Ident-No. 11.02-5003
vario EL III
CHNOS Elemental Analyzer
Operating Instructions
for instruments starting with serial-No.: 11054041
Issue May 2005
Elementar Analysensysteme GmbH, Donaustraße 7, D-63452 Hanau-Germany
Tel.: +49/6181-9100-0, Fax: +49/6181-9100-10, e-mail: info@elementar.de
Important Instructions
♦
♦
♦
♦
♦
The vario EL elemental analyzer is a fully automatic instrument which enables a
speedy quantitative analysis of CHNS. In different operation modes (depending on the
acquired equipment - see chapter 1), the instrument can determine the following
elements simultaneously from the weighed-in samples:
CHNS, CNS, CHN, CN, N, S and O.
The conversions to the above mentioned operation modes are described in chapter 7.3.
The suitability of the vario EL analyzer for the element analysis depends on the
controllable combustibility of the samples or sample quantities. Analyzing aggressive
chemicals, acids, alkaline solutions, solvents, explosives or materials that can
create explosive gas mixtures with the standard equipment of the vario El is
explicitly forbidden or can be executed at your own risk. It can lead to damages of
the instrument and to injuries of the operating personnel. For above applications or
applications that are especially difficult (if aggressive combustible products are to be
analyzed), please make use of the counseling possibilities of our Application
Laboratory in order to use special equipment or to work out safe processing
procedures. It is also possible that certain substances, as for instance fluorine, phosphate
or samples containing heavy metal have a negative influence on the analysis results or
the life time of instrument components.
Operation of the vario EL and peripheral equipment should only be carried out by
persons who have been authorized by E l e m e n t a r Analysensysteme GmbH.
Opening the transport packing by unauthorized personnel can lead to loss of warranty
rights! If the supplied instruments show damages, please contact the freight forwarder
and the manufacturer immediately.
For installation, the "Installations Requirements" have to be observed. For details,
please refer to the Appendix of this manual (chap. 12.4).
Operation, maintenance and repairs should only be carried out by trained
personnel. For a smooth and efficient operation of the vario EL, please read the
following operating instructions thoroughly. Please keep the operating instructions for
future questions. We reserve the right of deviations in illustrations and technical data
described in the operating instructions due to further development.
___________________________________________________________________________
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
01/04
•
•
•
The supplied operating instructions explain especially the operation and maintenance of
the vario EL. Since the operating and maintenance software of the vario EL is selfexplanatory, we have mentioned only several commands and menus. For further
information regarding the software, please read the notes in the PC-online-help.
The efficiency of the vario EL can be guaranteed only with original consumables as well
as original spare parts which can be obtained only through E l e m e n t a r Analysensysteme GmbH or authorized dealers. The use of different consumables or chemicals
of an unsuitable standard can lead to injuries as well as instrument damages. It can
also falsify the results of the analysis. Unsuitable spares lead to instrument damages
and loss of warranty.
All the operation dependent maintenance and exchange times mentioned in the operating
instructions depend very strongly on the respective test matrix. They are, therefore, only
examples and do not guarantee life times for consumables or wear and tear parts!
The analysis parameters described in the following are mean values. The operating
parameters that have been optimized for the individual instrument are included in the
furnished installation disk. Of course it is possible to optimize the analysis parameters any
time for special applications or unusual demands.
___________________________________________________________________________
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
01/04
Definitions
• Generally valid facts and examples have been explained only once in the following
operating instructions. However, in order to show the differences in the different operation
modes, we listed them in chapter 7.
If the general descriptions - as for instance the operation of the vario EL - depend only in
certain points on the operation mode - we continued the text in columns or as a table, to
enable the reader to read only the relevant passages (see for instance chapter 4.2.2).
• To clarify the input at the PC, we used the following definitions:
•
Definition in the text
Meaning
<Key>
key of the PC keyboard
e.g. <ESC> means the Escape-key
<CR> means the Return-key
<M>
means the letter M
{italic}
commands to be entered in the PC
e.g.: {vl <CR>} means, enter the letters
"vl" and push the return-key;
Edit or EditÖInput
dialog/menu or path to open a dialog
window;
click on menus one after the other. For
operation with the keyboard push the
underlined letters (”Hot Key”) together
with<Alt> ;
[OK] or [Help]
button (symbol) on the screen to be clicked
on with the mouse-cursor;
”Sleep at sample end”
definition of a function in a dialog window;
e.g.:
activate ”Sleep at sample end” in the
menu OptionsÖSleep-/WakeFunction.
___________________________________________________________________________
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
01/04
Abbreviations
• The following abbreviations are used in these operating instructions:
DF
daily factor
TCD
thermal conductivity detector
He
helium
O2
oxygen
H2O
water
CO2
carbon dioxide
SO2/ SO3
sulfur dioxide/sulfur trioxide
N2
molecular nitrogen
Nox
certain nitric oxides
___________________________________________________________________________
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
01/04
Contents
Page
I
Contents
1.
Scope of Delivery:
1-1
2.
Specifications and technical data
2-1
2.1
2.2
2.3
2.3.1
2-1
2-2
2-3
2-3
Specifications
Technical data
3-Tube furnace
Instructions for properoperation of the 3-tube furnace
3.
Safety Instructions
3-1
4.
Function of the vario EL
4-1
4.1
4.2
4.2.1
4.2.2
4.2.3
4.2.4
4-1
4-1
4-3
4-3
4-4
4-6
5.
6.
General Measuring Principle
Analysis
Sample loading
Substance digestion and removal of foreign gases
Separation of the measuring components
Detection
Installation and start-up
5-1
5.1
5.1.1
5.1.2
5.2
5.2.1
5.2.2
5.2.3
5.2.4
5.3
5.3.1
5.3.2
5.3.3
5.3.4
5.3.5
5-1
5-1
5-2
5-3
5-3
5-5
5-6
5-6
5-7
5-10
5-10
5-10
5-10
5-11
Preparations for operation
Working environment
Necessary gases and chemicals
Installation of the analyzer
Front view
Back view
Furnace
Safety features
Start-up
Connection of peripheral instruments
Connection of the supply lines
Instrument settings
Succession of instrument start-up
Parameter setting at the PC
Operating the vario EL
6-1
6.1 Sample preparation
6.1.1 Selection of sample weight
6.1.2 Possibilities of sample packing
6.1.3 Selection of oxygen dosing amounts
6.2 Daily measuring routine
6.2.1 Blank value limit determination
6.2.2 Factor determination
6.2.2.1 With calibration substances
6.2.3 Editing an analysis series
6.2.4 Data storage and print-out
6.2.5 Statistics
6-1
6-1
6-2
6-4
6-5
6-5
6-6
6-6
6-7
6-8
6-9
01.2005
Operating instructions vario EL III
Copyright by E l e m e n t a r Analysensysteme GmbH
Page
8.
9.
II
Contents
6.3 Checklist for analysis start
6.4 Calibration
6.4.1 Analysis of the calibration samples
6.4.2 Calibration evaluation
6.5 Shutdowns during analysis breaks
6.5.1 Short breaks
6.5.2 Longer shutdowns
6-11
6-12
6-12
6-14
6-18
6-19
6-21
7.
7-1
Particulars of the individual modes of operation
7.1 Modes with S-determination
7.1.1 CHNS-mode
7.1.2 CNS-mode
7.1.3 S-mode (with TCD)
7.2 Modes without S-determination
7.2.1 CHN-mode
7.2.2 CN-mode
7.2.3 N-mode
7.3 Instrument conversion and change of operation mode
7.3.1 Instrument conversion
7.3.1.1 Safety instructions for instrument conversion
7.3.1.2 Reassembly inside the furnace part
7.3.1.3 Tube conversion in the separation part
7.3.2 Mode conversion
7-1
7-2
7-4
7-7
7-9
7-10
7-14
7-16
7-19
7-19
7-20
7-22
7-22
7-25
Software
8-1
8.1 Installation and update
8.1.1 Installation of the software
8.1.2 Update of the software
8.1.3 Configuration of the balance
8.2 Main menu of the software
8.2.1 Title bar
8.2.2 Menu bar
8.2.3 Tool bar
8.2.4 Sample field
8.2.4.1 Text display
8.2.4.2 Graphic display
8.2.4.3 Statistic display
8.2.5 Status field
8.2.6 Recommendations for the software use
8.3 Processing of the vario EL data with MS Excel
8-1
8-1
8-1
8-1
8-2
8-2
8-3
8-10
8-11
8-11
8-11
8-12
8-12
8-14
8-14
Replacing consumables
9-1
9.1
9.1.1
9.1.2
9.1.3
9-3
9-3
9-6
9-9
Filling the reaction tubes
CHNS/ CNS/ S-mode
CHN/ CN/ N-mode
Filter plug
Operating instructions vario EL III
Copyright by E l e m e n t a r Analysensysteme GmbH
05.2005
Contents
9.2
9.2.1
9.2.2
9.2.3
9.2.4
9.3
9.3.1
9.3.2
9.4
9.5
9.6
9.6.1
9.6.2
9.7
9.7.1
9.7.2
Page
Installation, disassembly and conditioning of the reaction tubes
Disassembly from the 3-tube furnace
Installation into the 3-tube furnace
Installation of the absorption-U-tubes
Conditioning of newly installed tube
Ash finger
Emptying / Filling
Changing the ash finger
Changing the O2-lance
Cleaning the quartz glass bridge
Drying tubes
Filling the drying tubes
Installation/Disassembly and conditioning
Gas purification tube
Filling of the gas purification tube
Installation/disassembly and conditioning
10. Maintenance / Service
11.1
11.2
11.3
11.4
Main window
Title bar
Menu bar
Operating the program
9-10
9-10
9-13
9-14
9-16
9-17
9-17
9-18
9-19
9-20
9-21
9-21
9-21
9-22
9-22
9-23
10-1
10.1 Troubleshooting
10.1.1 Failure messages from the PC
10.1.2 Help to recognize failures
10.2 Service tips
10.2.1 Maintenance of the ball valve
10.2.2 Cleaning the carousel
10.2.3 Replacement of adsorption columns
10.2.4 Customer maintenance
10.25 Replacing fuses
10.2.6 Replacing the O-rings
11. Maintenance software
III
10-1
10-1
10-4
10-5
10-5
10-8
10-10
10-10
10-11
10-12
11-1
11-1
11-2
11-2
11-2
12. Appendix
List of Illustrations
Solving PC problems
List of Initial outfit
List of Consumables
Safety Data Sheets
Installation requirements
01.2005
Operating instructions vario EL III
Copyright by E l e m e n t a r Analysensysteme GmbH
Scope of delivery
Page 1-1
1. Scope of Delivery:
Basic unit :
♦
♦
vario EL
basic unit; fully automatic elemental analyzer for the quantitative determination of
CHNS or O  depending on the equipment  in solid or liquid samples, including
operation software in German or English, basic equipment . Basic equipment
sufficient for installation and training.
(for 230 V, 50/60 Hz, other current upon request)
Conversion sets
for the simultaneous determination of the listed operation modes with the recommended
working ranges
including set of chemicals for the initial set-up
order number
(incl.basic
instrument)
11.10-0000
operation mode
dynamic working range
[mg element absolute]
CHNS / CNS / S
11.60-0000
CNS / S
11.30-0000
CHN / CN / N
C : 0,03 - 20
mg abs.
H : 0,03 3
mg abs.
N : 0,03 2
mg abs.
S : 0,03 6
mg abs.
(upon request N to 10 mg abs.)
(upon request C to 30 mg abs.)
C : 0,03 - 30
mg abs.
N : 0,03 2
mg abs.
S : 0,03 6
mg abs.
(upon request N to 10 mg abs.)
C : 0,03 - 20
mg abs.
H : 0,03 3
mg abs.
N : 0,03 2
mg abs.
(upon request N to 10 mg abs.)
(upon request C to 30 mg abs.)
O : 0,03 2
mg abs.
O determination with TCD
[order no. 11.40-0002]
O determination with IRdetector for special application
[order no. 11.40-0001]
♦
♦
control- and evaluation unit
with German software
order no. 50 008 369
(for 230 V, 50/60 Hz, other voltages
upon request)
02/99
O : 0,03
-
2
mg abs.
control and evaluation unit
with English software
order no. 50 008 368
(for 230 V, 50/60 Hz, other voltages
upon request)
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
Page 1-2
Scope of delivery
Necessary Accessories :
♦
Matrix printer with printer cable
♦
Electronic micro balance
♦
O2 pressure reducing valve
♦
He pressure reducing valve
Order No. 50 031 857
(for 230 V, 50/60 Hz, other voltages upon request)
readability 0,001 mg
with V 24/ RS 232 interface
Order No. 22 133 042
two-stage, 2nd stage 0 - 3 bar with shut-off valve
for gas purity 99,995 % or better
Order No. 04 278 800
two-stage, 2nd stage 0 - 3 bar with shut-off valve
for gas purity 99,995 % or better
Order No. 04 278 810
♦
Forming gas pressure reducing valve
♦
Set of consumables for solid samples
♦
Set for a quick tube exchange
only for O-analysis with IR
two-stage, 2nd stage 0 - 3 bar with shut-off valve
Order No. 04 278 395
sufficient for approx. 4000 Analyses
Order No. 11.00-5012
CHNS / CNS / S
Order No. 11.00-5013
CHN / CN / N
Order No. 11.00-5014
O
to decrease process interruptions because of refilling the tubes
Order No. 11.00-5011
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
02/99
Scope of delivery
Page 1-3
Optional accessories :
For liquid or air sensitive samples:
♦
sealing press
for packing portioned samples in gas
tight tin capsules for liquid and
sensitive samples
incl. consumables for approx.
500 analyses
Order No. 22 160 062
♦
set consumables for liquid
samples
for use with capsule press sufficient for
approx. 2000 analyses
Order No. 22 133 012
For extreme acid and salt containing or aggressive samples
♦
Conversion set combustion tube of stainless steel
for routine operation of the analyzer with extremely acidy/salt containing, aggressive
and sensitive samples
including installation accessories
Order No. 11.12-0001/3
(Only suitable for operation mode CHN / CN / N !!!)
For heavier/more voluminous samples:
♦
♦
Pelletizer with pressing tool
for pelletizing prefabricated samples
packed in tin foil
Order No. 41.00-0000
♦
Hand pressing tool Ø 7 mm
for manual pelletizing of prefabricated
samples packed in tin foil
Order No. 41.01-0003/4
Carousel
for large samples with a volume of
1 cm³
with 39 positions
Order No. 12.00-0007/3
For further ordering information for spares or consumables, see appendix and the newest
catalog for consumables
02/99
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
Specifications and technical data
2.
Page
2-1
Specifications and technical data
2.1 Specifications
Method of analysis
Weigh-in/sample volume
Dynamic working range*
Elementary analysis of CHNS/ CNS/ S/ CHN/ CN
or N from one sample
Catalytic tube combustion of the samples, separation
of foreign gases, separation of the desired measuring
components, TCD-detection.
0,2 mg to 200 mg (substance dependent)
*
depends on the equipment and on the measuring mode
CHNS / CNS / S
CNS / S
CHN / CN / N
Precision /
Standard deviation
Recovery rate
Duration of analysis***
C:
0,03 - 20 mg abs.
H:
0,03 3 mg abs.
N:
0,03 2 mg abs.
S:
0,03 6 mg abs.
(on request N to 10mg abs.)
(on request C to 30mg abs.)
C:
0,03 - 30 mg abs.
N:
0,03 2 mg abs.
S:
0,03 6 mg abs.
(on request N to 10mg abs.)
C:
0,03 - 20 mg abs.
H:
0,03 3 mg abs.
N:
0,03 2 mg abs.
(on request N to 10mg abs.)
(on request C to 30mg abs.)
< 0,1 % abs.
at CHN and CHNS simultaneous determination. 5 mg
Acetanilide or sulphanilic acid
> 99,5 % for test substances
self optimizing,
6 - 12 minutes for CHN simultaneous
10 - 14 minutes for CHNS simultaneous
***
depending on the element content and weigh-in
Calibration
Data storage respectively
data output
01.04
curve adjustment; entire working range, if necessary in
2 sections
storage on hard disk or diskette.
LIMS-transfer possible.
Data output on monitor or printer.
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
Page
2-2
Specifications and technical data
2.2 Technical data
Detector
Thermal Conductivity Detector (TCD)
Control and evaluation unit
PC with Windows  operating system
printer (optional)
Software
German or English,
menu operated, status display during analysis, real
time graphic
Interfaces
RS 232 /V24, low safety voltage
according to DIN IEC 380/VDE 0806/08.81
Dimensions
Basic instrument: 780 x 560 x 700 mm (W x D x H)
plus 200 mm clearance from the walls
Weight
120 kg
Rated voltage
230 Volt AC ± 10 %, 50/60 Hz
Power consumption
0,6 kW
Connection value
1,4 kVA
Protection class
I, connection for earthed conductor wire
Protective system
IP 20, installation in dry rooms only
Noise level
55 dB (A), acc. DIN 45635 part 1
Ambient temperature
admissible max.: + 35°C
min.: + 15°C
Supply gases
He, purity 99,996 %, approx. 250 ml/min.
O2, purity 99,995 %;
(consumption per analysis: approx. 2 L He and
0,05 L O2)
Standard
CE-conformity according to EC guide lines
EMC 89/336/EWG and
LVD 73/23/EWG
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
02.99
Specifications and technical data
Page
2-3
2.3 3-Tube Furnace
Elementar Analysensysteme GmbH grants a 10 years' warranty on the 3-tube furnace.
In case of a manufacturing or material damage you will receive a replacement furnace
during a 10 years period starting with the date of purchase. This applies for all models
ordered from December 1, 2003 on.
Excluded from this warranty are of course damages that are caused by faulty
treatment/operation. Therefore, the following instructions for the operation of the 3tube furnace have to be followed by all means.
2.3.1 Instructions for proper operation of the 3-tube furnace
1. The instrument user has to observe the correct operation of the 3-tube furnace
according to the requirements of the operating instructions.
2. The furnace must not be heated above the maximum temperature stated in the
operating instructions.
3. The furnace must not be operated with a larger voltage than stated in the operating
instructions.
4. For breaks of several hours (e.g. over night) heater 1 shall be set to 900°C (for
CHNS, CNS, S mode only). For the operating modes CHN, CN, N and O the
corresponding operating temperatures remain the same.
5. For longer breaks over several days (5 days and more) the furnace shall be turned
off (set temperature control to 0.00°C).
6. The furnace shall be protected from liquids.
7. Short-circuits in connection with heating spirals and/or thermo elements have to be
avoided.
8. Inner and outer force to the heating spiral, to the thermo elements and to the
supply lines have to be avoided.
9. Only original parts by Elementar shall be used (e.g. combustion tubes, reductions
tubes, fillings, sealings, etc.)
10. In case of a breakdown, the 3-tube furnace shall be sent to the manufacturer's
works to Hanau in order to determine the error. If the inspection clearly shows that
the furnace became defective due to improper treatment, the warranty claim
expires.
01.04
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
02.99
Safety instructions
3.
page
3-1
Safety Instructions
Please adhere to the safety instructions and only operate
the unit in accordance with manufacturer's instructions.
The warnings on the individual instruments and in the
appropriate chapter of these instructions are also valid.
General instructions
• The analyzer vario EL is suitable only for the elemental analysis of samples or sample
sizes that have a controllable combustibility under combustion conditions, depending on
the mode of operation. Analyzing aggressive chemicals, acids, alkaline solutions,
solvents, explosives or materials that can form explosive gases is explicitly forbidden
with the basic vario El unit and must be performed at ones own risk. It can lead to
damages of the instrument and to injuries of the operating personnel. For difficult
applications, especially if aggressive combustion products can occur, we recommend to
use the counseling possibilities of our application laboratory, in order to use certain special
equipment and to work out safe operating procedures.
It is also possible that certain substances, as for instance fluorine, phosphate or samples
containing heavy metal have a negative influence on the analysis results or the life time of
instruments components.
• Operation, maintenance and repairs should only be carried out by trained personnel.
For a smooth and efficient operation of the vario EL, please read the following operating
instructions thoroughly. Please keep the operating instructions for future questions. We
reserve the right of deviations in illustrations and technical data described in the operating
instructions due to further development.
Installation / Start-up
• Operation of the vario EL and peripheral equipment should only be carried out by persons
who have been authorized by E l e m e n t a r Analysensysteme GmbH.
• Opening the transport packing by unauthorized personnel can lead to loss of
warranty rights! If the supplied instruments show damages, please contact the freight
forwarder and the manufacturer
02/99
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme
Page
3-2
Safety instructions
• The installation room must be well ventilated!
The exhaust gas pipes (connections M and R) must lead into the open air or into a
fume hood because it is possible that during operation toxic gases (e.g. SO2 in the
CHNS/CNS/S mode) emerge from the instrument. During constant operation the
respective gas concentration can exceed the permissible maximum workplace
concentration.
• The end of the gas pipes must lead to a sheltered (wind-free) place in the open air to avoid
fluctuations of the base line which would lead to detector instabilities.
Measuring process / calibration
• Since the operating and maintenance software of the vario EL is self-explanatory and is
equipped with an extensive on-line help program, we have mentioned only several
commands and menus. For further information regarding the software, please read the
notes in the PC-online Help program (menu HELPÖIndex).
• A faultless calibration of the instrument in the selected operation mode, covering the
required working range, is of crucial importance of the accuracy of the results. Calibration
procedures must, therefore, be carried out with utmost care. The Operating instructions
should be diligently observed.
• Insufficient oxygen reduces the catalysts and reduces, therefore, their effectiveness and life
span. The sample substances that have not been burnt remain inside the ash finger and
falsify the analysis results of the test samples to follow.
• When replacing the ash finger, the furnaces must be cooled down to room
temperature (nominal temperature 0°C). It is, however, still necessary to wear safety
goggles to protect the eyes from soot particles. It is also necessary to wear the supplied
protective gloves since hot components could still be inside the furnace chamber.
Maintenance / Tube Replacement
• The efficiency of the vario EL can only be guaranteed when original consumables as well
as original spare parts which can be obtained only through Elementar Analysensysteme
GmbH or their authorized dealers, are used. The use of different consumables or
chemicals of an unsuitable standard can lead to injuries as well as to instrument
damages. It can also falsify the results of the analysis. Unsuitable spares lead to
instrument damages and loss of warranty.
• All the operation dependent maintenance and exchange times mentioned in the Operating
instructions depend very strongly on the respective test matrix. They are, therefore, only
examples and do not guarantee life times for consumables or wear and tear parts!
• The described mode depending analysis parameters are mean values. The operating
parameters that have been optimized for the individual instrument are stored on the
supplied installation disk. Of course it is possible to optimize the analysis parameters any
time for special applications or unusual demands.
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
02/99
Safety instructions
page
3-3
• The walls of the vario EL should only be opened by authorized personnel for maintenance
and servicing purposes.
• Before opening a side or rear wall of the vario EL, disconnect all peripheral equipment
and the analyzer itself by turning the main switch and pulling the mains plug.
Attention: the 3-tube furnace must be cold otherwise components will become
overheated. The side and rear walls must be properly in place before starting a new
analysis (check safety linkage).
• To prevent leakage around the tube plugs, apply a slight coating of high-vacuum grease to
the O-rings and check them for damages. If too much grease is applied C blank values will
occur! The O-ring insert grooves in the plugs must be cleaned regularly. The high
temperature causes the O-rings to shrink, therefore, a resistance must be felt during O-ring
placement otherwise it might leak. Before inserting the plugs, the insides of the tubes must
be dusted.
• The vario EL and the gas pipe system must be checked periodically (at least once per
month) for leakage.
• When handling chemicals, observe the safety instructions of the chemical manufacturer
(see labels on bottles and safety data sheets)!
When handling Sicapent® (phosphorpentoxide) and NaOH (natrium hydroxide), it is
absolutely necessary to wear safety goggles and protective gloves.
!!!Danger of Cauterization !!!
• All tube fillings must be packed down as tightly as possible to avoid air pockets. To do
this, tap the side of the tube lightly with a wooden implement or cork ring while it is being
filled.
• Make sure that only WO3 granulate (11.02-0008) is used for tube filling!! WO3powder (11.02-0017) can only be used as sample additive.
a mix-up can cause clogging of the combustion tube.
• Replacing combustion or post combustion tubes can only be carried out when the
tubes are cold. For this purpose set furnaces to nominal temperature 0°C and let the tubes
cool down to room temperature (max. 100°C).
When working at hot furnaces or tubes there is danger of burning!!
Therefore, always wear the supplied protective gloves (order No. 05 000 094), because it is
possible that some components (e.g. heated tube line) are still hot. We are not liable for
accidents that are due to disregarding these warnings.
• Before replacing a tube turn off the gas supply into the instrument respectively activate the
function Options ÖMiscellaneousÖReplace .
• After a tube exchange, it is necessary to flush out the atmospheric nitrogen that entered the
unit for 5 minutes with He. This is accomplished automatically when leaving the function
OptionsÖMiscellaneousÖReplace.
• After changing the tubes wait until the 3-tube furnace as well as the new reaction tubes
have warmed up (ca. 10 to 15 minutes) before starting the next analysis. In addition, it is
necessary to adhere to the mode dependent conditioning rules for the tubes (see chapter
9.2.4).
02/99
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme
Page
3-4
Safety instructions
• Before installation into the 3-tube furnace all finger prints must be cleaned off the
quartz parts (for instance with acetone) to avoid crystallization areas which lead to
premature aging of the quartz. When handling cold quartz and glass parts wear the
supplied leather gloves to avoid danger of injuries in case of broken glass.
• Do not cut out O-rings with a sharp knife or a scalpel, since this might damage the
sealing area of the plugs etc. through scratches. There is also the danger of injury in case
the knife slips off!!
• Replacement of the ball valve can only be carried out when the tubes are cold. For this
purpose set furnaces to nominal temperature 0°C and let the tubes cool down to room
temperature (max. 100°C).
Always wear the supplied protective gloves (order No. 05 000 094), because it is possible
that some components in the furnace chamber are still hot.
• If the supply voltage has been interrupted for more than 15 minutes, the vario EL must be
checked for leakage. If necessary, replace all O-rings inside the furnace chamber since they
may have been brittle because of the interrupted ventilation.
Change of operation mode instrument conversion
• Conversion of the vario EL should only be carried out by trained personnel, who know
these operating instructions entirely.
• The max. permissible temperature limit values of combustion tube and reduction tube are
adjusted to the appropriate mode of operation. They are always approx. 50°C higher than
the necessary operating temperatures.
When changing the mode of operation make sure the tube fillings are adjusted to the
respective operating temperatures and cannot overheat. When overheating the tube
fillings they can melt, run into the furnace chamber and destroy the furnace.
• Replacement of adsorption columns can only be carried out when furnaces and
columns are cooled down and the vario EL is turned off.
For this purpose set the nominal temperature of the furnaces and the adsorption columns to
0°C and let them cool down to room temperature (max. 100°C). Turn off vario EL after it
has been cooled off, otherwise it might overheat because of missing ventilation.
• During a change of operation mode, the actual temperatures of the furnaces cannot be
higher than the nominal temperature of the furnaces in the newly selected mode, otherwise
the overtemperature-protection will be activated (see chapter 10.1.1).
• Please adhere to the safety instructions (safety steps I and II, chapter 7.3.1.1) for the
instrument conversion of the vario EL to the letter. We are not liable for accidents that are
due to disregarding these warnings.
