Method
APEX INSTRUMENTS, INC.
Method 6 Source Sampler – Model 623 (SK-25 Version)
Operator’s
Manual
METHOD 6
SOURCE SAMPLER
–MODEL MC623
Operator’s Manual
Apex Instruments, Inc.
204 Technology Park Lane
Fuquay-Varina, NC 27526
Phone 919-557-7300 • Fax 919-557-7110
Web: www.apexinst.com
E-mail: info@apexinst.com
Revision No: 2
Revision Date: April 2007
TABLE OF CONTENT
Introduction..............................................5
Appendix A .............................................43
System Description ....................................7
Electrical and Plumbing Diagrams ........... 43
Source Sampler Console ..........................8
Vacuum Subsystem ..............................10
Electrical Subsystem .............................11
Thermocouple Subsystem.....................11
Probe Assembly......................................12
Mini VersaCase.......................................14
VersaCase 2 ...........................................15
Umbilical Cable with Umbilical Adapter...16
Glassware Sample Trains .......................17
Operating Procedures ...........................19
Setup and Check of Source Sampling
System......................................................19
Initial Set-up Procedure ..........................19
System Check.........................................21
Main Power Circuit ................................21
Thermocouple Circuits ..........................21
Pump Power Circuit...............................21
Remote Auxiliary Power Circuit .............21
Elapsed Timer Circuit ............................21
Heater Circuits ......................................21
Initial Sampling System Leak Check.......22
Calibration and Maintenance ................23
Calibration Procedures.............................23
Dry Gas Meter.........................................23
Metering System Leak Check Procedure
..............................................................26
Initial or Semiannual Calibration of Dry
Gas Meter .............................................26
Post-Test Calibration of the Source
Sampler Console...................................28
Calibration of Thermocouples .................29
Initial Calibration of Probe Heater ...........30
Maintenance and Troubleshooting...........31
Source Sampler Console ........................31
Internal Diaphragm Pump .......................31
Dry Gas Meter.........................................33
Optical Encoder.....................................34
Digital Totalizer .......................................35
Program Mode ......................................35
Scale Factors ........................................36
Temperature Controllers .........................37
Probe, Filter and *Auxiliary Setup..........37
Temperature Display...............................38
Temperature Display Setup...................38
Temperature Controllers and Temperature
Display Maintenance...............................39
Pressure Meter Gauge............................39
Thermocouple Wiring and Thermocouple
Display ....................................................40
Electrical Power Circuits .........................41
Sample (Vacuum) Line on Umbilical Cable
................................................................41
Timer.......................................................42
Setup ....................................................42
Appendix B .............................................47
Calibration Data Sheets ........................... 47
Appendix C .............................................49
Applicable Method Procedures ................ 49
Leak-Check Procedures of Non-Isokinetic
Sampling Trains ......................................50
EPA Method 4 Moisture Approximation ..51
EPA Method 6 for Sulfur Dioxide ............52
EPA Method 11 for Hydrogen Sulfide in
Fuel Gas Streams ...................................54
EPA Method 15A for Total Reduced Sulfur
Compounds from Sulfur Recovery Plants in
Refineries................................................56
EPA Method 16A for Total Reduced Sulfur
Compounds.............................................58
EPA Method 18 for Organic Compounds 60
EPA Method 26 for Hydrogen Halides and
Halogens.................................................64
EPA Method 106 for Vinyl Chloride.........67
EPA Method 308 for Methanol ................68
EPA-SW-846 Method for Volatile Organic
Compounds.............................................70
EPA-SW-846 Method for Volatile Organic
Compounds.............................................72
EPA-SW-846 Method for Volatile Organic
Compounds.............................................75
EPA-SW-846 Method 0051 for HCl and Cl2
................................................................80
Appendix D .............................................83
Field Data Sheets..................................... 83
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Chapter
Introduction
The purpose of this manual is to provide a basic understanding of the Apex Instruments Model MC623 Source Sampler Console and gaseous sampling glassware systems. Sections of the manual
include description of sampling system hardware, set-up and system check, calibration procedures,
and troubleshooting and maintenance. Appendices contain electrical diagrams, calibration data sheets,
and specific test method sampling procedures. This manual is based so that a representative gas
samples can be collected according to the procedures established by the United States Environmental
Protection Agency (USEPA) for sampling trains which use midget impinger glassware trains and/or
adsorbent tube or gas bag sampling trains. The Model MC-623 Source Sampler Console and various
glassware sampling systems are applicable for the following test methods and pollutants listed in
Tables 1-1 and 1-2.
Table 1-1. List of US EPA Test Methods Applicable to MC-623 Source Sampler Console
Method No.
Pollutants
4
Stack Gas Moisture (Approximation Method)
6
Sulfuric Acid Mist and Sulfur Dioxide
6A
Sulfur Dioxide, Moisture and Carbon Dioxide
6B
Sulfur Dioxide and Carbon Dioxide
11
Hydrogen Sulfide in Petroleum Refinery Fuel Gas Streams
15A
Total Reduced Sulfur from Petroleum Refinery Sulfur Plants
16A
Total Reduced Sulfur
18
Integrated Bag Sampling for Organic Compounds
18
Adsorption Tube Sampling for Organic Compounds
26
Hydrogen Chloride and Chlorine
106
Integrated Bag Sampling for Vinyl Chloride
308
Methanol
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Table 1-2.
Hazardous Waste Combustion Source Test Methods in EPA-SW-846 Applicable to MC-623
Source Sampler Console
Method No.
Pollutants
0030
Volatile Organic Compounds (VOST)
0031
Volatile Organic Compounds (SMVOC or SuperVOST)
0040
Principle Organic Hazardous Constituents (POHCs) Using Tedlar Bags
0051
Hydrogen Chlorine and Chlorine
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System Description
The Apex Instruments MC-623 source sampling system consists of four (4) main components, shown
in Figure 1-1:
1. Source Sampler Console, which consists of dry gas meter, meter pressure gauge, internal
diaphragm vacuum pump, vacuum pump controls, and electrical controls.
2. Probe Assembly, which includes a probe sheath with glass probe liner, integrated tube heater
and thermocouple.
3. VersaCase sample glassware cabinet, which includes a probe clamp (33.9-mm standard),
monorail/handle bracket, adjustable framing for different types of glassware trains, coolant
reservoir brackets which accommodate standard modular impinger cases, removable front and
rear access doors, and bracket for umbilical and electrical connections.
4. Umbilical Cable, which connects the VersaCase and glassware train with the Source Sampler
Console.
5.
Figure 1-1. Apex Instruments Method 6 Source Sampling System.
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Source Sampler Console
The Source Sampler Console is the operator’s control station that monitors gas sample volume and
temperatures at the sampling location, and controls system sampling rate and system temperatures.
Figure 1-2 illustrates the Apex Instruments Model MC-623 Source Sampler Console’s front panel.
The Model 623 has an electronic digital gas meter display, with a reset function to start each test at
zero.
Figure 1-2. Model MC-623 Source Sampler Console Front Panel.
Assembly in the field is simple. The connections for sample line and Umbilical Cable electrical (4-pin
and thermocouple) are located on the front panel for easy access.
Table 1-3 presents the features and specifications of the MC-623 Apex Instruments Source Sampler
Console. The MC-623 Source Sampler Console has:

Coarse (on/off) and Fine Flow Control Valves make it simple to adjust sampling flow rates.

Dry Gas Meter which reads gas sample volume in liters to three decimal places.

Automatic Temperature Controllers with individual circuit breakers for filter (Method 26),
probe heat and auxiliary are standard equipment.
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
The Temperature Display and 6-channel Thermocouple Selector Switch enable the operator to
monitor temperatures throughout the sampling system.

The Vacuum Gauge reads system vacuum in the range 0-100 kPa (0-30 in. Hg).

The digital Elapsed Timer monitors sampling time in Hours/Minutes/Seconds by the on/off
toggle switch.
The front panel has four (4) latches -- one in each corner -- which unscrew and enable the operator to
pull out the Source Sampler Console from the cabinet using the convenient handle.
Table 1-3. Features and Specifications of Apex Instruments
Model MC-623 Source Sampler Console
Features
MC-623 Source Sampler Console
Gas Meter
Positive displacement diaphragm meter, 45 Lpm
maximum and 0.33 Lpm minimum flow rate
Meter Display
8-digit LCD, push button reset for volumetric
totalizer, factory set 0-99999.999 liter totalizer,
0.003 liter resolution
Temperature
Control
Digital solid-state autotuning controllers with
solid-state power relay external relay, 120
VAC/5A or 220 VAC/3A resistive load
Temperature
Display
3½ digit red LCD display, -200°C to 1250°C
range, 1°C resolution, with external 6-channel
selector switch
Sample Pump
Internal miniature diaphragm pump with 6.0 Lpm
capacity @ free flow conditions and 2.6 Lpm
capacity @ 254 mm Hg
Umbilical
Connections
Electrical: 4 pin Amphenol
Sample Line: 6.35 mm (1/4 inch) quick connect
Dimensions
36.8 x 40.6 x 26.7 cm (14½ x 16 x 10½ inches)
Power
110 V / 60 Hz standard,
220 V / 50 Hz optional
Weight
12.7 kg (28 lb)
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The Source Sampler Console has Vacuum, Electrical, and Thermocouple sub-systems.
VACUUM SUBSYSTEM

The vacuum subsystem consists of a sample inlet quick-connect fitting, Vacuum Gauge,
internal diaphragm vacuum pump assembly, internal fittings, two (2) control valves (Coarse
and Fine), Dry Gas Meter, Meter Pressure Gauge, and pair of orifices controlled by a solenoid
switch. Figure 1-3 is a diagram of the plumbing and gas flow direction.
Figure 1-3. Plumbing Flow Diagram of MC-623 Source Sampler Console.

The Internal Vacuum Pump is a miniature diaphragm-type and provides the vacuum for
extracting the gas sample from the stack and then through the various components of the
source sampling system.

The sample flow rate is controlled by the Coarse Control Valve and the Fine Increase Valve.
The Coarse Control Valve is a ball valve with a 90 handle rotation from CLOSED to full
OPEN. This valve blocks the flow from the SAMPLE INLET quick-connect to the Vacuum
Pump inlet.

The Fine Increase Valve is a needle-type valve with five (5) turns from closed to full open.
The Fine Increase Valve allows flow to re-circulate from the pump outlet back to the pump
inlet. This dual valve configuration enables very precise control of the sample flow rate.

The Dry Gas Meter is a positive displacement diaphragm volumetric totalizer meter with
optical encoder and digital LCD display and reset push button to start each sampling run at
0.000 liters.

A Meter Pressure Gauge (scale 0-100 mm H2O) is used to monitor sampling flow rate.
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ELECTRICAL SUBSYSTEM

The Source Sampler Console is factory-configured for 115 VAC / 60 Hz electrical power.
Configuration for 220 VAC / 50 Hz operation is an available option.

The electrical subsystem provides switch power to each circuit, controlled by seven switches:
MAIN POWER ON, PUMP POWER ON, TIMER ON, SPARE OUTPUT ON, PROBE ON,
FILTER ON and AUXILIARY ON.

All circuits are protected by four (4) front panel mounted circuit breakers. A 15 amp circuit
breaker protects main power, and two 5 amp breakers each protect probe and filter heat
circuits. These circuit breakers detect and interrupt overload and short circuit conditions,
providing an important safety factor. If the circuit breaker opens, or “trips,” indicating
interruption of the circuit, investigate and repair the electrical fault, and then reset the breaker
by pressing the circuit breaker switch. The Electrical Schematic for the Source Sampler
Console is presented in Appendix B.

A 4-pin electrical connection between Source Sampler Console and Umbilical Cable for probe
and filter heater. The pin configuration is presented in the Electrical Schematic in Appendix B.
THERMOCOUPLE SUBSYSTEM

The thermocouple subsystem measures and displays temperatures critical to sampling
operation. The thermocouple system consists of five (5) Type K thermocouples, extension
wires, male/female connectors, receptacles which accept both mini and standard Type K
thermocouple plugs, a 6-channel selector switch and a digital temperature display with internal
compensating junction.

There are automatic temperature controllers for probe and filter heat which receive an input
signal from the electrical subsystem and maintain these temperatures within a close range of
the set point. The temperature controllers are digital programmable temperature controllers.
The thermocouple electrical diagram is presented in the Electrical Schematic.
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Probe Assembly
The Probe Assembly consists of the following:

A probe liner (MPL-36_, where “_” is borosilicate glass (G) standard, quartz (Q), or Teflon
(T)), with several options for probe tip and connection end, and

A stainless steel probe sheath and probe tube heater (MPH-36).
Figure 1-4 illustrates a Probe Assembly. Table 1-4 presents maximum stack gas temperatures for
various probe liner materials. Probe lengths vary from 0.914-m (36-inches) to 1.828-m (72-inches)
nominal length.
Figure 1-4. Probe Assembly for MC-623 Sampling System.
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Table 1-4.
Maximum Stack Gas Temperatures for Probe Liner Materials
Probe Liner Material
Maximum
Temperature
Teflon
177C (350F)
Borosilicate Glass
480C (900F)
Stainless Steel
650C (1200F)
Quartz
900C (1650F)
The Probe Assembly connects to the VersaCase with several connections:

The probe sheath is mounted to the VersaCase using a hinged clamp with wing-nuts that is
attached to the VersaCase.

Extending from the probe assembly is a thermocouple male connector, which connects to
female thermocouple connector of the Umbilical Cable junction box.

An electrical plug connects to the electrical outlet on the Umbilical Cable junction box..

