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ASTM D7216-VGRA for Seals

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Proposal: Expanding VGRA for ASTM
D7216 - Annex A2
API BOI/VGRA Meeting October 2010
VGRA for ASTM D7216 Annex A2
Current Status
Extensive data was collected and analyzed to
support the existing VGRA adopted by API for the
SAE viscosity grades: 0W-20, 0W-30,5W-20,5W30,10W-30 and 10W-40
VGRA for ASTM D7216 Annex A2
Current Status
Extending the VGRA to other grades would be
beneficial since the API SN specification also
requires elastomer testing.
One company indicated that the elastomer data was
quite insensitive to viscosity grade changes and
that those parameters where differences were
seen were correlated to BOV
VGRA for ASTM D7216 Annex A2
Current Status
Since technology impacts the elastomer results and
limited data existed in some viscosity grades
individual companies performed data analyses.
Focus of analysis was to determine if there was
parameter sensitivity to change in viscosity grade
and if so whether BOV was appropriate to describe
the sensitivity.
Company A – ASTM D7216 A2
Extending VGRA
Study
Viscosity
Grade
Study
•
ASTM D7216 A2 VGRA study
– Same DI/VM/PPD system
•
– Gp II base stock slate
– Same Lab
– Viscosity grades tested
• Covered by Current VGRA table
– 5W-20
– 10W-30
– 10W-40
• Not covered by current VGRA table
– 15W-40
– 20W-50
– SAE 30
– SAE 40
For some seal parameters, the data showed correlation to viscosity
grade
Company A – ASTM D7216 A2 Extending VGRA Study
Explanation of Graphs
Seal parameter results were plotted verse formulation BOV @ 100C
• Line for Average of all results was added along ± reproducibility for
that parameter.
• Where correlation was found to be significant – that line is shown
along with R2 & p
Variable
R
Variable
R
ACM-1 Volume Change, %
0.48
FKM-1 Volume Change, %
0.50
ACM-1 Hardness Change, Points
1.71
FKM-1 Hardness Change, Points
2.91
ACM-1 Tensile Strength Change, %
13.86
FKM-1 Tensile Strength Change, %
10.95
HNBR-1 Volume Change, %
0.53
AEM-1 Volume Change, %
1.37
HNBR-1 Hardness Change, Points
2.44
AEM-1 Hardness Change, Points
2.02
HNBR-1 Tensile Strength Change, %
13.19
AEM-1 Tensile Strength Change, %
7.53
VMQ-1 Volume Change, %
7.48
VMQ-1 Hardness Change, Points
7.06
VMQ-1 Tensile Strength Change, %
8.46
R = Reproducibility: from EOEC Information Letter 09-2 (9/1/2009). Based on TMC reference oil 1006-1 from 2/19/09 to 4/30/09
Polyacrylate (ACM-1) vs. Base Oil Vis @ 100°C
-0.3
4.3
SAE 40
-6.1
SAE 40
SAE 40
12.0
Base Oil Viscosity @ 100C, cSt
11.0
20W-50
20W-50
20W-50
R2: 0.97
p: <0.0001
10.0
SAE 30
9.0
SAE 30
SAE 30
8.0
15W-40
7.0
6.0
15W-40
10W-40
10W-30
5.0
0.0
10W-40
10W-30
10W-40
10W-30
5W-20
5W-20
-5.0
15W-40
5.0
ACM-1 Volume
10.0 -10.0
-5.0
0.0
5.0
ACM-1 Hardness
10.0
5W-20
-40.0
-20.0
0.0
20.0
40.0
ACM-1 Tensile
May be significant if p <= 0.05
Hydrogenated Nitrile (HNBR-1) vs. Base Oil Vis @ 100°C
-0.6
SAE 40
-0.7
3.6
SAE 40
SAE 40
12.0
Base Oil Viscosity @ 100C, cSt
11.0
20W-50
20W-50
R2: 0.73
p: 0.014
10.0
9.0
20W-50
R2: 0.73
p: 0.014
SAE 30
SAE 30
SAE 30
8.0
15W-40
7.0
6.0
15W-40
10W-40
10W-30
5.0
10W-40
10W-30
5W-20
-5.0
0.0
15W-40
5.0
HNBR-1 Volume
10W-40
10W-30
5W-20
10.0
-10.0
-5.0
5W-20
0.0
HNBR-1 Hardness
5.0
-20.0
-10.0
0.0
10.0
HNBR-1 Tensile
May be significant if p <= 0.05
Silicon (VMQ-1) vs. Base Oil Vis @ 100°C
15.5
-13.4
-9.5
SAE 40