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
02/99
Function of the vario EL
4.
Page
4-1
Function of the vario EL
The elementary analyzer vario EL is a fully automatic instrument for a speedy and
quantitative determination of CHNOS. Depending on the purchased equipment (see chapter
1), the instrument can - in different operation modes - determine the following elements
simultaneously from one sample weigh-in:
CHNS, CNS, CHN, CN, N, and S.
The conversion possibilities into these operation modes are described in chapter 7.3.
The suitability of the vario EL analyzer for the element analysis depends on the controllable
combustibility of the samples or sample quantities.
It is also possible that certain substances, as for instance fluorine, phosphate or samples
containing heavy metal have a negative influence on the analysis results or the life time of
instruments components.
For difficult or contraversive applications (see for instance safety instructions below),
especially if aggressive combustible products are to be analyzed, please make use of the
counseling possibilities of our Application Laboratory.
Analyzing aggressive chemicals, acids, alkaline
solutions, solvents, explosives or materials that can
create explosive gas mixtures with the standard
equipment of the vario El is explicitly forbidden or
can be executed at your own risk. It can lead to
damages of the instrument and to injuries of the
operating personnel.
4.1 General Measuring Principle
The elementary analyzer vario EL works according to the principle of catalytic tube
combustion in an oxygenated CO2 atmosphere and high temperatures. The combustion gases
are freed from foreign gases (for instance volatile halogen). The desired measuring
components are separated from each other with the help of specific adsorption columns and
determined in succession with a thermal conductivity detector (TCD). Helium (He) serves as
flushing and carrier gas.
4.2 Analysis
The automatic control of the analysis procedure is accomplished through the software and the
sample specific nitrogen dosing is allocated through index numbers (O2-Index 1-5) to the
appropriate sample matrix. The oxygen dosing can be regulated by the operator (see chapter
6.1.3.).
02.99
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
Page
4-2
Function of the vario EL
We will now explain the timely and functional course of an analysis. With the help of
illustrations 4.1 and the figures/letters in brackets, it is possible to follow the location of the
described process. Illustration 4.1 shows the simplified flow diagram of the CHNS mode,
since all three possible adsorption columns (SO2, H2O, CO2) are built in. Depending on the
mode of operation, only the adsorption columns of the elements to be determined are built
into the gas line. To make it clear, the adsorption columns should not be seen as bridged. (For
conversions and detailed piping diagram see chapter 7ff.)
Illustration 4.1: functional diagram vario EL (CHNS-mode)
Legend
V2
V3
V4
V7
V8
V9
A
B
C
1
2
3
4
5
valves for
desorption path SO2
O2-input valve
He-input valve
valves for
desorption path H2O
SO2-adsorption column
H2O-adsorption column
CO2-adsorption column
carousel
ball valve
combustion tube
3-tube furnace
O2-lance
6
7
8
9
10
11
12
13
14
15
16
17
18
19
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
ash crucible
reduction tube
drying tubes
gas control insert
flow controller, measuring side
detector (TCD)
throttle, reference side
drying tube, reference gas
gauge, gas inlet pressure
flowmeter for O2 and He
gas cleaning tube
pressure sensor
drying tube, oxygen
needle valve for O2-dosing
02.99
Function of the vario EL
Page
4-3
4.2.1 Sample loading
The homogenized sample is packed in tin foil (see chapter 6.1.2), weighed and placed
into the carousel of the automatic sample feeder (1). The sample weight is entered into
the PC either from an on-line balance via an interface or manually with the keyboard.
The sample name and the matrix specific oxygen dosing (O2-Index 1-5) is allocated to
the sample weight (see chapter 6.2.3). Now the analysis can be started.
At the start of an analysis, the Auto-Zero Adjust of the measuring signal is carried out
through the detector (9). Thereafter the ball valve (2) opens through a 180° turn of the
blind hole ball. The carousel (1) moves up one position and the sample drops into the
blind hole of the ball valve (2). The ball valve (2) turns 90° into flushing position and
seals the apparatus. The atmospheric nitrogen that had entered is now flushed out and
after flushing is completed, the sample drops into the ash finger (6) of the combustion
tube (3) through another 90° turn of the ball valve (2).
4.2.2 Substance digestion and removal of foreign gases
Parallel to the sample feeding procedure, the oxygen dosing in the ash finger (6)
begins via V4 and the O2-lance (5), so that the sample drops into a highly oxygenated
atmosphere and combusts explosively. The time for switching on the oxygen dosing is
determined by the process time “O2-delay“ in the menu OptionsÖParameters. The
oxygen dosing amount is adjusted on the needle valve (19) and the combustion time is
selected beforehand for each sample individually by the PC using O2-Index (1-5) (see
chapter 6.1.3).
After the sample feeding, the integrator reset ensues and the integration display is set
to zero. A few seconds thereafter N-integration begins.
During oxydated combustion the elements C, H, N and S produce – in addition to the
molecular nitrogen (N2) – the oxidation products O2, H2O, NOx, SO2 and SO3.
If the sample contains halogens, volatile halogen compounds will be produced.
Depending on the mode of operation, please read the appropriate column.
CHNS/CNS/S
CHN/CN/N
Tungsten trioxide inside the combustion
tube (3) works as a catalyst in order to
bind alkaline or earth alkaline elements
and to avoid non-volatile sulfates.
02.99
A copper oxide filling inside the
combustion tube (3) works as catalyst for
quantitative oxidation, higher carbon
oxide weigh-ins and samples that are
difficult to combust.
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
Page
4-4
Function of the vario EL
CHNS/CNS/S
CHN/CN/N
A copper contact in the reduction tube (7)
quantitatively reduces nitrogen oxides
(NOx) and sulfur oxides (SO2/SO3) to N2
respectively SO2 and binds excess
oxygen. The volatile halogen compounds
are removed from the gas stream at the
exit of the reduction tube (7) with silver
wool.
The remaining gas stream contains only
the components CO2, H2O, SO2 and N2 in
the carrier gas (He).
In the CHNS-Mode this gas is guided to
the separation and measuring system.
In the CNS- respectively S-Mode the gas
stream is freed of H2O with the help of an
additionally built in absorption-U-tube
and subsequently guided to a modified
separation system (see chapter
7.1.2/7.1.3).
Volatile Fluor compounds are chemically
bound on a layer of ceroxide and the lead
chromate filling absorbs the sulfur
compounds (SO2/SO3). A copper contact
in the reduction tube (7) quantitatively
reduces nitrogen oxides (NOx) to N2 and
binds excess oxygen. The volatile halogen
compounds are removed from the gas
stream at the exit of the reduction tube (7)
with silver wool.
The remaining gas stream contains only
the components CO2, H2O and N2 in the
carrier gas (He).
In the CHN-Mode this gas is guided to
the separation and measuring system.
In the CN-Mode the gas stream is freed
of H2O with the help of an additionally
built in absorption U-tube and
subsequently guided to a modified
separation system (see chapter 7.2.2).
In the N-Mode a CO2 absorption U-tube
is built in addition to the H2O-tube (see
chapter 7.2.3). The reaction gas contains
then only nitrogen (N2) and can be
measured directly in the detector (for
further information see chapter 4.2.4).
To avoid the creation of H2SO4 out of H2O and SO2 as well as water condensation, all
tubes containing reaction gas with water are heated.
4.2.3 Separation of the measuring components
As the thermal conductivity detector (TCD, 11) cannot specifically distinguish
between the different components of the reaction gas, the desired reaction products
(CO2, H2O, SO2 or N2) must be flushed individually and one after the other by the
carrier gas (He) into the measuring module. This separation of measuring components
is carried out through specific adsorption on heatable columns (A,B,C), whereby the
adsorption columns (A,B,C) and the respective separation conditions are in
accordance with a reaction product [A = SO2-adsorption column, B = H2O-adsorption
column, C = CO2-adsorption column].
In each mode of operation only the necessary adsorption columns are built into the gas
path (see chapter 7ff). Nitrogen (N2), which is unaffected by the adsorption columns is
the first component that is measured in the thermal conductivity detector (11)
(exception: S-mode).
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
02.99
Function of the vario EL
Page
4-5
When the integration of a component is concluded, the integral value is stored, an
integrator reset is carried out and the next components is desorbed by the adsorption
column and measured.
Depending on the mode of operation, please read the appropriate section.
02.99
CHNS
Reactions gas: N2, CO2, H2O, SO2
The constantly tempered adsorption column (A) first removes SO2
quantitatively from the gas stream. Subsequently the reaction gas is dried
in the H2O-adsorption column (B). Adsorption column (C) finally adsorbs
the CO2. Now the measuring gas stream contains only N2, which is
measured directly in the TCD (11). After the N-measurement, the CO2 is
thermally desorbed and measured. Then follow desorption and
measurement of H2O and subsequently of SO2. These components
bypass the other adsorption columns and are guided via special desorption
paths to the detector.
CNS
Reaction gas: N2, CO2, SO2
The constantly tempered adsorption column (A) first removes SO2
quantitatively from the gas stream. Adsorption column (C) finally adsorbs
the CO2. Now the measuring gas stream contains only N2, which is
measured directly in the TCD (11). After the N-measurement, the CO2 is
thermally desorbed and measured. Then follow desorption and
measurement of SO2. This component bypasses the other adsorption
column and is guided via a special desorption path to the detector.
S
Reaction gas: N2, CO2, SO2
The constantly tempered adsorption column (A) first removes SO2
quantitatively from the gas stream. The remaining components of the
reaction gas (CO2, N2) are measured together as “Dummy Peak“ and the
integral is deleted after conclusion of the integration. After the “Dummy
Peak“, SO2 is thermally desorbed and guided to the detector.
CHN
Reaction gas: N2, CO2, H2O
First the H2O is adsorbed in the adsorption column (B). The CO2 remains
in the adsorption column (C). Now the measuring gas stream contains
only N2, which is measured directly in the TCD (11). After the Nmeasurement, the CO2 is thermally desorbed and measured. Then follow
desorption and measurement of H2O. This component bypasses the other
adsorption column and is guided via a special desorption path to the
detector.
CN
Reaction gas: N2, CO2
Only adsorption column (C) is available. This column adsorbs the CO2.
Now the measuring gas stream contains only N2, which is measured
directly in the TCD (11). After the N-measurement, the CO2 is thermally
desorbed and measured.
N
Reaction gas: N2
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
Page
4-6
Function of the vario EL
A separation through columns is not necessary because all other gas
components have been irreversibly removed. The reaction gas is guided
directly to the TCD (11) and measured.
4.2.4 Detection
The thermal conductivity detector (11) consists of two measuring chambers. The gas
flows through them at constant rate of flow. The carrier gas flow can be turned off
during measurement breaks because the measuring chambers are resistant against
oxygen. During operation the reference measuring chamber is flushed with pure
carrier gas He (reference gas flow) while the measuring gas flow, i.e. the respectively
desorbed fraction of the reaction gas (e.g. He/N2- or He/CO2-mixture) passes through
the other one.
The two chambers constitute a measuring bridge and its electrical imbalance provides
a direct gauge for the nitrogen content in the carrier gas. The detector output voltage is
recorded as a function of time and then digitized, integrated and represented as an
integral.
Through a calibration for each element, the integral is allocated to an absolute element
content of the sample. From the resulting content and the sample weight, the
percentage of the element content is calculated.
The timely course of the measuring signal can be displayed through the function
ViewÖGraphic on the monitor (see chapter 6.2.4). Illustrations of a typical measuring
peak can be seen in chapter 7 under the respective mode of operation.
Before starting an analysis, an Auto-Zero Adjust is carried out, to compensate a
possible zero point drift of the detector. Before every integration of a gas component,
the integrator reset to zero is carried out. The point of time of the integrator reset can
be influenced through the “Integrator-Reset-Delay“ in the Parameter-menu (see
chapter 5.3.5).
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
02.99
Installation and start-up
5.
Page
5-1
Installation and start-up
Installation and operation of the vario EL and peripheral
equipment should only be carried out by persons who
have been authorized by E l e m e n t a r
Analysensysteme GmbH. Opening the transport
packing by unauthorized personnel can lead to loss of
warranty rights! If the supplied instruments show
damages, please contact the freight forwarder and the
manufacturer immediately.
5.1 Preparations for operation
These prerequisites are absolutely adhered to for a smooth operation of the vario EL.
5.1.1 Working environment
The whole installation, consisting of the nitrogen analyzer vario EL and the
respective peripheral equipment as balance and PC should be protected from draught
and direct sources of heat. An air conditioned room is recommended as some parts of
the analyzer give off heat.
In addition, appropriate steps are to be taken to avoid electrostatic charges. Electrical
discharges on the unit can lead to malfunctions.
placement area
space requirement
(incl. PC and printer)
ambient temperature
power supply
connections
05/05
type of protection: IP 20
only in dry, well ventilated rooms; installation of the
vario EL only on a heat resistance surface.
length:
2.00 m
depth:
0.75 m
distance from the walls at least 20 cm at all sides,
otherwise the fans of the unit will not function properly.
constant temperature
permissible
min.:
+ 15°C
max.:+ 35°C
230 Volt AC ± 10 %, 50/60 Hz
connected load: 1.4 kVA
power supply and frequency must match the information
on the legend plate of the instrument
2 sockets and multipoint strip with 4 sockets for
connection of peripheral instrument or 5 sockets
protection class I, connection for earthed conductor wire
required fuse protection: 16 A/delay-action fuse
Operating instructions vario EL III
Copyright by E l e m e n t a r Analysensysteme GmbH
Page
5-2
Installation and start-up
gas connections
gas connections must be available in the immediate
vicinity of the instrument. Pressure reducing valves are
required for connection. Pressure reducing valves He and
O2, each with two steps (2nd step 0-3 bar) with shut-off
valve
(for order instructions see chapter 1)
exhaust pipes
atmospheric into the open air or into a fume hood
(see safety instructions)
The installation room must be well ventilated. The
exhaust gas pipes (connections M and R) must lead
into the open air or into a fume hood because during
operation toxic gases (e.g. SO2 in CHNS/CNS/S-mode)
come out of the instrument. It is possible that during
constant operation the gas content of the air exceed the
permissible maximum workplace concentration .
The end of the gas pipes must lead to a sheltered (windfree) place in the open air since pressure fluctuations, for
instance through wind, lead to detector instabilities.
5.1.2 Necessary gases and chemicals
When handling chemicals observe the safety instructions
of the chemical manufacturer (see labels on bottles and
safety data sheets )!
carrier gas
combustion gas
reagents
calibration standards
helium He ; purity 99.996 %
pre-pressure 2,0 bar
use : ca. 250 ml/min.
oxygen O2 ; purity 99.995 %
pre-pressure ca. 2.5 bar
use: 0,05 liter per analysis
chemicals for filling the reaction tubes (see chapter 9) are
included in the basic set of consumables.
For further analysis we suggest a set of consumables (see
chapter 1)
sulphanilic acid, acetanilide are supplied with the first set
of consumables.
If desired make other standards available (e.g. stearic acid
or benzoic acid).
Operating instructions vario EL II05/05
Copyright by E l e m e n t a r Analysensysteme GmbH
Installation and start-up
Page
5-3
5.2 Installation of the analyzer
The walls of the vario EL should only be opened by
authorized personnel for maintenance and servicing
purposes.
The design of the basic unit of the vario EL is as follows:
5.2.1 Front view
7
12
13
14
8
9
6
5
4
3
10
2
11
1
Illustration 5.1: front view of the vario EL (CHNS-mode)
05/05
Operating instructions vario EL III
Copyright by E l e m e n t a r Analysensysteme GmbH
Page
5-4
Installation and start-up
7
12
13
8
9
6
5
4
3
10
2
11
1
Illustration 5.2: front view of the vario EL (CHN-mode)
Legend to
Ill. 5.1/5.2
1
2
3
4
5
6
7
8
9
10
11
12
13
14
main switch with control light
pressure gauge for gas inlet pressure (1,25 bar)
He-flow meter
O2-flow meter
reference gas drying tube
oxygen drying tube
needle valve for oxygen dosage
gas purification tube
carousel
detector insert
front door in front of combustion furnace (the door is held by
magnets)
drying tube after the CO2-column
drying tube prior to the CO2-column
drying tube after the SO2-column
Operating instructions vario EL II05/05
Copyright by E l e m e n t a r Analysensysteme GmbH
Installation and start-up
Page
5-5
5.2.2 Back view
2
3
4
3
5
6
7
1
8
9
10
11
12
13
Illustration 5.3: rear view of the vario EL
legend:
05/05
No.:
1
2
3
4
5
6
7
8
9
10
11
12
13
inscription:
He IN
M OUT
R OUT
O2 IN
PC
RECORDER
BALANCE
explanation:
cooler fan for furnace or ball valve
cooler for SO2-column
hot air outlet of adsorption columns
He-gas inlet
TCD measuring gas outlet (200 ml/min.)
TCD reference gas outlet (ca. 50-100 ml/min.)
O2-gas inlet
Cooler for CO2- and H2O-adsorption column
PC-port
recorder port
balance port
vent supply insert
mains connection cable
Operating instructions vario EL III
Copyright by E l e m e n t a r Analysensysteme GmbH
Page
5-6
Installation and start-up
5.2.3 Furnace
The furnace is located behind the right front door (see illustration 5.1/5.2) of the
vario EL. The door is secured through magnets and can be removed easily.
The vario EL is equipped with a 3-tube-furnace with three heating tubes, each of
which works independently. The temperature for each tube is pre-selected through the
PC (see chapter 5.3.5). All heating tubes are monitored through the software and in
case of failure the heating system will be disconnected from all poles of the supplied
voltage.
The reaction tubes are inserted in the three-tube furnace - combustion tube on the
right and reduction tube in the middle (see chapter 9.2.2). The left heated tube is only
used for special applications. For fast and easy exchange of the reaction tubes, it is
possible to pull the three-tube furnace - after loosening of a few holding devices - out
of the unit on a rail.
5.2.4 Safety features
• Each heating system is monitored through an internal micro processor control for
the following failures:
1. A heater does not reach its set point temperature during a
selected time.
2. Thermocouple is defect or displays an invalid value.
3. The selected limit temperature is surpassed.
These failures will switch off the power supply for all heaters. Similar dangerous
failures will cause the furnace transformer to switch off.
The max. permissible temperature limit values of
combustion tube and reduction tube are always adjusted
to the respective mode of operation. They are always
approximately 50°C higher than the necessary operating
temperatures.
When changing the mode of operation make sure that the
tube fillings match the appropriate operating
temperatures and do not overheat. Overheating can
cause the tube fillings to melt. The melted material
can run into the furnace chamber and destroy the
furnace.
• The vario EL is equipped with a temperature limit control, which turns off all
furnaces automatically in case the temperature limit has been exceeded (e.g. if a
cooler is not working).
• He-supply is only possible when the mains switch is on.
Operating instructions vario EL II05/05
Copyright by E l e m e n t a r Analysensysteme GmbH
Installation and start-up
Page
5-7
5.3 Start-up
Operation of the vario EL and peripheral equipment
should only be carried out by persons who have been
authorized by E l e m e n t a r Analysensysteme
GmbH.
For start-up please follow these instructions successively:
Please also note the shut-down condition of the unit (see chapter 6.5)
a) For transport purposes of the vario EL, pull out the handles at the sides of the unit and tilt
them up (see illustration No. 5.4).
b) Set instrument up (for instructions regarding placement area see chapter 5.1.1) and connect
peripheral instruments (see chapter 5.3.1).
c) Connect supply gases and install exhaust gas outlets and drain pipes (see chapter 5.3.2).
d) Loosen transport guards.
The moveable 3-tube furnace must be secured during transport with a screwed on angle
piece (see illustration 5.5) to prevent accidental sliding. To loosen the transport guard
open the front door and right side panel. The screws holding the transport guard are now
accessible and be loosened.
Note:
For first start-up remove the cable bundle from the tube linkage pieces inside
the combustion chamber.
e) Fill quartz and glass parts and install (see chapter 9ff).
f) Turn PC and printer on and - if necessary - install software (see chapter 8.1) and wait for
booting procedure to be ended.
g) Remove carousel from the vario EL.
h) Turn on main switch of the vario EL (see illustration 5.1/5.2; No. 1). The instrument
carries out a reference run of ball valve and carousel. The reference run is correctly
performed only when the carousel is removed. Afterwards replace the carousel.
i) Turn on operation gases:
He
set pre-pressure (approx. 2.0 bar) so that inlet pressure gauge shows 1.25 bar
(see illustration 5.1/5.2; no.2)
O2
pre-pressure 2.5 bar (2nd step bottle pressure gauge).
05/05
Operating instructions vario EL III
Copyright by E l e m e n t a r Analysensysteme GmbH
Page
5-8
Installation and start-up
j) Start the vario EL-software by clicking on the corresponding icon.
The software is menu controlled, so that the user sees most of the operational steps
displayed on the screen. Moreover, most of the standard operation parameters have been
set in the factory (see chapter 7ff) which the user does not need to change.
k) Select desired mode of operation in the menu Mode (CHNS, CNS, CHN, CN, N or S).
When changing the mode of operation make sure that the
tube fillings match the appropriate operating
temperatures and do not overheat. Overheating can
cause the tube fillings to melt. The melted material
can run into the furnace chamber and destroy the
furnace.
l) Start heaters and check parameter setting at the PC (see chapter 7ff). Click to the menu
item OptionsÖParameter. In the Parameter-dialog the settings should be checked (see
chapter 7ff) and the operating temperatures must be entered. After confirming the changes
with [OK] you can observe in the status field how the furnace temperatures rise up. When
the heaters have reached the set temperatures (heating time approx. 45 minutes), the
vario EL is ready for analyzing procedures.
Note: for the temperature settings, corresponding access rights are required.
m) Perform leakage test (OptionsÖMiscellaneousÖleakage test).
If the leakage test is unsuccessful leave the operator software and activate the maintenance
software in order to locate the leak (see chapter 11).
n) In CHNS, CHN, CN and N mode, the newly filled reaction tubes must be conditioned
before operation (see chapter 9.2.4).
o) Check in the menu "Standards", whether or not the desired test substances (for instance
acetanilide or sulfuric acid) have been defined (see chapter 6.4.1).
p) Check if calibration coefficients have been loaded (Math.ÖCoeffs). With the new
vario EL we supply the calibration report of the quality control test.
q) Set oxygen dosing amount at the needle valve (illustration 5.1/5.2, no. 7) during a blank
value run. For this purpose place a small sample on to the carousel, enter this current
sample into the PC (weight = 1mg, name = blank, O2-Index = 1) and start with
SystemÖSingle. After the ball valve has turned into flush position, the needle valve is
adjusted in such a way that the O2-flow meter (see illustration 5.1/5.2, no.4) shows 1.8 to
2.0 scale divisions during O2-dosing time.
r) Check functionality of the vario EL (e.g. with “run-in“, blank value and standard measurements), thereby watching the gas flows and pressures (see chapter 6.1 to 6.3).
Operating instructions vario EL II05/05
Copyright by E l e m e n t a r Analysensysteme GmbH
Installation and start-up
Page
5-9
Illustration 5.4: handle carrying position
Illustration 5.5: transport guard
3-tube-furnace
5.3.1 Connection of peripheral instruments
Schreiber
Recorder
vario EL
Waage
Balance
PC
Drucker
Printer
Illustration 5.6: connection of peripheral instruments
As shown in illustration 5.6, the element analyzer consists of the basic instrument
vario EL and peripheral equipment. PC and printer are necessary for control and
evaluation. Recorder and balance are optional. The peripheral instruments are
connected (with the supplied cables) to the appropriate sockets at the back of the
vario EL (see illustration 5.3 and inscriptions on the instruments).
As an option, a recorder with the supplied cable can be connected for recording of the
following values:
05/05
Operating instructions vario EL III
Copyright by E l e m e n t a r Analysensysteme GmbH
Page
5-10
Installation and start-up
cable inscription
TCD comp (±)
measuring value
TCD-signal, compensated
TCD (±)
TCD-signal,
rest O2 (±)
pressure (±)
no function
system pressure [0 - 2.50 bar]
(pressure sensor signal
see illustr.4.1, No. 17)
recorder setting
0 to 10 V
according to height of peak
0 to 5 V
according to height of peak
0 to 5 V
(2 mV/mbar)
These measuring values can also be selected in the PC graphic. Chapter 6.2.4
describes how this graphic can be printed.
5.3.2 Connection of the supply lines
The installation room must be well ventilated. The
exhaust gas pipes (connections M and R) must lead
into the open air or into a fume hood because during
operation toxic gases (e.g. SO2 in CHNS/CNS/S-mode)
come out of the instrument. It is possible that during
constant operation the gas content of the air exceed the
permissible maximum workplace concentration .
The end of the gas pipes must lead to a sheltered (windfree) place in the open air since pressure fluctuations, for
instance through wind, lead to detector instabilities.
Illustration 5.3 shows the connections at the back of the vario EL. For easy
connection of the supply and discharge lines, the left cover plate at the top of the vario
EL can be unscrewed and removed.
5.3.3 Instrument settings
These are the suggested standard instrument settings:
gas pressure
flow
Set the O2-pre-pressure at the reducing valve to 2.5 bar. For He,
the pre-pressure is set to 2.0 bar. The inlet pressure gauge will
then show 1.20 to 1.25 bar.
the flow rates are factory set to:
measuring gas outlet (M OUT):
200 ml/min.
reference gar outlet (R OUT): 50 ml/min. - 100 ml/min.
5.3.4 Succession of instrument start-up
To ensure a smooth operation of the vario EL without any failures, it is absolutely
necessary to turn on the basic instruments and the peripheral equipment in a certain
succession.
Operating instructions vario EL II05/05
Copyright by E l e m e n t a r Analysensysteme GmbH
Installation and start-up
Page
5-11
a) Switch on PC with screen and printer and wait for booting procedure to be ended
a) Remove carousel from the vario EL.
b) Switch on the vario EL at the main switch (see illustration 5.1/5.2; no. 1) and wait
for the reference run..
Note:
The instrument carries out a reference run of ball valve and carousel.
The reference run is correctly performed only when the carousel is
removed.
d) Afterwards replace the carousel.
e) Start the vario EL-software by clicking the corresponding icon.
f) Now the gas supply lines He and O2 can be opened.
Note:
The gas O2 should only be turned off if no tests are run for a long time
(> 1 week).
5.3.5 Parameter setting at the PC
When changing the mode of operation make sure that the
tube fillings match the appropriate operating
temperatures and do not overheat. Overheating can
cause the tube fillings to melt. The melted material
can run into the furnace chamber and destroy the
furnace.
In every mode of the operation the parameters necessary for the analysis procedures
are filed in the menu OptionsÖParameter. Illustration 5.7 shows the Parameter
window for the CHNS mode with the factory set selections. Chapter 7 shows the
preselected parameters for every mode of operation. The following is only an
explanation of the individual parameters
Illustration 5.7: parameter-window in CHNS-mode
05/05
Operating instructions vario EL III
Copyright by E l e m e n t a r Analysensysteme GmbH
Page
5-12
Installation and start-up
Note:
The mode dependent analysis parameters are average values. The
optimized operating parameters of the first start-up are stored on the
supplied diskette. These settings can be optimized for special applications
or unusual requirement through the operator at any time.
For the meaning of the individual parameters, please note the following:
Parameter
Factory setting
Meaning
field of remarks of the operator.
Identifier
A sensible use is, for instance, to enter the
name of the stored file.
