proposal: expanding vgra for astm d7216 - annex a2 years... · 2010. 11. 8. · d7216 - annex a2...

Proposal: Expanding VGRA for ASTM D7216 - Annex A2

API BOI/VGRA Meeting October 2010

VGRA for ASTM D7216 Annex A2Current 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-20,5W-30,10W-30 and 10W-40


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


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.

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 GraphsSeal 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

Company A – ASTM D7216 A2 Extending VGRA Study

-5.0 0.0 5.0 10.0

ACM-1 Volume-10.0 -5.0 0.0 5.0 10.0

ACM-1 Hardness-40.0 -20.0 0.0 20.0 40.0

ACM-1 Tensile

5.0

6.0

7.0

8.0

9.0

10.0

11.0

12.0

Base

Oil

Visc

osity

@ 1

00C,

cSt

SAE 40

SAE 30

20W-50

15W-40

10W-4010W-30

5W-20

-0.3

SAE 40

SAE 30

20W-50

15W-40

10W-4010W-30

5W-20

4.3

SAE 40

SAE 30

20W-50

15W-40

10W-4010W-30

5W-20

-6.1

Polyacrylate (ACM-1) vs. Base Oil Vis @ 100°C

May be significant if p <= 0.05

R2: 0.97p: <0.0001

-5.0 0.0 5.0 10.0

HNBR-1 Volume-10.0 -5.0 0.0 5.0

HNBR-1 Hardness-20.0 -10.0 0.0 10.0

HNBR-1 Tensile

5.0

6.0

7.0

8.0

9.0

10.0

11.0

12.0

Base

Oil

Visc

osity

@ 1

00C,

cSt

SAE 40

SAE 30

20W-50

15W-40

10W-4010W-30

5W-20

-0.6SAE 40

SAE 30

20W-50

15W-40

10W-4010W-30

5W-20

-0.7SAE 40

SAE 30

20W-50

15W-40

10W-4010W-30

5W-20

3.6

Hydrogenated Nitrile (HNBR-1) vs. Base Oil Vis @ 100°C


R2: 0.73 p: 0.014

R2: 0.73 p: 0.014

0.0 10.0 20.0 30.0 40.0

VMQ-1 Volume-30.0 -20.0 -10.0 0.0 10.0

VMQ-1 Hardness-40.0 -20.0 0.0 20.0

VMQ-1 Tensile

5

6

7

8

9

10

11

12

Base

Oil

Visc

osity

@ 1

00C,

cSt

SAE 40

SAE 30

20W-50

15W-40

10W-4010W-30

5W-20

15.5

SAE 40

SAE 30

20W-50

15W-40

10W-4010W-30

5W-20

-13.4

SAE 40

SAE 30

20W-50

15W-40

10W-4010W-30

5W-20

-9.5

Silicon (VMQ-1) vs. Base Oil Vis @ 100°C


R2: 0.99 p: <0.0001

R2: 0.89p: 0.001

R2: 0.96p: <0.0001

-2.0 -1.0 0.0 1.0 2.0 3.0

FKM-1 Volume-6.0 -4.0 -2.0 0.0 2.0 4.0 6.0

FKM-1 Hardness-60.0 -40.0 -20.0 0.0

FKM-1 Tensile

5

6

7

8

9

10

11

12

Base

Oil

Visc

osity

@ 1

00C,

cSt

SAE 40

SAE 30

20W-50

15W-40

10W-4010W-30

5W-20

0.3

SAE 40

SAE 30

20W-50

15W-40

10W-4010W-30

5W-20

-0.4

SAE 40

SAE 30

20W-50

15W-40

10W-4010W-30

5W-20

-12.3

Fluorocarbon (FKM-1) vs. Base Oil Vis @ 100°C


0.0 10.0 20.0 30.0

AEM-1 Volume-20.0 -10.0 0.0 10.0

AEM-1 Hardness-30.0 -20.0 -10.0 0.0 10.0 20.0 30.0

AEM-1 Tensile

5

6

7

8

9

10

11

12

Base

Oil

Visc

osity

@ 1

00C,

cSt

SAE 40

SAE 30

20W-50

15W-40

10W-4010W-30

5W-20

13.4

SAE 40

SAE 30

20W-50

15W-40

10W-4010W-30

5W-20

-5.4

SAE 40

SAE 30

20W-50

15W-40

10W-4010W-30

5W-20

2.3

Ethylene Acrylate (AEM-1) vs. Base Oil Vis @ 100°C


R2: 0.96 p: <0.0001

R2: 0.97 p: <0.0001

Summary

• 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 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 A – Conclusions

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

Data Spread

Seal Variable Limits LimitSpread Data Range %LimitSpreadUsedEthylene Acrylic AEM-1 Volume % -5 to 30 35 8.79 25