The outlet ball or end of the Probe Liner is inserted through the entry hole of the VersaCase
compartment to connect with the desired sampling train glassware.
Table 1-5 lists available probe sheath and liner materials and maximum allowable stack temperature.
Table 1-5.
Probe Configuration Temperature Ratings
Probe Assembly Configuration
Maximum
Temperature
Stainless Steel Sheath and Glass Liner
480C (900F)
Stainless Steel Sheath and Liner
650C (1200F)
Inconel Sheath and Liner
980C (1800F)
Inconel Sheath and Quartz Liner
980C (1800F)
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Mini VersaCase
The VersaCase (VSB4) is used for support, protection and environmental control of the glassware in
the sampling train. It is a compact, lightweight portable lab frame for supporting complex and variable
glassware configurations. The VersaCase 4 consists of an aluminum cabinet, which is easily
configured for EPA Methods 6 (SO2) and 26 (HCI/CI). The VersaCase 4 features:

Handle and monorail attachment.

Aluminum cabinet with dimensions 16.83 cm deep x 24.13 cm wide x 31.75 cm high (6.625 x
9.5 x 12.5 inches), with overall height of 39.4 cm (15.5 inches).

Adjustable and removable stainless steel hinged probe clamp, (adjustment ±.125 inches).

Dual access doors.

Convenient high strength plastic bracket support the VU-Cord. (Umbilical Cord with Power
Box)
Figure 1-5 VSB4 VersaCase
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VersaCase 2
The VersaCase (VSB2) is used for support, protection and environmental control of the glassware in
the sampling train. It is a lightweight portable lab frame for supporting complex and variable
glassware configurations. The VersaCase consists of an aluminum cabinet with internal pre-punched
panel which is easily configured for various methods. Custom configuration kits are available for EPA
Methods 6 (SO2), 26 (HCl/Cl2), 0030 (VOST), 0031 (SMVOC), and 0040 (bag sampling). The
VersaCase features:

Handle and monorail attachment.

Aluminum cabinet with dimensions 27.9 cm deep x 30.5 cm wide x 61 cm high (11 x 12 x 24
inches), with overall height of 70.5 cm (27¾ inches)

Removable stainless steel hinged probe clamp.

Dual access doors.

Stainless steel guides for sliding on and off a removable impinger case for coolant reservoir
and re-circulation pump (methods with coil condenser).
Figure 1-6 VersaCase2 with pre-punched panel.
Figure 1-7 VersaCase Set-up for Midget Impinger Sampling Train.
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Umbilical Cable with Umbilical Adapter
The Umbilical Cable (VU-30) connects the VersaCase and Probe Assembly section of the source
sampling system to the MC-623 Source Sampler Console. Standard length is 9.14 meters (30-ft), but it
can be ordered in 18.3-m (60-ft) or 27.4-m (90-ft) lengths. The Umbilical Cable contains:

The primary gas sample line, 6.35-mm (¼-inch) with male quick-connect to the Source
Sampler Console and, at the opposite end on the Junction Box, a 6.35-mm (¼-inch) male
swagelok fitting.

Four (4) thermocouple extension cables for type K thermocouples, which terminate with full
size connectors for durability. The connectors have different diameter round pins to maintain
proper polarity, and will not fully connect if reversed. Each thermocouple extension wire in
the Umbilical Cable is numbered for temperature measurement of Probe heat, Filter heat,
Impinger Exit (or VOST adsorbent tube), and Auxiliary (spare).

AC power lines for the heaters in the Probe Assembly and Filter (if used). The power cable
terminates with an amphenol (military style) connector on each end. The body of the
amphenol is the ground conductor. A line-up guide is placed on each connector’s end, and the
retainer threads should be engaged for good contact.

The Umbilical Cable is covered with a woven nylon mesh sheath to restrain the cable and
reduce friction when moving the cable. Multiple Umbilical Cables can be connected together
if needed to reach longer lengths.

The Umbilical Cable junction box connects to the plastic bracket on the VersaCase. This
bracket serves as a strain relief between the Umbilical Cable and the glassware train and Probe
Assembly.
Figure 1-8. VersaCase Umbilical Cable
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Glassware Sample Trains
The sample glassware train contains the glass components necessary for execution of the chosen
sampling method. For example, a US EPA Method 6 train contains the impingers for absorption of
selected pollutants, and connecting glassware pieces. Figure 1-9 illustrates the glassware of the US
EPA Method 6 sampling train.
The order in which a typical USEPA Method 6 glassware train is constructed is as follows:
1. Three-way valve MGN-3 (connects to probe liner’s ball joint)
2. 1st Impinger MGN-1A (modified tip)
3. U-Tube MGN-2
4. 2nd Impinger MGN-1AO (orifice tip)
5. U-Tube MGN-2
6. 3rd Impinger MGN-1A (modified tip)
7. U-Tube MGN-2
8. 4th Impinger MGN-1A (modified tip)
9. Outlet Adapter with thermocouple well and 12/5 socket MGA-100, all held together with
Pinch Clamps (BS-12)
Figure 1-9 USEPA Method 6 Glassware Sampling Train Configuration.
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The order in which a typical US EPA Method 0031 glassware train, shown in Figure 1-10, is
constructed is as follows:
1.
Three-way valve VG-1 (connects to probe liner’s end with GA-15 screw-joint accessories)
and Charcoal Trap VG-6
2.
1st Coil Condenser VG-34 (screw-joints), surgical tubing 9.5-mm for water re-circulation
3.
1st Adsorbent Tube VG-6
4.
Adsorbent Tube Connector 4SC4-PFA (Teflon swage fitting)
5.
2nd Adsorbent Tube VG-6
6.
Water Trap, 40-mL with #15 screw-joints VG-54
7.
FEP Tubing, 6.35-mm x 61-cm
8.
2nd Coil Condenser VG-34 (screw-joints)
9.
3rd Adsorbent Tube VG-6
10.
Drying Tube with glass frit VG-2 (screw-joints)
11.
Vinyl Tubing, 6.35-mm x 61-cm
Figure 1-10 US EPA Method 0031 Glassware Sampling Train Configuration.
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Chapter
Operating Procedures
Setup and Check of Source Sampling System
Carefully unpack the contents, saving the packing material until the parts have been examined for
shipping damage and the sampling system has been completely assembled. Check each item against
the packing list. If any item is damaged or missing, notify your supplier or Apex Instruments
immediately. Table A-1 in Appendix A lists the items in a Source Sampling System that are
recommended for a system check and a spare parts list.
Initial Set-up Procedure
These instructions are for a “dry run” set-up of a midget impinger (USEPA Method 6) sampling train.
Do not load or charge liquids in the impingers. The objective is to set-up the equipment to check
whether everything works.
1. Remove all items from packaging and place in an open area.
2. Slide the Probe Liner into the Probe Assembly making certain the straight end of the Probe
Liner extends approximately 2.54 cm (1 inch) beyond the slotted end of the Probe Assembly.
Attach the ball joint to the Probe Liner using the bored cap and seal. Insert the Glass Wool
plug into the cup end of the Probe Liner as illustrated in Figure 2-4.
3. Place the Probe Assembly in the hinged probe clamp, which is attached to the VersaCase.
Tighten the probe clamp using the wing nut. Carefully insert the ball joint through the hole of
the VersaCase so that the ball end protrudes into the VersaCase allowing the elbow joint to be
readily attached to the ball joint.
4.
Connect the Umbilical Cable’s junction box to the VersaCase by sliding the support rod on the
back of the junction into the VersaCase’s plastic bracket. Plug the Probe Heater electrical
plug into the receptacle marked Probe on the junction box. Plug the probe thermocouple plug
into the thermocouple receptacle on the junction box.
5. Set up the impingers for the method 6 sampling train as illustrated in Figure 2-1. Connect the
U-Tubes to the impingers using the Pinch Clamps that are provided. Place the tray in the base
of the VersaCase and attach the elbow to the ball joint of the Probe Liner to the ball joint of
the first impinger. Complete the setup by attaching the Outlet Adapter (MGA-101) to the ball
joint of the last impinger. The final connection is the Outlet Adapter’s sample line to the
Umbilical Cable junction box, and the Outlet Adapter’s thermocouple to the Umbilical
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Cable’s No. 3 thermocouple receptacle. A diagram of the glassware configuration is shown in
Figure 1-9.
Top View
Figure 2-1. Midget Impingers and Ice Packs in an Insulated Sample Tray.
1. Connect the Umbilical Cable to the Source Sampler Console. Connect the Umbilical Cable
amphenol plug to the amphenol receptacle on the front panel of the Source Sampler Console.
Connect the numbered Umbilical Cable thermocouple plugs into the receptacles on the Source
Sampler Console front panel. Insert the Umbilical Cable sample line male quick-connect into
the Source Sampler Console female quick-connect.
2. Plug the Source Sampler Console into an appropriate electrical power source.
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System Check
Follow the set-up procedure in the previous section before starting system check procedure.
MAIN POWER CIRCUIT
Turn on the main power switch of the Source Sampler Console. The cabinet cooling fan should
operate when the power is switched on.
THERMOCOUPLE CIRCUITS
The temperature indicator display should illuminate and display ambient temperature when the sixchannel selector switch is set to 6 -- METER. Plug a single thermocouple into each of the five
thermocouple receptacles and dial the six-channel selector switch to each of the other five positions
and check for correct ambient temperature.
PUMP POWER CIRCUIT
Turn on the PUMP POWER ON switch to activate the pump motor. After hearing that it works, turn
the pump off.
REMOTE AUXILIARY POWER CIRCUIT
Plug in a test light or some other electrical test source into the REMOTE AUX receptacle on the lower
left corner of the front panel. Turn on the REMOTE AUX ON switch to activate the circuit and check
that power is supplied. (Controlled by Solid State Relay.)
ELAPSED TIMER CIRCUIT
The timer will begin to count when the TIMER ON switch is turned on and stops when the switch is
turned off. The display is reset to zero with a push button on the face of the timer display. The timer
is factory-set to read hour/minutes/seconds but can read minutes and tenths of minutes if specified in
the purchase order.
HEATER CIRCUITS
Turn on the power switches for the filter heater “FILTER ON” (only for USEPA Method 26 and
EPA-SW-846 Methods 0040 and 0051) and the probe heater “PROBE ON.” The indicator lights on
the automatic temperature controllers will illuminate and read ambient temperature. Adjust the
Temperature Controllers to approximately 120C (248F) and check the temperature display to verify
if the heaters are working. The procedure is as follows:
1.
Press and hold the SET button. (To set Heater Circuit Setpoint.)
2.
Press one of the arrow keys to alter the setpoint either upward or downward.
3.
Release SET to complete the change.
4.
Then turn off the filter and probe heaters.
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Initial Sampling System Leak Check
Apex Instruments, Inc. recommends that a leak check of the Source Sampler Console be conducted,
followed by a system leak check. The Source Sampler Console leak check and the system leak check
are to be “dry” runs as described.
1. Close the Coarse Valve (clockwise) and the Fine Control Valve (counter clockwise) on the
Source Sampler Console.
2. To conduct the Source Sampler Console leak check, insert a male quick-connect, with rubber
stopper into the SAMPLE INLET. In order to conduct the system leak check, insert a rubber
stopper into the probe inlet.
3. Turn on the Vacuum Pump -- marked PUMP POWER ON.
4. Slowly open the Coarse Valve to the full open position, and increase the Fine Increase Valve
(clockwise).
5. The pump vacuum, as indicated on the Vacuum Gauge, should read a system vacuum within
25 kPa (6-in Hg) of the barometric pressure. For example, if the barometric pressure is 100kPa (30-in Hg), then the Vacuum Gauge should read at least 75-kPa (23-in Hg).
6. Turn the Fine Increase Valve back (counter-clockwise), and slowly release the plug or seal.
Then turn off the Vacuum Pump.
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Chapter
Calibration and Maintenance
Calibration Procedures
Test results from a stack emission test are meaningless without calibration of the sampling and
analytical equipment components. The creation and maintenance of a regularly scheduled calibration
and record keeping program are critical to conducting any stack testing program. Without calibration,
sampling cannot be verified as having been conducted accurately.
Components of the MC-623 sampling system which require calibration are:
1. Dry Gas Meter.
2. Thermocouples (dry gas meter and sampling train components) and Digital Temperature
Indicator
Table 3-1 presents a summary of the calibrations required, equipment used for calibration, acceptance
limits, calibration frequency and actions required if calibration fails to meet acceptance limits.
Dry Gas Meter
The MC-623 Source Sampler Console’s dry gas meter is calibrated using the calibration procedures
contained in US EPA Method 6 (Sections 5.1.1 and 5.1.2), EPA-SW-846 Method 0051 (Sections
7.1.1.1 and 7.1.1.2), and in Handbook: Quality Assurance/Quality Control (QA/QC) Procedures for
Hazardous Waste Incineration, EPA/625/6-89/023 (Appendix A for EPA-SW-846 Method 0030).
An initial or full calibration is conducted at three (3) selected flow rate (Pm) settings for each flow
Orifice and with at least 5.0 liters of gas metered. The initial calibration should occur once every 6
months or if the results of a post-test 3-point calibration show that the dry gas meter calibration factor
(Y) has changed by more than 5% from the pre-test calibration value. The calibration factor (Y)
results for an initial calibration should fall within the interval Y  0.02Y, where Y is the average for all
three calibration runs.
Post-test calibrations use an abbreviated calibration procedure (described in Section 5.1.2 of US EPA
Method 6) with two independent calibration runs at a single intermediate flow rate (Pm) setting
corresponding to the test sampling flow rate, and with at least 3.0 liters of gas metered. Post-test
calibrations should be conducted after each field test series or quarterly, whichever is less. The tester
always has the option of conducting a more rigorous calibration check.
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Table 3-1.
Sampling System Equipment Calibration and Frequency
Calibrated
Against
Acceptance
Limits
Dry Gas Meter
1. Wet Test Meter
2. Secondary
Reference DGM
Yi = Yavg 
0.02Yavg
Semiannually
Recalibrate,
repair or
replace
Post-test 2-point
1. Wet Test Meter
2. Secondary
Reference DGM
Y = Y  0.05Yavg
After each
field test
Recalibrate at
3-points per
orifice and
 5.0 L
Pressure Meter
Measured during
DGM calibration
None; create curve
of Meter Pressure
vs. flow rate in
standard L/min
With DGM
Repair or
replace
Thermocouples
and Digital
Indicator
Certified Hg-inglass thermometer
in ice slush and
boiling water
Stack: 1.5% K
DGM: 3C
Filter: 3C
Exit: 1C
After each
field test
Recalibrate,
repair or
replace
Component
Frequency
Action If
Unacceptable
A wet test meter is used to calibrate the dry gas meter of the Source Sampler Console. It also must be
calibrated and have the proper capacity. The wet test meter should have a capacity of at least 1.0
L/min. No upper limit is placed on the capacity; however, a wet test meter should make at least one
complete revolution at the specified flow rate for each of the three independent calibration runs. Wet
test meters are calibrated by the manufacturer to an accuracy of  0.5%. Calibration of the wet test
meter must be checked about every two years. A certificate of its calibration should be maintained in
the quality assurance record keeping system.
Alternatively, a secondary dry gas meter which has been calibrated against a wet test meter or bell
prover liquid positive displacement technique and which remains in the laboratory may be used for
calibration.
Section 7.2 of Method 6 allows the use of critical orifices for volume and sampling rate
measurements. Basically, the procedure requires a calibration with a bubble flow meter before and
after each test run. For the volume measurement to be valid, the before and after flow rates must
agree to within ±5.0%. Method 6 currently does not specifically allow the use of critical orifices as
calibration standards for its metering system as does Method 5.
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Main
Powe r
Pump
Power
Timer
Spare
Out put
Probe
Filter
Temperature
Aux
OPEN
OPEN
Probe
Filter
Aux.
Fine
Increas e
Meter Volume Lite rs
Elapse d Time
00000
-15
-10
60
-20
20
50
0
30
40
20
-5
70
-30
40
60
80
0
10
-25
Flow
Contro l
10 0
0
0
mm of wat er
Vacuum
Meter Pre ssure
Coarse
Ope n
3
1. Probe
2. Filter
3. Aux
4.
2
4
Closed
5
1
6
Temperature Selection
Model 623 Source
Sampler
Sample
OPEN
Spare
Output
Remove
OPEN
CAUTION
Risk of Electric
Shock
115 VAC-60HZ
Figure 3-1. Diagram of Source Sampler Console Calibration vs. Wet Test Meter.
In calibrating the Source Sampler Console, the operator is determining the dry gas meter calibration
factor (Y), which is the ratio of accuracy of the wet test meter’s (or secondary reference dry gas
meter’s) volume measurement to the dry gas meter volume measurement, all corrected to standard
conditions. Note: US EPA standard conditions are 20C (293K) and 760 mm Hg. The equation for
the calibration factor (Y) is:
Yi =
Where Vw
Vw t d +273Pbar
P 

