Specification Test Methods
ASTM D6890/EN 15195 (IP498)
Ignition Quality g o Qua y
Tester (IQT™)
Technology Update
Technology Update
Fuel Rating Symposium
October, 2010
Welcome
• II would like to thank you for taking time out of would like to thank you for taking time out of
your busy schedules to come to attend presentation ‐ in particular to hear this presentation in particular to hear this
D6890/EN 15195 (IP 498) progress review update
Presentation Topics
Presentation Topics
IQT™ History
Test Method Development at EI and ASTM
Use of the IQT™ from a global perspective Th i ifi
The significance of the IQT™ in biodiesel fuel development f th IQT™ i bi di l f l d l
t
and commercialization
• The effective use of the IQT™ with cetane improver (2‐ethy hexyl nitrate ‐2EHN and ditertiary butyl peroxide ‐DTB)
• The effective use of the IQT™ in refinery diesel fuel blending opt
optimization (establish blend values for components)
at o (estab s b e d a ues o co po e ts)
• Regulatory use of the IQT™ for regular and premium diesel fuel
•
•
•
•
Presentation Topics Cont’d.
Presentation Topics Cont
d.
• Development of a high precision MDV Fuel Injection Pump that will further improve precision • Precision Update Status ( ASTM & EI Exchange Group Data)
• Update on Refinery On‐Line Model (ROLM) IQT
Update on Refinery On Line Model (ROLM) IQT™
• Preliminary Test Results for New Reference Fuel Blends
• Durability track record and recent durability improvements
• Update on near Totally Automated Laboratory Model (TALM) IQT™
• Ease of Maintenance
Ease of Maintenance
• Expansion of test method scope above 64 DCN and below 33 DCN
Presentation Topics Cont’d.
Presentation Topics Cont
d.
• Combined use of primary reference fuels with heptane and p
y
p
methylcyclohexane (MCH) to improve ease of calibration • Summary
IQT™ History
IQT
History
• The
The IQT
IQT™ was initially developed as a hand operated was initially developed as a hand operated
research tool by Southwest Research Institute (SwRI) in San Antonio, Texas
• AET acquired the technology from SwRI in 1994
IQT™ History Cont
IQT
History Cont’d.
d.
SwRI’ss hand
SwRI
hand‐operated
operated research CVCC device
research CVCC device
IQT™ History
IQT
History Cont
Cont’d.
d.
• Considerable
Considerable effort was required to determine the effort was required to determine the
major sources of error in order to further develop the instrument
• The main R&D focus was targeted towards developing a robust/optimized ignition delay
developing a robust/optimized ignition delay measurement algorithm that was based on a large data base of ASTM – NEG fuel remnants IQT™ History Cont
IQT
History Cont’d.
d.
SwRI hand‐operated research CVCC device in operation (c.1993)
IQT™ History Cont
IQT
History Cont’d.
d.
• The
The second main R&D focus was automating the second main R&D focus was automating the
instrument’s sequence of injection and combustion events.
IQT™ History
IQT
History Cont
Cont’d.
d.
SwRI/AET’s development of a first prototype IQT™, manufactured by SwRI
IQT™ History
IQT
History Cont
Cont’d.
d.
Prototype IQT™’s combustion chamber and injection pump
yp Q
j
p p
Handle for inlet valve
Pneumatic piston
Injection release mechanism
Handle for exhaust valve
IQT™ History
IQT
History Cont
Cont’d.
d.
