ASTM D7132-13
(Test Method)Standard Test Method for Determination of Retained Blowing Agent in Extruded Polystyrene Foam
Standard Test Method for Determination of Retained Blowing Agent in Extruded Polystyrene Foam
ABSTRACT
This test method covers the determination of retained blowing agent in extruded polystyrene foam. The internal standard preparation procedures of the material are presented in details. The procedures for determination of retained blowing agent in extruded polyester foam are presented in details.
SCOPE
1.1 This test method covers the determination of retained blowing agent in extruded polystyrene foam.
1.2 This test method applies to organic blowing agents which lend themselves to a convenient analysis by gas chromatography. The method is not applicable to blowing agents such as nitrogen, carbon dioxide, or water.
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 to determine the applicability of regulatory limitations prior to use. Note 1—There is no known ISO equivalent to this standard.
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Designation: D7132 − 13
StandardTest Method for
Determination of Retained Blowing Agent in Extruded
1
Polystyrene Foam
This standard is issued under the fixed designation D7132; 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* signal(s) from the blowing agent components. Test calibration
solutions with and without the polymer matrix to rule out any
1.1 This test method covers the determination of retained
interference.These calibration solutions shall contain about the
blowing agent in extruded polystyrene foam.
same amount of dissolved resin as in the foam sample being
1.2 This test method applies to organic blowing agents
analyzed.
which lend themselves to a convenient analysis by gas chro-
matography. The method is not applicable to blowing agents
4. Apparatus
such as nitrogen, carbon dioxide, or water.
4.1 Any GC equipped with a column suitable for resolving
1.3 The values stated in SI units are to be regarded as
blowing agent components is suitable for use. For example, if
standard. No other units of measurement are included in this
separating non-polar blowing agents, a 100 % dimethyl-
standard.
polysiloxane with 530-µm thick film and 30-m length is a
1.4 This standard does not purport to address all of the reasonable selection. If separating polar blowing agents, a 50
safety concerns, if any, associated with its use. It is the % dipheny/50 % dimethyl polysiloxane column with 530-µm
responsibility of the user of this standard to establish appro- thick film and 30-m length is suitable. Typical operating
priate safety and health practices and to determine the parameters for the GC are:
applicability of regulatory limitations prior to use.
Head pressure (kPa) 50
Initial oven temperature (°C) 50
NOTE 1—There is no known ISO equivalent to this standard.
Initial hold time (min) 3.5
Temperature program rate (°C/min) 25
2. Summary of Test Method Final temperature (°C) 150
Final hold time (min) 3
2.1 Polystyrene foams are made with a variety of blowing
Injector temperature (°C) 250
Detector temperature (°C) 300
agents such as hydrocarbons, hydrofluorocarbons, ethers,
Carrier gas He
ketones, and other volatile organic chemicals.Afraction of the
3
Carrier gas flow rate (cm /min) 30
blowing agent used in the manufacture of foam is retained in
Injection sample size (µL) 0.2
theproduct,someresidinginthecellwallsandsomeentrapped
NOTE 2—An autosampler is not recommended as the transfer of a
inside the cells. This test method is based on releasing the
solution containing volatile components can lead to loss of the volatile
retained blowing agent by dissolving the polystyrene foam in a
analyte.
solvent, such as toluene, and then analyzing the solution for its
4.2 Analytical balance with at least 150 g full scale and 0.1
components by gas chromatography. An internal standard is
mg resolution.
used as a reference analyte and calibration of the gas chro-
4.3 Instrument grade air supplied at 515 6 40 kPa, helium
matograph (GC) with standard solutions allows conversion of
at 450 6 40 kPa, and hydrogen at 380 6 40 kPa.
the GC response to the amount of blowing agent retained in the
3
foam matrix. 4.4 100-cm volumetric flasks.
3 3
4.5 1-cm syringe with Chaney Adapter, and 10-cm gas
3. Interferences
tight syringe with Chaney Adapter.
3.1 The gas chromatogram has the potential to contain a
4.6 1-µL syringe.
signal(s) from the polymer matrix that interferes with the
3
4.7 Tall, wide mouth 125-cm sample bottles with caps and
teflon/silicon septa.
1
This test method is under the jurisdiction ofASTM Committee D20 on Plastics
3
4.8 30-cm serum vials with crimp on teflon/silicon septa.
and is the direct responsibility of Subcommittee D20.70 on Analytical Methods.