(Vdf -Vdi )(t w +273) Pbar + m 
13.6 

= Volume measured by wet test meter, L
td
= Average temperature of dry gas meter, C
Pbar
= Barometric pressure at the meters, mm Hg
Vdf
= Final volume measured by the dry gas meter, L
Vdi
= Initial volume measured by the dry gas meter, L
tw
= Average temperature of wet test meter, C
Pm
= Pressure drop across the dry gas meter, mm H2O.
Both the initial and post-test calibration procedures are described here. Prior to conducting a
calibration run, the Source Sampler Console should be leak-checked.
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METERING SYSTEM LEAK CHECK PROCEDURE
Figure 3-2 shows a plumbing diagram of the MC-623 Source Sampler Console. Leak-check the
metering system (drying tube, Fine control valve, pump, pressure meter, and dry gas meter) as
follows:
1.
Temporarily attach a suitable rotameter (air flow range of 0-40 cc/min) to the outlet of the dry
gas meter, and place a vacuum gauge at the inlet of the drying tube.
2.
Plug the drying tube inlet. Turn on the pump, open the Coarse control valve and close (FINE
INCREASE) the Fine control valve to pull a vacuum of at least 34 kPa or 250 mm Hg (10 in.
Hg).
3.
Close the Coarse control valve, and note the flow rate as indicated by the rotameter.
4.
A leak of < 0.02 L/min (20 cc/min) must be recorded or leaks must be eliminated.
5.
Carefully release the vacuum gauge before turning off the pump.
Figure 3-2. MC-623 Source Sampler Console Plumbing Diagram.
INITIAL OR SEMIANNUAL CALIBRATION OF DRY GAS METER
The Source Sampler Console and dry gas meter are calibrated by connecting the Source Sampler
Console to a wet test meter or secondary reference dry test meter, according to the set-up shown in
Figure 3-1. A series of five (5) calibration runs are conducted using Flow Meter for desired flow
settings between .25 to 4 Lpm. For the initial or full recalibrations, at least 5.0-L of gas must pass
through the dry gas meter during each calibration run.
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If a wet test meter is used as the calibration standard, it should have a meter correction factor of 1.000.
Alternatively, a properly calibrated secondary reference dry gas meter may be used to calibrate the
Source Sampler Console’s dry gas meter. Use the following procedure:
1.
Before starting the calibration, fill out a meter calibration data sheet (can be a computer
spreadsheet) as shown in Appendix C. Record barometric pressure at the start of
calibration, the Source Sampler Console and wet test meter identification numbers, date
and time of calibration, and confirmation of acceptable leak checks on the Source Sampler
Console.
2.
Connect the outlet of the wet test meter to the inlet (SAMPLE INLET) of the Console
Meter, as shown in Figure 3-1. Connect the inlet side of the wet test meter to a saturator
(reverse impinger with water), which is open to atmosphere. Note: Do not use a drying
tube.
3.
Turn on the pump and adjust the Coarse and Fine control valves on the Source Sampler
Console to set the flow rate at about 1-L/min. Allow both meters to run in this manner for
at least 15 minutes to let the meter stabilize and the wet test meter to wet the interior
surfaces.
4.
Turn off the pump.
5.
Record initial settings of dry gas meter volume reading, wet test meter volume reading,
dry gas meter temperature, and wet test meter temperature.
6.
Start the pump and quickly adjust the Pressure Meter to the desired setting. Start the
Elapsed Timer on the Source Sampler Console at the same time that the pump is started.
7.
Let the pump run until a dry gas volume of at least 5.0-L is indicated by the dry gas meter.
Allow the calibration run to continue until the next minute elapses, then stop the pump
and Elapsed Timer.
8.
Record the final dry gas meter volume reading, wet test meter volume reading, dry gas
meter temperature, and wet test meter temperature. Calculate the dry gas meter and wet
test meter volumes by subtracting initial readings from final readings. Calculate the
average dry gas meter and wet test meter temperatures.
9.
Repeat the calibration run at each successive setting on the Pressure Meter. Suggested
values are 80, 50-60, and 20-35 mm H2O, recording same data as before.
10.
At the conclusion of the two sets of three calibration runs, calculate the average Y (ratio of
accuracy of the wet test meter to the dry gas meter). The tolerance for individual Y values
is  0.02 from the average Y. If a value in this range is not obtained, the orifice opening
should be adjusted or replaced, or the dry gas meter may require servicing.
11.
If the Y is acceptable, record the values on a label on the front face of the Console Meter,
and use for subsequent test runs. Plot the Pressure Meter reading for each calibration run
vs. the standardized flow rate in L/min, to develop a calibration curve for sample flow
rate, as shown in Appendix C. The completed forms should be forwarded to the
supervisor for approval and filed in the calibration log book.
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POST-TEST CALIBRATION OF THE SOURCE SAMPLER CONSOLE
A post-test, or 2-point, calibration of the Source Sampler Console should be conducted after each trip
to and from the field or test series to ensure that the dry gas meter correction factor (Y) has not
changed by more than 5%. A post-test calibration check is conducted with at least 3.0-L of gas run
through the dry gas meter. The Console Meter leak check is not conducted because a leak may be
corrected that was present during the test series. Use the following procedure:
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
Before starting the calibration, fill out a meter calibration data sheet (can be a computer
spreadsheet) as shown in Appendix B. Record barometric pressure at the start of
calibration, the Source Sampler Console and wet test meter (or secondary DGM)
identification numbers, and date and time of calibration.
Connect the outlet of the wet test meter to the inlet (SAMPLE INLET) of the Console
Meter, as depicted in Figure 3-1. Connect a saturator to the wet test meter inlet.
Turn on the pump and adjust the Coarse and Fine control valves on the Source Sampler
Console to set the flow rate at about 1-L/min. Allow both meters to run in this manner for
at least 15 minutes to let the meter stabilize and the wet test meter to wet the interior
surfaces.
Record initial settings of dry gas meter volume reading, wet test meter volume reading,
dry gas meter temperature, and wet test meter temperature.
Start the pump and quickly adjust the Pressure Meter to the average setting used for the
test series. Start the Elapsed Timer on the Source Sampler Console at the same time that
the pump is started.
Let the pump run until a dry gas volume of at least 3.0-L is indicated by the dry gas meter.
Allow the calibration run to continue until the next minute elapses, then stop the pump
and Elapsed Timer.
Record the final dry gas meter volume reading, wet test meter volume reading, dry gas
meter temperature, and wet test meter temperature. Calculate the dry gas meter and wet
test meter volumes by subtracting initial readings from final readings. Calculate the
average dry gas meter and wet test meter temperatures.
Repeat the calibration run at same setting on the Pressure Meter.
Calculate the percent change in the meter calibration factor Y.
If the calibration factor Y does not deviate by more than 5%, then the dry gas meter
volumes obtained are acceptable, and continue to use the initial Y-value on the faceplate.
If the dry gas meter Y values obtained before and after the test series differ by more than
5%, the test series shall be either voided, or calculations for the test series shall be
performed using the lower Y value (gives lower sample volume, therefore higher
concentration values).
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Calibration of Thermocouples
Apex Instruments suggests the following procedures for calibrating thermocouples and temperature
display readouts. Thermocouples should be checked for calibration at three temperatures, for
example, ice-point and boiling point of water and ambient temperature. Thermocouples such as the
stack gas thermocouple which are used at higher temperatures than boiling water can be checked for
calibration using a hot oil bath. Another more modern technique is to use a Thermocouple Simulator
Source (M5C-22), as shown in Figure 3-3. The M5C-22 can calibrate without external compensation
or icebaths, with a temperature range from 0 to 2,100F in divisions of 100F for 22 precise test
points.
A temperature sensor calibration form is provided in Appendix C. Acceptable reference materials are:

ASTM mercury-in-glass reference thermometers.

NIST-calibrated reference thermocouples/potentiometers.

Thermometric fixed points, e.g., ice bath and boiling water.

