ASTM F2466-10
(Practice)Standard Practice for Determining Silicone Volatiles in Silicone Rubber for Transportation Applications
Standard Practice for Determining Silicone Volatiles in Silicone Rubber for Transportation Applications
SIGNIFICANCE AND USE
Use of this practice in conjunction with realistic maximum volatility tolerance level can help minimize the risk of oxygen sensor dysfunction from formed-in-place-sealants in transportation applications. This practice provides a method for determination of percentage volatiles in silicone elastomers. The volatile silicones from a commercial silicone are primarily cyclo dimethyl-siloxane. Other species present having GC retention times similar to those of the cyclics are assumed to be silicone as well.
SCOPE
1.1 This practice covers a means to determine the percent silicone-producing volatiles present in heat-cured silicone rubber and room temperature-cured silicones (RTV).
1.2 Silicone-producing volatiles contribute to fouling of oxygen sensor systems used in the control of vehicle emissions.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
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Designation: F2466 − 10
Standard Practice for
Determining Silicone Volatiles in Silicone Rubber for
1
Transportation Applications
This standard is issued under the fixed designation F2466; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope oxygen sensor dysfunction from formed-in-place-sealants in
transportationapplications.Thispracticeprovidesamethodfor
1.1 This practice covers a means to determine the percent
determination of percentage volatiles in silicone elastomers.
silicone-producing volatiles present in heat-cured silicone
The volatile silicones from a commercial silicone are primarily
rubber and room temperature-cured silicones (RTV).
cyclo dimethyl-siloxane. Other species present having GC
1.2 Silicone-producing volatiles contribute to fouling of
retentiontimessimilartothoseofthecyclicsareassumedtobe
oxygen sensor systems used in the control of vehicle emis-
silicone as well.
sions.
1.3 This standard does not purport to address all of the
5. Apparatus
safety concerns, if any, associated with its use. It is the
5.1 Gas Chromatograph, fused silica capillary column sys-
responsibility of the user of this standard to establish appro-
tem equipped with a flame ionization detector, split-type
priate safety and health practices and determine the applica-
capillary column injector, temperature programming capability
bility of regulatory limitations prior to use.
and an appropriate data recording system. An alternative unit
may be an equivalent instrument equipped with a thermal
2. Referenced Documents
conductivity detector, or as agreed upon between producer and
2
2.1 ASTM Standards:
user. Specific column and operating conditions should be
D3182 PracticeforRubber—Materials,Equipment,andPro-
selected to optimize instrument response and chromatographic
cedures for Mixing Standard Compounds and Preparing
resolution, particularly separation of the internal standard from
Standard Vulcanized Sheets
extracted sample components.
E177 Practice for Use of the Terms Precision and Bias in
5.2 Column, suggested to be used is 30 to 60 m by 0.25 mm
ASTM Test Methods
with 0.25 to 1.5 µm DB-1 or DB-5 fused silica capillary
E691 Practice for Conducting an Interlaboratory Study to
column or equivalent.
Determine the Precision of a Test Method
5.3 Operating conditions are:
3. Summary of Practice
5.3.1 Column—50 to 320°C at 10°C/min (a post-analysis
3.1 This practice consists of four (4) basic steps: (1) the
period may be required to elute higher boiling components
silicone is cured to its elastomeric form, (2) the volatiles are
prior to subsequent analyses).
extracted from the cured material, (3) the extract is separated
5.3.2 Injector—290°C.
and measured by gas chromatography (GC), and (4) the GC
5.3.3 Detector—325°C.
results are quantified using a siloxane calibration.
5.3.4 Sample Size—1 µL.
4. Significance and Use
5.3.5 Injector Split Ratio—2:1 to 50:1 (adjusted as needed).
5.3.6 Helium or Nitrogen, for the carrier gas.
4.1 Use of this practice in conjunction with realistic maxi-
5.3.7 Carrier Gas Flow Velocity—1 to 2 mL/min (adjusted
mum volatility tolerance level can help minimize the risk of
as needed for column dimensions).
1
5.4 Humidity Chamber, or controlled lab environment.
ThispracticeisunderthejurisdictionofASTMCommitteeF03onGasketsand
is the direct responsibility of Subcommittee F03.50 on Analytical Test Methods.
