ASTM D5508-16
(Test Method)Standard Test Method for Determination of Residual Acrylonitrile Monomer in Styrene-Acrylonitrile Copolymer Resins and Nitrile-Butadiene Rubber by Headspace-Capillary Gas Chromatography (HS-CGC)
Standard Test Method for Determination of Residual Acrylonitrile Monomer in Styrene-Acrylonitrile Copolymer Resins and Nitrile-Butadiene Rubber by Headspace-Capillary Gas Chromatography (HS-CGC)
SIGNIFICANCE AND USE
4.1 A measurement of the residual acrylonitrile in nitrile rubbers (NBR), styrene-acrylonitrile copolymers or ABS terpolymers will determine the polymer's suitability for various applications.
4.2 Under optimum conditions, the minimum level of detection of RAN in NBR, SAN, or ABS terpolymers is approximately 50 ppb.
SCOPE
1.1 This test method covers the determination of the residual acrylonitrile (RAN) content in nitrile-butadiene rubbers (NBR), styrene-acrylonitrile (SAN) copolymers, and rubber-modified acrylonitrile-butadiene-styrene (ABS) resins.
1.2 Any components that can generate acrylonitrile in the headspace procedure will constitute an interference. The presence of 3-hydroxypropionitrile in latices limits this procedure to dry rubbers and resins.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 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. Specific precautionary statements are given in 6.3 and 6.4.
Note 1: There is no known ISO equivalent to this standard.
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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
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Designation:D5508 −16
Standard Test Method for
Determination of Residual Acrylonitrile Monomer in Styrene-
Acrylonitrile Copolymer Resins and Nitrile-Butadiene
Rubber by Headspace-Capillary Gas Chromatography (HS-
1
CGC)
This standard is issued under the fixed designation D5508; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope* the polymer, solvent, plus a known standard addition of
acrylonitrile (AN). Both vials are agitated for a specified time
1.1 This test method covers the determination of the re-
under ambient conditions. After agitation, the vials are ther-
sidual acrylonitrile (RAN) content in nitrile-butadiene rubbers
mally equilibrated in a constant-temperature bath.
(NBR), styrene-acrylonitrile (SAN) copolymers, and rubber-
modified acrylonitrile-butadiene-styrene (ABS) resins. 3.2 After completion of the timed equilibration, an aliquot
of the heated headspace gas from each vial is injected into a
1.2 Any components that can generate acrylonitrile in the
capillary gas-chromatographic column using an automated
headspace procedure will constitute an interference. The pres-
injection system. The capillary column will provide the chro-
ence of 3-hydroxypropionitrile in latices limits this procedure
matographic resolution necessary to isolate theAN from other
to dry rubbers and resins.
volatiles potentially present. The AN response is measured
1.3 The values stated in SI units are to be regarded as
using a nitrogen-specific detector (NPD). The raw data signal
standard. No other units of measurement are included in this
is converted to a relative RAN concentration through a
standard.
standard addition calculation.
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the 4. Significance and Use
responsibility of the user of this standard to establish appro-
4.1 A measurement of the residual acrylonitrile in nitrile
priate safety and health practices and determine the applica-
rubbers (NBR), styrene-acrylonitrile copolymers or ABS ter-
bility of regulatory limitations prior to use. Specific precau-
polymers will determine the polymer’s suitability for various
tionary statements are given in 6.3 and 6.4.
applications.
NOTE 1—There is no known ISO equivalent to this standard.
4.2 Under optimum conditions, the minimum level of de-
tection of RAN in NBR, SAN, orABS terpolymers is approxi-
2. Referenced Documents
mately 50 ppb.