NIST-traceable electronic thermocouple simulators.
Thermocouple Calibration procedure as follows:
1.
Prepare an ice-water bath in an insulated container (such as the Cold Box).
2.
Insert the thermocouple and a mercury reference thermometer into the bath.
3.
Allow the readings of both to stabilize, and record the temperatures on a thermocouple
calibration data sheet, as shown in Appendix C.
4.
Remove the thermocouple and allow it to stabilize at room temperature.
5.
Insert again the thermocouple into the bath, and record another reading.
6.
Repeat Steps 4 and 5.
7.
Calculate the average of the thermocouple readings and the average of the reference
thermometer readings. The averages should differ by less than 1.5% of the absolute
temperature (K) for the stack thermocouple.
1.
Place a beaker of distilled water on a hot plate, add a few boiling chips and heat to
boiling.
2.
Repeat Steps 2 through 7 as above.
1.
Set both the thermocouple to be checked and a mercury reference thermometer
side-by-side at ambient temperature.
2.
Repeat Steps 2 through 7 as above.
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1.
Place a container of oil on a hot plate and heat to a temperature below the boiling point.
DO NOT BOIL.
2.
Repeat Steps 2 through 7 as above.
Additional calibration procedures are performed on the temperature display. To check the linearity of
the temperature display, a thermocouple simulator (Apex Model M5C-22) is used. Connect the
simulator to the temperature display, as illustrated in Figure 3-3, and record on a calibration data sheet
the display reading at each temperature setting.
Figure 3-3. Thermocouple Simulator for Temperature Display Calibration Check.
Initial Calibration of Probe Heater
Apex Instruments calibrates the probe heater assembly before shipping according to procedures
outlined in USEPA APTD-0576. Probes are constructed according to specifications given in USEPA
APTD-0581, which is the original 1971 document entitled “Construction Details of Isokinetic SourceSampling Equipment,” by Robert M. Martin (available from National Technical Information Service
(NTIS) as document PB-203 060). The procedure in APTD-0576 involves passing heated gas at
several known temperatures through a probe assembly, and monitoring and verifying that the probe
assembly is capable of maintaining 120C  14C.
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Maintenance and Troubleshooting
Setting up and adhering to a routine maintenance program will help to ensure trouble-free operation of
the source sampling system. In addition, a carefully documented maintenance and calibration system
will help to assure that accurate results are obtained during stack testing activities. The following text
describes maintenance and troubleshooting procedures for the various subsystems of the MC-623
Source Sampler Console and sampling system.
Source Sampler Console
To inspect the inside components of the Source Sampler Console, make sure the power cord is
disconnected. Remove the front panel and tray from the cabinet by turning the four panel latches (in
corners of front panel) counterclockwise with your fingers or a flathead screwdriver until the latch
releases. Slide out the panel using the handle at the bottom-center of the faceplate. Once the panel is
partially pulled out, reach inside and disconnect (unplug) the fan wire from the fan assembly. Visually
inspect all of the mechanical and electrical components. Clean any accumulated dust off the
components.
Internal Diaphragm Pump
The Gast micro diaphragm pump (Model 15D AC) is an oil-less pump which never requires
lubrication. The sealed bearings are grease-packed. The required ambient temperature is 0 to 40C
(32 to 105F). For operation at temperatures outside this range, it is prudent to store the Source
Sampler Console in a warmed or cooled environment before use in source testing. The service life of
the diaphragm and head gasket will be reduced by petroleum or hydrocarbon products. Remember:
The pump is designed for pumping clean, dry air. Protect it against entrance of dirt, excessive
moisture and chemical contamination, and you will receive years of trouble-free service.
Figure 3-4 is an exploded view diagram of the Model 15D AC vacuum pump, with parts identified.
Servicing can include cleaning and replacement of the diaphragm and/or head assembly. Do not
attempt to replace the Connecting Rod or Motor Bearings. If after cleaning the unit and/or installing a
new diaphragm or head assembly, the unit still does not operate properly, contact Apex Instruments
and return the pump for repair or replacement. Before servicing, always disconnect the pump’s power
source before servicing, and always vent all air lines to the pump to remove pressure. Failure to do so
can result in personal injury and/or property damage.
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Head Screws
Head
Valve
Motor
Valve Plate
Fan
Retainer Plate
Diaphragm
Ground
Wire
Connecting
Rod Assembly
Bracket
Base
Figure 3-4. Diagram of Model 15D AC Mini Diaphragm Vacuum Pump.
Follow these steps to replace the diaphragm:
1.
Disconnect the pump from electrical service.
2.
Vent all air lines to the pump to remove pressure.
3.
Label the ports noting the direction of the arrows so you can orient the pump head
correctly during reinstallation.
4.
Remove the four corner head screws and remove the head, valve and valve plate. Remove
flat head screws on retainer plate.
5.
Remove the retainer plate and diaphragm.
6.
Clean the pump head and retainer using water-based solvents. CAUTION: Do not use
petroleum-base compounds, acids, caustics or chlorinated solvents to clean or lubricate
any parts. It will reduce the service life of the pump.
7.
Re-attach the retainer plate and diaphragm to rod with flat head screw. Torque to 0.09 kgmeters (8 inch-lb.). CAUTION: Do not overtighten head screw(s). To do so will damage
unit and will reduce performance.
8.
NOTE: Re-assemble the valve plate, valve and head as a unit before re-installing onto the
pump. These three parts assemble together in a single orientation. Once the parts are
assembled, place back onto the pump in the same orientation as before disassembly.
9.
Make certain the diaphragm lines up with the four screw holes, then re-install the valve
plate, valve and head. Tighten 4 head screws to 0.045 kg-meters (4 inch-lb.).
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The troubleshooting guide for the diaphragm pump is as follows:
SYMPTOM
POSSIBLE CAUSE
Won’t Start
-Electrical connection
-Dirty muffler
-Wrong or low voltage
-Pressure/vacuum on head
-Thermal overload tripped
-Too cold
-Ensure electrical power is supplied
-Is muffler clogged?
-Inspect power supply
-Inspect relief valve
-Inspect above points
-Check ambient temp
-Check plug or wire connection
-Replace muffler
-Apply proper voltage
-Reset or replace relief valve
-Replace unit
-Warm Source Sampler Console
-Wrong voltage
-Plumbing leak
-Check valve leaks
-Inspect power supply
-Inspect hoses for cracks
-Inspect check valve
-Apply proper voltage
-Replace hose
-Repair or replace check valve
Overheating
-Dirty filter
-Dirty muffler
-Low voltage
-Dirty valves
-Inspect filter
-Is muffler clogged?
-Inspect power supply
-Remove head and inspect valve
-Replace filter
-Replace muffler
-Apply proper voltage
-Clean/replace valve
Low Pressure
or
Low Vacuum
-Dirty filter
-Dirty muffler
-Low voltage
-Wrong AC voltage frequency
-Damaged or contaminated
diaphragm
-Dirty valves
-Inspect filter
-Inspect muffler
-Inspect power supply
-Inspect power supply
-Remove head and valve plate, inspect
diaphragm
-Remove head & inspect valve
-Replace filter
-Replace muffler
-Apply proper voltage
-Supply proper electrical power
-Replace diaphragm
Excessive Noise
POINT TO CHECK
REMEDY
-Clean/replace valve
Dry Gas Meter
The dry gas meter, shown in Figure 3-5, are not field adjustable. The routine maintenance consists of
performing the required periodic calibrations and calibration checks, described in Chapter 3.1. If the
dry gas meter fails repeatedly to calibrate against a wet test meter, then return the meter to Apex
Instruments or the factory for repair.
Optical
Digital
Figure 3-5. Dry Gas Meter (SK-25) with Digital Totalizer.
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OPTICAL ENCODER
To check the Optical Encoder follow the following guidelines:
Figure 3-6 SK-25 Dry Gas Meter with Optical Encoder
1. Disconnect Inlet and Outlet plumbing.
2. Remove screw from bracket underneath the floor panel.
3. Carefully pull meter back away from front panel and undo Optical Encoder wires.
4. Unscrew the four (4) plate screws and remove front plate.
5. Loosen first set screw and pull out Encoder.
6. Reconnect Encoder wiring making sure the wire colors are in the correct order.
7. Spin Optical Encoder armature and look at totalizer to see if any movement (increase for
forward movement and decrease for backwards movement.) If this movement occurs the
Encoder is working properly. If it does not, retrace wires per schematic in Appendix A of this
manual, and verify wiring is correct.
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Digital Totalizer
PROGRAM MODE
To enter the program mode, a connection must be made between terminals #1 and #5 on the back of
the totalizer. It is common to use a wire with alligator clips on each end to make this connection.
There are four program-mode screens. Upon making the connection between the terminals, the
totalizer will display screen 1 – Count Scale Factor. Press and hold the
key while repeatedly
key to advance to successive programming screens, as described in the following
pressing the
table:
Programming Screens
Screen
Function
1
Count Scale Factor
2
Count Decimal Point
3
Reset to Offset Value
4
Reset Key Enable/Disable
Screen 1 – Count Scale Factor
The count scale factor is used to convert the incoming count pulses to the desired unit of measure to
be displayed (cubic feet, cubic meters, liters, etc.). The Totalizer Scale Factor can be located on the
Apex Instruments Source Sampler Console Calibration Sheet.
1. The far right digit will be flashing upon making the connection between the terminals. Press
the
key until reaching the desired digit value. Note: Pressing and holding the
key
will cause the numbers to auto-scroll.
2. Press the
key to move the flashing digit one place to the left. Change this digit to the
desired value with the
key. Repeat this process until all digits are set correctly.
Screen 2 – Count Decimal Point
The scaler has six digits available with a user-defined fixed decimal point. The second screen is used
to enter the decimal point display on the totalizer screen. Press and hold the
key and then press
the
key to move from Screen 1 to Screen 2.
Press the
key to move the decimal point to the desired position.
Screen 3 – Reset to Offset Value
Do not make any adjustments to this field. The LCD should read P000.000.
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Screen 4 – Reset Key Enable/Disable
The fourth screen in the program mode allows the user to enable or disable the front panel (Zero)
Reset Key.
1. This program is ENABLED (R) as shipped from Apex Instruments, Inc. This allows the user
to re-zero the totalizer using the
key at any point. To change this setting (No R), press
key while in the programming mode.
the
2. The reset terminal on the rear panel is still active when the front reset button is disabled.
To Exit Programming Mode
Break the connection between terminals #1 and #5.
Your totalizer is now ready to be calibrated to the Source Sampler Console.(see Ch. 4 Calibration
Procedures, section Initial or Semiannual Calibration of Dry Gas Meter, pg 20.)
SCALE FACTORS
For Calibration Factor Y, the ratio of the reading of the calibration meter to the dry gas meter,
acceptable tolerance of individual values from the average is ±0.02. If the value range is not obtained
you must calculate a new Count Scale Factor as follows:

Multiply the Nominal Count Scale Factor programmed into the Totalizer by the Meter
Calibration Factor. For example, if the Meter Y was 0.98, then:

(CS)new = (CS) nominal X Y

(CS)new = 1.35000 x 0.98

Program (CS)new into the Totalizer (reconnect jumper wire and program.)