SAE 40
SAE 40
12
Base Oil Viscosity @ 100C, cSt
11
20W-50
20W-50
R2: 0.96
p: <0.0001
10
9
20W-50
R2: 0.99
p: <0.0001
SAE 30
R2: 0.89
p: 0.001
SAE 30
SAE 30
8
15W-40
7
6
15W-40
10W-40
10W-30
5
10W-40
10W-30
5W-20
0.0
10.0
20.0
30.0
VMQ-1 Volume
15W-40
10W-40
10W-30
5W-20
40.0
-30.0
-20.0
5W-20
-10.0
0.0
VMQ-1 Hardness
10.0
-40.0
-20.0
0.0
20.0
VMQ-1 Tensile
May be significant if p <= 0.05
Fluorocarbon (FKM-1) vs. Base Oil Vis @ 100°C
0.3
-0.4
SAE 40
-12.3
SAE 40
SAE 40
12
Base Oil Viscosity @ 100C, cSt
11
20W-50
20W-50
SAE 30
SAE 30
20W-50
10
9
SAE 30
8
7
6
15W-40
15W-40
10W-40
10W-30
10W-40
10W-30
5
5W-20
-2.0
-1.0
0.0
15W-40
10W-40
10W-30
5W-20
1.0
FKM-1 Volume
2.0
3.0
-6.0
-4.0
-2.0
5W-20
0.0
2.0
FKM-1 Hardness
4.0
6.0
-60.0
-40.0
-20.0
0.0
FKM-1 Tensile
May be significant if p <= 0.05
Ethylene Acrylate (AEM-1) vs. Base Oil Vis @ 100°C
13.4
12
-5.4
SAE 40
2.3
SAE 40
SAE 40
Base Oil Viscosity @ 100C, cSt
11
20W-50
20W-50
10
20W-50
R2: 0.97
p: <0.0001
R2: 0.96
p: <0.0001
9
SAE 30
SAE 30
SAE 30
8
7
15W-40
15W-40
15W-40
6
10W-40
10W-30
10W-40
10W-30
5W-20
5W-20
10W-40
10W-30
5
0.0
10.0
20.0
AEM-1 Volume
30.0
-20.0
-10.0
5W-20
0.0
AEM-1 Hardness
10.0
-30.0 -20.0 -10.0
0.0
10.0
20.0
30.0
AEM-1 Tensile
May be significant if p <= 0.05
Company A – Conclusions
•
Within the same Gp II slate,
8 out of 15 seal parameters
show a response to
formulation BOV
– BOV range for “ILSAC
grades” was 1cSt
– BOV range for “Non-ILSAC
grades” was 6.6cSt
•
Results from the other seal
parameters not responsive to
BOV fall within the
repeatability of the average
– repeatability defined by
reference oil T1006
Variable
Summary
BOV (Visgrade)
Impact
ACM-1 Volume Change, %
Yes
ACM-1 Hardness Change, Points
No
ACM-1 Tensile Strength Change, %
No
HNBR-1 Volume Change, %
Yes
HNBR-1 Hardness Change, Points
Yes
HNBR-1 Tensile Strength Change, %
No
VMQ-1 Volume Change, %
Yes
VMQ-1 Hardness Change, Points
Yes
VMQ-1 Tensile Strength Change, %
Yes
FKM-1 Volume Change, %
No
FKM-1 Hardness Change, Points
No
FKM-1 Tensile Strength Change, %
No
AEM-1 Volume Change, %
Yes
AEM-1 Hardness Change, Points
Yes
AEM-1 Tensile Strength Change, %
No
Company B Investigation of VGRA
extension – ASTM D7216 Annex A2
Company B analyzed by parameter across the
multiple seal materials
Three Group II basestocks were included in the
analysis with two different DI systems
Volume
Hardness
Tensile Strength
Company B – Data Range
Data Spread
Seal
Ethylene Acrylic AEM-1
Fluorocarbon FKM-1
Nitrile HNBR-1
Polyacrylate ACM-1
Silicone VMQ-1
Variable
Volume
Hardness
Tensile Strength
Volume
Hardness
Tensile Strength
Volume
Hardness
Tensile Strength
Volume
Hardness
Tensile Strength
Volume
Hardness
Tensile Strength
Limits
LimitSpread
%
-5 to 30
35
pts -20 to 10
30
% -30 to 30
60
%
-2 to 3
5
pts -6 to 6
12
% -65 to 10
75
%
-5 to 10
15
pts -10 to 5
15
% -20 to 15
35
% -5 to 10
15
pts
-10 to 10
20
% -40, 40
80
%
-5 to 40
45
pts -30 to 10
40
% -50 to 5
55
Data Range
8.79
8
14.9
0.79
3
19.7
4.12
3
15.1
4.05
7
10.9
20
19
39
%LimitSpreadUsed
25
27
25
16
25
26
27
20
43
27
35
14
44
48
71
Range of
Variable
%LimitSpreadUsed
Volume
16 to 44
Hardness
20 to 48
Tensile Strength
14 to 71
Company B Investigation of VGRA
extension – ASTM D7216 Annex A2
Company B Data spread is relatively narrow showing
that even when basestock slates and technologies
were modified the data for seal parameters were
not greatly influenced over a wide span of BOV.