Current edition approved Nov. 1, 2013. Published November 2013. Originally
4.9 Rubber sleeve stoppers for volumetric flask.
approved in 2005. Last previous edition approved in 2005 as D7132 – 05. DOI:
10.1520/D7132-13. 4.10 Septa for GC.
*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
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D7132 − 13
actually touching the balance pan.
4.11 Ice water bath.
3
8.4 Inject 0.2 to 0.4 cm heptane into the flask and weigh to
4.12 Weights to keep sample bottle submerged.
the nearest 0.1 mg (W ).
istd
4.13 Refrigerator for sample storage.
8.5 Dilute to the mark with toluene. It is acceptable to retain
4.14 Insulated mailing containers with ice packs for ship-
this internal standard (ISTD) so
...
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.
Designation: D7132 − 05 D7132 − 13
Standard Test Method for
Determination of Retained Blowing Agent in Extruded
1
Polystyrene Foam
This standard is issued under the fixed designation D7132; 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 Scope*
1.1 This test method covers the determination of retained blowing agent in extruded polystyrene foam.
1.2 This test method applies to organic blowing agents which lend themselves to a convenient analysis by gas chromatography.
The method is not applicable to blowing agents such as nitrogen, carbon dioxide, or water.
1.3 There is no similar or equivalent ISO standard. 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 to determine the applicability of regulatory
limitations prior to use.
NOTE 1—There is no known ISO equivalent to this standard.
2. Summary of Test Method
2.1 Polystyrene foams are made with a variety of blowing agents such as hydrocarbons, hydrofluorocarbons, ethers, ketones,
and other volatile organic chemicals. A fraction of the blowing agent used in the manufacture of foam is retained in the product,
some residing in the cell walls and some entrapped inside the cells. This test method is based on releasing the retained blowing
agent by dissolving the polystyrene foam in a solvent, such as toluene, and then analyzing the solution for its components by gas
chromatography. An internal standard is used as a reference analyte and calibration of the gas chromatograph (GC) with standard
solutions allows conversion of the GC response to the amount of blowing agent retained in the foam matrix.
3. Interferences
3.1 The gas chromatogram may has the potential to contain a signal(s) from the polymer matrix that interferes with the signal(s)
from the blowing agent components. Test calibration solutions with and without the polymer matrix to rule out any interference.
These calibration solutions shall contain about the same amount of dissolved resin as in the foam sample being analyzed.
4. Apparatus
4.1 Any GC equipped with a column suitable for resolving blowing agent components can be used. For is suitable for use. For
example, if separating non-polar blowing agents, a column such as HP-1 100 % dimethyl-polysiloxane with 530-μm thick film and
30-m length can be used. For is a reasonable selection. If separating polar blowing agents, a column such as HP-17 50 %
dipheny/50 % dimethyl polysiloxane column with 530-μm thick film and 30-m length can be used. is suitable. Typical operating
parameters for the GC are:
Head pressure (kPa) 50
Initial oven temperature (°C) 50
Initial hold time (min) 3.5
Temperature program rate (°C/min) 25
Final temperature (°C) 150
Final hold time (min) 3
Injector temperature (°C) 250
Detector temperature (°C) 300
Carrier gas He
3
Carrier gas flow rate (cm /min) 30
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.
Current edition approved July 1, 2005Nov. 1, 2013. Published August 2005November 2013. Originally approved in 2005. Last previous edition approved in 2005 as D7132
– 05. DOI: 10.1520/D7132-05.10.1520/D7132-13.
*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 ----------------------
D7132 − 13
Injection sample size (μL) 0.2
NOTE 2—An autosampler is not recommended as the transfer of a solution containing volatile components can lead to loss of the volatile analyte.
4.2 Analytical balance with at least 150 g full scale and 0.1 mg resolution.
4.3 Instrument grade air supplied at 515 6 40 kPa, helium at 450 6 40 kPa, and hydrogen at 380 6 40 kPa.
3
4.4 100-cm volumetric flasks.
3 3
4.5 1-cm syringe with Chaney Adapter, and 10-cm gas tight syringe with Chaney Adapter.
4.6 1-μL syringe.
3
4.7 I-Chem Tall 200 series Tall, wide mouth 125-cm sample bottles with caps and teflon/silicon septa.
3
4.8
...
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