Temperatures
Furnace 1
setting the nominal temperatures for
the 3-tube furnace.
Furnace 3
CO2-column
CHNS/CNS/S 1150°C
CHN/CN/N
950°C
CHNS/CNS/S 850°C
CHN/CN/N
500°C
0°C
130°C
SO2-Column
SO2-Column
H2O-Column
210°C
140°C
150°C
Furnace 2
Standby
Times
Flush
5s
O2-Delay
10 s
Auto Zero Delay
mode dependent
Integrator-ResetDelay
mode dependent
heater right, combustion tube
heater middle, reduction tube
heater left, mostly unused
desorption temperature1 of CO2-column
When analyzing C-quantities heavier than
20 mg abs. , the measuring signal becomes
higher than 10 V, i.e. the detector is
"overcontrolled". The heating temperature
of the CO2-column must then be reduced
to 80 to 90°C which means the peak
becomes flatter and wider.
desorption temperature1 SO2-column
adsorption temperature SO2-column
desorption temperature1 H2O-column
Here the run times of the instrument
control are entered
during this time, the blind hole of ball
valve is flushed free from the atmospheric
nitrogen that had entered.
begins after the analysis start and
thereafter the O2-dosing starts. This time is
optimized in such a way that for the
combustion the best possible initial O2concentration is available in the ash
finger.
the auto zero adjustment is delayed in
order to avoid the temporary fluctuations
of the base line after the start of the
analysis.
The integrator-reset prior to the first integration (mostly N) is delayed so that
temporary instabilities of the base line
during sample feeding are not integrated.
Operating instructions vario EL II05/05
Copyright by E l e m e n t a r Analysensysteme GmbH
Installation and start-up
1
Note:
Page
Desorption temperatures are optimized in such a way that at a low
concentration of the elements to be determined , a possibly high element
concentration occurs in the carrier gas after desorption (Purge and Trapmethod) in a possibly short analysis time. This means that narrow and high
peaks are formed.
Parameters
Factory setting
Peak-Anticipation
N
Peak-Anticipation
C
Peak-Anticipation
H
Peak-Anticipation
S
Peak-Anticipation
Dummy
Integr.-Reset-Delay
S
Meaning
70 s
100 s
CHNS
CHN
CHNS/CNS
S
only for S-mode
100 s
75 s
70 s
120 s
Dummy-Peak
CHNS/CNS
S
only in S-mode
3 mV
3 mV
5 mV
3 mV
2 mV
2 mV
O2-Dosing
Index 1
Index 2
Index 3
Index 4
Index 5
05/05
This time becomes effective after the
respective integrator reset. During this
time the integrator waits for a measuring
peak. If no measuring peak appears during
this time, integration is ended and the next
element is taken.
s. Peak-Anticipation N
s. Peak-Anticipation N
s. Peak-Anticipation N
s. Peak-Anticipation N
120 s
only for CHNS/CNS
60-80 s
Thresholds
N-Peak
C-Peak
H-Peak
S-Peak
5-13
This time is necessary in order to prevent
integration of underground signals arising
prior to the S peak. This time must be
optimized in such a way that 2 - 3 seconds
prior to begin of the S-peak the integrator
reset takes place. This is especially
important for low S-concentrations.
We recommend 60 sec. for sample
weights over 1 mg sulfanilic acid (resp.
185 µg S abs.) and 80 sec. for smaller
sample weights (resp. abs. sample
weights).
Here the termination thresholds for
peak-end detection is determined.
termination threshold for N-integration
termination threshold for C-integration
termination threshold for H-integration
termination threshold for S-integration
termination threshold for dummy-peakintegration
Here the O2-index-figures (1-5) are
allocated to the O2-dosing times.
(For application see chapter 6.1.3)
90 s
1s
120 s
150 s
180 s
Operating instructions vario EL III
Copyright by E l e m e n t a r Analysensysteme GmbH
Page
5-14
Parameters
Installation and start-up
Factory setting
Process
Gas/2 during Nintegration
off
Data-Transfer
off
Meaning
Here special modes of operation are
selected for the process control.
50% flow for N-integration causes
a) the sensitivity of the detector to double
during N-integration and b) an increase in
O2-concentration in the ash finger. This is
only recommended for substances with
difficult combustion with very low Ncontent (e.g. coal, graphite, ceramic
materials).
Please note: Peak-anticipation N and
integrator-reset-delay must be adjusted to
the mode of operation (these times are
usually doubled).
records all communication data between
PC and analyzer.
This function is to be activated for
servicing purposes only! Otherwise the
memory capacities of the PC will be used
up.
Operating instructions vario EL II05/05
Copyright by E l e m e n t a r Analysensysteme GmbH
Operating the vario EL
6.
Page
6-1
Operating the vario EL
The vario EL analyzer is suitable only for the element
analysis of samples or sample quantities which are
controlled combustible under mode dependent
combustion conditions.
Analyzing aggressive chemicals, acids, alkaline
solutions, solvents, explosives or materials that can
create explosive gas mixtures with the standard vario
EL equipment is explicitly forbidden. It can lead to
damages of the instrument and to injuries of the
operating personnel.(see also chapter "Important Notes",
point 2)
6.1 Sample preparation
Regarding sample preparation and homogenization, we recommend the special literature that
is commonly available. Special attention should be paid to sample reduction and drying,
because these procedures bear the danger of contamination and also the loss of volatile
components. When preparing the samples for the vario EL, keep in mind that an analysis of
the total nitrogen is performed which means that air trappings must be noted. When analyzing
carbon and hydrogen contamination could occur through touching the tin container or through
humidity. Also keep in mind that the moisture content of the samples influences the results of
the other elements.
6.1.1 Selection of sample weight
The best sample weight depends on the element content, the homogeneity and the
combustion behavior of the sample. The limits of the working ranges for each element
and the valid calibration must be adhered to. Combustion of the sample must be timely
limited and the pressure must be controllable.
The sample weight of a substance depends on the contents of the elements C,H,N and
S to be measured considering the dynamic working ranges of the modes of operation
(see chapter 2).
• If the substances are known (for instance in quality control) the possible weigh-in
range can be estimated by calculating for each element how much weight is
necessary for reaching the lowest and highest calibration value. The possible
weigh-in range of a substance results from the highest weight for reaching the
lowest calibration point and the lowest weight for reaching the highest calibration
point. The combustion respectively the O2-dosing must be optimized within these
limits. It could happen that a simultaneous determination of all elements of one
weigh-in is not possible.
01.04
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
Page
6-2
Operating the vario EL
Example: Stearic acid (76,0 %C; 12,76 %H) in CHN-mode:
C
H
working range/calibration
for CHN-mode
0.03
20 mg abs.
0.03
2 mg abs.
weigh-in [mg stearic acid]
0.039 mg
0.235 mg
26.31 mg
15.67 mg
This calculation shows that a minimum of 0.235 mg and a maximum of 15.67 mg
stearic acid can be measured.
• If the substances are unknown, a test measurement with 5 to 10 mg substance is
performed and the received rough values are used for the determination of the best
sample weight.
6.1.2 Possibilities of sample packing
Usually the sample is packed into tin containers since they combust exothermal and
the sample is, therefore, combusted with a high initializing temperature. For special
applications, boats made of other metal foils (e.g. Al, Ag) are available (see
consumables catalog).
Depending on the mode of operation and the analytical task, it is possible to add
additives to the samples to aid combustion or to bind interfering substances. For
analyses with the vario EL, tungsten trioxide powder (WO3-powder) as a sample
additive is used only in the CHNS/CNS/S-mode as a routine. For dosing and function
see chapter 7.1. Other additives or aids are usually not needed. If necessary, consult
the available literature on the subject or our application laboratory.
For sample packing the following points are especially important:
a) Contamination through body grease or perspiration must be avoided. Therefore, do
not touch the packing with your hands. Capsules for low C determination should be
washed with acetone and dried before packing.
b) Substance loss after weighing must be avoided. This is possible through exact
folding of the sample into the tin foil or through gas tight closing of the tin
capsules.
c) Air in the sample material must be minimized (falsifying of the N-value). This is
possible by compressing the sample packing or by flushing the capsules with gas.
For this purpose several aids are offered (see chapter 1).
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
05/05
Operating the vario EL
Page
6-3
Depending on the sample matrix, the following packing methods can be selected:
sample matrix
type of packing
procedure/remarks
•
“classical“
method
in
tin
foil
light to middle weigh-in
•
or tin boots
range
solid samples
•
•
(e.g. test substances,
chemicals, coal, rubber)
•
solid samples
•
•
•
•
(e.g. oil, petroleum,
plant extracts)
packing in tin
capsules
•
•
•
•
•
•
01.04
if necessary add sample additive (e.g. WO3powder) and counterbalance to zero;
fill in sample;
close tin with a pair of tweezers tightly
above the sample;
with a pair of tweezers shape sample into a
cube and press the air out;
When folding the sample, make sure that no
bits of tin foil protrude from the folds;
• weigh sample and enter the weight either
manually or from an online balance into the
PC;
• place sample into carousel;
packing in tin foil • shape paper into a pan or use tin boats;
high sample weight or
sample
voluminous samples
compressing with •
hand pressing
(e.g. soil, cellulose,
tool or pelletizer •
fiber glass filter)
paste like and
liquid samples
counterbalance tin boats or tin foil so that
the scale shows "0";
counterbalance to zero;
set tin to zero.
if necessary add sample additive (e.g. WO3powder) and counterbalance to zero;
fill in sample;
close tin with a pair of tweezers tightly
above the sample; if gloves are worn, it is
possible to twist the tin by hand above the
sample.
place packet into pressing tool and use
molding plug;
shape a pellet with the pelletizer (see
chapter 1) or a hand pressing tool;
weigh the pellet;
place pellet into carousel;
counterbalance tin capsule to zero and place
into capsule pressing tool (see chapter 1);
fill sample into capsule using a pipette or a
syringe;
flush capsule with CO2 if necessary and
close airtight;
in case the sample contains volatile compounds,
the capsule should be filled to the brim and
closed below the filling level. Sample rests
sticking to the outside must be removed with a
suitable solvent (e.g. acetone).
weigh sample;
place capsule into carousel.
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
Page
6-4
Operating the vario EL
6.1.3 Selection of oxygen dosing amounts
Insufficient oxygen dosing reduces the catalysts, thereby
decreasing their effectiveness and durability.
Sample substance that has not been burnt remains in the
ash finger and falsifies the result of the following
samples.
Through manual O2-dosing setting and individual allocation of an automatic dosing
time (O2-index 1-5) for every sample, the vario EL makes it possible to reach a high
dynamic in the weigh-in range for very different samples matrixes.
In any case, the O2-dosing (dosing time and amount) depends on the sample matrix
and the weight. Which means that an O2-index (1-5) with sufficient oxygen dosing
must be assigned to each sample.
The O2-dosing amount must also be regulated to reach a sufficient O2-concentration.
In general the O2-dosing is adjusted one time on the needle valve (illustration 5.1/5.2,
no. 7) during combustion of a starting sample and remains constant during the entire
analysis run. For normal combustible substances we recommend 20 - 25 ml/min. For
substances that are hard to combust we recommend - depending on sample weight and
application - 30 - 45 ml/min.
O2-dosing
amount
display O2-flow
meter
25 ml/min
35 ml/min
1,5 cm
2,0
50 ml/min
2,8 cm
65 ml/min
3,5 cm
application
standard setting
easy to normal combustible substances
(combustible weight approx. 10 mg)
easy to normal combustible substances
(combustible weight approx.. 20 mg)
hard to combust substances (e.g. graphite, coal
etc.)
Different combustion behaviors of several samples are compensated through
allocation of the O2-dosing time or combustion time (O2-Index 1-5).
O2-Index dosing time Application
1
90 s
2
3
1s
120 s
4
150 s
5
180 s
test substances and easy combustible substances
sample weight up to 10 mg
blank value without O2
sample weights from 10 - 20 mg substances of easy to normal
combustible
sample weights to 10 mg substances that are difficult to combust.
sample weights above 20 mg and substances that are very
difficult to combust
depending on the combustion behavior for substances that are
difficult to combust or substances that smolder
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
05/05
Operating the vario EL
Page
6-5
Remaining oxygen is bound at the copper contact in the reduction tube. Therefore, an
overdosing should be avoided in order not to drastically shorten the life of the tube.
For a constant sample matrix, we recommend to optimize the oxygen dosing for cost
reasons.
A representative sample material where the element contents are known is weighed
repeatedly (having the same weight - max. ± 1 mg deviation). During this procedure
the O2-dosing time is reduced systematically and if necessary also the O2-dosing
amount. If failures are registered, the settings of the last successful measurement are
the optimum for this matrix and sample. To be sure, some known samples similar to
this matrix should be measured as during a routine operation to check the applicability
of the determined O2-dosing.
Note:
Optimizing the life times of the reduction tube is very nice but it should
never lead to a bad sample combustion!
6.2 Daily measuring routine
Part of the daily measuring routine (after shutdowns for longer than 2 hours) is conditioning
the vario EL with several so-called “Run-in“-samples. During the conditioning phase the
correct process of the analysis, the function of the individual components and the flow and
pressure behavior of the gases should be checked.
The next step is a factor determination (see chapter 6.2.2), to adjust the calibration to the
atmospheric conditions of the analysis point in time. The reproducibility of the measurements
and the day-to-day fluctuations of the daily factor are a good criteria to judge the instrument
condition (catalyst aging, leaks in the gas lines, blockages etc.).
The determination of the blank value limit can be sensible for several reasons (see chapter
6.2.1).
After editing the sample data and assigning the respective O2-indices (1-5) the analysis can
start (see chapter 6.2.3).
6.2.1 Blank value limit determination
For blank value measurement enter the name of the sample with "blank". It is also
necessary to assign a hypothetical weight (for instance 1 mg) to the blank sample.
Blank value limit determination serves several purposes and can, therefore, be
performed in different procedures.
01.04
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
Page
6-6
Operating the vario EL
A) The blank value serves as a so-called "rough leak test" measure for gas
tightness of the vario EL. For this purpose, several blank value measurements
(without sample) with very little oxygen (O2-Index =5) are performed after
maintenance operations or tube exchanges. The integrals for N should not be at 20
to 50 after stabilization.
B) Blank value measurements [without sample but with oxygen (O2-index 1)]
between analyses of real samples show complete combustion. Complete
combustion of the previous sample is confirmed if the C-integral of the blank
value is max. 0.1 % of the integral value of the last analyzed sample or approx. 50
integrals. Blank value measurement should be performed to check O2-optimizing
(see chapter 6.1.3).
C) Blank value measurements between standard samples and real samples are for
reduction of the instrument equilibrium (for effects during S-determination see
chapter 7.1). These blank value measurements are necessary when the absolute
content of the samples is smaller than that of the standard sample. However, it is
also possible to weigh-in the test run samples or the daily factor samples with an
absolute content similar to that of the sample.
D) For blank value determination of additives (e.g. WO3-powder) or packing
materials blank values are measured. They are made without sample substance
but with the same sample preparation (additive amount, type of packing and
material). The O2-index (1-5) should be the same for real samples and for blanks.
The mean value of the blank value integral can then be edited and deducted from
the samples. Only if the blank value through sample preparation remains the same
it can be "calibrated in" during calibration and does not need to be deducted.
Standard substances for calibration and daily factors must then be prepared
identically as the samples.
6.2.2 Factor determination
Note:
For calibration computation the substances must be identified as
“calibration sample“.
For factor computation the substances must be identified as “Factor
sample“.
Identification in the menu "Standards" is also possible after the analysis.
6.2.2.1 With calibration substances
To adjust the calibration to the daily measuring conditions, it is necessary to measure
calibration standards which are very much like the samples in their integral range.
The daily factor can be determined in three ways.
a) Compute manually (nominal content/ real content) and assign to real samples
[EditÖInput]
For this purpose, any standard substance which does not have to be defined in the
Standards-menu can be used as sample.
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
05/05
Operating the vario EL
Page
6-7
b) With the function Math.ÖFactor the daily correction factor can be computed
automatically and assigned to the following samples.
For this purpose, the daily factor samples must have an identification that is defined in
the Standards-menu and the standard substance must be activated as “factor sample“.
c) In the menu Math.ÖSetup mode and degree of automation of the daily factor
computation can be set. The same conditions are valid as described under point b. (For
further information see online-help program HelpÖIndex).
Note:
For working continuous automatic analysis run, we suggest to activate the
function “Standard-Tolerance-Monitoring“ (OptionsÖError .......). With this
function, the fluctuations of the results of standard samples are checked and
in case of surpassing the “rel. tolerance“ which is defined in the Standardmenu, the analysis run will be stopped.
6.2.3 Editing an analysis series
For routine operation of the vario EL we suggest - depending on the mode of
operation - the following analysis sequence:
mode
analysis sequence
CHNS/CNS 4 x run-in
(5 mg sulphanilic acid, O2-Ind.=1)
4 x sulphanilic acid (daily factor; approx.. 5 mg sulphanilic acid, O2-Ind.=1)
real samples
at the end of an analysis run (max. 60 real samples) for checking the daily
factor
6 x sulphanilic acid (approx.. 5 mg sulfanilic acid, O2-Ind.=1) to be
measured.
S
CHN/CN/N
4 x run-in
(5 mg sulphanilic acid, O2-Ind.=1)
4 x sulphanilic acid (daily factor; approx.. 5 mg sulphanilic acid, O2-Ind.=1)
real samples
at the end of an analysis run (max. 60 real samples) for checking the daily
factor
6 x sulphanilic acid (approx. 5 mg sulfanilic acid, O2-Ind.=1) to be
measured.
2 x run-in
(5 mg acetanilide, O2-Ind.=1)
3 x acetanilide
(daily factor; approx. 5 mg acedanilide, O2-Ind.=1)
real samples
at the end of an analysis run (max. 70 real samples) for checking the daily
factor
4 x acetanilide
(approx. 5 mg acetanilide, O2-Ind.=1) to be measured.
Before weigh-in of a new analysis series, sample feeder must be on zero
(OptionsÖMiscellaneousÖSample Feeder), so that the running analysis number
matches the number of the carousel. Then the substances are packed and weighed (see
chapter 6.1.2).
01.04
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
Page
6-8
Operating the vario EL
The following data must be edited in the PC (EditÖInput):
•
weight [mg]
can either be entered manually or can be transmitted directly from an on-line
balance.
•
Name (max. 32 characters)
sample name or identifier
Daily factor and calibration samples must carry the name defined in the
Standards-menu. Blank samples must be identified with “blank“.
•
Method
defines the oxygen dosing (see chapter 6.1.3).
The other data in the input-menu can be entered before or after the analysis (see
online-help).
6.2.4 Data storage and print-out
After each analysis the measuring data are displayed on the screen and saved in a
temporary. Apart from the measuring data also all graphic information (pressure,
peaks etc.), (timely course) is stored in the temporary file.
In compliance to a GLP correct documentation we suggest to save the original
measuring file after every analysis series (FileÖSave and/or FileÖSave As). The
graphics information will also be saved.
These graphics data will be available upon a later reload of the document. Therefore,
not only the analysis results of each individual sample but also the timely course can
be viewed.
Of course the saved measuring values can be printed (FileÖPrint) or worked at any
time.
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
05/05
Operating the vario EL
Page
6-9
6.2.5 Statistics
After clicking on Math.ÖStatistics, the dialog Statistics: Define Groups appears (see
chapter 6.1). Here you can form measurement values into groups. The program then
calculates the mean value for each of these groups and the standard deviation (see also
HelpÖIndexÖCalculation Data). The values are displayed - after closing the dialog - in
the sample field of the statistics display (DisplayÖStatistics) (see chapters 7.3,
7.2.4.3).
Illustration 6.1: dialog statistics: define groups
The dialog shows two areas, one “Sample Area“ and one “Group Area“. The “Sample
Area“ contains all samples currently in the memory. The “Group Area" shows the
samples selected for statistics computation (for instance multiple determination of the
same sample). On the right side below the group area the “Group No.“ of the currently
displayed group is shown.
Groups can be built in two ways:
01.04
Automatic Group Formation:
With the button [Auto] the groups with the same
name are combined to groups.
Manual Group Formation:
The groups are formed individually through
selection and group assignment.
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
Page
6-10
Operating the vario EL
Selection Possibilities:
• Selecting the sample by clicking it on.
• Selecting sample successions by clicking on the first one and then by checking on
the last sample keeping the <Shift>-key depressed at the same time.
• Selecting individual samples by clicking on the first samples and then clicking on
the other samples by keeping the <Ctrl>-key depressed at the same time.
The function [Add] adds selected samples to the currently activated group. [Delete]
removes selected samples from the group area.
The buttons [Next], [Back], [<<] and [>>] permit opening of several groups.
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
05/05
Operating the vario EL
Page
6-11
6.3 Checklist for analysis start
♦Gases turned on?
♦Heaters up to nominal temperature?
CHNS/CNS/S
CHN/CN/N
combustion tube
1150 °C
950 °C
reduction tube
850 °C
500 °C
♦Pressures o.k.?
(inlet pressure gauge 1.25 ± 0.05 bar, PC-pressure display approx. 1.25 ± 0.05 bar)
♦Has flow meter been checked?
(He right side: 2.5 ± 0.5 cm; O2 left side: 1 ± 0.5 cm)
♦Enough capacity in drying tubes?
(last third still white? - see chapter 9.6)
♦Soot filter o.k.?
(see chapter 9)
♦Have maintenance intervals of the reaction tubes been observed?
Always check reduction tubes and if necessary absorption-U-tube and O2-lance directly
and empty ash finger (see chapter 9ff)
♦Detector signal low and stable?
(see TCD-signal in the status area)
Now the “run-in“-samples and blank values can be measured!
♦“run-in“-samples and blank values o.k.?
(see chapters 6.2 u. 6.2.1)
♦Has analysis sequence been edited with daily factor?
(see chapter 6.2.3)
♦Parameter (O2-Index =1-5) assigned correctly?
(see chapter 6.1.3)
♦
Are samples on carousel?
When everything is all right, the analysis can be started with [SystemÖAuto] or
[SystemÖSingle]!
01.04
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
Page
6-12
Operating the vario EL
6.4 Calibration
The element analyzer vario EL does not perform absolute measurements, i.e. the connection
between the CHNS content [mg absolute] and the CHNS measuring value [integral] must be
calculated by means of a calibration. In every mode of operation a calibration that covers the
desired working range for each element must be performed. For this purpose, test substances
(for instance sulphanilic acid, acetanilide) with given element content and different weights
are analyzed. The PC program automatically computes the calibration function (fourth power
equation).
A correct calibration covering the entire requested
working area for each element, is decisive for the
correctness of the results. Therefore, calibrations must be
performed with utmost care.
Observe the Operating instructions diligently!
Experience shows that the calibration of the vario EL remains stable for at least 6 months.
Recalibration is recommended when the daily factor is outside the range of 0.9 to 1.1 or if
components which influence the results (e.g. detector or adsorption columns) have been
exchanged. Changing the desorption temperature of adsorption columns can also require a
recalibration.
Note:
a successful calibration is only possible if the operator is familiar with the
operating instructions and the technical possibilities of the vario EL.
6.4.1 Analysis of the calibration samples
Note the following instructions:
• Calibration substances must be defined in the Standards-Menu and identified
as "Calibration Sample".
Using the sample identification the theoretical element content is assigned to the
calibration samples. If the element content of a sample substance is defined with
the value zero (0), the respective element will be ignored during computation.
recommended
standard substances
sulphanilic acid p.a.
acetanilide p.a.
stearic acid p.a.
(octadecanic acid)
bencoic acid p.a.
Ntheor. [%]
Ctheor. [%]
8,09
10,36
0
0
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
Htheor. [%]
41,61
71,09
76,00
4,07
6,71
12,76
68,80
5,00
Stheor. [%]
18,50
0
0
0
05/05
Operating the vario EL
Page
6-13
Note:
in the standard menu the „relative tolerance [%]“, i.e. the permitted
deviation range of the result for each element, is also defined.
Usually 5.0 % is assumed.
Note:
For calibration calculation, the appropriate samples must be identified
as "calibration sample".
For factor calculation, the appropriate samples must be identified as
"factor sample".
Identification in menu Standards is also possible after the analysis.
• Check parameter settings in the respective mode of operation
(factory set recommendations see chapter 7ff)
• Check and optimize instrument condition before calibration.
Example:
leaktest (see chapter 9.2.1), replacement of tube fillings
chapter 8ff)
replace ash finger
(see
• Packing of the calibration samples in tin boats (see chapter 6.1.2).
• To guarantee the best possible sample combustion, the following O2-dosing
quantities and combustion times are to be set.
weigh-in
approx. 0 to 10 mg
> 10 to 25 mg
> 25 mg
O2-quantity (see chapter 6.1.3)
[cm at O2-flow meter]
2.5 cm
2.5 cm
2.5 cm
O2-index
1=
4=
5=
90 s
150 s
180 s
• Suitable balances are required for weighing the calibration substances.
Usually a readability of 0.001 mg is sufficient.
• Editing the calibration process can be done in the dialog EditÖInput.
The following is a calibration recommendation which covers a sufficient measuring
range in the CHNS mode. Of course, an adjustment to customer specific
requirements is possible at any time. Recommendations for calibrations in different
modes are described in chapter 7.
The weight can also be entered directly through the balance interface. In that case
only the identifiers and the O2-Indices must be edited.
01.04
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
Page
6-14
Operating the vario EL
Calibration for vario EL in CHNS-mode
quantity
10
3
22
3
14
3
6
type of sample
conditioning
conditioning
calibration samples
description
sulphanilic acid
ea. 5.0 mg
sulphanilic acid
ea.0.1 - 0.15 mg
sulphanilic acid with weigh-ins in mg:
0.1-0.1-0.2-0.3-0.4-0.5-0.75-1.0-1.251.5-1.75-2.0-2.5-3.0-3.5-4.0-4.5-5-6-7911
conditioning
Acetanilide
ea. 5.0 mg
calibration samples acetanilide with weigh-ins in mg:
5-6-8-10
12-14-16-18-20-22-24
26-28-30
conditioning
stearic acid
ea.14.0 mg
calibration samples stearic acid with the following weighins in mg:
14-16-18-20-22-24
identifier
run-in
run-in
sulphanilic
acid
run-in
acetanilide
run-in
stearic acid
O2-index
1
1
1
1
1
4
1
1
4
5
4
5
• Now start calibration run by clicking the menu item SystemÖAuto.
• After the analysis of all calibration samples the original values should be saved
(with FileÖSave).
6.4.2 Calibration evaluation
a) Curve computation
• When all calibration samples have been processed, start the computation of the
calibration curve with the function Math.ÖCalibrate. At least four calibration
samples are required (see chapter 6.4.1, item 1).
• In the appearing dialog Configure Calibration, you can chose between the three
types of computations “linear“,“non- linear“ and “mixed“ for every element (see
illustration 6.2). Computation of the calibration curve is performed via clicking the
corresponding computing button.
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
05/05
Operating the vario EL
Page
Mode of calculation Form
linear
non-linear
(4th order polynom)
mixed
6-15
Remarks
y = a + bx
Only recommended if the
integral range is very narrow
(i.e. weight and N-content of
the samples are always equal).
Otherwise only applicable in the
low concentration range.
2
3
4
y = a + bx + cx + dx + ex Usual evaluation for the entire
range.
low range = linear
higher range = polynomial
If high accuracy is also required
for very low measuring values,
the working range is divided.