2
2.1 ASTM Standards:
E691Practice for Conducting an Interlaboratory Study to
5. Apparatus
Determine the Precision of a Test Method
5.1 Gas Chromatograph, equipped with a nitrogen-
phosphorus specific detector, backflush valve (see Fig. 1), split
3. Summary of Test Method
injector, and capable of accepting megabore (0.53 mm inside
3.1 Two dispersions (in o-dichlorobenzene) are prepared
diameter)fusedsilicacapillarycolumns.Detectormake-upgas
and sealed in headspace vials for each polymer; one vial
is required.
contains the polymer in solvent while the second vial contains
NOTE 2—The use of a backflush configuration will provide for
operating advantages, but its use is optional. Chlorinated solvents quench
1
ThistestmethodisunderthejurisdictionofASTMCommitteeD20onPlastics
the alkali bead in a nitrogen-phosphorous detector, producing a loss of
and is the direct responsibility of Subcommittee D20.70 on Analytical Methods and
signal. While the bead (signal) will recover as the solvent evacuates the
Section D20.70.02 on Chromatography.
detector, repeated quenching during a multi-run sequence may produce
Current edition approved Sept. 1, 2016. Published September 2016. Originally
instabilities in the signal (and precision) over the sequence period.
ε1
approved in 1994. Last previous edition approved in 2009 as D5508-94a(2009) .
DOI: 10.1520/D5508-16.
5.2 Automated Headspace Sampler, shall have a thermost-
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
atted sample tray capable of 90°C heating with constant
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
heatingtimes.Automatedsamplingoftheheadspacegasinthe
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. sample vials via a heated, constant-volume sample loop or
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959.
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM 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.
´1
Designation: D5508 − 94a (Reapproved 2009) D5508 − 16
Standard Test Method for
Determination of Residual Acrylonitrile Monomer in Styrene-
Acrylonitrile Copolymer Resins and Nitrile-Butadiene
Rubber by Headspace-Capillary Gas Chromatography (HS-
1
CGC)
This standard is issued under the fixed designation D5508; 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
ε NOTE—Reapproved with editorial changes in April 2009.
1. Scope*
1.1 This test method covers the determination of the residual acrylonitrile (RAN) content in nitrile-butadiene rubbers (NBR),
styrene-acrylonitrile (SAN) copolymers, and rubber-modified acrylonitrile-butadiene-styrene (ABS) resins.
1.2 Any components that can generate acrylonitrile in the headspace procedure will constitute an interference. The presence of
3-hydroxypropionitrile in latices limits this procedure to dry rubbers and resins.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 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. Specific precautionary statements are given in 6.3 and 6.4.
NOTE 1—There is no known ISO equivalent to this test method.standard.
2. Referenced Documents
2
2.1 ASTM Standards:
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
3. Summary of Test Method
3.1 Two dispersions (in o-dichlorobenzene) are prepared and sealed in headspace vials for each polymer; one vial contains the
polymer in solvent while the second vial contains the polymer, solvent, plus a known standard addition of acrylonitrile (AN). Both
vials are agitated for a specified time under ambient conditions. After agitation, the vials are thermally equilibrated in a
constant-temperature bath.
3.2 After completion of the timed equilibration, an aliquot of the heated headspace gas from each vial is injected into a capillary
gas-chromatographic column. An automated injection system is used to effect the transfer. column using an automated injection
system. The capillary column will provide the chromatographic resolution necessary to isolate the AN from other volatiles
potentially present. The AN response is measured using a nitrogen-specific detector (NPD). The raw data signal is converted to
a relative RAN concentration through a standard addition calculation.
4. Significance and Use
4.1 A measurement of the residual acrylonitrile in nitrile rubbers (NBR), styrene-acrylonitrile copolymers or ABS terpolymers
will determine the polymer’s suitability for various applications.
1
This test method is under the jurisdiction of ASTM Committee D20 on Plastics and is the direct responsibility of Subcommittee D20.70 on Analytical Methods and
Section D20.70.02 on Chromatography.
Current edition approved April 1, 2009Sept. 1, 2016. Published April 2009September 2016. Originally approved in 1994. Last previous edition approved in 20012009 as
ε1
D5508 - 94a(2001)(2009) . DOI: 10.1520/D5508-94AR09E01.10.1520/D5508-16.
2
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 Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D5508 − 16
4.2 Under optimum conditions, the minimum level of detection of RAN in NBR, SAN, or ABS terpolymers is approximately
50 ppb.
5. Apparatus
5.1 Gas Chromatograph, equipped with a nitrogen-phosphorus specific detector, backflush valve (see Fig. 1), split injector, and
capable of accepting megabore (0.53 mm inside diameter) fused silica capillary columns. Detector make-up gas is required.