Record the Count Scale Factor (CS)new on the Meter Calibration Sheet, and proceed with the
rest of the Meter Calibration as usual.
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Temperature Controllers
The Temperature Controllers for probe, filter box heat and auxiliary (PROBE, FILTER and AUX on
front panel), after setting temperature to the desired setpoint, receive a signal from the thermocouple
subsystem and maintain these temperatures within a close range of the setpoint. The standard
Temperature Controllers on the Model MC-623 are digital devices with push-button controls.
Although they can perform many programmable functions, these Temperature Controllers have been
pre-programmed and then “locked out” to perform only the functions required by the Source Sampler
Console and source sampling system.
PROBE, FILTER AND *AUXILIARY SETUP
1. Set the Setpoint.
a. Push and hold set key.
b. Use up or down key to change value to 121.
2. Set CNF9
a. Push up and down keys together until Aut is displayed.
b. Push down key until CNF9 displays.
c. Push set key and hold. Push up or down to change to YES.
d. Release key. IN will be displayed.
e. Push set key and hold. Push up or down until H is displayed. Release key.
f. Push down key to display C_F.
g. Push and hold set key and up or down until display reads °C.
h. Push up or down until dISP is displayed.
i. Push set key and hold. Push up or down until AcSP is displayed.
* To use Auxiliary as secondary output circuit follow the following procedure:
1. Set the setpoint as in 1b above.
2. Change the Thermocouple setpoint value to a number above the outside ambient temperature
(i.e. 426°).
3. Place a thermocouple bridge in AUX thermocouple panel jack.
Thermocouple
Bridge
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Temperature Display
The Temperature Display (TEMPERATURE on front panel) for thermocouple inputs was also a
temperature controller, but has been programmed and “locked out” to be used only as a temperature
display.
TEMPERATURE DISPLAY SETUP
1. Set CNF9
a. Push up and down keys together until Aut displays.
b. Push down key until CNF9 displays.
c. Push set key and hold. Push up or down to change to YES.
d. Release key. IN will be displayed.
e. Push set key and hold. Push up or down until H is displayed. Release key.
f. Push down key to display C_F.
g. Push set key and hold. Push up or down until display reads °C.
h. Push down key until Ot2 is displayed.
i. Hold set key and push up or down key until t 75 is displayed.
j. Push down key until tI 7 is displayed
k. Push set key and hold. Use down key to get to dLon.
l. Release keys and red light beside the #2 should be on.
m. Set disp on Temperature Display to AC.
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Temperature Controllers and Temperature Display Maintenance
Maintenance consists of removing the front panel from the cabinet, and making sure the electrical
contacts are free from dirt, dust and moisture.
If you see an Error Code on the display:
1. Be aware that most errors are input (sensor) related.
2. Read the table below and follow its recommendations:
Display
Probable Cause
Recommended Action
Er 1
Reversed thermocouple connection + to -
Change the sensor leads on Terminals 1 and 2.
Er 2
Sensor type mismatch or open RTD.
Check RTD, replace as necessary.
Er 3
Sensor type mismatch.
Check selection of sensor.
Er 4
No thermocouple, open thermocouple,
bad connection, or broken wire.
Check the sensor, replace or repair as
necessary.
Er 5
Electrical noise.
Cycle power to system. See if error clears.
Check system for electrical interference.
No
Display
Control is inoperable.
Check for line voltage at terminals 7 and 8.
Pressure Meter Gauge
No lubrication or periodic servicing is required for the Pressure Meter Gauge. Keep the case exterior
and cover clean. Occasionally disconnect pressure lines to vent both sides of the gauge to atmosphere
and re-zero. The gauge is calibrated and zeroed in the vertical position at the factory.
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Thermocouple Wiring and Thermocouple Display
The most commonly used thermocouple (TC) in stack testing applications is the Type K. Calibration
guidance is given by the USEPA in Emission Measurement Technical Information Center (EMTIC)
Guidance Documents GD-024 and GD-028. A Type K TC, even with large wire gauge sizes, will
eventually fail if subjected to sustained temperatures  1,090C (2,000F). Even short excursions will
shorten the useful life of the TC. Other types of TCs should be considered for sustained temperatures
above 1,090C.
TC Wire Not
Functioning Properly
Check to see if TC leads have not detached from screw posts inside TC plugs or
receptacles. This causes an open TC circuit when there is NO junction and reads “ER 4”
on the temperature display. This condition occurs when there is no device connected to
that channel, or when one of the wires in the circuit has broken or become disconnected.
TC Reads Lower
Value Than Expected
Under-reading is usually caused by second unintended junction in TC circuit, such as a
short in one wire (TC display reads average of two junctions). The most common place
for the short is in connectors, with unintended junction reading ambient temperature.
Quick check is to disconnect TC at connection farthest away from Source Sampler
Console. If display reads “ER 4” for an open circuit, then there is NOT a short in the
extension circuit. Check connector on the measuring device.
TC Display
Susceptible to Static
Electricity
When sampling hot dry gas across probe, ground with a grounding strap the either the
Probe Assembly (to the stack) or make sure the Umbilical Cable always connected.
TC Selector Switch
Clean contacts of accumulated dust periodically with electrical switch spray cleaner.
Check switch connections by connecting TC simulator to each receptacle on faceplate
and verifying that each channel reads temperature selected by simulator. Note: TC
attached to outlet of DGM is wired directly to selector switch and should read ambient
temperature.
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Electrical Power Circuits
Electrical power circuits include the Probe Assembly, Umbilical Cable and Junction Box, and Source
Sampler Console connections.
Amphenol Outlet on
Source Sampler
Console
Check the Amphenol outlet with a voltmeter or check light by connecting the leads to the
different terminals (see Electrical Schematic in Appendix B). When connected across
heater lines, voltmeter or check light should respond correspondingly. Solid-state
temperature controller circuits should be tested with a resistant load, such as test lamp or
heater.
Umbilical Cable
Check the electrical lines of the Umbilical Cable for continuity using an ohmmeter or
battery-light system. If there is no continuity in any of the lines, check the Amphenol
connectors. If this not the problem, replace the cord.
Connect the Umbilical Cable to the Source Sampler Console. Check the Umbilical Cable
outlet with a voltmeter by connecting the leads to a combination of the four pins: Pin A is
110/220 VAC for auxiliary power, Pin B is common neutral, Pin C is 110/220 VAC for
filter heat, and Pin D is 110/220 VAC for probe heat. Voltmeter should respond properly
when Amphenol is wired correctly and appropriate switches are thrown. Check ground
continuity wire with an ohmmeter between Amphenol body and electrical plug ground
pin. Ohmmeter should read less than 1 ohm.
Junction Box
Check the electrical heater receptacles with a check light for continuity.
Probe Assembly Tube
Heater
Inspect electrical connections to the tube heater and power cord for visible shorts or
burned spots in the high-temperature insulation. Connect power cord into suitable power
source and monitor temperature. Probe should become warm to touch over its entire
length in a few minutes. If probe does not heat, check power source for proper voltage
and loose connections in plug. Shorts are indicated by partial heating in rear section of
probe. Breaks in heating element and connections can be checked with an ohmmeter or a
battery-light system. Replace probe tube heater, if necessary.
Sample (Vacuum) Line on Umbilical Cable
Check the quick-connects and vacuum line on the Umbilical Cable as follows:
Quick-Connects
Wipe vacuum line and pitot line quick-connects clean before attaching to Source Sampler
Console. Mating quick-connects should be joined together when not in use to prevent
damage and dirt. A drop of penetrating oil on each keeps them in good working
condition.
Vacuum Line
Test vacuum line for leaks by plugging inlet with a 6.35-mm (-inch) quick-connect plug
and connect line to Source Sampler Console. Conduct leak-check by pulling vacuum. If
leakage is noted, check all connections first and then, if necessary, inspect the tubing
(look for crimps). If cause is not readily identified, slightly pressurize the line and check
for leaks using soapy water.
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Timer
SETUP
Figure 3-7 MC-T Timer Setup
Reset button (RST) is on the front of the unit. All timers are set by Apex Instruments to HMS (Hours,
Minutes, Seconds). Timers can be set to customer’s specifications.
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Appendix A
Electrical and Plumbing Diagrams
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Appendix B
Calibration Data Sheets
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Appendix C
Applicable Method Procedures
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Leak-Check Procedures of Non-Isokinetic Sampling Trains
A.
Procedure A
1.
If sampling train does not have a vacuum gauge, temporarily place a vacuum gauge at or
near the probe inlet. Otherwise, use Source Sampler Console’s existing vacuum gauge.
2.
Plug the probe inlet (or other specified point), and pull a vacuum of  255 mm Hg (10 in.
Hg).
3.
The vacuum must remain stable for  30 seconds.
4.
Carefully release the probe inlet plug before turning off the pump.
B.
Procedure B
1.
If sampling train does not have a vacuum gauge, temporarily place a vacuum gauge at or
near the probe inlet. Otherwise, use Source Sampler Console’s existing vacuum gauge.
2.
Plug the probe inlet (or other specified point), and pull a vacuum of  255 mm Hg.
3.
Note the time rate of change of the DGM dial (must be  2% of average sampling rate).
4.
Carefully release the probe inlet plug before turning off the pump.
C.
Procedure C
1.
If sampling train does not have a vacuum gauge, temporarily place a vacuum gauge at or
near the probe inlet. Otherwise, use Source Sampler Console’s existing vacuum gauge.
Temporarily attach a rotameter (0 to 40 cc/min) or a 50-cc soap bubble meter to the
DGM outlet.
2.
Plug the probe inlet (or other specified point), and pull a vacuum of  255 mm Hg.
3.
Note reading of rotameter or bubble meter (must be  2% of average sampling rate).
4.
Carefully release the probe inlet plug before turning off the pump.
D.
Procedure D
1.
For components after the pump, apply a slight positive pressure.
2.
Apply a surfactant liquid (for example, detergent in water) at each joint, and check for
gas bubbles.
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EPA Method 4 Moisture Approximation
The sampling procedure for US EPA Method 4 approximation method is as follows:
A.
Pre-Test Preparations
1.
Calibrate the metering system (see Calibration Procedure in Chapter 3)
2.
Prepare the sampling train as follows:
a. Add 5-mL of water in each midget impinger.
b. Assemble the sampling train as shown in the method Figure, with a drying tube to
protect the Source Sampler Console.
e. Adjust probe heater to a temperature sufficient to prevent water condensation.
f. Place crushed ice and water around the impingers.
B.
Sampling
1.
Optional: Leak-check the sampling train (see Appendix C).
2.
Record the initial DGM reading and barometric pressure.
3.
Position the tip of the probe in the stack, and start the pump.
4.
Adjust the sample flow (pressure meter) to a constant rate of about 2 L/min until the dry
gas meter registers about 31-L or until visible liquid droplets are carried over from the
first impinger to the second.
5.
Take readings (DGM, temperatures at DGM and impinger exit, flow rate meter, vacuum)
at least every 5 minutes.
6.
At the conclusion of the run, turn off the pump, remove the probe from the stack, and
record the final DGM reading.
7.
Mandatory: Leak-check the sampling train (see Appendix C).
C.
Sample Recovery
1.
After sampling, combine the contents of the two impingers, and measure the volume to
the nearest 0.5-mL. Alternative: Weigh each midget impinger (after wiping off liquid
from the outside surfaces) to the nearest 0.5-g (must have initial weights also).
2.
Calculate the moisture content.
D.
Alternatives
Use drying tubes, wet bulb-dry bulb techniques, condensation techniques, stoichiometric
calculations, previous experience, etc.
E.
Post-Test Calibrations
1.
Conduct post-test calibration checks of metering systems and temperature gauges
according to the Calibration Procedures in Chapter 3.
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EPA Method 6 for Sulfur Dioxide
The sampling procedure for US EPA Method 6 is as follows:
A.
Pre-Test Preparations
1.
Calibrate the metering system (see Calibration Procedure in Chapter 3)
2.
Determine the number and location of sampling points and sampling time.
3.
Prepare the sampling train as follows:
a. Add 15-mL of 80% isopropanol into the midget bubbler.
b. Add 15-mL of 3% H2O2 into the next two midget impingers.
c. Leave the final midget impinger dry.
d. Assemble the sampling train as shown in the Figure below, with a drying tube to
protect the Source Sampler Console.
e. Adjust probe heater to a temperature sufficient to prevent water condensation.
f. Place crushed ice and water around the impingers.
B.
Sampling
1.
Optional: Leak-check the sampling train (see Appendix C).
2.
Record the initial DGM reading and barometric pressure.
3.
Position the tip of the probe at the first sampling point, connect the probe to the bubbler,
and start the pump.
4.
Adjust the sample flow (pressure meter) to a constant rate of about 1.0 L/min. Maintain
this constant rate (10%) during the entire sampling run.
5.
Traverse, if applicable. Take readings (DGM, temperatures at DGM and impinger exit,
flow rate meter, vacuum) at least every 5 minutes.
6.
Add more ice during the run to keep the temperature of gases leaving the exit impinger at
 20C.
7.
At the conclusion of the run, turn off the pump, remove the probe from the stack, and
record the final DGM reading.
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8.
Mandatory: Leak-check the sampling train (see Appendix C).
C.
Sample Recovery
1.
Drain the ice bath, and purge the remaining part of the train by drawing clean ambient air
through the train for 15 min at the sampling rate. Pass air through a charcoal filter or
through an extra midget impinger with 15-mL H2O2 or use ambient air without
purification.
2.
Disconnect the impingers after purging. Discard the contents of the midget bubbler (80%
isopropanol). Note: Saving this portion until after analysis may be helpful in explaining
anomalies.
3.
Pour the contents of the midget impingers into a polyethylene sample container for
shipment.
4.
Rinse the three midget impingers and connecting U-tubes with DI water, and add the
washings to the same sample container.
5.
Seal and identify/label the sample container. Mark the fluid level.
D.
Alternatives
1.
If SO3 is expected to be insignificant, the midget bubbler containing 80% isopropanol may
be deleted from the sampling train.
2.
If an approximate SO3 concentration is desired, the midget bubbler contents may be
recovered in a separate polyethylene sample container.
E.
Post-Test Calibrations
1.
Conduct post-test calibration checks of metering systems and temperature gauges
according to the Calibration Procedures in Chapter 3.
F.
Elimination of Ammonia Interference
1.
When ammonia is suspected to be an interference, use the above procedure with the
following modifications:
a. Use a high-efficiency in-stack filter (glass fiber) that is un-reactive to SO2, for
example Whatman 934AH.
b. Maintain the probe at 274C.
c. Do not discard the isopropanol solution in the midget bubbler (Step C2), but
quantitatively recover the solution into container with solutions from midget impingers
(Step C3).
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EPA Method 11 for Hydrogen Sulfide in Fuel Gas Streams
The sampling procedure for US EPA Method 11 is as follows:
A.
Pre-Test Preparations
1.
Calibrate the metering system (see Calibration Procedure in Chapter 3)
2.
Prepare the sampling train as follows:
a. Add 15-mL of 3% H2O2 solution into the first midget impinger.
b. Leave the second midget impinger dry.
c. Add 15-mL of CdSO4 solution into the third, fourth and fifth midget impingers.
d. Assemble the sampling train as shown in the Figure in the method, with a drying