A factor correction must then
be performed in both ranges!
Illustration 6.2: dialog configure CHNS-calibration
• When the type of computation has been selected, click on [Configure N Calibration].
Depending on the selected type of computation the dialog Select/Linear/Polynomial Range
or Calibration appears. (For information see HelpÖIndexÖDialog Overview).
Since the non-linear polynomial calibration is sufficient for most applications, we will
discuss only this type of calculation.
Evaluating the curve adjustment
• After computation has been carried out, a dialog consisting of coordinate axis with
calibration points and the calibration curve is displayed on the screen. (see
illustration 6.3). In this graph the individual calibration points are shown as circles
and the curve resulting from computed calibration coefficients. The calibration
sample with the lowest index is marked at the beginning with a cursor cross.
• This graphic display can be changed in such a way that an optical control of the
curve adjustment is possible. This can be done through the functions [Zoom +],
[Zoom -] and [Center].
01.04
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
Page
6-16
Operating the vario EL
• Through functions [Prev] and [Next] any sample can be marked with the cursor so that its
position to the curve as well as the respective sample information is displayed.
Note:
a sample can be selected by clicking on its circle.
Illustration 6.3: graph of a calibration curve
Sample-Information Description
Sample No.
Area
Slope
theo.
act.
diff.
Curve-Information
a....e
Zoom
Q1 (actual)
Q2 (last)
shows the analysis number (running No.) of the marked sample
(with cursor);
integral value of the marked sample
slope of the curve at the calibration point (marked sample)
[integr./mg]
theoretical N-absolute content of the marked sample [mg]
N-absolute content of the marked sample computed with actual
curve [mg]
difference between “theo“ and “act“
Description
coefficients of the computed polynom.
shows the magnified graph (zoom factor).
Quality measure of the degree of adaptation of the actual curve
computation.
If the computation is linear, Q is the correlation coefficient
(Optimum = 1).If the computation is polynomial, Q is the sum
of all error squares (Optimum = 0).
Quality measure for the degree of adaptation of the last curve
computation.
Serves for comparison with Q1, to check, for instance, the
effectiveness of sample elimination.
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
05/05
Operating the vario EL
Page
6-17
The quality of the degree of adaptation is calculated according to the following
formulas:
linear
computation
r2 =
2
 xiyi − ∑ xi ∑ yi 
∑
n 
2
( ∑ yi)

( ∑ xi )  
2
i
−
x
∑ yi 2 −

∑
n  
n

2



whereby:
r2
xi
yi
n
correlation coefficient
integral of the respective sample
absolute content [mg abs.] of the respective sample
total quantity of samples
polynomial
computation
Q=
SFQ
( n − 1)
n ( act. − theo ) ⋅ 100 
SFQ = ∑ 
theo i

i = 1

whereby:
Q:
n:
SFQ:
acti:
theoi:
2
quality
quantity of calibration samples
sum of error squares
computed absolute content of the respective sample
theoretical absolute content of the respective sample
Illustration 6.4: formulas for quality computation
• The displayed sample information and the quality (Q1) of the curve information provide
information for optimizing the curve adaptation.
For polynom computation the following is valid:
Obtainable quality values are usually between 3 to 1 (optimum = 0) for N, 1.5 to 0.5 for C,
3 to 1 for S and 12 to 6 for H.
The difference (between theoretical and actual) of the individual samples should be as low
as possible, whereby the differences for larger weigh-in can become greater.
(e.g.
weigh-in
< 5 mg
permissible diff.
0.002 - 0.003 mg
5 - 15 mg
0.004 - 0.008 mg)
The slope of the curve can be used to judge so-called "outliers". The dependence of the
integrals on the absolute N-content is a constant function, so that "outliers" will drop out of
a defined course of slope which means the “Slope“ (Integr./mg) of an outlier will be
noticed.
01.04
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
Page
6-18
Operating the vario EL
c) Elimination of outliers
• Illustration 6.5 shows a marked sample, which can be recognized as outlier visibly as well
as through the sample information “Slope“ and “Diff“.
Illustration 6.5: calibration menu with marked outliers
• These marked outliers can be eliminated through the function [Kill]. Thereafter the curve
is computed again. The effect of the elimination can be evaluated through the new quality
(Q1). The eliminated samples are shown as light gray circles and can be reactivated
through the function [Unkill] if necessary.
d) Closing
• By clicking on [Close], the calibration dialog (illustration 6.3) will be closed and the
dialog Configure Calibration re-appears (illustration 6.2). After all calibration coefficients
have been computed, function [OK] is active. With [OK] this computation can be accepted.
If another mode of computation is desired, the calibration data can be processed again but
the coefficients of the previous computation that have not been saved will be lost.
• After clicking on [OK], the dialog with newly computed calibration coefficients appears
(see illustration 6.6).
• Through the function [OK], the coefficients will be accepted as the actual calibration.
Through the function [Cancel], the dialog is closed and the coefficients are rejected (for
further information see online-help HelpÖIndexÖDialog).
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
05/05
Operating the vario EL
Page
6-19
Illustration 6.6: dialog CHNS Calibration-Coefficients
6.5 Shutdowns during analysis breaks
6.5.1 Short breaks
During analysis breaks for one night or several days (2 - 5 days), the vario EL and the
PC remain in a state of readiness. Only the following steps should be taken:
a) Manual
• Reduce temperature of the combustion tube to 900°C in CHNS/CNS/S mode
[OptionsÖParameters]
Note: for setting the furnace temperatures, the corresponding access rights are
required.
• Turn off He-supply. (O2-supply should remain open for flushing purposes.) To cut
down the He-supply, reduce the prepressure at the bottle or the supply-source until
the He flow meter shows 0.3cm.
• Turn down screen lighting.
01.04
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
Page
6-20
Operating the vario EL
b) Through the software (see also Online-Help)
• Click on OptionsÖSleep-/Wake-Up-Function.
In this dialog (see illustration 6.7) it is possible to select the shut-down conditions.
• Select "Activate Gas Reduction Option “ and set “Gas Reduction to“ to 0%.
• Select "Activate Sleep Temperature“ and set the reduction temperatures.
“Reduce Furnace 1 to“ 900 °C.
Illustration 6.7: dialog sleep-/wake-function
• Ways to activate the Sleep-Function:
[Sleep Now]
starts the shut-down conditions immediately
“Sleep after End of Samples“
The vario EL is brought into shut-down
condition after the last sample has been
The vario EL is brought into shut-down
condition before the respective sample is
processed.
“Sleep at Sample No.“
• Ways to activate the Wake-Up-Function:
[Wake-Up]
“Wake-Up Time“
Heats up the vario EL to the appropriate
operation temperature and flushes the instrument
with gas.
With this function a “Time“ can be defined at
which on a certain “Date“, “daily“ or on
weekdays Wake-Up is performed.
“Continue Analysis after Wake-Up “ permits the
automatic analysis start, provided there are
unprocessed samples in the data memory.
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
05/05
Operating the vario EL
Page
6-21
6.5.2 Longer shutdowns
Note:
To transport the vario EL, lock the moveable 3-tube-furnace with the
supplied transport safety guard (see chapter 5.3 and illustration 5.5)
For longer shutdowns lasting several days or weeks, proceed as follows:
• Cool down all heaters and adsorption columns and wait (approx. 2 hours) until the
temperatures are lowered to room temperature (max. 100°C). For this purpose set
nominal temperatures to 0°C OptionsÖParameters.
• Exit software program via SystemÖOffline and FileÖExit.
• Turn off gas supply (He and O2).
• Turn off vario EL and peripheral instruments.
Note:
To restart operation of the vario EL proceed in reverse order (see also
chapter 5.3.4).
If operation is re-started (see also chapter 5.3), tube
fillings must be checked respectively renewed.
Adhere to conditioning instructions!
From used tubes at least the moisture should be removed
through 2 hour heating.
01.04
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
Particulars of the individual modes of operation
Page
7-1
7. Particulars of the individual modes of operation
7.1 Modes with S-determination
Modes of operation during which sulfur is determined simultaneously, work with the
combustion tubes and the reduction tube as described in chapter 9.1.1. The operating
temperature of these tubes is very high (combustion tube = 1150 °C, reduction tube =
850 °C).
The sample preparation (see chapter 6.1.2) requires the use of a WO3-sample additive so
that alkali and earth alkali elements from the sample do not react with the quartz glass of the
tubes and destroy the tubes. It also prevents forming of alkali sulfates which are hard to
combust.
• Test substance or known samples without alkali content (organic chemicals, organic
liquids) do not require WO3-sample additives.
• Samples with a low alkali content (coal, rubber) require at least one time the sample
weight of WO3-powder.
• Samples with a high alkali content (soil, sediments) require at least three times the
sample weight of WO3-powder.
Note:
If in doubt, it is better to use too much WO3-powder than not enough. Only a
few alkali containing samples without WO3 are enough to contaminate the ash
finger which leads to failure results for S.
Make sure that WO3-powder (11.02-0017) is only
used as additive and WO3-granulate (11.02-0008) as
tube filling!!!
A mix-up can clog the combustion tube.
Application tip: S-determination reacts very sensitive to a balance change in the reaction
tube. Therefore, the following effects can be observed if the S-contents of the samples vary
considerably:
1. S-wash-out: depending on the H-content of the current sample, S-wash-outs from the
conditioned equilibrium occur when analysing samples with a high S-content before
samples with a low or no S-content. This means that the S-results for 1 to 2 analyses will
be too high (until the new equilibrium is reached).
This effect is not caused through bad sample combustion or delay, which would be
indicated through higher C-values.
Recommendation: sort samples according to their S-content or - if content differences are
very high - analyses "run-in samples" with a low weight or low absolute content in
between.
05.05
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
Page
7-2
Particulars of the individual modes of operation
2. S-failure results: on the other hand, failure results occur for 1 or 2 analyses when
measuring samples with a low S-content, followed by samples with a high S-content until
the reaction tube has reached the new equilibrium.
7.1.1 CHNS-mode
Illustration 7.1: tubing scheme vario EL, CHNS-mode
________________________________________________________________________________________
Operating Instructions vario EL
03.04
Copyright by E l e m e n t a r Analysensystem GmbH
Particulars of the individual modes of operation
Legend:
c to 143
V2 + V3
V4
V7
V8 + V9
V10
A
B
C
D
E
to illustration 7.1
Page
F
G
H
numbers of tubes
valves for desorption path SO2
O2 inlet valve
He inlet valve
valves for desorption path H2O
flushing gas valve
SO2-adsorption column
H2O-adsorption column
CO2-adsorption column
drying tubes
I
J
K
L
M
N
O
P
He-flow meter
Q
7-3
gas purification tube
combustion tube
reduction tube
parting wall
O2-flow meter
mass flow controller (MFC)
needle valve
flow controller
measuring gas
reference gas
magnet valve (without current from 2 to 3
open)
pressure gauge, gas inlet pressure
Illustration 7.1 shows the tubing scheme of the CHNS-mode with complete tubing
numbering. This illustration enables the operator to control all gas streams in the
vario EL because the tubes and valves inside the instrument are also marked (for
identification of instrument components see also illustration 4.1).
The factory set parameters, which should be entered under OptionsÖParameters are
shown in illustration 5.7 (for information regarding the meaning of the parameters see
chapter 5.3.5).
If mostly large amounts of carbon (> 20 mg C abs.) are to be analyzed, the desorption
temperature of the CO2-adsorption column must be reduced to 80 °C so that the peak
of C becomes flatter (below 10 V) and wider. This change requires a new Ccalibration!
The operation mode “half of the gas flow during N-Integration“ (Gas/2 during NIntegr.) may not be activated for this parameter set because the process times do not
match. For this mode of operation a time adjustment must be performed (see chapter
5.3.5). If necessary, contact our application laboratory.
The course of the analysis has already been discussed in chapter 4.2. Illustration 7.2
shows the typical measuring peak course for the CHNS-mode with the factory set
parameters (illustration 5.7).
A recommendation for a CHNS-calibration was made in chapter 6.4. An individual
adjustment to the respective analytical tasks or the necessary working range can be
made by the operator.
05.05
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
Page
7-4
Particulars of the individual modes of operation
Legend:
1
2
3
4
5
sample feeding peak
detector fluctuations
N2-peak
CO2-peak
H2O-peak
SO2-peak
Illustration 7.2: typical course of measuring peak
7.1.2 CNS-mode
Illustration 7.3 shows the tubing scheme of the CNS-mode with complete tube
numbering. This illustration enables the operator to control all gas streams in the
vario EL because the tubes and valves inside the instrument are also marked (for
identification of instrument components see also illustration 4.1).
Combustion and reduction tubes are identical with the CHNS-mode. Only a H2Oabsorption-U-tube is installed between reduction tube-exit and tube # 9(see chapter
9.2.3). Furthermore the H2O-adsorption column is removed and replaced by the tube
#146 (see chapter 7.3).
The factory set parameters, which should be entered under OptionsÖParameters are
shown in illustration 7.4 (for information regarding the meaning of the parameters see
chapter 5.3.5).
Note: parameters can only be changed with the corresponding access rights.
If mostly large amounts of carbon (> 20 mg C abs.) are to be analyzed, the desorption
temperature of the CO2-adsorption column must be reduced to 80 °C so that the peak
of C becomes flatter (below 10 V) and wider. This change requires a new Ccalibration!
The operation mode “half of the gas flow during N-Integration“ (Gas/2 during NIntegr.) may not be activated for this parameter set because the process times do not
match. For this mode of operation a time adjustment must be performed (see chapter
5.3.5). If necessary, contact our application laboratory.
________________________________________________________________________________________
Operating Instructions vario EL
03.04
Copyright by E l e m e n t a r Analysensystem GmbH
Particulars of the individual modes of operation
Page
7-5
Illustration 7.3: tubing scheme vario EL, CNS-mode
05.05
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
Page
7-6
Particulars of the individual modes of operation
Legend:
c to 143
V2 + V3
V4
V7
V8 + V9
V10
A
B
C
D
E
to illustration 7.1
F
G
H
numbers of tubes
valves for desorption path SO2
O2 inlet valve
He inlet valve
valves for desorption path H2O
flushing gas valve
SO2-adsorption column
H2O-adsorption column
CO2-adsorption column
drying tubes
I
J
K
L
M
N
O
P
He-flow meter
Q
gas purification tube
combustion tube
reduction tube
parting wall
O2-flow meter
mass flow controller (MFC)
needle valve
flow controller
measuring gas
reference gas
magnet valve (without current from 2 to 3
open)
pressure gauge, gas inlet pressure
The course of the analysis process has been discussed in chapter 4.2. The typical
course of the measuring peak for the CNS-mode is derived from the CHNS-mode
(illustration 7.2), only the H2O-peak (4) is missing.
Calibration is described in chapter 6.4. For the CNS-calibration the sulfanilic acid
and acetanilide is weighed-in as for the CHNS-calibration. For further calibration of
the C-working-range up to 30 mg, we recommend benzoic acid. An individual
adjustment to the respective analytical tasks or the necessary working range can be
made by the operator.
Illustration 7.4: Parameter-menu, CNS-mode
________________________________________________________________________________________
Operating Instructions vario EL
03.04
Copyright by E l e m e n t a r Analysensystem GmbH
Particulars of the individual modes of operation
Page
7-7
7.1.3 S-mode (with TCD)
Illustration 7.5: tubing scheme vario EL, S-mode (with TCD)
05.05
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
Page
7-8
Particulars of the individual modes of operation
Legend:
c to 143
V2 + V3
V4
V7
V8 + V9
V10
A
B
C
D
E
to illustration 7.1
F
G
H
numbers of tubes
valves for desorption path SO2
O2 inlet valve
He inlet valve
valves for desorption path H2O
flushing gas valve
SO2-adsorption column
H2O-adsorption column
CO2-adsorption column
drying tubes
I
J
K
L
M
N
O
P
He-flow meter
Q
gas purification tube
combustion tube
reduction tube
parting wall
O2-flow meter
mass flow controller (MFC)
needle valve
flow controller
measuring gas
reference gas
magnet valve (without current from 2 to 3
open)
pressure gauge, gas inlet pressure
Illustration 7.5 shows the tubing scheme for the S-mode with thermal conductivity
detection. This complete numbering of the tubes enables the operator to control all gas
streams in the vario EL because the tubes and valves inside the instrument are also
marked (for identification of instrument components see also illustration 4.1).
Combustion and reduction tubes are identical with the CHNS-mode. Only a H2Oabsorption-U-tube is installed between reduction tube-exit and tube # 9(see chapter
9.2.3). Furthermore only the SO2-adsorption column is in the gas line and its exit is
directly connected with the detector entrance (see chapter 7.3).
The factory set parameters, which should be entered under OptionsÖParameters are
shown in illustration 7.6 (for information regarding the meaning of the parameters see
chapter 5.3.5).
Note: parameters can only be changed with the corresponding access rights.
Illustration 7.6: Parameters-menu, S-mode
________________________________________________________________________________________
Operating Instructions vario EL
03.04
Copyright by E l e m e n t a r Analysensystem GmbH
Particulars of the individual modes of operation
Page
7-9
o
Legend:
1
2
n
“Dummy Peak“
SO2-peak
Illustration 7.7: typical course of measuring peak, S-mode
The course of the analysis process has been discussed in chapter 4.2. Illustration 7.7
shows a typical course of the measuring peak for the S-mode with factory set
parameters (illustration 7.7). Since the so-called “Dummy-Peak“ does not have to be
computed, an exceeded measuring range (peak higher than 10 V) does not matter.
Calibration is described in chapter 6.4. For the S-calibration the sulfanilic acid is
weighed-in as for the CHNS-calibration. For higher S-working ranges pure sulfur can
be used as standard substance. An individual adjustment to the respective analytical
tasks or the necessary working range can be made by the operator.
7.2 Modes without S-determination
Modes of operation without simultaneous S-determination work with the combustion tubes
and the reduction tube as described in chapter 9.1.1. The operating temperature of these tubes
is not as high as for the operation modes with S-determination (combustion tube = 950 °C,
reduction tube = 500 °C).
Tube filling of combustion and reduction tubes in
CHN/CN/N modes (see chapter 9.1.2) must not be
overheated, because of occurring melts which destroy
the furnaces.
When changing the mode of operation always cool
down the furnaces to room temperature. Watch for
the current furnace temperatures in the status
display!
05.05
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
Page
7-10
Particulars of the individual modes of operation
Sample preparation (see chapter 6.1.2) does not require a sample additive because the
operating temperatures of the quartz tubes do not cause a considerable reaction with alkali and
earth alkali elements.
7.2.1 CHN-mode
Illustration 7.8: tubing scheme vario EL, CHN-mode
________________________________________________________________________________________
Operating Instructions vario EL
03.04
Copyright by E l e m e n t a r Analysensystem GmbH
Particulars of the individual modes of operation
Legend:
c to 143
V2 + V3
V4
V7
V8 + V9
V10
A
B
C
D
E
to illustration 7.1
Page
F
G
H
numbers of tubes
valves for desorption path SO2
O2 inlet valve
He inlet valve
valves for desorption path H2O
flushing gas valve
SO2-adsorption column
H2O-adsorption column
CO2-adsorption column
drying tubes
I
J
K
L
M
N
O
P
He-flow meter
Q
7-11
gas purification tube
combustion tube
reduction tube
parting wall
O2-flow meter
mass flow controller (MFC)
needle valve
flow controller
measuring gas
reference gas
magnet valve (without current from 2 to 3
open)
pressure gauge, gas inlet pressure
Illustration 7.8 shows the tubing scheme for the CHN-mode with the complete
numbering of the tubes. This illustration enables the operator to control all gas streams
in the vario EL because the tubes and valves inside the instrument are also marked
(for identification of instrument components see also illustration 4.1).
The factory set parameters, which should be entered under OptionsÖParameters are
shown in illustration 7.9 (for information regarding the meaning of the parameters see
chapter 5.3.5).
Note: parameters can only be changed with the corresponding access rights.
If mostly large amounts of carbon (> 20 mg C abs.) are to be analyzed, the desorption
temperature of the CO2-adsorption column must be reduced to 80 °C so that the peak
of C becomes flatter (below 10 V) and wider. This change requires a new Ccalibration!
The operation mode “half of the gas flow during N-Integration“ (Gas/2 during NIntegr.) may not be activated for this parameter set because the process times do not
match. For this mode of operation a time adjustment must be performed (see chapter
5.3.5). If necessary, contact our application laboratory.
05.05
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
Page
7-12
Particulars of the individual modes of operation
Illustration 7.9: Parameter-menu, CHN-mode
The course of the analysis process has been discussed in chapter 4.2. Illustration 7.10
shows a typical course of the measuring peak for the CHN-mode with factory set
parameters (illustration 7.9).
p
Legend:
1
2
3
4
sample feeding peak
detector fluctuations
N2-peak
CO2-peak
H2O-peak
o
n
q
time [sec.]
Illustration 7.10: typical course of measuring peak, CHN-mode
________________________________________________________________________________________
Operating Instructions vario EL
03.04
Copyright by E l e m e n t a r Analysensystem GmbH
Particulars of the individual modes of operation
Page
7-13
Calibration is described in chapter 6.4. A recommendation for a CHN-calibration is
given below. An individual adjustment to the respective analytical tasks or the
necessary working range can be made by the operator.
Calibration for vario EL in CHN-mode
quantity type of sample
description
10
3
29
acetanilide
ea.5.0 mg run-in
acetanilide
ea.0.1 - 0.15 mg run-in
acetanilide with following weighins in acetanilide
mg:
0.1-0.1-0.2-0.3-0.4-0.5-0.75-1.0-1.25
1.5-1.75-2.0-2.5-3.0-3.5-4.0-4.5-5.0
6-7-8-10
12-14-16-18-22 26-30
3
6
05.05
conditioning
conditioning
calibration
samples
conditioning
calibration
samples
identifier
stearic acid
ea.14.0 mg run-in
stearic acid with following weighins in stearic acid
mg:
14-16-18-20-22-24
O2Index
1
1
1
1
1
4
5
4
4
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
Page
7-14
Particulars of the individual modes of operation
7.2.2 CN-mode
Illustration 7.11: tubing scheme vario EL, CN-mode
________________________________________________________________________________________
Operating Instructions vario EL
03.04
Copyright by E l e m e n t a r Analysensystem GmbH
Particulars of the individual modes of operation
Legend:
cto 143
V2 + V3
V4
V7
V8 + V9
V10
A
B
C
D
E
to illustration 7.1
Page
F
G
H
numbers of tubes
valves for desorption path SO2
O2 inlet valve
He inlet valve
valves for desorption path H2O
flushing gas valve
SO2-adsorption column
H2O-adsorption column
CO2-adsorption column
drying tubes
I
J
K
L
M
N
O
P
He-flow meter
Q
7-15
gas purification tube
combustion tube
reduction tube
parting wall
O2-flow meter
mass flow controller (MFC)
needle valve
flow controller
measuring gas
reference gas
magnet valve (without current from 2 to 3
open)
pressure gauge, gas inlet pressure
Illustration 7.11 shows the tubing scheme for the CN-mode with the complete
numbering of the tubes. This illustration enables the operator to control all gas streams
in the vario EL because the tubes and valves inside the instrument are also marked
(for identification of instrument components see also illustration 4.1).
Combustion and reduction tubes are identical with the CHN-mode. Only a H2Oabsorption-U-tube is installed between reduction tube-exit and tube # 9(see chapter
9.2.3). Furthermore the H2O-adsorption column is blind and tube # 9 is - through tube
# 145 - directly connected with the CO2-adsorption column (see chapter 7.3).
The factory set parameters, which should be entered under OptionsÖParameters are
shown in illustration 7.12 (for information regarding the meaning of the parameters
see chapter 5.3.5).
Note: parameters can only be changed with the corresponding access rights.
If mostly large amounts of carbon (> 20 mg C abs.) are to be analyzed, the desorption
temperature of the CO2-adsorption column must be reduced to 80 °C so that the peak
of C becomes flatter (below 10 V) and wider. This change requires a new Ccalibration! The operation mode “half of the gas flow during N-Integration“ (Gas/2
during N-Integr.) may not be activated for this parameter set because the process times
do not match. For this mode of operation a time adjustment must be performed (see
chapter 5.3.5). If necessary, contact our application laboratory.
The course of the analysis process has been discussed in chapter 4.2. The typical
course of the measuring peak for the CN-mode derives from the CHN-mode
(illustration 7.10), only the H2O-Peak (4) is missing.
Calibration is described in chapter 6.4. For CN-calibration only acetanilide - as for
the CHN-calibration - is weighed in. For further calibration of the C-working range up
to 30 mg, we recommend benzoic acid. An individual adjustment to the respective
analytical tasks or the necessary working range can be made by the operator.
05.05
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
Page
7-16
Particulars of the individual modes of operation
Illustration 7.12: parameter-menu, CN-mode
7.2.3 N-mode
Illustration 7.13 shows the tubing scheme for the N-mode with the complete
numbering of the tubes. This illustration enables the operator to control all gas streams
in the vario EL because the tubes and valves inside the instrument are also marked
(for identification of instrument components see also illustration 4.1).
Combustion and reduction tubes are identical with the CHN-mode. Only a H2Oadsorption-U-tube and a CO2-adsorption-U-tube are installed between reduction tubeexit and tube # 9(see chapter 9.2.3). Furthermore, all adsorption columns are blind and
tube #9 is - through tube #47 - directly connected with the measuring gas inlet of the
detector (tube #19) (see chapter 7.3).
The factory set parameters, which should be entered under OptionsÖParameters are
shown in illustration 7.14 (for information regarding the meaning of the parameters
see chapter 5.3.5).
The operation mode “half of the gas flow during N-Integration“ (Gas/2 during NIntegr.) may not be activated for this parameter set because the process times do not
match. For this mode of operation a time adjustment must be performed (see chapter
5.3.5). If necessary, contact our application laboratory.
The course of the analysis process has been discussed in chapter 4.2. The typical
course of the measuring peak for the N-mode derives from the CHN-mode (illustration
7.10), only the H2O-peak (4) and the CO2-peak (3) are missing.
________________________________________________________________________________________
Operating Instructions vario EL
03.04
Copyright by E l e m e n t a r Analysensystem GmbH
Particulars of the individual modes of operation
Page
7-17
Calibration is described in chapter 6.4. For N-calibration only acetanilide - as for the
CHN-calibration - is weighed in. An individual adjustment to the respective analytical
tasks or the necessary working range can be made by the operator.
Illustration 7.13: tubing scheme vario EL, N-mode
05.05
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
Page
7-18
Legend:
c to 143
V2 + V3
V4
V7
V8 + V9
V10
A
B
C
D
E
Particulars of the individual modes of operation
to illustration 7.1
F
G
H
numbers of tubes
valves for desorption path SO2
O2 inlet valve
He inlet valve
valves for desorption path H2O
flushing gas valve
SO2-adsorption column
H2O-adsorption column
CO2-adsorption column
drying tubes
I
J
K
L
M
N
O
P
He-flow meter
Q
gas purification tube
combustion tube
reduction tube
parting wall
O2-flow meter
mass flow controller (MFC)
needle valve
flow controller
measuring gas
reference gas
magnet valve (without current from 2 to 3
open)
pressure gauge, gas inlet pressure
Illustration 7.14: parameter-menu, N-mode
________________________________________________________________________________________
Operating Instructions vario EL
03.04
Copyright by E l e m e n t a r Analysensystem GmbH
Particulars of the individual modes of operation
Page
7-19
7.3 Instrument conversion and change of operation mode
The vario EL can be operated in modes CHNS, CNS, S, CHN, CN and N. For additional
modes (e.g. O or CH) read the respective operating instructions.