Updated prototype IQT™ under test at AET
p
p
yp Q
Pneumatically actuated valves
Solenoid actuator
Data acquisition and control computer
Test Method Development at EI and ASTM • The
The first test method was written in accordance with first test method was written in accordance with
the Energy Institute (EI) format and was first approved by EI as IP 498 • The EI version was then utilized to commence the ASTM version and approved in 2002 as D6890
ASTM version and approved in 2002 as D6890
Test Method Development at EI and ASTM Cont’d. ’d
• AET
AET continues to be grateful for the knowledgeable continues to be grateful for the knowledgeable
help of John Jones with this initial ASTM test method • B
Both test methods were developed in a totally open th t t
th d
d l
d i t t ll
and transparent manner
Test Method Development at EI and ASTM Cont’d. ’d
• Throughout
Throughout the test method development the IQT
the test method development the IQTTM
Instrument User Group (UG) played a major role in test method development and round robin testing
• The IQTTM UG met by teleconference call every two weeks for several years – these teleconference calls weeks for several years these teleconference calls
were kindly hosted by BP Oil
Test Method Development at EI and ASTM Cont’d. ’d
• More
More recently, the UG helped with the Independent recently, the UG helped with the Independent
Laboratory Study (ILS) for B100 materials and their use in D6751 • AET and the UG has supplied test data for the development of ASTM D7467 – Fuel Specification for development of ASTM D7467 Fuel Specification for
B6 to B20
Test Method Development at EI and ASTM Cont’d. ’d
• AET
AET has planned additional testing of B100 for D613 has planned additional testing of B100 for D613
and D6890 by UG and AET (on two B100 feedstocks
that meet D6751)
Use of the IQT™ from a Global Perspective
Region
g
Number of IQT
Q ™s
Europe
50
North America
46
Eastern Asia & Australia
17
South America
10
Middle East, Western Asia & India
Middle East, Western Asia
6
Africa
3
Use of the IQT™ from a Global Perspective Cont’d.
’d
Organization Type
g
yp
Number of IQT
Q ™s
Refinery
57
Government Laboratory
19
Independent Testing Laboratory
18
Oil Company Laboratory
18
University/Research Laboratory
13
Other
7
Use of the IQT™ from a Global Perspective Cont’d.
’d
Use of the IQT™ from a Global Perspective Cont’d.
’d
Use of the IQT™ from a Global Perspective Cont’d.
’d
Use of the IQT™ from a Global Perspective Cont’d.
’d
Use of the IQT™ from a Global Perspective Cont’d.
’d
Some of our Major IQT™ Users
Some of our Major IQT
Users
The Significance of the IQT™ in Biodiesel Fuel Development and Commercialization
l
l
d
i li i
• Over
Over the past 10 years, the IQT
the past 10 years, the IQT™ has been utilized to has been utilized to
test B100 development fuels from approximately 50 different bio sources
• On all of these bio sources, there was never a single problem in providing a DCN indication (many of
problem in providing a DCN indication (many of these fuels were tested well before the development of ASTM D6751) )
Effective use of the IQT™ with cetane improver (2‐ethy
(2
ethy hexyl
hexyl nitrate nitrate ‐2EHN
2EHN and ditertiary
and ditertiary butyl butyl
peroxide ‐DTBP)
• Unlike the CFR engine, the IQT™ is sensitive to small concentrations of cetane improvers such as 2‐ethyl hexyl nitrate (2‐EHN) and ditertiary butyl peroxide (DTB).
Refinery use of the IQT™ with Cetane Improver
• Numerous
Numerous refineries and research centers have been refineries and research centers have been
using their IQT™s to determine the level of boost for different base fuels with various cetane improver concentrations
IQT™ with Cetane Improver Cont
IQT
with Cetane Improver Cont’d.
d.
20
High response fuel
Ce
etane Boostt
15
10
5
0
0
Low response fuel
1000
2000
3000
Amount of Additive (ppm)
4000
Ghosh ‐ Energy & Fuels 2008
Predicting the Effect of Cetane Improvers on Diesel Fuels
Effective use of the IQT™ in refinery diesel fuel blending optimization (establish blend values for
blending optimization (establish blend values for component blending)
• Establish DCN blend values for the blend components
• Determine the optimal dose rates for cetane
improver
Effective use of the IQT™ in refinery diesel fuel blending optimization (establish blend values for
blending optimization (establish blend values for component blending)
• Determine cetane improver response with individual components • As a result of IQT™ precision, a blend curve can be produced with as few as 4 tests for DCN Regulatory use of the IQT™ for regular and premium diesel fuel
d
d
lf l
• Many
Many countries, states, regions in the world have countries, states, regions in the world have
adopted fuel specifications that utilize ASTM D 6890 or EN 15195 in similar manner to that of ASTM D975, EN 590, D6751
Development of a high precision MDV Fuel Injection Pump that will further improve
Injection Pump that will further improve precision Pump #
Fuel
Pump Statistics
A
B
C
E
AVE
StdDev.