tube to protect the Source Sampler Console.
e. Place crushed ice and water around the impingers.
B.
Sampling
1.
Optional: Leak-check the sampling train as follows:
a. Connect the rubber bulb and manometer to the first impinger, as shown in method
Figure. Close the petcock on the DGM outlet.
b. Pressurize the train to 254 mm H2O (10 in. H2O) with the bulb, and close off the
tubing connected to the rubber bulb.
c. Time the pressure drop (must be  10-mm drop in pressure in 1-min)
2.
Purge the connecting line between the sampling valve and the first impinger as follows:
a. Disconnect the line from the first impinger, and open the sampling valve.
b. Allow process gas to flow through the line for 1 to 2 min. Close the sampling valve,
and reconnect the line to the impinger train.
3.
Open the petcock on the DGM outlet. Record the initial DGM reading and barometric
pressure.
4.
Open the sampling valve, and then adjust the valve to obtain about 1.0 L/min (pressure
meter). Maintain this constant rate (10%) during the entire sampling run.
5.
Sample for at least 10-min. Take readings (DGM, temperatures at DGM and impinger
exit, flow rate meter) at least every 5 minutes.
6.
Add more ice during the run to keep the temperature of gases leaving the exit impinger at
 20C.
7.
At the conclusion of the run, close the sampling valve, and record the final DGM reading.
8.
Mandatory: Leak-check the sampling train (see Step A2).
C.
Sample Recovery
1.
Disconnect the impinger train from the sampling line, and connect the charcoal tube and
the pump, as shown in method Figure.
2.
Purge the train at 1 L/min with clean ambient air for 15-min.
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3.
After purging, cap the open ends, and remove the impinger train to a clean, well-lighted
area that is away from sources of heat or direct sunlight.
4.
Discard the contents of the H2O2 midget impinger.
5.
Carefully transfer the contents of the third, fourth, and fifth midget Impingers into a 500mL iodine flask.
6.
Rinse the three midget impingers and connecting U-tubes with DI water, and add the
washings into the iodine flask.
7.
For a blank, add 45-mL CdSO4 absorbing solution to an iodine flask.
8.
Because analysis must immediately follow sample recovery, conduct the iodometric
titration described in the method procedure.
D.
Post-Test Calibrations
1.
Conduct post-test calibration checks of metering systems and temperature gauges
according to the Calibration Procedures in Chapter 3.
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EPA Method 15A for Total Reduced Sulfur Compounds from Sulfur
Recovery Plants in Refineries
The sampling procedure for US EPA Method 15A is as follows:
A.
Pre-Test Preparations
1.
Calibrate the metering system (see Calibration Procedure in Chapter 3)
2.
Prepare the sampling train as follows:
a. Add 15-mL of 80% isopropanol into the midget bubbler.
b. Add 20-mL of 3% H2O2 into the next two midget impingers.
c. Leave the final midget impinger dry.
d. Assemble the sampling train as shown in the method Figure, with a drying tube to
protect the Source Sampler Console.
e. Set the oxidation furnace at 1100  50C.
f. Adjust probe and filter heaters to a temperature sufficient to prevent water
condensation.
g. Place crushed ice and water around the impingers.
B.
Sampling
1.
Optional: Leak-check the sampling train (see Appendix C).
2.
Optional: Conduct two 30-min system performance checks in the field according to
Section D.
3.
Adjust the pressure on the second stage of the regulator on the combustion air cylinder to
10 psig and the combustion air flow rate to 0.50 L/min ( 10%). See method Figure.
4.
Record the initial DGM reading and barometric pressure.
5.
Inject combustion air into the sampling train, start the sample pump, and open the stack
sample gas valve. Do all these operations within 30-sec to avoid pressurizing the
sampling train.
6.
Adjust the sample flow (pressure meter) to a constant rate of about 2.0 L/min. Maintain
this constant rate (10%) during the entire sampling run of 1-hr for three sampling runs
total (3-hr).
7.
Take readings (DGM, temperatures at DGM and impinger exit, flow rate meter, vacuum)
at least every 5 minutes. Monitor and record the combustion air manometer at regular
intervals, also.
8.
Add more ice during the run to keep the temperature of gases leaving the exit impinger at
 20C.
9.
At the conclusion of the run, turn off the sample pump and combustion air simultaneously
(within 30-sec of each other), turn off the sample gas valve, and record the final DGM
reading.
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10.
Mandatory: Leak-check the sampling train (see Appendix C).
C.
Sample Recovery
1.
Drain the ice bath. Disconnect the impingers. Discard the contents of the midget bubbler
(80% isopropanol). Note: Saving this portion until after analysis may be helpful in
explaining anomalies.
2.
Pour the contents of the midget impingers into a polyethylene sample container for
shipment.
3.
Rinse the three midget impingers and connecting U-tubes with DI water, and add the
washings to the same sample container.
4.
Seal and identify/label the sample container. Mark the fluid level.
5.
Optional: Rinse and brush the probe and replace the filter before the next run.
6.
Mandatory: Conduct a performance system check after each 3-hr run or after three 1-hr
samples. See Section D.
D.
System Performance Check
1.
Adjust the flow rates to generate COS concentration in the range of the stack gas or within
 20% of the applicable emission standard at a total flow rate of at least 2.5 L/min. See
method Figure, if dilution is required.
2.
Calibrate the flow rate from both sources with a soap bubble flow meter.
3.
Collect 30-min samples, and analyze in the normal manner. Collect the samples through
the probe of the sampling train using a manifold or some other suitable device. Do not
replace the particulate filter and do not clean the probe before this performance check.
4.
Analyze the samples as in the method procedure for SO2. Analyze field audit samples,
too, if applicable.
E.
Post-Test Calibrations
1.
Conduct post-test calibration checks of metering systems and temperature gauges
according to the Calibration Procedures in Chapter 3.
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EPA Method 16A for Total Reduced Sulfur Compounds
The sampling procedure for USEPA Method 16A is as follows:
A.
Pre-Test Preparations
1.
Calibrate the metering system (see Calibration Procedure in Chapter 3)
2.
Prepare the sampling train as follows:
a. Add 15-mL of 80% isopropanol into the midget bubbler.
b. Add 20-mL of 3% H2O2 into the next two midget impingers.
c. Leave the final midget impinger dry.
d. Assemble the sampling train as shown in method Figure, with a drying tube to
protect the Source Sampler Console.
e. Set the oxidation furnace at 800  100C.
f. Add 100-mL citrate buffer into the first and second impingers of the SO2 scrubber;
leave the third impinger empty. Keep the Teflon line between the heated filter and
citrate scrubber as short as possible.
g. Adjust probe and filter heaters to a temperature sufficient to prevent water
condensation.
h. Place crushed ice and water around the impingers.
3.
Bypassing all sample collection components, draw stack gas into the citrate scrubber for
10-min at 2 L/min. Then final assemble the train.
B.
Sampling
1.
Optional: Leak-check the sampling train (see Appendix C).
2.
Optional: Conduct two 30-min system performance checks in the field according to
Section D.
3.
Record the initial DGM reading and barometric pressure.
4.
Adjust the sample flow (pressure meter) to a constant rate of about 2.0 L/min. Maintain
this constant rate (10%) during the entire sampling run of 1-hr for three sampling runs
total (3-hr).
5.
Take readings (DGM, temperatures at DGM and impinger exit, flow rate meter, vacuum,
oxidation furnace temperature) at least every 5 minutes.
6.
Add more ice during the run to keep the temperature of gases leaving the exit impinger at
 20C.
7.
At the conclusion of the run, turn off the sample pump and record the final DGM reading.
8.
Mandatory: Leak-check the sampling train (see Appendix C).
C.
Sample Recovery
1.
Drain the ice batch. Disconnect the impingers. Discard the contents of the midget
bubbler (80% isopropanol). Note: Saving this portion until after analysis may be helpful
in explaining anomalies.
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2.
Pour the contents of the midget impingers into a polyethylene sample container for
shipment.
3.
Rinse the three midget impingers and connecting U-tubes with DI water, and add the
washings to the same sample container.
4.
Seal and identify/label the sample container. Mark the fluid level.
5.
Optional: Rinse and brush the probe and replace the filter before the next run.
6.
Mandatory: Conduct a performance system check after each 3-hr run or after three 1-hr
samples. See Section D.
D.
System Performance Check
1.
Adjust the flow rates to generate H2S concentration in the range of the stack gas or within
 20% of the applicable emission standard and an O2 concentration >1% at a total flow
rate of at least 2.5 L/min. See method Figure.
2.
Calibrate the flow rate from both sources with a soap bubble flow meter.
3.
Collect 30-min samples, and analyze in the normal manner. Collect the samples through
the probe of the sampling train using a manifold or some other suitable device. Do not
replace the particulate filter and do not clean the probe before this performance check.
4.
Analyze the samples as in the method procedure for SO2, except for 1-hr samples, use a
40-mL aliquot, add 160-mL of 100% isopropanol, and four drops of thorin. Analyze field
audit samples, too, if applicable. Sample recovery must be 100  20% for data to be valid.
Do not use recovery data to correct the test results.
E.
Post-Test Calibrations
1.
Conduct post-test calibration checks of metering systems and temperature gauges
according to the Calibration Procedures in Chapter 3.
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EPA Method 18 for Organic Compounds
The sampling procedure for USEPA Method 18 using gas bags is as follows:
A.
Pre-Test Preparations
1.
Calibrate the metering system (see Calibration Procedure in Chapter 3)
2.
Obtain from pre-test surveys, literature surveys, experience, discussions with plant
personnel, etc. all information necessary to design the emission test.
3.
Obtain pre-test survey samples (glass flasks, purged flasks, gas bags, adsorbent tubes) of
the gas and analyze to confirm the identity and approximate concentrations of the specific
compounds.
B.
Sampling
1.
Mandatory: Leak-check both the bags and the lung container sampling train as follows:
a. Connect a water manometer using a tee connector between the bag or rigid
container and a pressure source.
b. Pressurize the bag or container to 50 to 100 mm H2O, and allow it to stand
overnight. A deflated bag or loss of pressure indicates a leak.
c. Evacuate the bag by pulling a vacuum until a rotameter indicates no flow.
2.
Assemble the sampling train as shown in the method Figure.
3.
Record the initial DGM reading and barometric pressure.
4.
Purge the probe as follows: Connect the vacuum line from the Source Sampler Console to
the Teflon line from the probe, place the probe at the stack centroid or  1-m from the
stack wall, and purge at 0.5-L/min for sufficient time to purge the line several times. If
the gas concentration may harm the Source Sampler Console, then use a squeeze bulb to
purge the probe and line.
5.
Reconfigure the sample and vacuum lines for sampling, and sample proportional to the
stack velocity with a starting sampling rate of about 0.5-L/min. Measure the moisture
content using Method 4 or psychrometry (<59C). Measure the stack gas static pressure.
6.
Take readings (stack gas velocity, DGM, temperatures at DGM and stack gas, flow rate
meter, vacuum) at least every 5 minutes. Adjust sampling rate proportionally if stack gas
velocity varies by >20%.
7.
At the conclusion of the run, shut off the pump, record the final DGM reading, disconnect
the sample line from the bag, and disconnect the vacuum line from the bag container.
C.
Sample Recovery
1.
Disconnect the bag from the rigid container, and close the bag’s valve so as to not lose or
contaminate the sample.
2.
Protect the Tedlar bag from sunlight.
3.
When possible, perform the analysis within 2-hr of sample collection. For longer hold
times, perform a stability study that demonstrates  85% recovery for the actual hold
times of the test.
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Alternatives
If condensation occurs in the bag during sample collection (and a direct interface GC
system cannot be used), use one of the following modifications:
1.
Heating: Heat (conforming to safety restrictions) the rigid sampling container to the
source temperature (assuming system can withstand this temperature). Maintain the
temperature until analysis.
2.
Pre-Dilution: Using the setup shown in the method Figure, meter an inert gas into the
Tedlar bag before sampling. Take the partly filled bag to the source, and meter the source
gas through heated sample lines into the bag. As a quality control check, dilute and
analyze a gas of known concentration and validate this techniques by checking the
dilution factor.
3.
Condensate Trap: Insert a midget impinger(s) with shortened tube in an ice bath between
the probe and rigid container to collect condensate. Recover the collected condensate
into a VOA vial and top off with HPLC-grade water to eliminate and headspace. Submit
condensate samples and blank water for analysis.
E.
Post-Test Calibrations
1.
Conduct post-test calibration checks of metering systems and temperature gauges
according to the Calibration Procedures in Chapter 3.
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EPA Method 18 for Organic Compounds
The sampling procedure for USEPA Method 18 using adsorbent tubes is as follows:
A.
Pre-Test Preparations
1.
Calibrate the metering system (see Calibration Procedure in Chapter 3)
2.
Obtain from pre-test surveys, literature surveys, experience, discussions with plant
personnel, etc. all information necessary to design the emission test.
3.
Obtain pre-test survey samples (glass flasks, purged flasks, gas bags, adsorbent tubes) of
the gas and analyze to confirm the identity and approximate concentrations of the specific
compounds.
4.
After the normal clean up, clean the probe with extraction solvent. Although borosilicate
glass or stainless steel probes are acceptable, use Teflon probes and connecting lines as
much as possible.
B.
Sampling
1.
Assemble the sampling train as shown in the Figure in the method. Mount the adsorption
tubes in a vertical direction to prevent channeling during sampling. Use minimal length of
flexible tubing between the probe and adsorption tubes.
2.
Optional: Leak-check the sampling train (see Appendix C).
3.
Record the initial DGM reading and barometric pressure.
4.
Place the probe at the stack centroid or  1-m from the stack wall, and sample at a
constant rate, using the pressure meter or rotameter as an indicator. Obtain a total sample
volume commensurate with the expected concentration(s) of the volatile organic(s)
present, and recommended sample loading factors (weight of sample per weight of
adsorption material).
5.
Measure the moisture content using Method 4 or psychrometry (<59C). Measure the
stack gas static pressure.
6.
Take readings (stack gas velocity, DGM, temperatures at DGM and stack gas, flow rate
meter, vacuum) at least every 5 minutes. Adjust sampling rate proportionally if stack gas
velocity varies by >20%.
7.
At the conclusion of the run, shut off the pump, and record the final DGM reading.
Remove the probe from the stack.
8.
Mandatory: Leak-check the sampling train (see Appendix C).
C.
Sample Recovery
1.
Remove the adsorption tubes and cap tightly. Label the tubes.
2.
Rinse the probe and sampling lines up to the first adsorption tube with desorption solvent.
Store in glass bottles, and refrigerate (if necessary). Seal and label the bottle.
D.
Recovery Study (Mandatory)
Obtain triplicate samples:
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1.
Set up two identical sampling trains. Designate one train as “S” for spiked, and the other
as “U” for un-spiked.
2.
Spike all the compounds of interest (in gaseous or liquid form) onto the adsorbent tube(s)
in the spiked train before sampling (at about 40-60% of mass expected from stack samples
or 5X the method detection limit). Adsorbent tube spiking can be done in the laboratory
before the trip to the field.
3.
Collocate the probes in the stack of the duplicate trains. Position the probe nozzles on the
same plane, 2.5-cm apart.
4.
Sample as in Step A.
5.
Analyze the samples along with the other field samples and determine the fraction of
spiked compound recovered for each compound. Determine the average R of all three