The vario EL works with 3 different adsorption columns (SO2, CO2, H2O), which are
installed in the vario EL according to the ordered equipment. For converting the instrument
to another mode of operation, it may be necessary to order additional adsorption columns or
chemicals (see information in the conversion matrix).
The following table provides general information about the adsorption columns.
adsorption column
CO2-adsorption column
order no. 11.00-0084/4
H2O-adsorption column
order no. 11.00-0086/4
SO2-adsorption column
mode of operation
CHN/CN
CHNS/CNS
CHN
CHNS
CHNS/CNS/S
order no. 11.02-0007/4
function
CO2-adsorption
C-measuring range to
approx. 30 mg C abs.
H2O-adsorption
H-measuring range to
approx. 3 mg H abs.
SO2-adsorption
S-measuring range to approx.
6 mg S abs.
advantages
large dynamic
optimized to low blank Hvalues and large Hmeasuring range
optimized to separation of
SO2 and H2O and large Smeasuring range
For a mode conversion, the instrument tubing must be converted first (see chapter 7.3.1).
Then the software must be adjusted according in the menu Mode (see chapter 7.3.2).
7.3.1 Instrument conversion
The following conversion matrix (see illustration 7.15) provides conversion
possibilities based on the available basic equipment. The following procedures
necessary for conversion regarding
• safety instructions (Safety I or II)
• conversion in the furnace chamber (a to e)
and
• changing of the tubing in the separation part (A to K)
are mentioned. Areas with a light gray background list the necessary materials
(chemicals or adsorption columns, etc.).
05.05
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
Page
7-20
Particulars of the individual modes of operation
vario EL basic
equipment
possible conversions
to →
from ↓
CHNS
CHNS
order no. 11.10-0000
CNS
Best. No. 11.60-0000
CNS
S
CHN
CN
N
Safety I
Safety I
Safety II
Safety II
Safety II
c
A
c
B
a
C
a+c
D
a+d
E
Safety II
Safety I
e
F
c
B
order no. 11.30-0000
a+e
G
H2O-column
11.00-0086
set of
consumables
CHN
11.00-5013
H2O-column
order no.
11.00-0086
CHN
set of consumables CHN
order no. 11.00-5013
Safety II
Safety II
Safety II
a
D
a+d
E
set of consumables
CHN
order no. 11.00-5013
Safety II
Safety II
Safety II
Safety I
Safety I
b
H
b+c
H+A
b+c
K
c
D
d
E
conversion set CHNS-determination
order no. 11.10-0002
Illustration 7.15: conversion matrix vario EL
7.3.1.1 Safety instructions for instruments conversion
Safety provisions for the protection of the operator and the instrument must be made.
Therefore, before working on electrical connections - as the electrical connections of
the adsorption columns - or before changing reaction tubes, the vario EL must be
cooled down and turned off. Also, please adhere to the safety instructions in the
mentioned chapters.
Conversion of the vario EL may only be performed by
trained personnel. Exact knowledge of these operating
instructions is a prerequisite for instrument conversion.
________________________________________________________________________________________
Operating Instructions vario EL
03.04
Copyright by E l e m e n t a r Analysensystem GmbH
Particulars of the individual modes of operation
Page
7-21
The following is an explanation of the safety instructions mentioned in the
conversion matrix:
Safety level I (Safety I):
• Before converting the vario EL, switch off the gas supply and
activate the function OptionsÖMiscellaneousÖReplace Parts.
• When changing the absorption-U-tubes in the hot furnace
chamber wear the protective gloves which are part of the delivery
(order no. 05 000 094) .
• Newly installed absorption-U-tubes must be conditioned
(see chapter 9.2.4).
• After completion of the conversion the atmospheric nitrogen
which entered the instrument must be removed through 5 minutes
flushing with e. This is carried out automatically when leaving the
function OptionsÖMiscellaneousÖReplace Parts .
Safety level II (Safety II):
• Before converting the vario EL, all furnaces and adsorption
columns must be cooled down to room temperature. For this
purpose set the nominal temperatures to 0°C in the menu
OptionsÖParameters and leave the menu with [OK]. Wait approx.
2 hours until the actual temperatures (display in the status line)
have gone down to room temperature (max. 100 °C).
Note: parameters can only be changed with the corresponding
access rights.
• Leave software by clicking on SystemÖOffline and exit through
FileÖExit.
• Now turn off the mains switch of the vario EL (illustration
5.1/5.2, no. 1). The carrier gas He is turned off automatically.
• After conversion turn the vario EL and peripheral instruments on
(see chapter 5.3.4). After changing the mode of operation (see
chapter 7.3.2) re-heat the furnaces and adsorption column and
flush the instrument with He during the heating phase.
05.05
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
Page
7-22
Particulars of the individual modes of operation
7.3.1.2 Reassembly inside the furnace part
• For this purpose the right front door (illustration 5.1/5.2, no. 11) must be opened.
Caution: When the furnaces are hot and the 3-tube-furnace has not been pulled
out, the door should not be opened too long because this might impair
the ventilation and overheat instrument components (e.g. switch). If
the inner temperature is too high, the temperature safety will become
activated and turn off the furnaces (see chapter 10.1.1).
• The following is an explanation of the procedures mentioned in the conversion
matrix:
identification
in the matrix
conversion procedure
a
fill combustion and reaction tubes for CHN-mode
(see chapter 9.1.2) and install (see chapter 9.2.1/ 9.2.2).
b
fill combustion and reaction tubes for CHNS-mode
(see chapter 9.1.1) and install (see chapter 9.2.1/ 9.2.2).
c
fill H2O-absorption-U-tube (see chapter 9.1.1) and install between
reduction tube exit and tube no. 9 (see chapter 9.2.3).
fill H2O- and CO2-absorption-U-tubes (see chapter 9.1.2) and
install between reduction tube exit and tube no. 9 (see chapter
9.2.3).
d
e
remove H2O-absorptions-U-tube by connecting tube no.9 and
reduction tube exit with each other and removing U-tube together
with connection lines out of the holding device. Close with clamps
if necessary.
7.3.1.3 Tube conversion in the separation part
When changing the tubes in the separation part of the vario EL, the gas line of the
desired operation mode is assembled according to the tubing scheme. The bridged
components and tubes of the previous mode are closed with blind stoppers.
• To have access to the separation part of the vario EL, the left cover plate at the top
of the instrument must be removed (remove 4 screws and lift off cover plate).
• The following is a description of the procedures mentioned in the conversion matrix:
________________________________________________________________________________________
Operating Instructions vario EL
03.04
Copyright by E l e m e n t a r Analysensystem GmbH
Particulars of the individual modes of operation
Page
7-23
identification
tube conversion in the separation part
in the matrix (the mentioned tubes are either in the instrument or belong to the supplied
A
B
• loosen ground-in balls at the outlet of the SO2-adsorption
column (tube no. 10). Tube no. 19 must be clamped off valve
V2. Connect outlet of the SO2-adsorption column and tube no.
19 with each other through the additional tube no. 147.
• The open tube no. 10 and the valve V2 must be closed with
blind stoppers.
C
• loosen tube no. 9 from the inlet of the SO2-adsorption column
and clamp directly onto the inlet of the H2O-column (see
illustration 10.3).
• Clamp the open tube no. 141 onto the open inlet of the SO2adsorption column or close both with blind stoppers.
D
• loosen tube no. 9 from the inlet of the adsorption column and
connect to the inlet of the CO2-adsorption column (see
illustration no. 10.3) through the additional tube no. 145.
• Close the open tube no. 15 and the open inlet of the adsorption
column with blind stoppers.
E
• loosen tube no. 9 from the inlet of the adsorption column. Tube
no. 19 must be clamped off valve V2. Connect tube no. 9 with
tube no. 19 through the additional tube no. 47.
• The open valve V2 and the open adsorption column must be
closed with blind stoppers.
• Remove tube no. 146 (dummy column) (see chapter 10.2.3,
items a-e), thereby removing the blind plug from the electric
connection socket for the H2O-adsorption column (see
illustration 10.3).
• Install H2O-adsorption column (see chapter 10.2.3, item f)
• After changing the mode of operation (see chapter 7.3.2) heat
out the H2O-column (see chapter 10.2.3, item g-i) and connect
then the outlet of the adsorption column to tube no. 140.
• Remove tube no. 146 (dummy column) (see chapter 10.2.3,
items a-e), thereby removing the blind plug from the electric
connection socket for the H2O-adsorption column (see
illustration 10.3).
• Install H2O-adsorption column (see chapter 10.2.3, item f)
• Loosen tube no. 9 from the inlet of the SO2-adsorption column
and connect to the inlet of the H2O-adsorption column.
• Close the open SO2-adsorption column and tube no. 141 with
blind stopper.
• After changing the mode of operation (see chapter 7.3.2) heat
out the H2O-column (see chapter 10.2.3, item g-i) and connect
then the outlet of the adsorption column to tube no. 140.
F
G
05.05
equipment)
• loosen ground-in screws at the inlet and outlet of the H2Oadsorption column and close with blind stoppers.
• The additional tube no. 146 (dummy column) is clamped into the
open tubes instead of the H2O-adsorption column.
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
Page
7-24
Particulars of the individual modes of operation
identification
tube conversion in the separation part
in the matrix (the mentioned tubes are either in the instrument or belong to the supplied
H
equipment)
The conversion set “CHNS-determination“ contains all tubes that were
not included with the basic CHN-instrument as well as components and
the SO2-adsorption column).
• Remove tube no. 146 (dummy column) (see chapter 10.2.3,
items a-e), thereby removing the blind plug from the electric
connection socket for the SO2-adsorption column (see
illustration 10.3).
• Install SO2-adsorption column (see chapter 10.2.3, item f)
• Loosen tube no. 9 from the inlet of the H2O-adsorption column
and connect to the inlet of the SO2-adsorption column.
• Fill a drying tube (see chapter 9.6.1). Install the third drying
tube at the front side (see illustration 5.1, no. 14) (see chapter
9.6). The connections of tubes no. 142 and 143 are already
installed.
• The entrance of the H2O-adsorption column is connected to tube
no. 141 (already installed).
• After changing the mode of operation (see chapter 7.3.2) heat
out the SO2-column (see chapter 10.2.3, item g-i) and connect
then the outlet of the SO2-adsorption column to tube no. 10
(already installed).
H+A
K
• First follow instructions H and then instructions A. Thereafter,
the mode conversion (see chapter 7.3.2) and the heating of the
SO2-adsorption column (see chapter 10.2.3, item g-i) are carried
out.
Then close the outlet of the SO2-adsorption column with tube
no. 10 (already installed).
The conversion set “CHNS-determination“ contains all tubes that were
not included with the basic CHN-instrument as well as components and
the SO2-adsorption column).
• Remove tube no. 146 (dummy column) (see chapter 10.2.3,
items a-e), thereby removing the blind plug from the electric
connection socket for the SO2-adsorption column (see
illustration 10.3).
• Install SO2-adsorption column (see chapter 10.2.3, item f).
• Loosen tube no. 9 from the inlet of the H2O-adsorption column
and connect to the inlet of the SO2-adsorption column.
• Clamp off the measuring gas inlet of the detector (tube no. 19)
from valve V2 and connect to additional tube no.147.
• Close the inlet of the H2O-adsorption column and valve V2
with blind stoppers.
• After changing the mode of operation (see chapter 7.3.2) heat
out the SO2-column (see chapter 10.2.3, item g-i) and connect
then the outlet of the SO2-adsorption column to tube no. 147.
________________________________________________________________________________________
Operating Instructions vario EL
03.04
Copyright by E l e m e n t a r Analysensystem GmbH
Particulars of the individual modes of operation
Page
7-25
7.3.2 Mode conversion
During a mode conversion the current furnace
temperatures must not be higher than the nominal
furnace temperatures of the newly selected mode,
otherwise the overtemperature protection becomes
activated (see chapter 10.1.1).
During a mode conversion make sure that the tube
fillings match the respective operating temperatures and
do not overheat. Overheated tube fillings can cause
the tubes to melt. This melt may run into the inside
of the furnace and destroy it.
• After conclusion of the instrument conversion, the instrument and the carrier gas He
can be turned on again (see chapter 5.3.4).
• Now the desired mode of operation can be selected through the menu Mode (see
illustration 7.16) and confirmed with [OK].
• Now the dialog Changing Mode appears (see illustration 7.17) with the following
questions. These safety questions must be confirmed explicitly before the dialog can
be closed with [OK] and the mode change is really carried out (see also Onlinehelp).
Illustration 7.16: mode-menu
05.05
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
Page
7-26
Particulars of the individual modes of operation
Illustration 7.17: dialog changing mode
question in the dialog
Changing Mode
(illustration 7.17)
temperature of furnace 1 = °C
correct tube filling?
correct tubing?
CH/CHN-switch position?
CAUTION: data saved?
Coefficients Identifier
meaning
The currently saved nominal temperature of furnace 1
[OptionsÖParameters] for the new mode is displayed here.
Check whether:
1. the actual furnace temperature is lower than the displayed
nominal temperature (exception: nominal = 0°C). Otherwise
error message „temperature limit surpassed“ (see chapter
10.1.1) will appear;
2. the currently installed tube filling can withstand the displayed
temperature. If necessary set new nominal temperatures in the
Parameter-menu immediately after mode conversion.
does the tube filling of the combustion and reduction tube match
the new mode?
does the tubing match the tubing scheme of the new mode?
confirm, unless you own a special model for CH-determination.
when changing modes the memory will be deleted. Check
whether the last data was saved.
the coefficient identification of the new mode is displayed here.
• In the new mode check the parameters in OptionsÖParameters first (see chapter 7) and
set the nominal temperatures of the furnaces and adsorption columns. The furnaces
will heat out after confirmation.
Note: parameters can only be changed with the corresponding access rights.
________________________________________________________________________________________
Operating Instructions vario EL
03.04
Copyright by E l e m e n t a r Analysensystem GmbH
Particulars of the individual modes of operation
Page
7-27
• If new adsorption columns have been installed, they must be heated up (see chapter
10.2.3, item g-i).
Attention: watch heating succession of the adsorption columns.
Lower gas pre-pressure and re-set to 2 bar. Close the open column
outlets according to the tubing scheme and fasten the cover plate on the
top of the instrument.
• Perform a leakage test (see chapter 11). If the instrument is gas tight, the vario EL is
now ready for operation.
• If new absorption-U-tubes have been installed, they must be conditioned (see chapter
9.2.4).
• Now the function of the vario EL can be tested with run-in, blind value and standard
samples.
05.05
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
Software
8.
page
8-1
Software
The vario EL is operated with the operating
software WinVar version no. V5.01.
Since the operating software of the vario EL is selfexplanatory and contains an extensive online help
program, we have mentioned only several
commands and menus. For further information
regarding software or instrument control, please read
the notes in the PC-online help program HelpÖIndex.
8.1 Installation
8.1.1 Installation and update of the software
• For the installation of the software insert the furnished CD into the CD-ROM drive of
the PC
• The CD will start automatically.
• If the CD does not run automatically a start with AUTORUN.EXE will be possible.
• Choose Software Installation in order to start the setup program.
• For the first installation choose "New Installation".
Please also refer to "Installation Instructions vario EL Software".
8.1.2 Configuration of the balance
The parameters of the serial interface of a connected balance must match the parameters
which are set in the setup-program. The setup-program sets the parameters as follows:
2400
7
1
odd
05.2005
Baud
Databit
Stopbit
Parity
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
page
8-2
Software
8.2 Main menu of the software
The program is started by clicking on the vario EL icon. Depending on the condition of the
initialization files, it will take a while until the main menu appears. If the program finds a
connected analyzer, a second window appears with the information that the modules are being
initialized.
After program start the main menu looks like illustration 8.1.
title bar
menu bar
tool bar
sample field
status field
Illustration 8.1: main menu of the vario EL-software
8.2.1 Title bar
The name of the document of the current process appears in the title bar. For a new
document the document name is “untitled“. The title bar also contains the usual buttons
for opening the system menu and for minimizing and maximizing the application
window.
Operating instruction vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
05.2005
Software
page
8-3
8.2.2 Menu bar
The menu bar shows the top level of the menu structure. The following is a short
description of the individual menus:
FileÖNew
Creates a new document, the database will be cleared.
The name of the new document is set to Untitled.
FileÖLoad
Opens an existing document. A dialog for selecting a
document appears. Since all of these documents usually
contain the respective calibration coefficients, a
warning will appear if these calibration coefficients do
not match to the current ones.
Note:
If a document is opened regardless of the
warning, the current coefficients will be written over.
With FileÖNew the previous coefficients are reloaded
automatically as long as no analysis process was started
with the old file.
FileÖSave
Actualizes the currently active document. If the
document name is Untitled, a dialog for selecting a
document and/or input will appear.
FileÖSave As
stores the currently active document under a different
name. A dialog appears for selecting and/or entering a
document name.
FileÖDelete
deletes the currently active document.
FileÖSend AQS-Data
allows transmitting samples to another AQS program
running in background for keeping control charts etc. A
dialog appears where it can be determined which
samples shall be transmitted to the AQS program and
for what purpose.
FileÖSend LIMS-Data
transmits the database's data of the samples to a
overriding LIM-system. The mode of transmission can
be selected in the dialog OptionsÖLIMS.
FileÖGraphics
opens the graphic information of a sample. After a
graph has been opened a graphical screen
representation is possible through ViewÖGraphics (see
chapter 6.2.4).
05.2005
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
page
8-4
Software
FileÖPrint
creates an analysis report of the currently active
document. In an appearing dialog, the operator can
perform certain functions as for instance enter a head
line, give the document with the current parameters or
calibration coefficients first priority etc.
FileÖProtocol Setup
The same dialog appears as described under FileÖPrint
in which printing options can be selected without the
actual printing.
FileÖPrint Preview
displays the analysis report on the screen.
FileÖPrinter Setup
opens a dialog in which the printing options can be
selected.
FileÖExport
exports a document into a file. A dialog appears for
selecting the equivalent document and subsequently
another dialog for determining name and type of the
destination file.
FileÖImport
imports data from an external file into the database. A
dialog appears where the file to be imported can be
selected.
Note: only those files can be imported which were
generated by the vario EL software or by the balance
program before.
FileÖUser Logon
makes login of another user possible.
FileÖExit
leaves the software. This function is disabled as long as
the system is not in standby or sleep condition.
EditÖPointer
opens a dialog in which the current sample and the
current weight can be defined. The current sample is
the one which is to be processed next (sleep condition)
or current (during analysis) respectively. The current
weigh-in is the sample which the data from the
connected balance are assigned to next.
EditÖSwap
enables to swap two samples. Of course, swapping
takes place only in the database. Swapping of the
original samples in the carousel must be carried out by
hand.
EditÖInput
opens an application window where sample data can be
entered or modified.
Operating instruction vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
05.2005
Software
page
8-5
EditÖChange
allows additional changes of already analyzed samples.
The user has to enter the number of the equivalent
sample and a dialog opens where the sample data can
be changed.
EditÖClear Tags
removes the markings of all tagged samples.
Mode
opens a dialog where the analysis mode, type of
detector as well the size of the carousel etc. can be
defined. Changing the operation mode deletes the
sample memory automatically and causes an
initializing of the module.
During a mode conversion make sure that the tube
fillings match the respective operating temperatures
and do not overheat. Overheated tube fillings can
cause the tubes to melt. This melt may run into the
inside of the furnace and destroy it.
ViewÖText
switches the sample field to the regular text display.
The sample data of all samples are displayed (see
chapter.
ViewÖStatistics
switches the sample field to statistics display. The
statistical values for each sample group is displayed.
ViewÖGraphics
switches the sample field to graphics display. Different
analysis courses are displayed as a graph. Usually the
course of the current sample is displayed. With the
function FileÖPeak Graphic it is possible during
standby mode to display the course of any sample.
ViewÖWeight
flashes a window in or out (alternating) which shows
the weights of the last four samples. This window can
be moved to any position on the screen.
ViewÖTool bar
flashes the tool bar in or out (alternating).
ViewÖStatus Field
flashes the Status field in and out (alternating).
ViewÖPrevious
If the text display is activated, this function scrolls the
display field back to the previous sample line. If the
graphic display is activated and the peak graphic is
open this function changes to the peak graphic of the
previous sample.
ViewÖNext
If text display is activated, this function scrolls the
display field upwards to the next sample line. If the
05.2005
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
page
8-6
Software
graphic display is activated and the peak graphic is
open this function changes to the peak graphic of the
next sample.
ViewÖPos 1
If the text display is activated, this function moves the
display field to the first position of the database.
ViewÖEnd
If the text display is activated, this function moves the
display field to the last position of the database.
ViewÖZoom In
If the graphic display is activated the enlarging factor
of the graphic course can be doubled. Upon clicking on
this function the mouse arrow changes into a
magnifying glass. If it is placed inside the graphic field
and the left mouse key is clicked again, the graphic
course is enlarged by the factor two. The pixel at which
the left mouse key was clicked moves in the center of
the graphic field. It is possible to enlarge up to a zoom
factor of 64.
ViewÖZoom Out
If the graphic display is activated, the enlarging factor
is cut in half and the graphic course appears anew.
ViewÖCenter
At activated graphic display and a zoom factor > 1, this
function moves a certain point within the graphic field
into the center. The mouse arrow changes into a cross.
Click again and the point is centered.
ViewÖConfiguration
If text display is activated, this function enables to
show and/or remove individual columns. Furthermore,
the input of two operator specific formulas is possible.
If the graphic display is activated, this function
determines the graph that is to be shown with a certain
display area.
SystemÖAuto
starts a continuous operation. Samples will be analyzed
until there are no more weights left. The activated
sleep/wake-up function can also stop continuous
operation at a particularly defined sample.
SystemÖSingle
starts a single analysis or terminates a continuos
operation.
Operating instruction vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
05.2005
Software
page
8-7
SystemÖStop
cancels, if possible, a started analysis.
Note:
An immediate stop is not always possible,
because the vario EL would become
contaminated through not combusted
samples, which would effect the following
tests negatively. This function should only
be carried out before a carousel
movement and after completed O2dosing.
SystemÖStatus
shows a status field, displaying the current state of the
individual modules.
Standards
opens a dialog for defining standard samples regarding
their identification as well as their theoretical contents.
Math.ÖCalibrate
performs instrument calibration (see chapter 6.4).
Different dialogs appear for determining the mode of
computation, possible determination of the linear and
non-linear calibration areas, visual judgement of the
calibration graphs, possible elimination of outlier
samples as well as saving the calibration coefficients.
Math.ÖStatistics
Statistical computation (see chapter 6.2.5). Through the
appearing dialog the operator forms the respective
samples into groups. The program then calculates the
mean value for each group and the standard deviation.
Math.ÖFactor
computes the daily factors. Computation is carried out
as selected through function MathÖSetup.
Math.ÖFactor Setup
opens a dialog for setting the mode of daily factor
computation.
Math.ÖCoefficients
opens a dialog in which the user can enter calibration
coefficients, modify, load or save.
Math.ÖRecalculate
recalculates the whole content of the database.
OptionsÖParameters
opens a dialog for entering instrument parameters,
modify, load or save them (see chapter 5.3.5).
OptionsÖMethods
allows creating, modifying and deleting of methods.
Methods define where the O2 dosing for the
corresponding sample shall take place. A method can
be allocated to a sample by its name via the dialog.
OptionsÖSleep/Wake-Up
opens a dialog for activating or modifying the
Sleep/Wake-Up functions (see chapter 6.5)
05.2005
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
page
8-8
Software
OptionsÖLIMS
opens a dialog for determining how the LIMS
transmission is to be carried out. Transmission to an
overriding system can either be carried out through an
available serial interface or through copying the file
into a target path of a computer within the network. In
this dialog you can also define which components are
contained in one file.
OptionsÖMaintenance
opens a dialog for defining up to 5 maintenance
activities (see chapter 9).
OptionsÖError Index
opens a dialog which lists all possible errors of the
controller and combustion module. By entering the
appropriate error code its meaning is displayed (see
chapter 10).
OptionsÖError Buffer
opens a dialog which lists the errors in chronological
order. Up to 50 errors can be stored, thereafter the
oldest error is deleted. Double clicking on an error
message lets the dialog ErrorIndex appear and
displays the respective explanation.
OptionsÖError Handling
opens a dialog in which the operator can activate the
"Standard Tolerance Control" for defining how many
samples in succession can have non-critical error before
the analysis series is stopped.
Note:
the analysis is always stopped if critical errors occur
OptionsÖConfiguration
opens a dialog where the entries of the individual
initialization files can be modified.
OptionsÖDatabase
allows the setting and execution of scripts that create
access to the database.
OptionsÖBackup
opens a dialog where the program behavior for data
safety can be configured.
OptionsÖClean
deletes all sample data from the database. The
initialization and configuration data are not influenced.
OptionsÖRestore
allows to restore database files previously saved via the
backup function.
Operating instruction vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
05.2005
Software
page
OptionsÖMiscellaneousÖ
Sample Feeder
8-9
causes to move the sample feeder to a desired
position. This function operates only if the
carousel has been removed.
OptionsÖMiscellaneousÖReplace Part
cuts off the carrier gas, reduces pressure and
permits changing of different spare parts.
When the dialog is ended, the carrier gas is
turned on again and a gas pre-run will be
performed before the system is ready for the
next analysis.
OptionsÖMiscellaneousÖH2O column
permits heating the H2O-adsorpion column
after a change; without function in CN and
CNS mode.
OptionsÖMiscellaneousÖCO2 column
permits heating the CO2-adsorption column
after a change.
OptionsÖMiscellaneousÖSO2 column
permits heating the SO2-adsorption column
after a change.
OptionsÖMiscellaneousÖRough Leak Check This function performs a rough leak check of
the analysis system.
HelpÖContent
shows the vario EL user help and activates the index card
"Content".
HelpÖFind
shows the vario EL user help and activates the index card
"Find".
HelpÖIndex
shows the vario EL user help and activates the index card
"Index".
HelpÖElementar on the web
if the PC has internet access, this command opens the
internet home page of Elementar Analysensysteme where
you can order further information on the requested
analytical instruments.
HelpÖRegistry
opens a dialog where your product registration data is
displayed.
HelpÖAbout vario EL
opens a dialog which displays the different version
numbers of the software and modules, the serial number of
the instrument as well as the Copyright-remarks.
05.2005
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
page
8-10
Software
8.2.3 Tool bar
The tool bar permits access to the most important menu points without going through the menu
levels. The following illustration shows the tool bar and the menu points that can be reached.
View_End
File_Print
Context Sensitive
System_Single
File_Save
View_Pos 1
System_Auto
File_New
View_Text
View_Graphic
File_Open
View_Reverse
View_Forward
View_Statistics
Help_vario EL
View_Zoom in
View_Zoom out
View_Center
Illustration 8.2: tool bar
8.2.4 Sample field
The display of the sample field depends on the selected display mode (Menu View).
In the text-mode it appears in the Text Display with sample specific input or measuring
data respectively.
In the graphic-mode the sample field has a frame (graphic display), representing the
timely course of an analysis.