CF 12
CF‐12
57 2
57.2
57 2
57.2
57 3
57.3
57 3
57.3
57 3
57.3
.05
05
Cf‐13
42.0
42.2
42.4
41.9
42.1
.23
Cf‐14
51.2
51.8
51.1
51.2
51.3
.33
1013
42.5
43.2
42.6
42.9
42.8
.32
0811
57.7
57.2
58.0
57.6
.37
0810
52.3
52.0
52.3
52.2
.19
1030
38.9
39.5
39.9
39.4
.40
39.4
Development of a high precision MDV Fuel Injection Pump that will further improve
Injection Pump that will further improve precision cont’d.
ASTM/EI Test Results
Fuel
DCN
StdDev
CN
StdDev
1013
42 7
42.7
1 15
1.15
44 0
44.0
1 42
1.42
0811
57.2
0.79
55.4
1.78
0810
52.6
0.81
51.0
0.58
1030
38.4
0.34
38.8
1.10
Precision Update
Precision Update
• There
There were 4 ballots to update the precision of were 4 ballots to update the precision of
D6890 at the December 2009 ASTM meeting
–
–
–
–
ASTM/EI Research Report
Update Reproducibility
Expand Scope Update Between Method Reproducibility
• All items are going to publication
Precision Update Cont’d.
Precision Update Cont
d.
DCN / CN
D6890‐2008
D6890‐2010
((approved)
pp
)
D613‐2008
40
2.56
2.23
2.8
45
2.85
2.43
3.4
51
3 20
3.20
2 66
2.66
42
4.2
55
3.43
2.81
4.7
Table: Reproducibility p
y
DCN / CN
D6890‐2008
D6890‐2010
(approved)
D613‐2008
40
3 57
3.57
3 15
3.15
N/A
45
4.17
3.71
N/A
51
4.90
4.37
N/A
55
5.38
4.81
N/A
Table: Between Method Reproducibility Precision Update Status
Precision Update Status
• ASTM
ASTM D6890
D6890‐10a
10a was published by ASTM in late was published by ASTM in late
September 2010
– Reproducibility, repeatability and between‐method reproducibility were recalculated using much larger data set than original calculation
• Original
Original 2002 inter
2002 inter‐laboratory
laboratory study data, ASTM NEG fuel study data ASTM NEG fuel
exchange program data, and Energy Institute IP fuel exchange program data
– Significant improvement in reproducibility and Significant impro ement in reprod cibilit and
between‐method reproducibility
Precision Update Status Cont’d
Precision Update Status Cont
d
DCN/CN
r
33
34
35
37
39
40
41
43
45
47
49
51
53
55
56
57
59
61
63
64
0.85
0.85
0.85
0.85
0.85
0.85
0.85
0.85
0.85
0.85
0.85
0.85
0.85
0.85
0.85
0 85
0.85
0.85
0.85
0.85
0.85
D6890‐09
R
Rxy
r
2.15
2.21
2.27
2.39
2.50
2.56
2.62
2.74
2.85
2.97
3.08
3.20
3.32
3.43
3.49
3 55
3.55
3.67
3.78
3.90
3.96
2.72
2.84
2.97
3.21
3.45
3.57
3.69
3.93
4.17
4.42
4.66
4.90
5.14
5.38
5.50
5 62
5.62
5.86
6.11
6.35
6.47
0.67
0.69
0.70
0.73
0.75
0.77
0.78
0.81
0.83
0.86
0.88
0.91
0.94
0.96
0.98
0 99
0.99
1.02
1.04
1.07
1.08
D6890‐10a
R
1.96
2.00
2.04
2.12
2.19
2.23
2.27
2.35
2.43
2.50
2.58
2.66
2.73
2.81
2.85
2 89
2.89
2.96
3.04
3.12
3.16
D613‐08
Rxy
r
R
2.40
2.51
2.62
2.84
3.06
3.17
3.28
3.50
3.72
3.94
4.16
4.37
4.59
4.81
4.92
5 03
5.03
5.25
5.47
5.69
5.80
0.8
0.8
0.8
0.8
0.8
0.8
0.8
0.9
0.9
0.9
0.9
0.9
1.0
1.0
1.0
10
1.0
1.0
1.0
1.1
1.1
1.9
2.1
2.2
2.4
2.7
2.8
2.9
3.2
3.4
3.7
3.9
4.2
4.4
4.7
4.8
49
4.9
5.2
5.4
5.7
5.8
Areas in lighter shaded regions are for published precision, hence values in darker shaded regions are an extrapolation of published values
Precision Update Status Cont’d
Precision Update Status Cont
d
Precision Update Status Cont’d
Precision Update Status Cont
d
Precision Update Status
Precision Update Status
• ASTM NEG Fuel Exchange Program