5.5 Wrist-Action Mechanical Shaker.
Current edition approved May 1, 2010. Published June 2010. Originally
approved in 2005. Last previous edition approved in 2005 as F2466 – 05. DOI:
5.6 Analytical Balance, with glass draft shield capable of
10.1520/F2466-10.
2
0.0001 g accuracy.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
5.7 30-mL Vials, flint glass, with screw cap (polyethylene
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. lined).
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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F2466 − 10
5.8 Syringe, capable of accurately delivering 20 6 0.1 µL
ADn = the area under the curve for each siloxane species
(no plastic elements used due to solvents used).
from4to10
DoD = thedodecanestandard,whichisarbitrarilygivena
5.9 Solvents and standards used are pentane (99 %) and
response factor of “1” (one), and is used as the
dodecane (99 %), both spectral grade.
basis for calculating the response factors of the
5.10 Rigid Pla
...
This document is not anASTM standard and is intended only to provide the user of anASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation:F2466–05 Designation:F2466–10
Standard Practice for
Determining Silicone Volatiles in Silicone Rubber for
1
Transportation Applications
This standard is issued under the fixed designation F2466; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope
1.1 This practice covers a means to determine the percent silicone-producing volatiles present in heat-cured silicone rubber and
room temperature-cured silicones (RTV).
1.2 Silicone-producing volatiles contribute to fouling of oxygen sensor systems used in the control of vehicle emissions.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory
limitations prior to use.
2. Referenced Documents
2
2.1 ASTM Standards:
D3182 Practice for RubberMaterials, Equipment, and Procedures for Mixing Standard Compounds and Preparing Standard
VulcanizedSheetsMaterials,Equipment,andProceduresforMixingStandardCompoundsandPreparingStandardVulcanized
Sheets
E177 Practice for Use of the Terms Precision and Bias in ASTM Test Methods
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
3. Summary of Practice
3.1 This practice consists of four (4) basic steps: (1) the silicone is cured to its elastomeric form, (2) the volatiles are extracted
from the cured material, (3) the extract is separated and measured by gas chromatography (GC), and (4) the GC results are
quantified using a siloxane calibration.
4. Significance and Use
4.1 Use of this practice in conjunction with realistic maximum volatility tolerance level can help minimize the risk of oxygen
sensordysfunctionfromformed-in-place-sealantsintransportationapplications.Thispracticeprovidesamethodfordetermination
of percentage volatiles in silicone elastomers. The volatile silicones from a commercial silicone are primarily cyclo
dimethyl-siloxane. Other species present having GC retention times similar to those of the cyclics are assumed to be silicone as
well.
5. Apparatus
5.1 Gas Chromatograph, equipped with a dual column, dual thermal conductivity detectors, differential flow control, linear
temperature programming capability, and an appropriate 1 mV potentiometric recorder.An alternative unit may be the equivalent
ofaHewlettPackard5880A,equippedwithaflameionizationdetector,orasagreeduponbetweenproduceranduser.,fusedsilica
capillary column system equipped with a flame ionization detector, split-type capillary column injector, temperature programming
capability and an appropriate data recording system.An alternative unit may be an equivalent instrument equipped with a thermal
conductivity detector, or as agreed upon between producer and user. Specific column and operating conditions should be selected
to optimize instrument response and chromatographic resolution, particularly separation of the internal standard from extracted
sample components.
5.2 Column, to be used with the first GC is 2.4 m by 0.32 cm stainless steel with a 5% OV-101 coating and 80/100 Chromosorb
1
This practice is under the jurisdiction of ASTM Committee F03 on Gaskets and is the direct responsibility of Subcommittee F03.50 on Analytical Test Methods.
Current edition approved March 1, 2005. Published April 2005. DOI: 10.1520/F2466-05.
CurrenteditionapprovedMay1,2010.PublishedJune2010.Originallyapprovedin2005.Lastpreviouseditionapprovedin2005asF2466 – 05.DOI:10.1520/F2466-10.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. ForAnnualBookofASTMStandards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1
---------------------- Page: 1 ----------------------
F2466–10
W, HP. The HP 5880Atype GC uses a column 60 m by 0.25 mm with 0.25-1 µm DB-1 or SE30 fused silica capillary column or
equivalent.
5.3Operating conditions for first GC type are: , suggested to be used is 30 to 60 m by 0.25 mm with 0.25 to 1.5 µm DB-1 or
DB-5 fused silica capillary column or equivalent.
5.3 Operating conditions are:
5.3.1 Colum
...
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