In the statistics-mode (statistics display) the statistical data of defined sample groups are
listed (see chapter 6.2.5).
8.2.4.1 Text display
In the text-mode the sample data is listed line-by-line (see illustration 8.1). With the
scroll bar at the right side and the lower edge of the sample field, the operator can move
the desired segment as necessary. The width and the sequence of the individual columns
can be determined by by adequate moving of the mouse pointer in the top bar of the text
display. Showing and removing of unneeded columns can be done with
ViewÖConfiguration. The two left columns, however, “No.“ and “Sample name“ can
be adjusted in width but cannot be moved.
Operating instruction vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
05.2005
Software
page
8-11
8.2.4.2 Graphic display
In the graphic mode, the display field where the graphic course of an analysis is shown
is integrated in the sample field (see illustration 8.3). The right and lower edges of the
display field are dimensioned according to the existing settings. In the graphic display,
the sample field has no scrolling bars since the entire display is shown completely
through standard VGA resolution (640x480 pixels).
Illustration 8.3: main window with graphic display
8.2.4.3 Statistic display
In the statistic mode, the statistical data of pre-selected sample groups is listed line by
line (see illustration 8.4). Through the scrolling bar at the right and lower edges of the
sample field, the operator can position the desired segment as needed. A configuration
of the column sequence is not possible. For the definition of sample groups see
chapter 6.2.5.
05.2005
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
page
8-12
Software
Illustration 8.4: main window with statistic display
8.2.5 Status field
The status field gives the operator the most important information regarding the current
state of the system. It consists of four status lines whereby the upper three lines are
subdivided into three columns (see illustration 8.4).
Maint:
(here: OK):
shows the current state of maintenance. This display is
linked to the menu OptionsÖMaintenance and watches
that the set maintenance intervals are adhered to. If “OK“
is flashing, at least one maintenance procedure will be
necessary during the analysis run. If a message is
flashing, the respective interval has been reached or
surpassed.
Mode:
shows the current mode of operation, e.g. CNS, CN,
CHN. Mode conversions are carried out through the
dialog Mode.
Note: When changing the mode of operation, the tubing
scheme and the reaction tube filling must be changed
also. Tube fillings must not be overheated !!
Operating instruction vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
05.2005
Software
page
In the right hand column of the first line “Offline“ is
shown when there is no communication with the analyzer.
This is usually the case when no analyzer is connected to
the PC or after opening the function SystemÖOffline. If
there is communication with the analyzer, either sleepstate will appear if the system is sleeping or the respective
process phase.
Process phase
(here: Offline
Furnaces:
TCD:
[°C]
[mV]
[integral]
shows the current temperatures of the three-tube furnace.
Furnace 1 = combustion tube, Furnace 2 = post
combustion tube, Furnace 3 = reduction tube
shows the current measuring signal in mV and the current
integral value during analysis.
Press.:
[bar]
shows the current system pressure at the pressure sensor
Columns
(H/C/S)
[°C]
shows the current temperatures of the adsorption
columns.
(Succession: H2O/ CO2)
Flow
05.2005
8-13
[ml/min]
shows the current flow through the measuring cell
right column of the third
line
is usually empty. Only if an error has occurred or if the
gas-pre-run is active, an error message or the waiting time
will be displayed.
fourth line
shows a help text on the left side which refers to the
currently selected menu of the menu bar or tool bar. If
neither a menu of the menu bar nor a menu of the tool bar
has been selected, the text “for help, press F" appears. By
depressing F1 the help system is activated.
In the middle the data of the currently logged in user and
his access rights appear.
The right side displays whether the keyboard mode
NUMLOCK is activated or not. If the NUMLOCK mode
is activated, entering of number is possible via the
number block.
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
page
8-14
Software
8.2.6 Recommendations for the software use
As is common through Windows, it is possible to activate several applications at the
same time. Multiple instances of the vario EL program is, however, not possible. If the
operator tries to load another instance of this program, an error message will appear.
However, it is possible to let the vario EL program run in the background while working
on another application. In this case, please note the following:
• programs, which burden the PC drastically (regarding the CPU-time) or which have
long access times to reach disk drives can cause disturbances in the program course
of the vario EL program.
• Furthermore, every mouse activity, enlarging or reducing the frame of an
application, has the effect that as long as the mouse has picked up the frame,
everything else stops. This can also cause disturbances in the program of the
vario EL.
• Please note, that programs which (purposely or inadvertently) use the same serial
port as the vario EL program will definitely cause a total failure of the vario EL
system.
We, therefore, recommend the following:
Avoid simultaneous operation of several programs when using the vario EL
program, unless you are absolutely sure that these programs do not have the
uncertainties described above. Avoid also unnecessary enlarging, reducing or
moving of frames and windows during an analysis.
8.3 Processing of the vario EL data with MS-Excel
The data files created and filed by the vario EL program can be further processed under MSExcel. Proceed as follows:
1. Invoke the menu point FileÖExport and select the document name in the opening dialog
"Select document name" that you would like to have further processed with Excel. Click
"OK" to take the selected document.
2. Another dialog opens "Save File under". Select "MSExcel-files(*.xls)" in field "Files of
type". The name of the previously selected document appears as a suggestion in the field
"File name". If required, the name can now be changed. Also if required, the suggested path
where the file shall be stored can be changed. The Excel file will be created by clicking
"OK".
3. Now start MS-Excel and load the recently created file for further processing.
Operating instruction vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
05.2005
Replacing consumables
9.
Page 9-1
Replacing consumables
Please note the following
safety instructions !!!
• The efficiency of the vario EL can be guaranteed only with original
consumables as well as original spare parts which can be obtained only
through E l e m e n t a r Analysensysteme GmbH or authorized
dealers. The use of different consumables or chemicals of an
unsuitable standard can lead to injuries as well as instrument
damages. It can also falsify the results of the analysis. Unsuitable
spares lead to instrument damages and loss of warranty.
• All the operation dependent maintenance and exchanges times
mentioned in the operating instructions depend very strongly on the
respective test matrix. They are, therefore, only examples and do not
guarantee life times for consumables or wear and tear parts!
• All tube fillings must be packed down as tightly as possible to avoid air
pockets. For this purpose, tap the side of the tube lightly while it is being
filled with a wooden implement or a piece of cork.
• To prevent leakage around the tube plugs, apply a slight coating of high
vacuum grease to the O-rings and check them for damage before fitting
them in. Too much grease causes C-blank-values. The tube insertgrooves in the plug must be cleaned regularly.
O-rings shrink due to temperature influences. The high temperature
causes the O-rings to shrink, therefore, a resistance must be felt during
O-ring placement otherwise it might leak.
Before inserting the plugs, the sealing areas of the tubes (inner walls)
should be dusted off.
• Replacing combustion or reduction tubes can only be carried out when
the tubes are cold. For this purpose set furnaces to nominal
temperature 0°C and let the tubes cool down to room temperature
(max. 100°C).
When working at hot furnaces or tubes there is danger of burning!!
Therefore, always wear the supplied protective gloves
(order No. 05 000 094), because it is possible that some components
(e.g. heated tube line) are still hot. We are not liable for accidents that
are due to disregarding these warnings.
Please note the following safety instructions!!!
_________________________________________________________________________________
10/02
Operating Instructions vario EL
Copyright y E l e m e n t a r Analysensystem GmbH
Page 9-2
Replacing consumables
• Before replacing a tube turn off the gas supply into the instrument
respectively activate the function Options ÖMiscellaneousÖReplace.
• After a tube exchange, it is necessary to flush out the atmospheric
nitrogen that entered the unit for 5 minutes with CO2. This is
accomplished automatically through the function
OptionsÖMiscellaneousÖReplace.
• After changing the tubes wait until the 3-tube furnace as well as the new
reaction tubes have warmed up (approx. 10 to 15 minutes) before
starting the next analysis. Also, please observe the mode dependent
conditioning instructions (see chapter 9.2.4).
• When handling cold quartz and glass parts wear the supplied leather
gloves to avoid danger of injuries in case of broken glass.
• When handling chemicals, observe the safety instructions of the
chemical manufacturer (see labels on bottles and safety data sheets)!
To simplify following up on the maintenance and change intervals, it is possible to define five
different replacement or maintenance functions and their due dates through the menu
OptionsÖMaintenance. Illustration 9.1 shows the Maintenance dialog. The preset intervals
(illustration 9.1, right) are monitored by the software through the progressive analysis count in the
respective counter (illustration 9.1, left). A message is displayed in the Status field (see chapter 8.2.5)
if the preset interval has not been reached or has been exceeded. After maintenance or a tube
replacement has been carried out, the counter must be set to zero (for further information see OnlineHelp).
Illustration 9.1: menu OptionsÖMaintenance
_________________________________________________________________________________
Operating Instructions vario EL
12.04
Copyright by E l e m e n t a r Analysensystem GmbH
Replacing consumables
Page 9-3
Before changing a tube or the ash finger, always turn off the carrier gas. This can be
accomplished automatically through the function OptionsÖMiscellaneousÖReplace. After the
respective part has been changed and the button [OK] was activated, the vario EL is flushed
for 1 minute with O2 and for 5 minutes with He. If a tube has been replaced, wait until the
new tube has reached the correct temperature.
Note:
Maintenance intervals may vary depending on sample type (e.g. salt content) or operation
mode (e.g. oxygen dosing). The entered intervals are therefore only of statistical nature. They
can be changed according to the experiences of the respective application.
9.1 Filling the reaction tubes
Finger prints must be cleaned off all quartz parts
before installing them into the 3-tube-furnace (for
instance with acetone). Otherwise crystallization zones
can form and cause a premature aging of the quartz.
9.1.1 CHNS/ CNS/ S-mode
A.)Combustion tube
During the operation mode with simultaneous S-determination a combustion tube is
used that is empty in the bottom and filled in the middle (hottest zone) with WO3
granulate. Quartz wool serves as an intermediate layer. As a separation layer between
WO3 granulate and ash finger, a 3mm layer of corundum balls is used. The ash finger
and a protection tube are installed last (see chapter 9.3). Illustration 9.2 shows the
filling and the best filling levels.
Operating temperature: 1150 °C (max. 1180 °C)
Note:
•
For CHNS determination freshly filled combustion tubes must be conditioned (see
chapter 9.2.4).
•
The position of the ash finger is decisive for the best sample combustion. The
WO3 granulate sinters during operation. Therefore, the filling level must be
checked from time to time and if necessary, WO3 must be refilled. If necessary,
corundum balls have to be refilled when changing the ash finger.
•
If the analysis values ( also for standard substances) become bad before the
regular maintenance interval, a regeneration of the WO3-filling can be tried
through 10 blank value measurements with lots of oxygen (O2-Index 5 = 180 s).
_________________________________________________________________________________
10/02
Operating Instructions vario EL
Copyright y E l e m e n t a r Analysensystem GmbH
Page 9-4
Replacing consumables
Legend:
1
2
3
4
5
6
7
protective tube
ash finger
corrundum balls 3 mm
(approx. 2 g)
WO3 granulate 55 mm
quartz wool 10 mm (approx.
0,2 g)
support tube 65 mm
quartz wool 15 mm (approx.
0,2 g)
Illustration 9.2: combustion tube CHNS/CNS/S-mode
Make sure that only WO3 granulate (11.02-0008) is
used for tube filling!!!
WO3-powder (11.02-0017) may only be used as sample
additive. A mix-up can cause clogging of the
combustion tube.
B.) Reduction tube
Please also refer to chapter 9.1.3 filter plug and filling instructions.
The reduction tube for CHNS/CNS/S determination is filled as described in illustr. 9.3.
Operating temperature: 850 °C (max. 880 °C)
Note:
• For CHNS determination freshly filled reduction tubes must be conditioned (see
chapter 9.2.4).
•
Already used silver wool can be used again as long as the surface is still shiny
(silvery). Used-up silver wool turns white and dull.
_________________________________________________________________________________
Operating Instructions vario EL
12.04
Copyright by E l e m e n t a r Analysensystem GmbH
Replacing consumables
Page 9-5
1.2
1.1
1
1.3
2
3
4
Legend:
1
1.1
1.2
1.3
2
3
4
5
6
5
6
7
8
plug
11.01-1004/4
square gasket 05 000 353
wire mesh ronde
11.00-1313/4
quartz wool 03 679 908
o-ringes 2 pcs.
Art. No. 03 654 627
silver wool 26 mm
corundum balls
45 mm
copper 170 mm
quartz wool 10 mm
support tube 65 mm
quartz wool 5 mm
7
8
Illustration 9.3: reduction tube CHNS/CNS/S-mode
C.) H2O-absorption-U-tube for CNS/S-mode
Only for CNS and S determination is the H2O-absorption-U-tube installed into the
furnace chamber after the reduction tube (see chapter 9.2.3).
The U-shaped glass tube is filled with Sicapent® and closed with 2 filters on both sides
(see illustration 9.4). Make sure that enough absorption material is inside the bend of
the U-tubes. Clean any Sicapent® residue from the tube ends. At last the connection
pieces are fitted into the seal rings and the closing caps are screwed onto the glass
tube.
When handling Sicapent® (phosphor pentoxide) it is
absolutely necessary to wear safety goggles and
protective gloves!
!!! Caution - Danger of Cauterization !!!
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Page 9-6
Replacing consumables
Legend:
1
2
2 filter 03 022 399
both sides
Sicapent®
Illustration 9.4: H2O-absorption-U-tube
Note:
•
•
In every mode of operation the freshly filled H2O-absorption-U-tubes must be
conditioned (see chapter 9.2.4).
Sicapent® has an indicator which shows the used-up zones of the tube through
blue discoloring. For a safe automatic operation, Sicapent®-tubes must be
exchanged if ¾ of their capacity is discolored.
9.1.2 CHN/ CN/ N-mode
A.) Combustion tube
For operation modes without S determination, a combustion tube is used which filled
as described in illustration 9.5. The filling levels should be as exact as possible so that
the ash finger is located in the hottest zone of the tubular furnace. At last the ash finger
(see chapter 9.3) and a protective tube are inserted.
Operating temperature: 950 °C (max. 980 °C)
Note:
•
•
Freshly filled combustion tubes for CHN/CN/N-mode must always be conditioned
before operation (see chapter 9.2.4).
The position of the ash finger is decisive for the best sample combustion. If
necessary, corundum balls have to be refilled when changing the ash finger.
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Operating Instructions vario EL
12.04
Copyright by E l e m e n t a r Analysensystem GmbH
Replacing consumables
Page 9-7
Legend:
1
2
3
4
5
6
7
8
9
protective tube
ash finger
corundum balls
3 mm
copper oxide
90 mm
quartz wool 5 mm
ceroxide 20 mm
quartz wool 5 mm
lead chromate
20 mm
quartz wool 5 mm
Illustration 9.5: combustion tube CHN/CN/N-mode
B.) Reduction tube
Please also refer to chapter 9.1.3 filter plug and filling instructions.
The reduction tube in the CHN/CN/N-mode is filled as described in illustration 9.6.
Operating temperature: 500 °C (max. 550 °C)
Note:
•
In the CHN mode, freshly filled reduction tubes must be conditioned because of
moisture (see chapter 9.2.4).
•
Already used silver wool can be used again as long as the surface is still shiny
(silvery). Used-up silver wool turns white and dull.
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Copyright y E l e m e n t a r Analysensystem GmbH
Page 9-8
Replacing consumables
1.2
1.1
1
1.3
2
3
Legend:
1
1.1
1.2
1.3
2
4
3
4
5
plug
11.01-1004/4
square gasket
05 000 353
wire mesh ronde
11.00-1313/4
quartz wool
03 679 908
o-rings 2 pcs.
03 654 627
silver wool 20 mm
copper
quartz wool 5 mm
5
Illustration 9.6: reduction tube CHN/CN/N-mode
C.) H2O-/CO2-absorptions-U-tube for CN/N-mode
In the CN mode the H2O-absorptions-U-tube and in the N-mode both absorption-Utubes are installed in the furnace chamber after the reduction tube (see chapter 9.2.3).
For filling the H2O-absorption-U-tube see illustration 9.4 and chapter 9.1.1 point C.
The U-shaped CO2-absorption tube is filled with a 1:1 mixture of quartz splinters and
NaOH on a carrier material and closed on both sides with 2 filters (see illustration
9.7). It is important that enough absorption material is in the bend of the tube. The
tube ends must be cleaned from NaOH residue. At last the connection pieces are fitted
into the seal rings and the closing caps are screwed onto the glass tube.
Please check if there is resulting a free space between filter and filling material while
operating the U-shaped tubes (may be possible due to compaction of the filling
material). Fill this new free space with filter too.
_________________________________________________________________________________
Operating Instructions vario EL
12.04
Copyright by E l e m e n t a r Analysensystem GmbH
Replacing consumables
Page 9-9
When handling NaOH (natrium hydroxide) it is
absolutely necessary to wear safety goggles and
protective gloves!
!!! Caution Cauterization !!!
Legend:
1
2
2 filters 03 002 399
both sides
mixture (1:1) of
NaOH on carrier /
quartz splinters
Illustration 9.7: CO2-absorption-U-tube
Note:
• In every mode of operation the freshly filled CO2-absorption-U-tubes must be
conditioned (see chapter 9.2.4).
• NaOH on carrier becomes light through CO2,-absorption. Used-up zones in the
filling become therefore visible. It is furthermore necessary to watch for clogging
in this tube during operation because this reaction creates water which lets the
filling bake.
9.1.3 Filter plug
For protection puroposes of the detection system und the ad- and desorption column
we recommend the filter plug. The filter plug (quartz wool) works as a mechanical
filter and holds back a number of contaminations.
The filter plug has a bore of approx. 7 mm at the massive part. It shall be filled with
approx. 0.1 g quartz wool and put on the reduction tube. In addition, a wire mesh is
put on it at the outle, subsequently the o-ring. As usual, the outlet of the reduction tube
is connected with the heated tube which leads to the SO2 and/or the H2O column. The
wire mesh shall hold back fine quartz wool particles. It is important that the thermal
cover of aluminim is placed on the reduction tube in order to avoid water
condensation. The quartz wool should be exchanged after each reduction copper
exchange. In case of extremely strong contaminations, a more often exchange interval
is possible.
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Page 9-10
Replacing consumables
9.2 Installation, disassembly and conditioning of the reaction
tubes
Combustion and/or reduction tubes can only be exchanged when they are cooled off. For this purpose set
furnaces to nominal temperature 0°C and let the
tubes cool down to room temperature (max. 100°C).
!!! DANGER OF BURNING!!!
The tubes are made of quartz glass.
!!! DANGER OF BREAKAGE!!!
When working on the 3-tube furnace wear the supplied
protective gloves (order no.05 000 094) because there
are always hot components inside the furnace chamber.
9.2.1 Disassembly from the 3-tube furnace
a)
Set temperature of the furnaces to 0 °C [OptionsÖParameters] and wait until they
have cooled down to room temperature (approx. 2 hours).
b)
For assembly and disassembly of tubes, the gas supply is turned off [OptionsÖ
MiscellaneousÖReplace Parts]. Wait for the pressure to be reduced and remove the
right front door.
c)
Now remove the O2-supply line to the combustion tube flange by loosening the
two ground-in clamps (illustration 9.8, no. 1 + 2).
d)
Loosen combustion tube flange (illustration 9.8, no. 3), i.e. turn to the right.
e)
Remove ground-in clamps (illustration 9.8, no. 4) from reduction tube.
f)
Pull the 3-tube furnace towards the front out of the instrument.
g)
Remove the combustion tube flange (illustration 9.9, no. 1) from the combustion
tube. Loosen the combustion tube flange slowly with carefully rocking
movements (o-rings tend to stick to the hot tube) from the combustion tube (see
illustration 9.9) and pull upwards out of the tube (see illustration 9.10). If the
flange becomes wedged, the combustion tube and the O2-lance could get
damaged.
h)
Place the combustion tube flange up side down on the tube stand (see illustration
9.11).
i)
Remove thermal shield from reduction tube (illustration 9.9, no. 3).
_________________________________________________________________________________
Operating Instructions vario EL
12.04
Copyright by E l e m e n t a r Analysensystem GmbH
Replacing consumables
Page 9-11
j)
Remove thermal shield from quartz glass bridge under the 3-tube furnace by
pulling the handle towards the front.
k)
Disassemble quartz glass bridge (see illustration 9.12) by holding the bridge and
loosening the ground-in clamps.
l)
Then pull the respective tube out of the furnace towards the top and place in tube
stand.
6
5
7
1
3
8
4
Illustration 9.8: furnace chamber vario EL
Legend:
1+2
3
4
5
6
7
8
ground-in clamps O2-supply
handle for bayonet catch
ground-in clamp between reduction tube and tube
no. 9
heated tube no. 9
ball valve
He-supply valve (flushing gas)
He-supply (carrier gas)
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Copyright y E l e m e n t a r Analysensystem GmbH
Page 9-12
4
Replacing consumables
1
Legend:
1
2
3
2
3
4
combustion tube flange
O2-connection of the
combustion tube flange
thermal cover
reduction tube
plug
reduction tube
Illustration 9.9: pulling off/replacing the combustion tube flange
Illustration 9.10: pulling out/inserting the
combustion tube flange
Illustration 9.11: placing the combustion
tube flange in the tube
stand
_________________________________________________________________________________
Operating Instructions vario EL
12.04
Copyright by E l e m e n t a r Analysensystem GmbH
Replacing consumables
Page 9-13
Illustration 9.12: quartz glass bridge
9.2.2 Installation into the 3-tube furnace
a) Close the reduction tube with the plug (illustration 9.9, no 4) and the combustion
tube with the combustion tube flange (illustration 9.9, no 1). During insertion of
the combustion tube flange do not rest the O2-lance on the edge of the ash finger
(danger of breakage). Then check the position of the O2-lance in the ash finger (see
chapter 9.4).
b) Install the tubes into the 3-tube furnace (combustion tube = right, reduction tube =
middle), thereby inserting the O2-connection of the flange into the holding device
(illustration 9.9, no. 2) and placing the seal on top of the flange.
Caution: This seal should not be greased and should therefore be checked more
often for mechanical damage.
c) Pull the thermal cover (illustration 9.9, no. 3) over the reduction tube and check
whether there is a seal in the plug.
d) Install the quartz glass bridge between combustion tube and reduction tube (see
illustration 9.12) and push the thermal cover on the angle plates over it.
Note:
When closing the ground-in ball connectors an elastic resistance must
be felt through pressure on the o-rings in the quartz glass bridge. Otherwise the orings must be replaced.
e) Now push the 3-tube furnace back, thereby lifting the bayonet catch lightly so that
the seal on the combustion tube flange is not damaged. Then close the bayonet
catch (turn left).
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Page 9-14
Replacing consumables
f) If necessary carry out conditioning procedures (see chapter 9.2.4).
g) Connect reduction tube exit or H2O-absorption-U-tube exit to heated tube no. 9 (see
illustration 9.8, nos. 4+5).
h) Connect O2-supply (see illustration 9.8, nos. 1+2).
i) Insert left front door and leave the dialog OptionsÖMiscellaneousÖReplace Parts in
the PC. The gas will be turned on automatically and the atmospheric nitrogen will
be removed by flushing for 5 minutes with helium.
j) Reset operating temperature through menu OptionsÖParameters and wait for the
tubes to heat up again.
9.2.3 Installation of the absorption-U-tubes
When working on hot furnaces wear the supplied
protective gloves (order no.05 000 094).
Danger of burning !!
For modes CNS/S/CN and N a H2O-absorption-U-tube must be installed inside the
furnace (see illustration 9.13). For the N-mode it is necessary to clamp the CO2absorption-U-tubeRohr into the gas path (see illustration 9.14).
All necessary tubing is supplied with the standard equipment of the vario EL.
_________________________________________________________________________________
Operating Instructions vario EL
12.04
Copyright by E l e m e n t a r Analysensystem GmbH
Replacing consumables
Page 9-15
Please read the appropriate mode column.
CNS/S/CN
N
a) Open the ground-in clamp (illustration 9.8,
no. 4) at the reduction tube outlet and the
heated tube no. 9.
b) Press the H2O-absorptions-U-tube into the
two left holding devices at the 3-tube
furnace (see illustration 9.13).
Note: Hold that part of the glass tube that
needs to be fastened. Otherwise the bend
of the U-tube will break!
c) The reduction tube outlet is connected to
the inlet of the H2O-absorption-U-tube
through tube no. 111 (right leg of the Utube) (illustration 9.13, nos. 1+2).
d) The H2O-absorption-U-tube outlet (left
leg) is connected to the heated tube no. 9
through tube no. 110 (illustration 9.13,
nos. 2+3).
a) Open the ground-in clamp (illustration 9.8,
no. 4) at the reduction tube outlet and the
heated tube no. 9.
b) Press the H2O-absorption-U-tube into the
left and the CO2-absorption-U-tube into
the right holding device at the 3-tube
furnace (see illustration 9.14).
Note:
Hold that part of the glass tube
that needs to be fastened. Otherwise the
bend of the U-tube will break!
c) The reduction tube outlet is connected to
the inlet of the CO2-absorption-U-tube
(left leg of the U-tube) through tube no.
111 (illustration 9.14, nos. 1+3).
d) The right leg of the CO2-absorption-Utube and the right leg of the H2Oabsorption-U-tube are connected to tube
no. 109 (illustration 9.14, nos. 2,3,4).
e) The H2O-absorption-U-tube outlet (left
leg) is connected to the heated tube no. 9
through tube no. 110 (illustration 9.14,
nos. 4+5).
Newly installed absorption-U-tubes must be flushed free of atmospheric nitrogen
(see conditioning instructions in chapter 9.2.4).
3
1
Legend:
1
2
3
tube no. 111
H2O-absorptionU-tube
tube no. 110
2
Illustration 9.13: built-in H2O-absorption-U-tube (CNS/S/CN-mode)
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Operating Instructions vario EL
Copyright y E l e m e n t a r Analysensystem GmbH
Page 9-16
Replacing consumables
1
5
2
Legend:
1
2
3
4
3
4
5
tube no. 111
tube no. 109
CO2-absorptionU-tube
H2O-absorptionU-tube
tube no. 110
Illustration 9.14: built-in H2O- and CO2-absorption-U-tube (N-mode)
9.2.4 Conditioning of newly installed tube
Due to air in the filling materials, all tubes filled with Sicapent® as well as the CO2absorption-U-tube must be flushed free of atmospheric nitrogen before operation. We
therefore recommend blind value measurements (at least 20) without oxygen (O2Index 2 = 1 s) until the N blind value is stable and low
(usually integral approx. 20 - 50).
In some operation modes conditioning of the freshly filled or newly installed
combustion tubes or reduction tubes becomes necessary. The following table shows
conditioning instructions and thereafter the general procedure is explained.
mode
reaction tube
CHNS
combustion tube (illustration 9.2) to remove moisture from the tube
reduction tube (illustration 9.3) fillings, these tubes must be heated 1 ½
hours at operating temperature (see
chapter 9.2.1).
combustion tube (illustration 9.5) to remove moisture from the tube and
interfering components of CeO2 , this
tube must be heated for one night (12 14 hours) at 950°C .
reduction tube (illustration 9.6) because of moisture, this tube must be
heated for 1 ½ hours at 500°C.