Parameters may show no correlation within the span
but, at a minimum, bracketing by BOV should
provide ample measure of seal compatibility.
Company C Investigation of VGRA
extension – ASTM D7216 Annex A2
Company C evaluated two Group II and a Group II /
Bright Stock mixture
Data was collected over a 6 month period and
included two laboratories
Company C Elastomer Data Overview
•
ASTM D7216 A2 data - same DI/PPD system
– For multigrade oils, the same VM is used
– Oils are from two Group II base stock slates and one Group II/Bright
Stock mix
– Data is from two independent test labs
– Data was generated in the past 6 months (majority from the last 2
months)
– Viscosity grades tested
• Covered by current VGRA table
–
–
–
–
5W-20
5W-30
10W-30
10W-40
• Not covered by current VGRA table
– 20W-50
– SAE 30
– SAE 40
Company C Correlation Summary
•
•
•
•
Across this single DI/PPD
system, 7 out of 15 seal
parameters show a response
to formulation BOV
BOV impact determined
based on the P-value
threshold of 0.1
BOV range for “ILSAC
grades” is 0.9 cSt
BOV range for “Non-ILSAC
grades” is 6.0 cSt
Variable
BOV (Visgrade)
Impact
ACM-1 Volume Change, %
Yes
ACM-1 Hardness Change, Points
No
ACM-1 Tensile Strength Change, %
Yes
HNBR-1 Volume Change, %
No
HNBR-1 Hardness Change, Points
No
HNBR-1 Tensile Strength Change, %
No
VMQ-1 Volume Change, %
Yes
VMQ-1 Hardness Change, Points
Yes
VMQ-1 Tensile Strength Change, %
Yes
FKM-1 Volume Change, %
No
FKM-1 Hardness Change, Points
No
FKM-1 Tensile Strength Change, %
Yes
AEM-1 Volume Change, %
Yes
AEM-1 Hardness Change, Points
No
AEM-1 Tensile Strength Change, %
No
Polyacrylate (ACM-1) vs. Base Oil Vis @ 100°C Company C
Hydrogenated Nitrile (HNBR-1) vs. Base Oil Vis @ 100°C Company C
Silicon (VMQ-1) vs. Base Oil Vis @ 100°C Company C
Fluorocarbon (FKM-1) vs. Base Oil Vis @ 100°C Company C
Ethylene Acrylate (AEM-1) vs. Base Oil Vis @ 100°C Company C
Company C Conclusion and Request
• Data suggests that VGRA can be extended
• BOV appears to be appropriate measure foe
those parameters showing viscosity grade
sensitivity
Company D Investigation of VGRA
extension – ASTM D7216 Annex A2
Dataset Description
 All data run in certified stands in 2010
 10 oils, 3 10W-30, 2 10W-40, 3 15W-40,
1 15W-50, 1 20W-50.
 Constant DI and Treat rate.
 Constant VI.
 Same Grp II Basestock Slate,
4 oils mixed with minor amount Grp III
% Volume Change Company D
Silicone (VQM)
Nitrile (HNBR)
PolyAcrylate (ACM)
Fluorocarb (FKM)
Ethyl Acryl (AEM)
12.00
11.00
B OB V , cS t
10.00
9.00
8.00
7.00
6.00
5.00
-5
0
5
10
-5
0
5
10
-5
10
25
40
-2
-1
0
1
2
3
-5
5
15
25
X Axis width of each graph is GF-5 Specification Passing Range for that elastomer.