ASTM NEG Fuel Exchange Program
Year
DCN
σ
# Labs
CN
σ
# Labs
2003
45.58
1.12
5
45.09
1.19
17
2004
48.06
0.82
4
48.18
1.34
18
2005
45.18
0.80
6
45.04
1.55
19
2006
47 38
47.38
0 99
0.99
7
47 74
47.74
1 50
1.50
21
2007
44.90
0.96
6
44.67
1.26
20
2008
47.05
0.93
8
47.70
1.19
21
2009
45.90
0.95
8
45.34
1.37
21
2010*
47.11
0.97
10
47.49
1.26
22
Average
46 36
46.36
0 94
0.94
7
46 36
46.36
1 34
1.34
20
* 2010 data up to August 2010
Precision Update Status
Precision Update Status
• Energy Institute IP Fuel Exchange Program
Energy Institute IP Fuel Exchange Program
Year
DCN
σ
# Labs
CN
σ
# Labs
2006
52.90
1.00
9
52.30
1.42
18
2007
51.46
0.78
12
51.29
1.53
18
2008
52.46
0.89
14
52.63
1.10
15
2009
52 30
52.30
0 88
0.88
15
52 01
52.01
1 33
1.33
18
2010*
51.97
0.83
18
51.94
1.54
18
Average
52.23
0.91
12
51.94
1.40
18
* 2010 data up to August 2010
Update on Refinery On‐Line Model (
(ROLM) IQT™
)
• Automated Bleed Valve System
Automated Bleed Valve System
– Fuel system flushing between samples
– Torque‐limiting mechanism
New Reference Fuels
New Reference Fuels
• Primary
Primary reference fuel blends of cetane and reference fuel blends of cetane and
heptamethylnonane (HMN) are being experimented with in the range from 65‐100
• The reference fuels are being blended according to the Cetane Scale – CN = %vol Cetane + 0.15 * %vol HMN
• As anticipated, the DCN results from the IQT™ match the Cetane Scale New Reference Fuel Blends Cont’d.
New Reference Fuel Blends Cont
d.
Derived Cetan
ne Number (D
DCN)
120
IQT A
IQT020
IQT077
IQT
B
IQT120
IQT
C
DCN/ID Relationship
110
100
90
80
70
60
22
2.2
24
2.4
26
2.6
28
2.8
Ignition Delay (ms)
3
32
3.2
Scope Expansion (>65CN, <30CN)
Scope Expansion (>65CN, <30CN) • The results from the experiments are very promising
e esu s o
e e pe e s a e e y p o s g
• Additional tests have shown that HMN is 15DCN using the IQT, which is its definition
• The primary reference fuels will be used to expand the scope of D6890 from 15‐33 and 65‐100 DCN
• This would permit the IQT™ conversion equation to be anchored at three additional points: 15, 65, and 100 DCN • Anchoring the IQT™ conversion equation to the Cetane Anchoring the IQT™ conversion equation to the Cetane
Scale will enable it to be considered a standalone method
Reference Fuels Package
Reference Fuels Package
• Quality
Quality controlled reference fuels are available for all controlled reference fuels are available for all
operators from AET:
–
–
–
–
–
Heptane
MCH
Low Cetane Check Fuel
High Cetane Check Fuel
65.2 DCN Fuel
Durability track record and recent d bl
durability improvements
• Some
Some heavy use refineries have utilized the IQT
heavy use refineries have utilized the IQT™ for for
more than 28,000 tests or 1,250,00 combustion events
• Exhaust and intake air valves have been removed as a frequent repair component
• Fuel injection nozzles can last from 6 months to 2 or more years
Update on Near ‐ Totally Automated Laboratory Model (n ‐
b
d l ( TALM) IQT™
)
• Electronic pressure control (UG Driven)
Electronic pressure control (UG Driven)
Gas hook‐ups
Set point adjustment
adjustment controls
Nitrogen pressure display
Update on Near ‐ Totally Automated Laboratory Model (n ‐
b
d l ( TALM) IQT™ Cont’d.