CHN/CN/N
CHN
instruction
_________________________________________________________________________________
Operating Instructions vario EL
12.04
Copyright by E l e m e n t a r Analysensystem GmbH
Replacing consumables
Page 9-17
General procedure for conditioning:
a) Install tube (see chapter 9.2.2, point a-e) and leave outlet open, i.e. either do not
fasten the quartz glass bridge at the end of the combustion tube or do not clamp the
ground-in connection at the outlet of the reduction tube.
b) Restart the gas flow (leave function Replace Parts) and reduce He-prepressure at
the source until the He-flow meter shows 3 cm.
c) After reaching the respective operating temperature (if necessary set temperatures
in menu Parameters) wait the required conditioning time.
d) Stop gas flow through function Replace Parts and close open gas lines
(see point a).
e) Restart gas flow and reset He-pressure again to 2.0 bar at the bottle pressure gauge
(inlet pressure gauge shows then 1.25 bar, He-flow meter shows 2.0 cm).
9.3 Ash finger
9.3.1 Emptying / Filling
type of ash
finger
filling
emptying
application
ash finger open on
both sides, slotted
at the side
(order no.
11.00-1170/4)
place ash finger on a
plane surface and fill
with Al2O3-wool
(approx. 0,4 g) packed
down firmly using the
supplied tool to a
10 mm thick bottom.
when cooled off
push stuffed
bottom out and
refill the ash
finger.
commonly used ash
finger
when cooled off
empty ash finger
and if necessary
scrape out.
when substances are not
easily combustible. The
gas tight bottom causes a
higher local O2-concentration.
ash finger with
bottom
(order no.
11.00-1319/4)
Note: when using new
ash fingers, the Al2O3bottom does not stick
well to the polished
quartz wall. It is
therefore necessary to
stuff especially firmly.
fill with approx.
2-3 mm quartz splinters
to remove the ash more
easily.
when samples are heavy.
The stuffed bottom could
break through.
Note:
The end of the O2-lance must reach into the ash finger by at least
5 - 10 mm! Therefore, the appropriate lance length must be selected (see
chapter 9.4).
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Operating Instructions vario EL
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Page 9-18
Replacing consumables
9.3.2 Changing the ash finger
When changing the ash finger, furnaces must be
cooled down to room temperature (nominal
temperature 0°C). Nevertheless safety goggles must
be worn to protect the eyes from ash particles. The
supplied protective gloves must also be worn because
hot components are inside the furnace.
As a rule, the ash finger must be replaced after 120 to 140 analysis. Its filling can vary
a great deal, as the amount of ash depends on the mineral content of the samples. An
extremely high mineral content may cause a finger replacement to be necessary after
just 60 samples (e.g. soil samples with a weight of 100 - 200 mg).
It could also happen that at a very low mineral content, the ash in the ash finger is so
toxic that after 50 samples the measuring values fluctuate strongly and the peak
widens extremely. In this case the ash finger must be exchanged and the contaminated
ash finger must be removed.
Note:
The position of the ash finger in the combustion tube must constantly be
checked. If necessary refill WO3-granulate or corundum balls.
Ash fingers are usually replaced when furnaces are cooled off.
a)
b)
c)
d)
e)
For changing the ash finger, follow the points a) through h) described in chapter
9.2.1.
Lower the crucible tongs provided with the delivery into the combustion tube
(see illustration 9.15) and pull out the protective tube towards the top.
When the crucible tongs are clamped inside the ash finger, it can easily be pulled
out of the combustion tube.
Caution: Ash finger and protective tube have a temperature of approx.
1150°C or 950°C, if the cool-down instructions have not been observed!
When the ash finger has been almost completely removed from the combustion
tube, it can be gripped by pliers or strong tweezers (see illustration 9.16). Place
the ash finger in a fume hood to cool off.
If corundum balls are sticking to the bottom of the ash finger it might be
necessary to refill corundum balls into the combustion tube.
Subsequently, the new ash finger which has been prepared beforehand, is
installed with the pliers carefully and slowly so that the stuffed bottom of the ash
finger is not pushed upwards.
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Operating Instructions vario EL
12.04
Copyright by E l e m e n t a r Analysensystem GmbH
Replacing consumables
f)
g)
Page 9-19
The prepared combustion tube flange is inserted into the combustion tube from
the top at a lightly slanting position, so that the O2-lance does not touch the
upper edge of the ash finger (see illustration 9.10). The end of the lance must
reach down into the ash finger by about 5 to 10 mm. The ball connection of the
flange must be centered in the sheet clamp and the seal must be placed on top of
the flange.
Re-assembly is the same as described in chapter 9.2.2. items e) to j).
Illustration 9.15: inserting the crucible tongs
Illustration 9.16: removing the ash finger
9.4 Changing the O2-lance
The O2-lance has the function to bring oxygen for combustion as close as possible to the
sample (i.e. near the ash finger bottom).
Two types of lance are available (both supplied with the standard equipment):
•
•
one standard-O2-lance (length: 140 mm) and
one extended O2-lance (length: 150 mm).
The extended O2-lance reached approx. 15 - 20 mm into the ash finger and brings the oxygen
closer to the sample (better combustion), but the available room for ashes is then shortened by
10 mm (i.e. ash finger must be exchanged more often). This type of lance should be used for
the analysis of hard to combust substances (e.g. copper phtalocyanine, graphite, carbon) and
when using an ash finger with bottom.
The standard-O2-lance reaches approx. 5 - 10 mm into the ash finger and is recommended
for the analysis of easily to normal combustible substances.
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Operating Instructions vario EL
Copyright y E l e m e n t a r Analysensystem GmbH
Page 9-20
Replacing consumables
Every time the ash finger has been changed, the O2-lance must be removed from the
combustion tube flange and checked. If necessary the gasket from the special sealing tube
must be renewed. The O2-lance must be checked for blockage caused by molten ash or tin
particles.
For disassembly or installation of the combustion tube flange see chapter 9.2.1, point a-h
respectively 9.2.2, point a and e-j.
The O2-lance is installed into the combustion tube flange as follows:
• Take the special sealing tube 4 mm (order No. 05 000 247) and stick it in one end of the
O2-lance.
• Insert the O2-lance with the gasket in the bore in the combustion tube flange until stop
(see illustration 9.17). Breaking of the lance can be avoided with a slight twist.
Illustration 9.17: inserting the O2-lance
9.5 Cleaning the quartz glass bridge
The quartz glass bridge connects combustion tube and reduction tube and is located below the
3-tube furnace (see illustration 9.12) behind a thermal shield. For disassembly see chapter
9.2.1 (points b-f and j-k). For installation see chapter 9.2.2 (point d-h).
The quartz glass bridge must be checked for dirt during every tube change. Black residue
(maybe tar) mean a bad combustion and wrong O2-dosing (see chapter 6.1.3). Blind value
measurements with oxygen (O2-index 1 respectively 3) after installation of the cleaned quartz
glass bridge ( and maybe after changing the ash finger) are therefore necessary until the blind
values (especially C) have come down to a normal level (see chapter 6.2.1).
In the CHNS/CNS/S-mode the quartz glass bridge can turn blue due to tungsten acids. This
necessitates a cleaning but otherwise it is harmless.
_________________________________________________________________________________
Operating Instructions vario EL
12.04
Copyright by E l e m e n t a r Analysensystem GmbH
Replacing consumables
Page 9-21
It is best to clean the quartz glass bridge in an ultrasonic bath with commonly used cleaning
solution. Then it should be carefully rinsed with distilled water and then dried. The seals of
the quartz glass bridge must be removed before cleaning. They should be checked for
damages and if necessary replaced.
Note:
when installing the quartz glass bridge an elastic resistance through pressing
the o-rings into the quartz glass bridge should be felt. Otherwise leakage might
occur, therefore the o-rings should be replaced.
9.6 Drying tubes
9.6.1 Filling the drying tubes
Legend:
1
2
3
empty space approx.
5 mm
filter 03 002 399
Sicapent®
Illustration 9.18: drying tube
Illustration 9.18 shows the filling of the drying tubes. At first a filter is stuffed into the
straight tube. The rest of the tube is filled with Sicapent® and covered with a filter.
Any Sicapent® residue must be cleaned off the tube ends and have an empty space of
approx. 5mm. Then the connection pieces are fitted into the gaskets, the caps are put
on and the connection with the glass tube is made.
9.6.2 Installation/Disassembly and conditioning
Before changing a tube, the gas supply into the
instrument must be turned off and the function
OptionsÖ MiscellaneousÖReplace parts must be
activated.
The five (respectively four) drying tubes are mounted in the front on the left side
behind the door (see illustration 5.1 respectively 5.2). These tubes are the reference
drying tube (no. 5), the O2-drying tube (no. 6) and the drying tubes between adsorption
columns or in the desorption paths (no. 12+13 respectively 14). They prevent
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Page 9-22
Replacing consumables
that
a) moisture traces in the carrier gas or oxygen lead to increased blind H values
and
b) if the H measuring range has been surpassed, steam which has not been
adsorbed on the H2O-adsorption column, does not lead to falsified
measuring results.
Disassembly/installation if carried out by opening or closing the ground in clamps.
For conditioning of the freshly filled drain tubes see chapter 9.2.4.
Change intervals:
Caution:
Sicapent® has an indicator which shows the used-up zones of the
tube through blue discoloring. Before every analysis it should be
checked if the unused Sicapent® is sufficient. The use of Sicapent® is very sparingly so that a change becomes necessary only
after several weeks.
Not absorbed moisture falsifies measuring results!
9.7 Gas purification tube
9.7.1 Filling of the gas purification tube
The gas purification tube (large U-tube) is filled as shown in illustration 9.19. First a
layer of NaOH on a carrier is filled in the bend of the U-tube. Then a quartz wool layer
(approx. 5 mm) is stuffed in both legs of the U-tube and the rest of the tube is filled
with Sicapent and closed with a filter. Any Sicapent® residue must be cleaned off the
tube ends before filling in the filter. At last the connection pieces are fitted into the
seals, the caps are put on and connected with the glass tube.
_________________________________________________________________________________
Operating Instructions vario EL
12.04
Copyright by E l e m e n t a r Analysensystem GmbH
Replacing consumables
Legend:
1
2
3
4
Page 9-23
2 filters 03 002 399
(both legs)
Sicapent® (both legs)
quartz wool approx. 5 mm
(both legs)
NaOH on carrier
Illustration 9.19: gas purifying tube
9.7.2 Installation/disassembly and conditioning
Before changing a tube, the gas supply must be turned
off and the function OptionsÖ MiscellaneousÖReplace
Parts must be activated.
The gas purifying tube is located at the front of the unit (see illustration 5.1/5.2, no. 8).
It removes traces of moisture and sour gases from the carrying gas. For installation
grip the tube at the right leg and push it carefully into the holding brackets until the
ground-in connections. Then the two ground-in connections are secured with clamps.
To compensate glass tolerances one of the two connection pieces at the instrument is
moveable.
For conditioning of the freshly filled gas purifying tubes see chapter 9.2.4.
Change intervals:
Caution:
Sicapent® has an indicator which shows the used-up zones of the
tube through blue discoloring. Before every analysis it should be
checked if the unused Sicapent® is sufficient. The use of Sicapent® is very sparingly so that a change becomes necessary only
after several weeks.
Not absorbed moisture and CO2 falsifies the measuring results!
_________________________________________________________________________________
10/02
Operating Instructions vario EL
Copyright y E l e m e n t a r Analysensystem GmbH
Page 9-24
Replacing consumables
_________________________________________________________________________________
Operating Instructions vario EL
12.04
Copyright by E l e m e n t a r Analysensystem GmbH
Maintenance/Service
Page
10-1
10. Maintenance / Service
Before opening a side or rear wall of the vario EL,
disconnect all peripheral equipment and the vario EL
itself by turning the main switch and pulling the
mains plug. Attention: the 3-tube furnace must be
cold otherwise components will become overheated. The
side and rear walls must be properly in place before
starting a new analysis (check safety linkage).
10.1 Troubleshooting
After a power supply failure of more than 15 minutes,
the vario EL must be checked for leaks. If necessary
replace all o-rings inside the furnace chamber since they
may have become defect due to the missing ventilation.
10.1.1 Failure messages from the PC
The unit is equipped with an internal failure diagnosis. When the diagnosis recognizes
a failure, it will be displayed, and either the unit will be stopped immediately (critical
failure) or after a defined number of samples (non-critical failure). For non-critical
failures, the quantity of permitted repetitions is defined on the menu OptionsÖError
Handling. The occurring failures are displayed and also saved in the report as error
code. The error code can be decoded any time in the menu OptionsÖError Index (see
illustration 10.1).
Illustration 10.1: menu OptionsÖError Index
05/05
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
Page
10-2
Maintenance/Service
We will now mention several error messages and the remedies that can be activated by
the operator:
Failure message from the
measuring module
Unsuccessful
Auto-Zero Adjust
Peak Termination not
recognized
Analysis without 2nd S-Peak
Start without sample
carousel
Cause:
Remedy
The change of the zero point of
the detector is higher than 2mV
in 10 seconds
After a completely new start of
the vario EL wait approx. 1.5
hours.
After turning on the gas when
That happens when the unit is
the vario EL is already switched
started immediately after turning on, wait approx. 15 minutes.
on the gas.
At the end of the peak the
• replace ash finger
detector signal does not become • check stability of the base
smaller than the N-Peak-End
line of the detector
defined in the menu
• check combustion
OptionsÖParameters. The
• check threshold
integration is aborted after 8
minutes.
not applicable !
Carousel not in position
place carousel in correct position
TCD thermostat
TCD-temperature not stable. The contact service;
deviation from the nominal
value is more than 12°C.
MS not ready
Cabinet temperature too
high
not applicable !
• Fan defect.
Internal temperature of the
vario EL is higher than 90°C.
• Front door (illustration
5.1/5.2, No.11) was open too
The heaters will be switched
long.
off parallel to this failure
message.
Overtemperature safety
circuit responded
System pressure too low
Integration overflow
The furnace monitoring system
has responded and switched of
the furnace transformer (see
chapter 5.2.4) Cause for this is
usually a failure message of the
combustion module (see
following pages).
• Operating pressure at the
pressure sensor < 0,5 bar
during analysis
• gas bottle empty?
• leakage
• defective pressure sensor
•
• Integral too high
• Auto-Zero value too low
push thermal switch above 3tube furnace back in, then restart
the vario EL and PC (see chapter
5.3.4);
if unsuccessful contact service.
• Restart unit and software and
adhere to the prescribed
succession (see chapter
5.3.4)
• correct failure message of the
combustion module.
• if unsuccessful contact
service.
• change gas bottle
• Leak test (see chapter 11)
• check the reaction tubes
• insufficient gas flush before
analysis start
• check base line during
standby condition
_________________________________________________________________________________
Operating instructions vario EL
02/99
Copyright by E l e m e n t a r Analysensysteme GmbH
Maintenance/Service
Failure message from
measuring module
Process error
Measuring range exceeding
time-out Sample Carousel
(zero position)
Measure memory overflow
Illegal Command to the
measuring module
Time-Out ball valve (flush
position)
Time-Out; heaters 1 - 6
Page
Cause
Remedy
• temporary disturbance of the
serial interface
• Start command incomplete or
new start of an analysis
during an analysis
TCD signal was higher than
10 V
Carousel did not recognize zero
position during reference run.
if this error occurs after a restart, contact service.
• Analysis takes too long
• Occurs mostly in
combination with other
failures
• wrong start-up succession
• disturbance at the serial
interface
ball valve does not reach end
position in defined time
(flush position only CHNS
analyzer)
heater 1-3 did not reach the
nominal temperatures during a
defined time.
• voltage too low
• heater is defective
• defective solid state relay
05/05
10-3
Temperature heaters 1-6
exceeds limit
a defined limit temperature was
exceeded
• defective thermocouple
• electrical connection of
adsorption column or blind
plug not plugged in (see
chapter 10.2.3).
Temperature difference
heaters 1-6
Actual temperature is not
approaching nominal
temperature.
Difference > 70°C during
overheating
• sample weight too high
• leakage
• try to move to another
position through the menu
OptionsÖMiscellaneousÖCarousel (without the
carousel)
• check if turn-off-knob is still
in the carousel drive.
• contact service
• check parameters, O2-Index
and sample weight
• check gas supply He + O2
• adhere to the prescribed
switch-on succession (see
chapter 5.3.4.)
• otherwise contact service
• clean and adjust ball valve
(see chapter 9.2.1)
• otherwise contact service
• heat up heaters in two steps
• heater power supply
defective. Check fuses
• wrong nominal temperature
in the parameter file?
• contact service if the
respective heater remains
totally cold.
• check connections of adsorption columns.
• wrong nominal temperature
in the parameter file?
• contact service.
• short circuited thermocouple
• defective heater
• contact service
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
Page
10-4
Failure message PCmonitoring
Threshold values for test
substances are exceeded
Maintenance/Service
Cause
Remedy
The threshold defined in the
standards menu has been
exceeded
• insufficient run-in samples?
• check combustion
• perform leakage test (see
chapter 11).
• chosen threshold too narrow?
• weight error
“Standard-ThresholdControl“ must be activated
[OptionsÖParameters].
10.1.2 Help to recognize failures
Failure
Cause
Remedy
Variations in the measuring
values, increase in analysis
times, occurrence of blanks
poor sample
combustion
Remedies in the following order of
priority:
1. has the minimum combustion time
to be increased?
2. does the end of the O2-lance reach
into the ash finger?
It should be about 5-10mm; or is
the O2-lance clogged?
3. is the seal in the O2-lance in the
VR flange intact? If not replace it;
4. how old are the catalyst fillings?
if necessary change combustion
tube;
5. is the filling of the reduction tube
used up? Replace if necessary;
6. is the O2-supply correct during
combustion?
check at the O2-flow meter (left)
during analysis (see chapter 6.1.3).
1. leak test (see chapter 11).
Remedies in the following order of
priority:
1. check quartz wool at the
combustion tube outlet and at the
reduction inlet to see if it is felted;
2. check the quartz glass bridge
between the combustion tube and
reduction tube for blockages;
3. the filling of the combustion tube
could possible be "baked",
especially if the samples contain a
lot of salt;
normal blank value:
N:
20 - 50 Int.
C:
0 - 50 Int.
H:
150 - 300 Int.
S:
0 - 50 Int.
it is especially
noticeable when the
results are alternating
too low or too high
Clogging
• flow meter at the PC
shows decreasing values,
• pressure gauge and He
remain stable,
• analysis results increase.
_________________________________________________________________________________
Operating instructions vario EL
02/99
Copyright by E l e m e n t a r Analysensysteme GmbH
Maintenance/Service
Page
10-5
Failure
Cause
increased N blank values
(normal 20 - 50 integrals)
1. N-blank value without O2-dosing
• leakage
(O2-Index = 2), i.e. instrument
• insufficient sample
leaks;
flashing in the ball
2. N blank value only with O2valve
dosing, i.e. leak in the O2-supply
line or inferior O2-quality;
3. is ball valve flushing working
during sample placement?
Is the quantity of flushing gas
sufficient?
The pressure at the pressure gauge
decreases to 1 bar during flushing.
If not, the flushing gas quantity
must be re-adjusted at the throttle
of the ball valve;
perform a manual leak test (see
probably a leakage
chapter 11).
Variations in measuring
values without the
occurrence of any other
irregularities
N-value too high
S-values too low
Variations in the measuring
values of all elements
which means: CHNS value
always too high or too low.
Stable CN relation
reduction tube filling
is used up
• copper filling in the
reduction tube is in
the wrong place
(too cold)
• tar in the quartz
glass bridge
• not enough WO3sample additive
Probably a weighing
error
Remedy
Replace reduction tube (see chapter
9.1ff).
• replace reduction tube (see chapter
9.1.1)
• clean quartz glass bridge (see
chapter 9.5)
• replace ash finger and use samples
with more WO3-additive.
Check the balance with a test weight
regarding stability and consistency.
Avoid electrostatic charging during
weighing.
Please ensure that the tin boats do not
burst while folding.
Contact service if the problem persists.
10.2 Service tips
Note:
Regarding this subject, please read also the description of the maintenance
software (see chapter 11 and Online-Help). For further problems and question
please contact the respective service.
10.2.1 Maintenance of the ball valve
If dust, sample particles, ashes or tin oxide particles get between the ball and the
Teflon shells of the ball valve, it can lead to leakage. We, therefore, suggest to clean
05/05
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
Page
10-6
Maintenance/Service
and check the ball valve after analyzing 1500 samples. The tool set "ball valve" (order
No. 12.00-0100) is part of the initial outfit of delivery.
For disassembly or installation of the ball valve, furnaces
must have been cooled down. For this purpose set
furnaces to nominal temperature 0°C and let them
cool down to room temperature (max. 100°C). The
supplied protective gloves must also be worn because hot
components are inside the furnace.
Steps
Procedure
Prerequisites
Bring instrument in standby position, turn off gas and
wait for pressure decrease.
• Pull out the combustion furnace from the analyzer
(see chapter 9.2.1, a-f);
• open the right side wall of the vario EL;
• loosen He-line to the ball valve (illustration 9.8,
no.7+8);
• loosen the two hexagonal nuts (inscription: M6) on
the right side of the ball valve;
• pull out the ball valve together with the holding plate
towards the front out of the drive coupling and
remove it from the unit.
• loosen the safety screw on the driving axle of the
opposite casing side;
• loosen and remove the spring flange of the Teflon
shells by means of a hooked wrench;
• loosen and remove holding plate (4 Philips screws)
• loosen and remove drive bearings (4 Philips screws)
• the ball as well as the upper Teflon shell must be
pushed out with the tool supplied in the tool set "ball
valve". For this purpose push onto the ball with the
pushing tool from the side of the bayonet lock until
the ball and the upper shell glide out of the housing;
• the lower Teflon shell falls out of the ball valve
housing when it is turned around;
Disassembly of the ball valve
Dismantling the ball valve (see
illustration 10.2)
Cleaning the Teflon shells and
the ball
• clean the Teflon shells and the ball with acetone;
• check Teflon shells for tangible grooves. In case of
grooves the Teflon shells have to be replaced;
_________________________________________________________________________________
Operating instructions vario EL
02/99
Copyright by E l e m e n t a r Analysensysteme GmbH
Maintenance/Service
Mounting the ball valves
(see illustration 10.2)
Page
10-7
• install the lower teflon shell considering the O-ringsealing and the notch for the drive bearing;
• install the ball valve with the blind hole downwards;
note the position of the cutout for the drive axle;
• install drive bearing and tighten (take care of the Oring sealing);
• put in the upper teflon shell, considering the cutout
for the drive bearing;
• place the spring flange in position and tighten with a
hooked wrench;
• at the same time measure the torque of the ball valve
with a torque wrench; torque wrench has to be
adjusted to 350 Ncm before use!
at approx. 300 to 350 Ncm the ball valve is usually
tight;
• tighten safety screw of spring flange - not too tight;
• bring ball valve into basic position (open) and check
torque again; if necessary, repeat adjustment
procedure;
• install ball valve into the unit;
• close the side wall on the right;
03 774 793
11.02-1012/4
05 000 425
O-Ring
11.00-0053/o.Z.
11.00-1164/4
05 000 353
Square gasket
11.00-1323/4
05 000 425
O-Ring
11.00-0905/4
03 654 627
O-Ring
11.00-0910/4
03 654 629
05 000 371
11.00-1191/4
05 000 372
Illustration 10.2: ball valve
05/05
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
Page
10-8
Maintenance/Service
10.2.2 Cleaning the carousel
In due course, dust particles can soil the carousel. Because of this there is a risk that
dusty abrasion may occasionally enter the combustion apparatus during sample
feeding and lead to a distortion of measuring values.
For cleaning purposes, dismantle the carousel into two parts: 1. the metallic base plate
and 2. the plastic upper part with three holding magnets. Separate the parts by holding
the plate in one hand and press lightly against the base plate with a pencil (do not use a
sharp pointy implement).
Clean with a soft cloth or a brush, if necessary use a little water with laboratory
detergent (do not use sharp or abrasive cleaners).
Caution: damage to the base plate by scratches etc. impairs the function of the
carousel!
After cleaning and drying the base plate, insert it into the plastic upper part. Take care
not to insert it the wrong way around!
If the base plate is wrongly inserted. the sample feeder cannot be started at position 1.
10.2.3 Replacement of adsorption columns
Replacement of adsorption columns can be necessary for the following reasons:
1. Changing the mode of operation (see chapter 7.3).
2. Aging of the column filling (e.g. through fluor connection) which
decreases the adsorption/desorption ability and causes extreme peak
widening.
All columns are available as a new part or replacement part (only with a new filling)
(for order instructions see chapter 7.3).
For replacement of adsorption columns, furnaces and
columns must have been cooled down and the
vario EL must have been shut off. For this purpose set
furnaces and adsorption columns to nominal temperature
0°C and let them cool down to room temperature (max.
100°C). Turn off vario EL after it has cooled down so
that it does not overheat because of missing ventilation.
Procedure for the replacement of adsorption columns:
a) Set furnaces and adsorption columns to nominal temperature 0°C and let them cool
down to room temperature (max. 100°C). For this purpose set nominal temperatures in
OptionsÖParameters to 0°C and wait until they have cooled off (approx. 2 hours).
Note: temperature setting can only be done with the corresponding access rights.
_________________________________________________________________________________
Operating instructions vario EL
02/99
Copyright by E l e m e n t a r Analysensysteme GmbH
Maintenance/Service
Page
10-9
b) Leave vario EL-software with SystemÖOffline and FileÖExit.
c) Turn main switch of vario EL off (see illustration 5.1/5.2, no. 1).
d) Remove left cover plate from instrument top by removing two Philips screws.
The separation part of the vario EL is now accessible. Illustration 10.3 shows the
lay-out of the adsorption columns and their electrical connection sockets.
gas inlets
gas outlet
electrical connection
sockets of the adsorption
columns
Illustration 10.3: lay-out of the adsorption columns (top view)
e) Disassembly of the adsorption column for replacement:
Š
Š
Š
Š
Š
Loosen ground-in screws at inlet and outlet.
Loosen two Philips screws of the holding device.
Pull plug from the appropriate socket.
Remove adsorption column.
Close adsorption column with blind stopper.
Store adsorption column in a cool, dry place where it is not subjected to
vibrations or send in to be refilled.
f) Installation of a new adsorption column:
♦ Insert adsorption column into its retainer.
Š Fasten holding device with two screws.
Š Plug the adsorption column in (see illustration 10.3).
The electrical connection sockets are marked and coded so that a mistake
is not possible.
Š Remove blind stoppers and close the ground-in connections at the inlet of the
adsorption column according to the pipe diagram (see chapter 7)
Š The outlet of the adsorption column remains open because the new adsorption
column must be heated up before operation.
05/05
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
Page
10-10
Maintenance/Service
g) Heating the new adsorption column:
Š turn vario EL on (see chapter 5.3.4).
Š reduce He-prepressure at the source to 0,5 - 0,6 bar.
Š load vario EL software and start the heating program with function
OptionsÖMiscellaneousÖ SO2-Column (respectively H2O- or CO2Column).
Š After heating time is over close the outlet of the adsorption column
according to the tubing diagram (see chapter 7).
Note: If several adsorption columns have been replaced it is necessary
to strictly adhere to the order of the gas supply (first SO2, then H2O and
thereafter CO2). This is the only way not to flush interfering components
from one adsorption column to the other.
h) Reset He-prepressure at the source to 2.0 bar and remount the cover plate on the
top of the unit.
i) The vario EL is now ready for operation.