Arrows depict Volume Change ASTM Reproducibility Range for each elastomer.
Hardness Change Company D
Ethyl Acryl (AEM)
Nitrile (HNBR)
PolyAcrylate (ACM)
Silicone (VQM)
Fluorocarb (FKM)
12.00
11.00
B OB V , cS t
10.00
9.00
8.00
7.00
6.00
5.00
-10 -5
0
5
10
-10
-5
0
5
-30 -20 -10
0
10
-6 -4 -2
0
2
4
6
-20
-10
0
X Axis width of each graph is GF-5 Specification Passing Range for that elastomer.
Arrows depict Hardness Change ASTM Reproducibility Range for each elastomer.
10
Tensile Strength % Change Company D
PolyAcrylate (ACM)
Silicone (VQM)
Nitrile (HNBR)
Fluorocarb (FKM)
EthylAcryl(AEM)
12.00
11.00
BOBV, cSt
10.00
9.00
8.00
7.00
6.00
5.00
-40 -20
0
20
40
-20
-10
0
10
-30
-20
-10
0
10 -65
-40
-15
10 -30
-15
0
15
X Axis width of each graph is GF-5 Specification Passing Range for that elastomer.
Arrows depicts Tensile Strength ASTM Reproducibility Range for each elastomer.
30
Seal Type /
Parameter
Observed Range of
results
ASTM R as
1.33
0.90
-0.65
Supports BOBV trend.
Also supports Full VGRA.
Hardness
4
2.9
-0.02
Supports Full VGRA
Tensile
14.0
19.2
-0.32
Supports Full VGRA
HNBR Volume
1.31
1.7
-0.66
Supports BOBV trend.
Also supports Full VGRA.
2
2.4
0.06
Supports Full VGRA.
No evidence of BOBV impact.
10.1
13.6
0.03
Supports Full VGRA
0.20
0.42
-0.04
Supports Full VGRA
Hardness
1
2.8
-0.16
Supports Full VGRA
Tensile
10.4
12.2
-0.01
Supports Full VGRA
7.25
7.5
-0.72
Supports BOBV trend.
Also supports Full VGRA.
6
5.7
+0.79
Indicates BOBV trend.
Also supports Full VGRA.
11.8
10.6
+0.40
Supports BOBV Trend.
Also supports Full VGRA.
3.16
2.2
- 0.81
Data indicates BOBV trend.
Also supports Full VGRA.
2
2.5
+0.30
Data supports Full VGRA.
Weakly supports BOBV trend.
7.9
10.8
+0.06
Supports Full VGRA.
ACM
Volume
Hardness
Tensile
FKM
VMQ
Volume
Volume
Hardness
Tensile
AEM
Volume
Hardness
Tensile
of July 15 2010
Trend R2
Conclusion
Conclusions – Company D
 All data within expected Statistical Range
 10 of 15 within ASTM R, all others within
95 % Confidence Studentized Range, “q” @
n=10
 Results thus support Full VGRA between all
SAE grades up to 20W-50.
 Supports BOBV Trends seen in other data.
Conclusions
4 Companies with 5 technologies have data supporting extending VGRA for
this elastomer test for grades beyond those already covered.
Proposal is to ADD additional VGRA beyond existing viscosity grade table
Majority of data indicates that over a very wide range of viscosity grades and
BOV there is little effect to most seal parameters
All data sets support the concept of bracketing by Base Oil Viscosity for the
parameters where some variation is seen.
Proposal to Expand current VGRA for D7216
Annex A2
For Viscosity Grades not currently on the VGRA
table
For Now: BOV Bookends, all Parameters
Consider later Dropping Bookend on Parameters as
indicated by further data.
Proposal to Expand current VGRA for D7216
Annex A2
Augment the current VGRA Table with the following:
For viscosity grades not listed in the table above, bracketing two passing
formulations for a given technology may be used to waive additional testing.
VGRA is allowed if the candidate’s base oil viscosity @100°C falls within the
range of the base oil viscosity @100°C of the 2 passing formulations.
Base Oil Viscosity @
100°C, cSt
D7216 A2 Result
Test Required?
Reason
Matrix Oil 1
Matrix Oil 2
Candidate Oil A
Candidate Oil B
4.6
10.9
9.0
12.4
Pass
Pass
No
Yes
Formulation falls
within the base oil
viscosity range
Formulation does
not fall within the
base oil viscosity
range
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