Hardness pts -20 to 10 30 8 27Tensile Strength % -30 to 30 60 14.9 25

Fluorocarbon FKM-1 Volume % -2 to 3 5 0.79 16Hardness pts -6 to 6 12 3 25

Tensile Strength % -65 to 10 75 19.7 26Nitrile HNBR-1 Volume % -5 to 10 15 4.12 27


Polyacrylate ACM-1 Volume % -5 to 10 15 4.05 27Hardness pts -10 to 10 20 7 35

Tensile Strength % -40, 40 80 10.9 14Silicone VMQ-1 Volume % -5 to 40 45 20 44

Hardness pts -30 to 10 40 19 48Tensile Strength % -50 to 5 55 39 71

VariableRange of

%LimitSpreadUsedVolume 16 to 44

Hardness 20 to 48Tensile Strength 14 to 71

Seal Variable Limits LimitSpread Data Range %LimitSpreadUsedEthylene Acrylic AEM-1 Volume % -5 to 30 35 8.79 25


Fluorocarbon FKM-1 Volume % -2 to 3 5 0.79 16Hardness pts -6 to 6 12 3 25

Tensile Strength % -65 to 10 75 19.7 26Nitrile HNBR-1 Volume % -5 to 10 15 4.12 27


Polyacrylate ACM-1 Volume % -5 to 10 15 4.05 27Hardness pts -10 to 10 20 7 35

Tensile Strength % -40, 40 80 10.9 14Silicone VMQ-1 Volume % -5 to 40 45 20 44

Hardness pts -30 to 10 40 19 48Tensile Strength % -50 to 5 55 39 71

VariableRange of

%LimitSpreadUsedVolume 16 to 44

Hardness 20 to 48Tensile Strength 14 to 71

Company B – Data Range

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

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

Company D Investigation of VGRA extension – ASTM D7216 Annex A2

% Volume Change Company D

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.

Ethyl Acryl (AEM)

-5 5 15 25

Nitrile (HNBR)

-5 0 5 10

PolyAcrylate (ACM)

5.00

6.00

7.00

8.00

9.00

10.00

11.00

12.00

-5 0 5 10

BO

BV,

cSt

Fluorocarb (FKM)

-2 -1 0 1 2 3

Silicone (VQM)

-5 10 25 40

Hardness Change Company D

PolyAcrylate (ACM)

5.00

6.00

7.00

8.00

9.00

10.00

11.00

12.00

-10 -5 0 5 10

BO

BV,

cSt

Ethyl Acryl (AEM)

-20 -10 0 10

Fluorocarb (FKM)

-6 -4 -2 0 2 4 6

Silicone (VQM)

-30 -20 -10 0 10

Nitrile (HNBR)

-10 -5 0 5

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.

Tensile Strength % Change Company D

PolyAcrylate (ACM)

5.00

6.00

7.00

8.00

9.00

10.00

11.00

12.00

-40 -20 0 20 40

BO

BV,

cSt

Nitrile (HNBR)

-20 -10 0 10

Fluorocarb (FKM)

-65 -40 -15 10

EthylAcryl(AEM)

-30 -15 0 15 30

Silicone (VQM)

-30 -20 -10 0 10

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.

Seal Type / Parameter

Observed Range of results

ASTM R as of July 15 2010

Trend R2 Conclusion

ACM Volume1.33 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 Volume1.31 1.7 -0.66 Supports BOBV trend.


Hardness 2 2.4 0.06 Supports Full VGRA. No evidence of BOBV impact.

Tensile 10.1 13.6 0.03 Supports Full VGRA

FKM Volume 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

VMQ Volume7.25 7.5 -0.72 Supports BOBV trend.


Hardness 6 5.7 +0.79 Indicates BOBV trend.Also supports Full VGRA.

Tensile 11.8 10.6 +0.40 Supports BOBV Trend.Also supports Full VGRA.

AEM Volume3.16 2.2 - 0.81 Data indicates BOBV trend.


Hardness 2 2.5 +0.30 Data supports Full VGRA. Weakly supports BOBV trend.

Tensile 7.9 10.8 +0.06 Supports Full VGRA.

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.

For Viscosity Grades not currently on the VGRA table

For Now: BOV Bookends, all ParametersConsider later Dropping Bookend on Parameters as

indicated by further data.

Proposal to Expand current VGRA for D7216 Annex A2

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.

Matrix Oil 1 Matrix Oil 2 Candidate Oil A Candidate Oil B

Base Oil Viscosity @ 100°C, cSt

4.6 10.9 9.0 12.4

D7216 A2 Result Pass Pass

Test Required? No Yes

Reason Formulation falls within the base oil

viscosity range

Formulation does not fall within the base oil viscosity

range

proposal: expanding vgra for astm d7216 - annex a2 years... · 2010. 11. 8. · d7216 - annex a2...

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