runs (must be 0.70  R  1.30).
6.
Adjust the field sample concentrations using R for each compound.
E.
Post-Test Calibrations
1.
Conduct post-test calibration checks of metering systems and temperature gauges
according to the Calibration Procedures in Chapter 3.
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EPA Method 26 for Hydrogen Halides and Halogens
The sampling procedure for USEPA Method 26 is as follows:
A.
Pre-Test Preparations
1.
Calibrate the metering system (see Calibration Procedure in Chapter 3)
2.
Prepare the sampling train as follows:
a. Add 15-mL of 0.1N H2SO4 acidic absorbing solution into each of the first two midget
impingers.
b. Add 15-mL of 0.1N NaOH alkaline absorbing solution into each of the next two
midget impingers.
c. Optional: Place an empty midget impinger with shortened stem for knockout
condensate collection in front of the absorbing impingers.
d. Assemble the sampling train as shown in the Figures below, with a drying tube to
protect the Source Sampler Console.
e. Adjust and maintain the probe, filter and 3-way valve heaters to a temperature
 20C above source temperature, but  120C.
f. Place crushed ice and water around the impingers.
g. Connect the purge line to the 3-way valve, and turn the valve to purge the probe
(see Figure below), and purge at a rate of 2 L/min for  5-min before sampling.
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B.
Sampling
1.
Optional: Leak-check the sampling train (see Appendix C).
2.
Record the initial DGM reading and barometric pressure.
3.
Position the tip of the probe at the first sampling point, start the sampling pump, pull a
slight vacuum of ~4 kPa (1 in. Hg) on the impinger train, then turn the 3-way valve to
sample stack gas through the midget impinger train.
4.
Adjust the sample flow (pressure meter) to a constant rate of about 2.0 L/min. Maintain
this constant rate (10%) during the entire sampling run.
5.
Traverse, if applicable. Take readings (DGM, temperatures at DGM and impinger exit,
flow rate meter, vacuum) at least every 5 minutes.
6.
Add more ice during the run to keep the temperature of gases leaving the exit impinger at
 20C.
7.
Sample  1-hr. Shorter sampling times may introduce a significant negative bias in the
HCl concentration.
7.
At the conclusion of the run, turn off the pump, remove the probe from the stack, and
record the final DGM reading.
8.
Mandatory: Leak-check the sampling train (see Appendix C).
C.
Sample Recovery
1.
Acidic Absorbing Impingers
a. Disconnect the impingers after sampling and quantitatively transfer the contents of
the knockout impinger (if used) and acid impingers to a leak-free sample storage
bottle.
b. Add the water rinses of each of these impingers and connecting glass ware to the
sample storage container.
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2.
Alkaline Absorbing Impingers
a. Quantitatively transfer the contents of the alkaline impingers to a leak-free sample
storage bottle.
b. Add the water rinses of each of these impingers and connecting glass ware to the
sample storage container.
c. Multiply 25-mg sodium thiosulfate per “ppm” of halogen anticipated in the stack gas
by the “dscm” stack gas sampled, and add this amount to the storage container.
Note: This amount of sodium thiosulfate includes a safety factor of ~5 to assume
complete reaction with the hypohalous acid to form a second Cl- ion in the alkaline
solution.
3.
Blanks
a. Save portions of both absorbing reagents equivalent to the amount used in the
sampling train. Dilute to the approximate volume of the corresponding samples
using rinse water directly from the wash bottle being used.
b. Add the same amount of sodium thiosulfate to the alkaline absorbing solution blank.
c. Save a portion of the rinse water directly from the wash bottle.
4.
Seal all sample and blank sample bottles, shake to mix, and label. Mark the fluid level.
E.
Post-Test Calibrations
1.
Conduct post-test calibration checks of metering systems and temperature gauges
according to the Calibration Procedures in Chapter 3.
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EPA Method 106 for Vinyl Chloride
The sampling procedure for USEPA Method 106 for vinyl chloride using gas bags is as follows:
A.
Pre-Test Preparations
1.
Calibrate the metering system (see Calibration Procedure in Chapter 3)
2.
Establish the sampling rate at half the bag volume (60-L minimum) divided by the
sampling time.
B.
Sampling
1.
Mandatory: Leak-check both the bags and the lung container sampling train as follows:
a. Connect a water manometer using a tee connector between the bag or rigid
container and a pressure source.
b. Pressurize the bag or container to 50 to 100 mm H2O, and allow it to stand
overnight. A deflated bag or loss of pressure indicates a leak.
c. Evacuate the bag by pulling a vacuum until a rotameter indicates no flow.
2.
Assemble the sampling train as shown in the Figure in the method.
3.
Record the initial DGM reading and barometric pressure.
4.
Place the probe at the stack centroid or  1-m from the stack wall, and purge the probe and
line at 0.5-L/min for sufficient time to purge the line several times. If the gas
concentration may harm the Source Sampler Console, then use a squeeze bulb to purge the
probe and line.
5.
Reconfigure the sample and vacuum lines for sampling, and sample proportional to the
stack velocity with a starting sampling rate of about 0.5-L/min.
6.
Take readings (stack gas velocity, DGM, temperatures at DGM and stack gas, flow rate
meter, vacuum) at least every 5 minutes. Adjust sampling rate proportionally if stack gas
velocity varies by >20%.
7.
At the conclusion of the run, shut off the pump, record the final DGM reading, disconnect
the sample line from the bag, and disconnect the vacuum line from the bag container.
C.
Sample Recovery
1.
Disconnect the bag from the rigid container, and close the bag’s valve so as to not lose or
contaminate the sample.
2.
Protect the Tedlar bag from sunlight until analysis.
D.
Post-Test Calibrations
1.
Conduct post-test calibration checks of metering systems and temperature gauges
according to the Calibration Procedures in Chapter 3.
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EPA Method 308 for Methanol
The sampling procedure for USEPA Method 308 is as follows:
A.
Pre-Test Preparations
1.
Calibrate the metering system (see Calibration Procedure in Chapter 3)
2.
Prepare the sampling train as follows:
a. Add 20-mL of deionized, distilled water into the two midget impingers.
b. Attach the silica gel adsorbent tube (520-mg/260-mg) behind the midget impingers.
c. Assemble the sampling train as shown in Figure in the method.
d. Place crushed ice and water around the impingers.
B.
Sampling
1.
Optional: Leak-check the sampling train as follows:
a. Temporarily attach a suitable (0-40 cc/min) rotameter to the outlet of the DGM.
b. Place a vacuum gauge near the probe inlet.
c. Plug or seal the probe inlet, and pull a vacuum of at least 34 kPa (10 in. Hg).
d. Note the flow rate as indicated by the rotameter. A leak rate of  2% of the average
sampling rate is acceptable.
e. Carefully release the probe inlet seal before turning off pump.
2.
Record the initial DGM reading and barometric pressure.
3.
Position tip of probe at sampling point, connect probe to impingers, and start the pump.
4.
Adjust the sample flow (pressure meter) to a constant rate of about 0.2 L/min. Maintain
this constant rate (10%) during the entire sampling run.
5.
Take readings (DGM, temperatures at DGM and impinger exit, flow rate meter, vacuum)
at least every 5 minutes.
6.
Add more ice during run to keep temperature of gases leaving exit impinger at  20C.
7.
At the conclusion of the run, turn off the pump, remove the probe from the stack, and
record the final DGM reading.
8.
Mandatory: Leak-check the sampling train.
C.
Sample Recovery
1.
Disconnect the impingers. Pour contents of midget impingers into a polyethylene sample
container for shipment.
2.
Rinse the two midget impingers and connecting U-tubes with reagent water, and add the
washings to the same sample container.
3.
Seal and identify/label the sample container. Mark the fluid level.
4.
Remove and seal silica gel tube(s) and place in an ice chest for shipment to laboratory.
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D.
Post-Test Calibrations
1.
Conduct post-test calibration checks of metering systems and temperature gauges
according to the Calibration Procedures in Chapter 3.
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EPA-SW-846 Method for Volatile Organic Compounds
The sampling procedure for EPA-SW-846 Method 0030 (VOST) using adsorbent tubes is as follows:
A.
Pre-Test Preparations
1.
Calibrate the metering system (see Calibration Procedure in Chapter 3)
2.
Obtain from pre-test surveys, literature surveys, experience, discussions with plant
personnel, etc. all data necessary to calculate a safe sampling volume designed to
minimize adsorbent breakthrough and still demonstrate the desired DRE results. This
procedure is applicable for organic compounds with boiling points from 30C to about
140C. If the boiling point is  30C, breakthrough on the adsorbent may occur unless
sampling volumes are adjusted.
3.
The glass tubes, condensers and other glassware should be cleaned with a nonionic
detergent in an ultrsonic bath, rinsed well with organic-free water, and dried at 110C.
4.
Have the laboratory prepare the VOST tubes and ship them to the site. After receiving
them, keep the tubes cool and away from any chemical contamination sources.
5.
Assemble the sampling train as shown in the Figure below. Mount the adsorption tubes in
a vertical direction to prevent channeling during sampling. Minimize the time that
adsorbent tubes are uncapped and open to exposure from fugitive emissions. If the
sampling site is contaminated, consider moving the sampling train to a clean area and
mounting adsorbent tubes there, then returning to the sampling site. Attach a
thermocouple between the first condenser and the first adsorbent tube to monitor the
temperature (must be  20C). Use minimal length of flexible Teflon tubing between the
condensate collector and second water-cooled condenser.
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B.
Sampling
1.
Optional: Leak-check the sampling train. Close the valve at the inlet of the first
condenser and slowly pull a vacuum of 250 mm Hg (10 in. Hg). Isolate the tubes and
condensers from the pump by shutting off the Coarse control valve, and observe the leak
rate on the vacuum gauge. The leak rate should be less than 2.5 mm Hg/min. The train is
returned to atmospheric pressure by turning the 3-way valve at the train inlet to the
charcoal-filled tube and admitting ambient air filtered through the charcoal. This
procedure will minimize contamination from fugitive emissions.
2.
Record the initial DGM reading and barometric pressure.
3.
Place the probe in the stack, open the 3-way valve at the inlet of the first condenser, and
turn on the pump. Sample at a rate of 1.0-L/min for 20-min or 0.5-L/min for 40-min.
Collect enough samples to have at least 120-min of total sampling time. The volume of
sample for any pair of tubes should not exceed 20-L, corrected to standard conditions.
4.
Take readings (DGM, temperatures at DGM and condenser(s), flow rate meter, vacuum)
at least every 5 minutes. Maintain a constant sampling rate.
5.
At the conclusion of the run, shut off the pump, close the 3-way valve, and record the final
DGM reading.
6.
Mandatory: Leak-check the sampling train (see B1), except use the highest vacuum
observed during the sampling run.
C.
Sample Recovery
1.
Remove the adsorption tubes, replace their end caps and hand-tighten. Place each
adsorbent tube in the glass culture tube in which it was shipped. Label the culture tubes,
and place on bagged ice or on cold packs (no dry ice or solid CO2) for storage. Minimize
time exposed to ambient conditions to prevent contamination of adsorbent tubes.
2.
A new pair of adsorbent tubes is mounted in the sampling train, and the procedure is
repeated until at least 120-min of sampling time has been collected.
3.
Depending on condensate volume collected, recovery of the condensate may be performed
with each tube change or at the end of the run (  120-min). Recover by transferring any
liquid in the condensate trap to a 40-mL VOA vial, rinsing the trap three times with a
minimal amount of organic-free reagent water, and adding the rinses to the VOA vial. If
necessary, add more water to the VOA vial to eliminate headspace before sealing and
labeling. Place the VOA vial(s) with the set of tubes in a self-sealing plastic bag and store
on cold packs until analysis.
4.
Store and ship the adsorbent tubes on cold packs until ready for analysis. Keep tubes
away from organic reagents and organic waste samples.
D.
Post-Test Calibrations
1.
Conduct post-test calibration checks of metering systems and temperature gauges
according to the Calibration Procedures in Chapter 3.
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EPA-SW-846 Method for Volatile Organic Compounds
The sampling procedure for EPA-SW-846 Method 0031 (SMVOC or SuperVOST) using adsorbent
tubes is as follows:
A.
Pre-Test Preparations
1.
Calibrate the metering system (see Calibration Procedure in Chapter 3)
2.
Obtain from pre-test surveys, literature surveys, experience, discussions with plant
personnel, etc. all data necessary to calculate a safe sampling volume designed to
minimize adsorbent breakthrough and still demonstrate the desired DRE results. This
procedure is applicable for organic compounds with boiling points from -15C to 121C.
If the boiling point is  0C, field application of the method should be supported by data
from laboratory gaseous dynamic spiking and GC/MS analysis to demonstrate the
efficiency of the method.
3.
All glass components of the train should be cleaned by sonicating for 1-hr in a solution of
nonionic laboratory detergent, rinsed with copious amounts of hot tap water, rinsed 3X
with HPLC-grade water, oven dried at 110C, and capped for shipment with Teflon tape
or aluminum foil.
4.
Have the laboratory prepare the adsorbent tubes and ship them to the site. After receiving
them, keep the tubes cool (<10C) and away from any chemical contamination sources.
Conditioned tubes should be held no more than 14 days before sampling.
5.
Assemble the sampling train as shown in the Figure below. Mount the adsorption tubes in
a vertical direction to prevent channeling during sampling. The removed end caps of the
adsorbent tubes should be placed in a clean screw-capped glass container (culure tube)
during sample collection to prevent contamination. Minimize the time that adsorbent
tubes are uncapped and open to exposure from fugitive emissions. If the sampling site is
contaminated or exposed to fugitive emissions, consider moving the sampling train to a
clean area and mounting adsorbent tubes there, then returning to the sampling site.
Attach a thermocouple between the first condenser and the first adsorbent tube to monitor
the temperature (must be  20C). Use minimal length of flexible Teflon tubing between
the condensate collector and second water-cooled condenser.
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B.
Sampling
1.
Optional: Leak-check the sampling train from the probe to the pump. Seal the end of the
probe and turn the 3-way valve at the inlet of the first condenser to the open position.
Turn on the pump and slowly pull a vacuum of 254 mm Hg (10 in. Hg). Allow the
pressure meter to drop to zero, and allow the dry gas meter to stop. Isolate the tubes and
condensers from the pump by shutting off the Coarse control valve, and observe the leak
rate on the vacuum gauge. The leak rate should be less than 2.5 mm Hg/min. Turn off the
pump and return the train to atmospheric pressure by turning the 3-way valve at the train
inlet to the charcoal-filled tube and admitting ambient air filtered through the charcoal.
This procedure will minimize contamination from fugitive emissions.
2.
Record the initial DGM reading and barometric pressure.
3.
Place the probe tip at the centroid of the stack or at a point  1-m from the stack wall.
Purge the probe with stack gas by attaching a pump (or squeeze bulb) to the 3-way valve
and drawing stack gas to purge the probe of ambient air. Open the 3-way valve at the inlet
of the first condenser, and turn on the pump. Sample at a rate of 1.0-L/min for 20-min or
0.5-L/min for 40-min. Collect enough samples to have 120-min of total sampling time.
The volume of sample for any set of tubes should not exceed 20-L, corrected to standard
conditions.
4.
Take readings (DGM, temperatures at DGM and condenser(s), flow rate meter, vacuum)
at least every 5 minutes. Maintain a constant sampling rate.
5.
At the conclusion of the run, shut off the pump, close the 3-way valve, and record the final
DGM reading.