Note:
1. After replacement of a H2O-adsorption column, we recommend to
measure several blanks without oxygen (O2-index 2 = 1s) until low
and stable blank values (150 to 300 integrals) have been achieved.
2. If after an adsorption column replacement the daily factor is not
within the range of 0.9 to 1.1, a calibration becomes necessary
(see chapter 6.4).
10.2.4 Customer maintenance
Maintenance
Recommended interval Reference
Changing the ash finger
depends on sample matrix
max. 140 samples
chapter
9.3.2
Checking or replacing the O2-lance and
gasket
every time the
ash finger is replaced
chapter 9.4.
Changing fillings or replacing tubes with
simultaneous checking of the plugs and
O-rings
Cleaning or checking the quartz glass
bridge between combustion and
reduction tube incl. checking of the orings
for changing intervals see
maintenance menu
OptionsÖMaintenance
at every tube replacement
chapter
9.1/9.2
chapter 9.5
_________________________________________________________________________________
Operating instructions vario EL
02/99
Copyright by E l e m e n t a r Analysensysteme GmbH
Maintenance/Service
Page
Maintenance
10-11
Recommended interval Reference
Checking or replacing the absorption-U- daily sight check
tubes in the CNS/S/CN/N-mode
Checking or replacing the drying tubes
daily sight check
and the gas purifying tube
Cleaning the carousel
if necessary
Cleaning the ball valve, if necessary
replacing the gaskets
every 1500 analyses
chapter
9.1/9.2
chapter
9.6/9.7
chapter
10.2.2
chapter
10.2.1
Checking the capacity of the hard disk, if backup every week
storage on disks as necessary
necessary storage of data on disks
Checking the supply gases for correct
before every test series
pre-pressure and sufficient volume
Leak test of the vario EL and the supply min. every two months
lines for the gases
chapter
5.1.2
chapter 11
Recommendation: an annual maintenance contract for a complete maintenance
saves time and money.
For more information contact your service.
10.2.5 Replacing fuses
Note:
If the overload releases jumped out, please always inform your respective
service. The causes could be serious.
To replace the fuses, the left side wall of the vario EL must be removed.
Table of the vario EL fuses
F1
F2 + F3
F4
F5
F6
F7
F8
F9 + F10
F11 + F12
05/05
furnace 1
furnace 2, furnace 3
adsorption columns
heater for the tubes
24 VDC card
TCD-heater
Haltec power supply IRdetector
furnace transformer
electronic-transformer
42 V AC; 15 A
42 V AC; 10 A
42 V AC; 10 A
13 V AC; 10 A
18 V AC; 10 A
24 V AC; 6 A
230 V AC; 2 A
230 V AC; 15 A
230 V AC; 6 A
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
Page
10-12
Maintenance/Service
10.2.6 Replacing the O-rings
The o-rings in the drying tubs, in the plugs of the combustion and reduction tubes and
in the quartz glass bridge are particularly susceptible to chemical corrosion and
mechanical and thermal stress, which alter their material properties, so that after a
while they become leaky.
O-rings in the drying tubes
The o-rings are immediately accessible after removing the sealing plugs. They only
have to be slipped over the cylindrical tube connections.
A replacement is advisable when the o-rings show cracks or permanent damage
caused by the sharp edges of the drying tube.
O-rings in the quartz glass bridge
After disassembly of the quartz glass bridge (see chapter 9.5) the o-rings are freely
accessible in the ground-in connections of the quartz glass bridge.
Always replace the o-rings in the quartz glass bridge if only a slight pressure
resistance or non at all can be felt on closing the ground ball connector.
O-rings in the combustion tube flange or in the sealing plug of the reduction tube
These o-rings are subject to long-term thermal wear and tear. In the course of time
they are pressed flat and become leaky. During cooling-off the plug / flange shrinks a
little and if the o-rings are old and not elastic anymore they cause leaks or the sealing
plug or flange can fall out of the tube. For disassembly and installation of the
combustion tube flange see chapter 9.2.
Always replace the o-rings in the sealing plugs if only a slight pressure resistance can
be felt on inserting the plug into the tube. A visual check is helpful, to see if the orings still protrude from the recesses of the plugs (see illustration 10.4).
O-rings are in good
condition
O-rings must be replaced
Illustration 10.4: condition of o-rings in sealing plugs
_________________________________________________________________________________
Operating instructions vario EL
02/99
Copyright by E l e m e n t a r Analysensysteme GmbH
Maintenance/Service
Page
10-13
To remove an o-ring from a sealing plug, push it with thumb and index finger
sideways out of the plug until it forms a loop at the side (see illustration 10.5). Grip
this loop with a pair of tweezers and pull the o-ring off the plug completely.
Illustration 10.5: removing the o-ring
Using a sharp knife or scalpel to cut out o-rings can
damage the sealing surface underneath the o-ring
through scratches. There is also the danger of injuries
through slipping!!
05/05
Operating instructions vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
Maintenance software
Page 11-1
11. Maintenance software
Since the maintenance software of the vario EL is
self-explanatory and has an extensive Online-Help
program, we have mentioned only the most important
menus and commands. For further information
regarding software please read the notes in the menu
HelpÖIndex.
Start the program by clicking on the vario EL Maintenance-symbol. Depending on the
condition of the initializing files, a certain amount of time will pass until the main window
appears. If the program recognizes a connected analyzer, an additional window will appear
with the message that the modules are being initialized.
11.1 Main window
After program start, the main window appears as shown in illustration 11.
Illustration 11.1: main window of the vario EL maintenance software
02/99
Operating instructions
Copyright E l e m e n t a r Analysensysteme GmbH
Page 11-2
Maintenance software
11.2 Title bar
the title bar is equipped with the usual click areas to call up the system menu as well as the
buttons for minimizing and maximizing the application window.
11.3 Menu bar
The menu bar shows the top level of the menu structure. The following is a short description
of the individual menus:
End
To end the program. the program can only be ended when the leak test
modus is not active!
Leaktest
Enables to call up different leak test steps.
Privilege
Enables selection between service personnel and operator. For service
personnel selection a password is necessary.
Error
Serves to reset error messages of the measuring module and the
combustion module.
Help
Detailed help for the program can be called up.
11.4 Operating the program
The program can be operated by clicking on different components of the diagram. Please read
the detailed description in
HelpÖContentsÖGeneral.
Operating instructions
Copyright E l e m e n t a r Analysensysteme GmbH
02/99
Appendix
Page
A-1
12. Appendix
12.1 Index of illustrations
Illustration 4.1: functional diagram vario EL (CHNS-mode)
Illustration 5.1: front view of the vario EL (CHNS-mode)
Illustration 5.2: front view of the vario EL (CHN-mode)
Illustration 5.3: rear view of the vario EL
Illustration 5.4: handle carrying position
Illustration 5.5: transport guard 3-tube-furnace
Illustration 5.6: connection of peripheral instruments
Illustration 5.7: parameter-window in CHNS-mode
Illustration 6.1: dialog statistics: define groups
Illustration 6.2: dialog configure CHNS-calibration
Illustration 6.3: graph of a calibration curve
Illustration 6.4: formulas for quality computation
Illustration 6.5: calibration menu with marked outliers
Illustration 6.6: dialog CHNS Calibration-Coefficients
Illustration 6.7: dialog sleep-/wake-function
Illustration 7.1: tubing scheme vario EL, CHNS-mode
Illustration 7.2: typical course of measuring peak
Illustration 7.3: tubing scheme vario EL, CNS-mode
Illustration 7.4: parameter-menu, CNS-mode
Illustration 7.5: tubing scheme vario EL, S-mode (with TCD)
Illustration 7.6: parameters-menu, S-mode
Illustration 7.7: typical course of measuring peak, S-mode
Illustration 7.8: tubing scheme vario EL, CHN-mode
Illustration 7.9: parameter-menu, CHN-mode
Illustration 7.10: typical course of measuring peak, CHN-mode
Illustration 7.11: tubing scheme vario EL, CN-mode
Illustration 7.12: parameter-menu, CN-mode
Illustration 7.13: tubing scheme vario EL, N-mode
Illustration 7.14: parameter-menu, N-mode
Illustration 7.15: conversion matrix vario EL
Illustration 7.16: mode-menu
Illustration 7.17: dialog changing mode
Illustration 8.1: main menu of the vario EL-software
Illustration 8.2: tool bar
Illustration 8.3: main window with graphic display
Illustration 8.4: main window with statistic display
Illustration 9.1: menu OptionsÖMaintenance
Illustration 9.2: combustion tube CHNS/CNS/S-mode
Illustration 9.3: reduction tube CHNS/CNS/S-mode
Illustration 9.4: H2O-absorption-U-tube
Illustration 9.5: combustion tube CHN/CN/N-mode
05.2005
4-2
5-3
5-4
5-5
5-9
5-9
5-9
5-11
6-9
6-15
6-16
6-17
6-18
6-19
6-20
7-2
7-4
7-5
7-6
7-7
7-8
7-9
7-10
7-12
7-12
7-14
7-16
7-17
7-18
7-20
7-25
7-26
8-2
8-10
8-11
8-12
9-2
9-4
9-5
9-6
9-7
Operating instruction vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
Page
A-2
Appendix
Illustration 9.6: reduction tube CHN/CN/N-mode
Illustration 9.7: CO2-absorption-U-tube
Illustration 9.8: furnace chamber vario EL
Illustration 9.9: pulling off/replacing the combustion tube flange
Illustration 9.10: pulling out/inserting the combustion tube flange
Illustration 9.11: placing the combustion tube flange in the tube stand
Illustration 9.12: quartz glass bridge
Illustration 9.13: built-in H2O-absorption-U-tube (CNS/S/CN-mode)
Illustration 9.14: built-in H2O- and CO2-absorption-U-tube (N-mode)
Illustration 9.15: inserting the crucible tongs
Illustration 9.16: removing the ash finger
Illustration 9.17: cutting the special sealing tube
Illustration 9.18: inserting the O2-lance
Illustration 9.19: drying tube
Illustration 9.20: gas purifying tube
Illustration 10.1: menu OptionsÖError Index
Illustration 10.2: ball valve
Illustration 10.3: lay-out of the adsorption columns (top view)
Illustration 10.4: condition of o-rings in sealing plugs
Illustration 10.5: removing the o-ring
Illustration 11.1: main window of the vario EL maintenance software
Operating Instructions vario EL III
Copyright by E l e m e n t a r Analysensysteme GmbH
9-8
9-9
9-11
9-12
9-12
9-12
9-13
9-15
9-16
9-19
9-19
9-20
9-20
9-21
9-22
10-1
10-7
10-9
10-12
10-13
11-1
05.2005
Appendix
Page
A-3
Solving PC problems
Occasionally, there are problems with the PCs which probably are in connection with the
Elementar instrument software. Possible problems may be occasional system crashes or a
freeze of the instrument software. The cause can be explained by the connection of the
settings in the operation system for the power management of the PC. The settings shall be
checked in the power management under Control Panel-> Power Option Properties and/or
Power Schemes. The options for "Turn off monitor", "Turn off hard disks", "System standby"
and "System hibernates" shall be set to "Never". If possible, also the power management in
the BIOS of the PC shall be deactivated.
If the PC is connected to a network a further measure can be the deactivation of the network.
If possible, deactivate the network adapter under Systemsteuerung-> Gerätemanager or
remove the network cable and restart the PC without network.
Under Windows NT4.0, Windows 2000 Professional and Windows XP Professional the
instrument software has to be started under equivalent user rights in order to be able to change
files in the instrument software directory (e.g. c:\variomax) and in the system directory (e.g.
c:\windows).
General Note
For future generations of the Elementar instrument software the operation systems Windows
2000 Professional or Windows XP Professional will be a prerequisite. Windows 9x/ME and
Windows NT will not be supported anymore. This has to be taken under consideration when
purchasing new PC hardware.
05.2005
Operating instruction vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
Page
A-4
Appendix
12.2 Data sheets for the spare parts lists
The following blow-up drawings show several components. The order numbers for individual
parts as gaskets etc. are shown.
Operating Instructions vario EL III
Copyright by E l e m e n t a r Analysensysteme GmbH
05.2005
Appendix
05.2005
Page
A-5
Operating instruction vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
Page
A-6
Appendix
12.3 List for spare parts and consumables/Safety Data Sheets
The enclosed lists (initial outfit and consumables sets) are valid at the time these Operating
instructions are supplied. For further order information for spare parts and consumables
please contact your local dealer or Elementar, Hanau, Germany.
Operating Instructions vario EL III
Copyright by E l e m e n t a r Analysensysteme GmbH
05.2005
Appendix
Page
A-7
initial outfit vario EL for installation and training
Erstausstattung vario EL für Inbetriebnahme und Einweisung
Date: 30.1.03
art.-no.:
11.00-5010
article-no.
description
Artikelname
03 001 248
tweezers 145 mm lg.
Pinzette 145 mm lg.
(Te)
Menge
units
1
pcs
03 002 399
filter, 14 x 20 mm
Filter, 14 x 20 mm
15
pcs
03 651 010
pressure hose
Druckluftschlauch 5 x 1
25
m
03 674 010
clamp, large
Schliffklammer, groß
5
pcs
03 679 908
quartz wool, 10 g
Quarzwolle
1
pcs
03 679 942
acetanilide, 5 g
Acetanilid , pulverförmig
1
pcs
03 710 717
multiple plug box (5 entries)
Steckdosenleiste
1
pcs
03 950 005
micro spatula
Mikrospatel
1
pcs
03 968 006
vacuum grease 100 gr
Vakuumfett 100 g
1
pcs
05 000 086
Al2 O3-wool, 20 g
Aluminiumoxid-Wolle, 20 g
1
pcs
05 000 088
O2 - lance, 140 mm
O2 - Lanze, 140 mm
1
pcs
05 000 094
gloves, temp. resistant
Handschuhe, 1 Paar
1
pcs
05 000 247
Lance-sealing (10 pcs)
Lanzendichtung (10 St.)
1 pcs
05 000 249
o-ring 4.5 x 1.5, green
O-Ring 4,5 x 1,5, grün
5
pcs
05 000 287
clamp, small
Schliffklammer, klein KS 7
4
pcs
05 000 308
sample plate for 24 samples
Probenplatte für 24 Proben
3
pcs
05 000 353
square gasket, black
Quad-Ring, schwarz
7
pcs
05 000 354
O2 - lance, 150 mm
O2 - Lanze, 150 mm
1
pcs
05 000 358
leather gloves, 1 pair
Lederhandschuhe
1
pcs
05 000 397
ball, d=12 mm
Kugel D = 12 mm
2
pcs
05 000 416
o-ring 7.5 x 2.5, green
O-Ring 7,5 x 2,5, grün
2
pcs
05 000 699
copper, wire 100 g
Kupfer, drahtförmig
7
pcs
05 000 933
mouse pad
Mouse - Pad
1
pcs
05 001 255
hexagon socket screw key
Inbuschlüssel Gr 4
1
pcs
11.00-0035
tool kit for ball valve
Satz Werkzeug für Kugelhahn
1
pcs
11.00-0109/4
copper tube no. 47
Rohrleitung Nr. 47
1
pcs
11.00-1150/4
combustion tube, reduct. tube
Verbrennungs-, Reduktionsrohr
2
pcs
11.00-1170/4
ash finger, quartz
Aschefinger
5
pcs
11.00-1173/4
stuffing tool
Stopfwerkzeug
1
pcs
11.00-1317/4
protective tube
Schutzrohr
1
pcs
11.00-1331/4
quartz bridge vario EL
Quarzglasbrücke
1
pcs
11.00-5017
tin boats assortment
Zinnschiffchen Sortiment
3
pcs
11.00-5047/4
leakage set vario EL, rapid N
Lecksuchsatz varioEL
1
pcs
11.01-0015/4
U-tube with GL 18 connection
U-Rohr, GL 18,kpl.,vario/rapid
2
pcs
11.01-0016/4
copper tube , cpl. No. 110
Rohrleitung Nr. 110
1
pcs
11.01-0017/4
copper tube No. 111
Rohrleitung Nr. 111
1
pcs
11.01-0021/4
copper tube No.109
Rohrleitung, vollst., Nr. 109
1
pcs
11.02-0009/4
copper tube no. 145
Rohrleitung Nr. 145
1
pcs
11.02-0010/4
copper tube no. 146
Rohrleitung Nr. 146
1
pcs
11.02-0011/3
copper tube no. 147
Rohrleitung Nr. 147
1
pcs
12.00-1008/3
crucible tongs
Fingerzange
1
pcs
22 131 365
silver wool, 50 g
Silberwolle
1
pcs
34.00-0051/4
funnel, complete,
Trichter, komplett für GL 14
1
pcs
34.00-0099/4
funnel, complete for GL 18
Trichter, komplett für GL 18
1
pcs
01/04
Operating instruction vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
Page
A-8
Appendix
set of consumables for approx. 4.000 analysis (vario EL / CHNS, CNS, S)
Satz Verbrauchsmaterial/ca.4000 Analysen
(vario EL / CHNS, CNS, S)
Date: 31.1.03
art.-no.:
11.00-5012
article-no.
description
Artikelname
03 001 118
sulfanilic acid 5 g
Sulfanilsäure 5 g
1 pcs
03 002 399
filter, 14 x 20 mm
Filter, 14 x 20 mm
30 pcs
Menge
units
03 654 627
o-ring 20 x 2, green
O-Ring 20 x 2, grün
8 pcs
03 679 908
quartz wool, 10 g
Quarzwolle
2 pcs
03 679 942
acetanilide, 5 g
Acetanilid , pulverförmig
1 pcs
05 000 086
Al2 O3-wool, 20 g
Aluminiumoxid-Wolle, 20 g
5 pcs
05 000 088
O2 - lance, 140 mm
O2 - Lanze, 140 mm
5 pcs
05 000 247
lance sealing (10 pcs)
Lanzendichtung (10 St.)
1 pcs
05 000 353
square gasket, black
Quad-Ring, schwarz
6 pcs
05 000 354
O2 - lance, 150 mm
O2 - Lanze, 150 mm
5 pcs
05 000 416
o-ring 7.5 x 2.5, green
O-Ring 7,5 x 2,5, grün
05 000 699
copper, wire 100 g
Kupfer, drahtförmig
11.00-1150/4
combustion tube varioEL,
Verbrennungs-, Reduktionsrohr
11.00-1170/4
ash finger, quartz
Aschefinger
11.00-1172/4
support tube, 65 mm
Stützrohr, 65 mm
8 pcs
22 pcs
6 pcs
20 pcs
6 pcs
11.00-1317/4
protective tube
Schutzrohr
2 pcs
11.02-0008
tungsten(VI)-oxide,60 g
Wolfram(VI)-Oxid Granulat 60 g
4 pcs
11.02-0017
tungsten(VI)-oxyd powder 25g
Wolfram(VI)-Oxid Pulver 25 g
3 pcs
22 131 365
silver wool, 50 g
Silberwolle
1 pcs
22 137 418
tin boats
Zinnschiffchen
2 pcs
22 137 419
tin boats
Zinnschiffchen
4 pcs
50 008 467
corundum balls, 40 g
Korund - Hohlkugeln, 40 g
1 pcs
Operating Instructions vario EL III
Copyright by E l e m e n t a r Analysensysteme GmbH
01/04
Appendix
Page
A-9
set of consumables for capsule press for appr. 2.000 samples
Satz Verbrauchsmaterial Kapselpresse für ca. 2.000 Proben
art.-no.:
22 133 012
article-no.
description
Artikelname
03 951 619
tin capsules, 250 pcs.
Zinnkapsel,Füllvolumen 0,05 ml
1 pcs
03 951 620
tin capsules, 250 pcs.
Zinnkapsel,Füllvolumen 0,025ml
7 pcs
03 951 621
micro pipette 100 pcs.
Mikro-Pipette, 100 St.
03 951 622
GZ 383 ABS bottles, 300 pcs.
ABS Fläschchen
01/04
Date: 15.1.02
Menge
units
20 pcs
1 pcs
Operating instruction vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
Page
A-10
Appendix
Set of consumables for approx. 4.000 analysis (O) (vario EL)
Satz Verbrauchsmaterial/ca. 4.000 Analysen (O) (vario EL)
Date: 15.01.02
art.-no.:
11.00-5014
article-no.
description
Artikelname
03 002 399
filter, 14 x 20 mm
Filter, 14 x 20 mm
30 pcs
03 654 603
o-ring 11.3 x 2.4, red
O-Ring 11,3 x 2,4, rot
20 pcs
03 654 627
o-ring 20 x 2, green
O-Ring 20 x 2, grün
5 pcs
03 654 814
o-ring 14 x 3.5, red
O-Ring 14 x 3,5, rot
12 pcs
03 679 900
sodium hydroxide
Natriumhydroxid gekörnt
1 pcs
03 679 907
quartz chips, 100 g
Quarzsplitter, 100 g
1 pcs
03 679 908
quartz wool, 10 g
Quarzwolle
2 pcs
03 679 910
lamp black, 80 g
Gasruß
2 pcs
03 679 941
square gasket, red
Quad-Ring Z 261, rot
5 pcs
05 000 369
o-ring 4 x 4, green
O-Ring 4 x 4, grün
10 pcs
05 000 400
benzoic acid, 5 g
Benzoesäure , 5 g
1 pcs
22 131 365
silver wool, 50 g
Silberwolle
1 pcs
Menge
units
22 133 210/3
crack tube GZ 384 for O2 anal.
Crackrohr
4 pcs
22 133 211/4
quartz tube insert
Quarzfinger
6 pcs
22 133 212
silver boats
Silberschiffchen
2 pcs
22 137 418
tin boats
Zinnschiffchen
4 pcs
34.00-1339/4
u-tube, GL 18
U-Rohr, GL 18
2 pcs
xx
Operating Instructions vario EL III
Copyright by E l e m e n t a r Analysensysteme GmbH
2
01/04
Appendix
Page
A-11
12.4 Installation requirements
Dear User,
we thank you for your order and the confidence expressed to our representative and
Elementar by this decision.
You have made you choice for a CHNOS analyzer of highest analytical performance and
reliability. In order to secure a fast and smooth installation of the instrument in your
laboratory, we kindly ask you to take the following hints into consideration:
Installation location
• The analyzer can be installed under normal laboratory conditions, i.e. no fume hoods or air
condition (ambient temperature between +15°C max. +35°C) are necessary.
• However, like for all analytical equipment direct sun beams, draft or other inconvenient
conditions for precision instruments should be avoided.
• For the installation of the unit (without PC, printer and balance) a stable laboratory table with
heat resistant surface is sufficient.
•
Minimum dimensions: length 1.20 m * depth 0.80 m
•
Weight vario EL approx. 120 kg.
Gas supply
For the operation of the analyzer the following gases are required which should be kept ready
by you on the spot for installation:
• helium (purity 99.996 %)
• oxygen (purity 99.995 %)
Unless delivered from us, the availability of two-step high precision pressure reducers (Air
Liquide or similar) is necessary. Pressure reducers of inferior quality will influence negatively
the analysis results!
! Pay attention to the bottle pressure !
Instrument control
If PC and balance were not delivered from Elementar, we reserve the right to perform the
installation with own instruments. Possible modifications to our analyzer have to be done by the
customer.
We would like to emphasize that the PC is the central control system of the analyzer. The
operating ability of the analyzer depends on a failure-free operation of the PC. Due to
experiences in the past with the use of control PC in mixed operation as office workplace
impairments due to software instabilities may occur.
Therefore, we recommend to only use programs on this PC for operation and data evaluation of
this analyzer.
01/04
Operating instruction vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
Page
A-12
Appendix
Control PC
In case the PC was not delivered by us, the following minimum requirements have to be met:
For operation without modem:
• PC with Pentium III Processor 500 MHZ (or equivalent) or faster
• Operating system
•
Windows 2000 Professional (SP3 or later), with 128 Mbyte RAM
or
•
Windows XP Professional (SP1 or later), with 256 Mbyte RAM
• At least 100 MB fee momory on hard disc
• 1 free serial port RS 232
• CD-ROM or DVD-ROM drive
For operation with modem:
• 2 free serial ports RS 232
• CAUTION: The mouse must not occupy any of these ports.
• 1 analog telephone socket TAE-6N in 6 m periphery from the PC.
• This connection is necessary to guarantee the remote control maintenance of the instrument
via an analog modem.
• 1 analog modem with at least 56 kBaud transfer rate.
• Remote control maintenance software Symantec PC-Anywhere 10.5 or later.
Installation requirements for the instrument software:
To install the instrument software correctly, administrator rights for the PC have to be made
available.
Requirements for the correct operation of the instrument software:
The instrument software has to be operated under a user account that is provided with writing
rights in the instrument software directory (e.g. c:\varioel) and in the system directory (e.g.
c:\windows).
The PC where the instrument software will be installed should be checked for settings in the
control panel under Control PanelÖPower Option Properties and/or Power Schemes. Setting
should be made as follows: "Turn off monitor", "Turn off hard disks", "System stand by" and
"System hibernates" should always be set to "Never". If possible, also deactivate the power
management in the BIOS of the PC.
As screen saver use only the Windows standard screen saver.
Generally, it is not recommended to overload the PC where the instrument software is installed
with other software programs. This may lead to instable operation of the instrument software.
Operating Instructions vario EL III
Copyright by E l e m e n t a r Analysensysteme GmbH
01/04
Appendix
Page
A-13
Balance
Requirements for the balance: readability of 0.001 mg,
weighing range
to 5,1 g
tara
to 5,0 g
If the balance was not furnished by us, we reserve the right to enter the weights manually.
Possible adjustments to our analyzer have to be made by the customer.
General remarks
The instrument will be installed by a factory trained service engineer and the analytical
performance will be demonstrated by max. 10 standard calibration samples.
In case of specific handling and application questions, you are kindly invited to contact our
representative for assistance. The elaboration of specific operation procedures can be ordered
there against separate charge.
The instrument is calibrated over a standard measuring range from works`side which is stable
for a long time. If specific applications are not within this range, the user can perform an
extended calibration by himself.
Our agent and Elementar will of course assist you at all arising questions.
Please do not hesitate to contact us under:
Service:
Application Lab:
Sales Department:
01/04
+49/6181/91 00-16
+49/6181/91 00-26
+49/6181/91 00-12
Operating instruction vario EL
Copyright by E l e m e n t a r Analysensysteme GmbH
Page
A-14
Appendix
Specifications:
1. Electrical connection values for complete analyzer unit:
Power connection value:
Voltage value:
16A
100V AC
120V AC
230V AC
50/60 Hz
± 10%
± 10%
± 10%
A separate static bonding connection (safety earth) is necessary.
Connector:
1 x connector (customary in place)
Mode of protection: IP 20, installation in dry rooms only.
2. Gas supply:
Emission-free parts should be used in the entire gas supply (copper, stainless steel, etc.)
Pressure reducer:
Output pressure:
0-3 bar
two step precision reducer
Example:
Type AIR LIQUIDE
HSB 315/3
!CAUTION: Pay attention to the bottle pressure!
Necessary gas connection behind the pressure reducers 2 x clamping ring screwing for tube
diameter 6 mm /Swadgelock, Serto)
Initial operation and instructions:
Please make sure that the direct user of the
Instrument is available for instrument delivery
and training over the whole period of time.
If additional instructions or training time by our
service technician are required, they will have to
charge separately.
Operating Instructions vario EL III
Copyright by E l e m e n t a r Analysensysteme GmbH
01/04