NOTE 2—The use of a backflush configuration will provide for operating advantages, but its use is optional. Chlorinated solvents quench the alkali bead
in a nitrogen-phosphorous detector, producing a
...
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D5508 − 16
Standard Test Method for
Determination of Residual Acrylonitrile Monomer in Styrene-
Acrylonitrile Copolymer Resins and Nitrile-Butadiene
Rubber by Headspace-Capillary Gas Chromatography (HS-
1
CGC)
This standard is issued under the fixed designation D5508; 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* the polymer, solvent, plus a known standard addition of
acrylonitrile (AN). Both vials are agitated for a specified time
1.1 This test method covers the determination of the re-
under ambient conditions. After agitation, the vials are ther-
sidual acrylonitrile (RAN) content in nitrile-butadiene rubbers
mally equilibrated in a constant-temperature bath.
(NBR), styrene-acrylonitrile (SAN) copolymers, and rubber-
modified acrylonitrile-butadiene-styrene (ABS) resins. 3.2 After completion of the timed equilibration, an aliquot
of the heated headspace gas from each vial is injected into a
1.2 Any components that can generate acrylonitrile in the
capillary gas-chromatographic column using an automated
headspace procedure will constitute an interference. The pres-
injection system. The capillary column will provide the chro-
ence of 3-hydroxypropionitrile in latices limits this procedure
matographic resolution necessary to isolate the AN from other
to dry rubbers and resins.
volatiles potentially present. The AN response is measured
1.3 The values stated in SI units are to be regarded as
using a nitrogen-specific detector (NPD). The raw data signal
standard. No other units of measurement are included in this
is converted to a relative RAN concentration through a
standard.
standard addition calculation.
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the 4. Significance and Use
responsibility of the user of this standard to establish appro-
4.1 A measurement of the residual acrylonitrile in nitrile
priate safety and health practices and determine the applica-
rubbers (NBR), styrene-acrylonitrile copolymers or ABS ter-
bility of regulatory limitations prior to use. Specific precau-
polymers will determine the polymer’s suitability for various
tionary statements are given in 6.3 and 6.4.
applications.
NOTE 1—There is no known ISO equivalent to this standard.
4.2 Under optimum conditions, the minimum level of de-
tection of RAN in NBR, SAN, or ABS terpolymers is approxi-
2. Referenced Documents
mately 50 ppb.
2
2.1 ASTM Standards:
E691 Practice for Conducting an Interlaboratory Study to
5. Apparatus
Determine the Precision of a Test Method
5.1 Gas Chromatograph, equipped with a nitrogen-
phosphorus specific detector, backflush valve (see Fig. 1), split
3. Summary of Test Method
injector, and capable of accepting megabore (0.53 mm inside
3.1 Two dispersions (in o-dichlorobenzene) are prepared
diameter) fused silica capillary columns. Detector make-up gas
and sealed in headspace vials for each polymer; one vial
is required.
contains the polymer in solvent while the second vial contains
NOTE 2—The use of a backflush configuration will provide for
operating advantages, but its use is optional. Chlorinated solvents quench
1
This test method is under the jurisdiction of ASTM Committee D20 on Plastics
the alkali bead in a nitrogen-phosphorous detector, producing a loss of
and is the direct responsibility of Subcommittee D20.70 on Analytical Methods and
signal. While the bead (signal) will recover as the solvent evacuates the
Section D20.70.02 on Chromatography.
detector, repeated quenching during a multi-run sequence may produce
Current edition approved Sept. 1, 2016. Published September 2016. Originally
instabilities in the signal (and precision) over the sequence period.
ε1
approved in 1994. Last previous edition approved in 2009 as D5508 - 94a(2009) .
DOI: 10.1520/D5508-16.
5.2 Automated Headspace Sampler, shall have a thermost-
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
atted sample tray capable of 90°C heating with constant
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
heating times. Automated sampling of the headspace gas in the
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. sample vials via a heated, constant-volume sample loop or
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D5508 − 16
7. Sampling and Storage
...
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