6.
Mandatory: Leak-check the sampling train (see B1), except use the highest vacuum
observed during the sampling run. The sampling run is considered invalid if the leak test
does not meet specifications.
C.
Sample Recovery
1.
Remove the adsorption tubes, replace their end caps and hand-tighten. Place each
adsorbent tube in the glass culture tube in which it was shipped. Label the culture tubes,
and place on bagged ice or on cold packs for storage. Use of dry ice (solid CO2) for
cooling should be avoided as adsorbent will take up CO2 as the solid coolant vaporizes
and analysis will be made more difficult. Minimize time exposed to ambient conditions to
prevent contamination of adsorbent tubes.
2.
A new pair of adsorbent tubes is mounted in the sampling train, and the procedure is
repeated until at least 120-min of sampling time has been collected.
3.
Depending on condensate volume collected, recovery of the condensate may be performed
with each tube change or at the end of the run (  120-min). Recover by transferring any
liquid in the condensate trap to a 40-mL VOA vial, rinsing the trap three times with a
minimal amount of organic-free reagent water, and adding the rinses to the VOA vial. If
necessary, add more water to the VOA vial to eliminate headspace before sealing and
labeling. Place the VOA vial(s) with the set of tubes in a self-sealing plastic bag and store
on cold packs at  10C until analysis.
4.
Store and ship the adsorbent tubes on cold packs until ready for analysis (  14 days).
Keep tubes away from organic reagents and organic waste samples.
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5.
Field Blanks: Collect a field blank set for at least every 120-min sampling period. A set
of adsorbent tubes are attached to sampling train while the train is leak-checked. The
tubes are removed, labeled and stored with the actual samples.
6.
Trip Blanks: At least one set of blank adsorbent tubes should be included with each
shipment of tubes to the sampling site, which should remain unopened, be treated like any
other tubes, and then be labeled and return-shipped to the laboratory.
D.
Post-Test Calibrations
1.
Conduct post-test calibration checks of metering systems and temperature gauges
according to the Calibration Procedures in Chapter 3.
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EPA-SW-846 Method for Volatile Organic Compounds
The sampling procedure for EPA-SW-846 Method 0040 Tedlar bag sampling is as follows:
A.
Pre-Test Preparations
1.
Calibrate the metering system (see Calibration Procedure in Chapter 3)
2.
Obtain from pre-test surveys, literature surveys, experience, discussions with plant
personnel, etc. all data necessary to calculate a sample concentration sufficient to
demonstrate the desired DRE results. This procedure is applicable for organic compounds
with boiling points < 121C and having a concentration below the condensation point.
During laboratory validation studies, the loss of a compound from a Tedlar bag must be
less than 20% over a 72-hr storage time above 0C. Longer storage times must be
demonstrated before testing.
3.
Clean sampling train glassware with non-ionic detergent (Alconox or equivalent) and hot
water in an ultrasonic bath. Rinse each component 3X with distilled, deionized water,
then rinse 3X with 10% HNO3, followed by an additional 3X rinse with distilled,
deionized water. Dry in an oven at 130C for >2-hr.
4.
Clean all Teflon lines as in Step A3, except air-dry in an organic-free area. Use clean
Teflon tubing for each test series or test condition.
5.
Ensure that all bags are clean before use by first flushing 3X with high-purity N2
(99.998%), then filling each bag with N2 and analyzing the bag contents at the highest
sensitivity setting using the same analytical technique that will be used for the test. An
acceptable level of contamination is a response <5X the IDL or 1/2 the level of concern,
whichever is less.
6.
Mandatory: Leak-check the Tedlar bags and rigid bag container as follows:
a. Connect a water manometer using a tee connector between the bag or container
and a pressure source (high purity N2).
b. Pressurize the bag or container to 50 to 100 mm H2O, and allow it to stand
overnight. A deflated bag or loss of pressure indicates a leak.
c. Evacuate the bag by pulling a vacuum until a rotameter indicates no flow.
7.
Determine whether the source has a constant (<20% change in p) or variable stack gas
flow rate. Use constant rate sampling for a constant rate source and proportional rate
sampling for a variable source.
8.
Assemble the sampling train as shown in the Figure (top of next page). The probe, filter
and 3-way valve must be heated to between 130C and 140C during sampling. All
sample lines upstream of the condenser must be heated to between 130C and 140C.
Attach a thermocouple between the water-circulating condenser and the condensate trap or
on the outlet of the condensate trap to monitor the temperature (must be  20C during
sampling). Circulate cooling water from the ice bath to the condenser and back until the
temperature is stabilized  20C. Use a minimal length (  1.5-m) of flexible Teflon
tubing between the condensate collector and rigid bag container.
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9.
Conduct a preliminary velocity and temperature traverse in accordance with EPA Methods
1 and 2, to determine the point of average velocity. Mark the probe of the Method 0040
train to position the probe tip at the point of average velocity.
10.
Determine the moisture content of the gas stream before or during actual sampling.
B.
Sampling
1.
Mandatory: Bag Evacuation and Leak-Check Procedure: Before sampling, ensure that
the Tedlar bag is fully evacuated and leak-free.
a. Disconnect the vacuum line from the rigid bag container and attach this
quick-connect fitting to the outlet of the Bag Isolation Valve. Turn on the pump in
the Source Sampler Console and turn the Bag Isolation Valve to empty the bag.
b. Open the Coarse control valve on the Source Sampler Console and adjust the Fine
control
valve until the vacuum rises to 127-mm Hg (5 in. Hg).
c. Observe the dry gas meter and pressure meter on the Source Sampler Console as the
bag is
evacuated. The bag is completely evacuated when no flow is indicated on the dry
gas meter and the vacuum rises to 127-mm Hg.
d. Allow the pressure meter to drop to zero. Time and record the leak rate indicated
on the vacuum gauge (must be  2.54 mm Hg).
e. If all connections are found to be leak-tight and leak rate cannot meet set criteria,
discard the bag and test another clean bag.
f. Turn the Bag Isolation Valve to pull on the condenser to seal the evacuated bag,
and turn off the pump.
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2.
Mandatory: Pre-Test Leak-Check:
a. Ensure the Bag Isolation Valve is in the position from the condenser to the vacuum
line (not to bag), and the end of the probe is sealed.
b. Turn the Probe Isolation Valve to connect the filter and condenser, turn on the pump,
and open the Coarse control valve.
c. Allow the sampling train to evacuate and adjust the Fine control valve to increase
the vacuum to 127-mm Hg.
d. When the pressure meter drops to zero and the dry gas meter slows to a stop, time
and record the leak rate as in Section B.1.d. (must be  2.54 mm Hg).
e. If the leak rate is exceeded, check all connections, valves and probe seal for
tightness. Any leak found must be corrected and the leak check repeated and
passed before sampling may begin.
f. After completing a satisfactory leak-check, return the sampling train to ambient
pressure by turning the Probe Isolation Valve to connect the purge with condenser
and turning off the pump.
g. When the vacuum gauge drops to zero, immediately turn the Probe Isolation Valve
to connect the filter to purge. Disconnect the vacuum line from the Bag Isolation
Valve quick-connect fitting, then connect the vacuum line to the rigid bag container
to return the sampling train to a ready position.
3.
Remove the seal from the end of the probe and place the probe tip at the point of average
velocity.
4.
Purge the sampling train (probe, valve and filter assembly ONLY) as follows:
a. Disconnect the vacuum line quick-connect fitting from the rigid bag container, and
connect it to the Probe Isolation Valve quick-connect fitting.
b. Ensure that the Probe Isolation Valve is turned so that filter is connected to purge
line, and turn on the pump.
c. Draw at least 8X the sample volume of flue gas or purge for 10-min, whichever is
greater.
d. Adjust the sample flow rate to desired settings and check out all temperature and
flow readings during the purge to ensure proper settings.
e. When purge is complete, shut off the pump, and return the train to its initial
configuration.
5.
Record the initial DGM reading and barometric pressure.
6.
Turn on the pump to start sample collection. Use constant rate sampling (unless
proportional rate sampling was indicated) to collect about 25 to 35-L.
7.
Take readings (DGM, temperatures at DGM and condenser(s), flow rate meter, vacuum)
at least every 5 minutes.
8.
At the conclusion of the run, shut off the pump, close the Probe Isolation Valve, and
record the final DGM reading.
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9.
Mandatory: Post-Test Leak-Check:
a. Ensure that the Bag Isolation Valve Leak connects the condenser to bag and that
the Probe Isolation Valve connects filter to purge line when pump is shut off.
b. Remove the probe from the stack and seal the probe end.
c. Disconnect the vacuum line from the rigid bag container and attach it to the outlet
of the Bag Isolation Valve. Turn the Probe Isolation Valve to connect the filter to
condenser. Turn on the pump and adjust the Fine control valve until a vacuum of
>25.4-mm Hg (1 in. Hg) above the highest vacuum recorded during the run is
reached.
d. Time and record the leak rate as in B.1.d. The sampling run is considered invalid if
the leak test does not meet specifications.
e. Return the sample train to ambient pressure and disconnect the sample and vacuum
lines from the bag and rigid container to prepare train for next sampling run.
C.
Sample Recovery
1.
Remove the Tedlar bag from the rigid container, close the bag valve, and label the bag.
Store to protect the bag from sharp objects or surfaces, direct sunlight, and low
temperatures (below 0C that could cause condensation of analytes). Store bags in rigid
opaque containers for all storage, shipping or handling operations. Ship the bags using
ground transportation. Analyze the bags within 72-hr of sample collection unless it can be
shown that significant (<20%) sample degradation does not occur over a longer period of
sample storage.
2.
Depending on condensate volume collected, recovery of the condensate may be performed
with each bag change or at the end of a test condition. Recover by transferring any liquid
in the condensate trap to a 40-mL VOA vial, rinsing the trap three times with a minimal
amount of organic-free reagent water, and adding the rinses to the VOA vial. If
necessary, add more water to the VOA vial to eliminate headspace before sealing and
labeling. Place the VOA vial(s) in a self-sealing plastic bag and store on cold packs at 
10C until analysis.
3.
Field Blanks: Collect at least one field blank sample daily and per source. Collect high
purity air or N2 from a compressed gas cylinder in the same manner as source emissions.
The field blank bag samples are leak-checked, labeled and stored with the actual samples.
4.
Trip Blanks: Take at least two Tedlar bags labeled “trip blanks” and filled with inert
gas from the laboratory to the sampling site, which should be treated like any other
samples except not be opened, and then be labeled and return-shipped to the laboratory.
5.
Field Spike Samples: Take at least one field spike per 10 bag samples, or a minimum of
one field spike per test. Spike the chosen bag sample with a known mixture (gaseous or
liquid) of isotopically-labeled analogues of all target pollutants using either gaseous or
liquid injection into the bag. Spiking concentration should be 2X the concentration
anticipated in the stack gas. The syringe volume for gaseous injection should not exceed
200-mL and for liquid injection should not exceed 1-mL. The final volume of spiked gas
must not exceed 1% of total sample volume. Store, transport and analyze with the source
test samples. Compound recoveries in the spiked sample must be 80-120%.
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D.
Post-Test Calibrations
1.
Conduct post-test calibration checks of metering systems and temperature gauges
according to the Calibration Procedures in Chapter 3.
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EPA-SW-846 Method 0051 for HCl and Cl2
The sampling procedure for USEPA Method 26 is as follows:
A.
Pre-Test Preparations
1.
Calibrate the metering system (see Calibration Procedure in Chapter 3)
2.
Prepare the sampling train as follows:
a. Add 15-mL of 0.1N H2SO4 acidic absorbing solution into each of the first two midget
impingers. If moisture is to be determined, pre-weigh each impinger.
b. Add 15-mL of 0.1N NaOH alkaline absorbing solution into each of the next two
midget impingers. If moisture is to be determined, pre-weigh each impinger.
c. Optional: Place an empty midget impinger with shortened stem for knockout
condensate collection in front of the absorbing impingers.
d. Assemble the sampling train as shown in the Figures below, with a drying tube to
protect the Source Sampler Console. If moisture is to be determined, pre-weigh the
drying
tube.
e. Leak-check the probe and 3-way valve prior inserting the probe into the stack.
f. Adjust and maintain the probe and 3-way valve heaters to a temperature sufficient
to prevent condensation. Adjust the filter temperature 121C.
g. Place crushed ice and water around the impingers.
h. Connect the purge line to the 3-way valve, and turn the valve to purge the probe
(see Figure below), and purge at a rate of 2 L/min for  5-min before sampling.
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B.
Sampling
1.
Optional: Leak-check the sampling train (see Appendix C).
2.
Record the initial DGM reading and barometric pressure.
3.
Position the tip of the probe at the first sampling point, start the sampling pump, pull a
slight vacuum of ~4 kPa (1 in. Hg) on the impinger train, then turn the 3-way valve to
sample stack gas through the midget impinger train.
4.
Adjust the sample flow (pressure meter) to a constant rate of about 2.0 L/min. Maintain
this constant rate (10%) during the entire sampling run.
5.
Traverse, if applicable. Take readings (DGM, temperatures at DGM and impinger exit,
flow rate meter, vacuum) at least every 5 minutes.
6.
Add more ice during the run to keep the temperature of gases leaving the exit impinger at
 20C.
7.
Sample  1-hr. Shorter sampling times may introduce a significant negative bias in the
HCl concentration. If expected condensate catch exceeds capacity of the sampling train, a
larger knockout impinger may be used or two (2) sequential 30-min sampling runs may be
conducted.
8.
At the conclusion of the run, turn off the pump, remove the probe from the stack, and
record the final DGM reading.
9.
Mandatory: Leak-check the sampling train (see Appendix C).
C.
Sample Recovery
If performing a moisture determination, wipe off any moisture on the outside surfaces of
each impinger and weigh to the nearest 0.5-g and record weight.
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1.
Acidic Absorbing Impingers
a. Disconnect the impingers after sampling and quantitatively transfer the contents of
the knockout impinger (if used) and acid impingers to a leak-free sample storage
bottle.
b. Add the water rinses of each of these impingers and connecting glass ware to the
sample storage container.
2.
Alkaline Absorbing Impingers
a. Quantitatively transfer the contents of the alkaline impingers to a leak-free sample
storage bottle.
b. Add the water rinses of each of these impingers and connecting glass ware to the
sample storage container.
c. Add 2-mL or more of sodium thiosulfate (Na2S2O3) to the storage container.
3.
Blanks
a. Save portions of both absorbing reagents equivalent to the amount used in the
sampling train. Dilute to the approximate volume of the corresponding samples
using rinse water directly from the wash bottle being used.
b. Add the same amount of sodium thiosulfate to the alkaline absorbing solution blank.
c. Save a portion of the rinse water directly from the wash bottle.
4.
Seal all sample and blank sample bottles, shake to mix, and label. Mark the fluid level.
E.
Post-Test Calibrations
1.
Conduct post-test calibration checks of metering systems and temperature gauges
according to the Calibration Procedures in Chapter 3.
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Appendix D
Field Data Sheets
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