)
’d
• Automatic flushing (fuel injector nozzle)
Automatic flushing (fuel injector nozzle)
Pneumatic actuator
Solenoid valve
Standard IQT™ bleed valve
Update on Near ‐ Totally Automated Laboratory Model (n ‐
b
d l ( TALM) IQT™ Cont’d.
)
’d
• Automatic flushing (fuel injection pump)
Automatic flushing (fuel injection pump)
Pneumatic actuator
Standard IQT™ bleed valve
bleed valve
Solenoid valve
Update on Near ‐ Totally Automated Laboratory Model (n ‐
b
d l ( TALM) IQT™ Cont’d.
)
’d
• New drip free fuel reservoir (UG Driven)
New drip free fuel reservoir (UG Driven)
Update on Near ‐ Totally Automated Laboratory Model (n ‐
b
d l ( TALM) IQT™ Cont’d.
)
’d
• New
New enclosure design will be unveiled in November enclosure design will be unveiled in November
2010
Update on Near ‐ Totally Automated Laboratory Model (n ‐
b
d l ( TALM) IQT™ Cont’d.
)
’d
• Automated
Automated control of nozzle tip and combustion control of nozzle tip and combustion
chamber pressure transducer temperature
Update on Near ‐ Totally Automated Laboratory Model (n ‐
b
d l ( TALM) IQT™ Cont’d.
)
’d
• Automated
Automated control of nozzle tip and combustion control of nozzle tip and combustion
chamber pressure transducer temperature
Flow sensor with rate output
rate output
Flow indicator
Update on Near ‐ Totally Automated Laboratory Model (n ‐
b
d l ( TALM) IQT™ Cont’d.
)
’d
• Updated
Updated graphical user interface (test and parameter graphical user interface (test and parameter
status at a glance) (UG driven)
Update on Near ‐ Totally Automated Laboratory Model (n ‐
b
d l ( TALM) IQT™ Cont’d.
)
’d
• Updated
Updated graphical user interface (test and parameter graphical user interface (test and parameter
status at a glance) (UG driven)
Update on Near ‐ Totally Automated Laboratory Model (n ‐
b
d l ( TALM) IQT™ Cont’d.
)
’d
• Automated Automated ‐ Self checking of calibration
Self checking of calibration
– Verify SQC fuel test results against quality control limits
– Prompt to start automatic calibration procedure if required
• Automated ‐ Self calibration
– Determine change in set point required to achieve ARV for g
p
q
n‐heptane and verify that new set point is correct
– Verify the instrument’s measurement sensitivity using methylcyclohexane
th l l h
– Perform post‐calibration quality control test
Update on Near ‐ Totally Automated Laboratory Model (n ‐
b
d l ( TALM) IQT™ Cont’d.
)
’d
• Precision improvement data
Precision improvement data
1L Fuel Reservoir
Update on Near ‐ Totally Automated Laboratory Model (n ‐
b
d l ( TALM) IQT™ Cont’d.
)
’d
• Precision improvement data
Precision improvement data
Deriived Cetan
ne Numbe
er (DCN
N)
44.0
43.5
43.0
42.5
42.0
41.5
41 0
41.0
40.5
40.0
9:00 AM
1:00 PM
5:00 PM
9:00 PM
1:00 AM
5:00 AM
Experimental Results
9:00 AM
1:00 PM
Update on Near ‐ Totally Automated Laboratory Model (n ‐
b
d l ( TALM) IQT™ Cont’d.
)
’d
• The
The new enclosure will further improve instrument new enclosure will further improve instrument
safety
Ease of Maintenance
Ease of Maintenance
• Use
Use of bellville
of bellville washers on the three combustion washers on the three combustion
chamber studs mean that high temperature gasket life is greatly extended
• The new enclosure will permit easier access for periodic maintenance
periodic maintenance
Summary
• From
From 1993 to 2010 work has been ongoing to 1993 to 2010 work has been ongoing to
improve the capability, precision, and durability of the IQT™
• New developments for the Totally Automated Laboratory Model (TALM) IQT™ will further its Laboratory Model (TALM) IQT
will further its
capability and durability characteristics for use with a broad range of fuel options over a cetane range of 15 g
p
g
to 100