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ASTM D4526-96(2007)

(Practice)

Standard Practice for Determination of Volatiles in Polymers by Static Headspace Gas Chromatography

Standard Practice for Determination of Volatiles in Polymers by Static Headspace Gas Chromatography

SCOPE
1.1 Headspace gas chromatography (GC) involves the determination of volatile components in a polymer solution by gas chromatography of a vapor phase in thermal equilibrium with the sample matrix. Volatiles in finely ground insoluble polymers can also be determined with and without an extracting solvent.
1.2 This practice provides two procedures:
1.2.1 Procedure A - Automatic headspace analysis.
1.2.2 Procedure B - Manual injection headspace analysis.
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 Section 6.Note 1
There is no equivalent ISO standard.

General Information

Status
Historical
Publication Date
31-Aug-2007
ICS
83.080.01 - Plastics in general
Technical Committee
D20 - Plastics
Drafting Committee
D20.70 - Analytical Methods
Current Stage
Ref Project

Relations

Replaces
ASTM D4526-96(2001)e1 - Standard Practice for Determination of Volatiles in Polymers by Static Headspace Gas Chromatography
Effective Date
01-Sep-2007
Replaced By
ASTM D4526-12 - Standard Practice for Determination of Volatiles in Polymers by Static Headspace Gas Chromatography
Effective Date
15-Dec-2012
Referred By
ASTM D3749-19 - Standard Test Method for Residual Vinyl Chloride Monomer in Poly(Vinyl Chloride) Resins by Gas Chromatographic Headspace Technique
Effective Date
01-Sep-2007

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ASTM D4526-96(2007) - Standard Practice for Determination of Volatiles in Polymers by Static Headspace Gas ChromatographyASTM D4526-96(2007) - Standard Practice for Determination of Volatiles in Polymers by Static Headspace Gas Chromatography
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ASTM D4526-96(2007) - Standard Practice for Determination of Volatiles in Polymers by Static Headspace Gas Chromatography
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Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D4526 − 96(Reapproved 2007)
Standard Practice for
Determination of Volatiles in Polymers by Static Headspace
1
Gas Chromatography
This standard is issued under the fixed designation D4526; 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* 3. Significance and Use
3.1 For various reasons, one may want to measure the level
1.1 Headspace gas chromatography (GC) involves the de-
of unreacted or residual monomer, water, or other volatile
termination of volatile components in a polymer solution by
components in a polymer sample.
gas chromatography of a vapor phase in thermal equilibrium
with the sample matrix. Volatiles in finely ground insoluble
3.2 Volatiles of interest are often at trace concentrations.
polymers can also be determined with and without an extract- Headspace analysis is suited for determination of these trace
ing solvent. componentswhichoftencannotbedeterminedbyconventional
gas chromatography because of sample decomposition or
1.2 This practice provides two procedures:
interferences.
1.2.1 Procedure A—Automatic headspace analysis.
3.3 For polymer analysis, sample treatment for headspace
1.2.2 Procedure B—Manual injection headspace analysis.
analysis is simpler than conventional gas chromatography,
where precipitation steps may be required to prevent polymer
1.3 This standard does not purport to address all of the
contamination of the chromatographic column.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
3.4 This headspace practice will be able to determine
priate safety and health practices and determine the applica-
qualitatively any component with sufficient vapor pressure. It
bility of regulatory limitations prior to use. Specific precau-
is capable of yielding semiquantitative results and can be used
tionary statements are given in Section 6.
for relative comparisons between samples.
NOTE 1—There is no equivalent ISO standard.
4. Apparatus
4.1 Gas Chromatograph, equipped with an appropriate
2. Referenced Documents
detector and backflush valve.
2
2.1 ASTM Standards:
4.1.1 For Procedure A, an Automated Headspace Sampler,
4,5
D4322Test Method for Residual Acrylonitrile Monomer
including backflush capability, thermostated sample tray,
Styrene-Acrylonitrile Copolymers and Nitrile Rubber by
and associated accessories fulfill these requirements while
3
Headspace Gas Chromatography (Withdrawn 2010) providing for automatic sequential sampling of headspace
E260Practice for Packed Column Gas Chromatography
vapors.
E355PracticeforGasChromatographyTermsandRelation- 4.1.2 Procedure B requires the following additional equip-
ment:
ships
4.1.2.1 Constant-Temperature Bath, capable of maintaining
E594Practice for Testing Flame Ionization Detectors Used
90 6 1°C.
in Gas or Supercritical Fluid Chromatography
4.1.2.2 Gas-Tight Gas Chromatographic Syringes, which
can be heated to 90°C for sampling and injection.
4.1.2.3 Valve, 6-port for backflush assembly.
1
ThispracticeisunderthejurisdictionofASTMCommitteeD20onPlasticsand
is the direct responsibility of Subcommittee D20.70 on Analytical Methods.
NOTE 2—Appropriate detectors could include the following:
Current edition approved Sept. 1, 2007. Published November 2007. Originally
(a) Flame ionization (FID) for general organic volatiles,
´1
approved in 1985. Last previous edition approved in 2001 as D4526-97(2001) .
DOI: 10.1520/D4526-96R07.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
4
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Thesolesourceofsupplyoftheapparatusknowntothecommitteeatthistime
Standards volume information, refer to the standard’s Document Summary page on is Perkin-Elmer Corp., Main Ave., Norwalk, CT 06856.
5
the ASTM website. If you are aware of alternative suppliers, please provide this information to
3
The last approved version of this historical standard is referenced on ASTM International Headquarters. Your comments will receive careful consider-
1
www.astm.org. ation at a meeting of the responsible technical committee, which you may attend.
*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 ----------------------
D4526 − 96 (2007)
(b) Electron capture (EC) for halogenated species,
6. Safety Precautions
(c) Nitrogen-phosphorous (NPD) for acrylonitrile,
6.1 Volatiles such as vinyl chloride and acrylonitrile should
(d) Thermal
...

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4.1 The test methods are intended to be rapid empirical tests which have been found to be useful in the relative comparison of materials having the same nominal thickness.
Note 2: When the plastic material contains plasticizer, loss from the plastic is assumed to be primarily plasticizer. The effect of moisture is considered to be negligible.  
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1.1 These test methods cover the determination of volatile loss from a plastic material under defined conditions of time and temperature, using activated carbon as the immersion medium.  
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Note 1: This standard and ISO 176 address the same subject matter, but differ in technical content.  
1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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1.1 This terminology covers definitions of technical terms used in the plastics industry. Terms that are generally understood or adequately defined in other readily available sources are not included.  
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1.6.2 For terms related to electrical or electronic insulating materials, the applicable definitions are contained in Terminology D1711.  
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1.6.4 For terms relating to precision and bias and associated issues, the applicable definitions are contained in Terminology E456.  
1.6.5 For terms related to plastic piping systems, the applicable definitions are contained in Terminology F412.  
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4.1 This test method is designed to provide load versus deformation response of plastics under essentially multi-axial deformation conditions at impact velocities. This test method further provides a measure of the rate sensitivity of the material to impact.  
4.2 Multi-axial impact response, while partly dependent on thickness, does not necessarily have a linear correlation with specimen thickness. Therefore, results must be compared only for specimens of essentially the same thickness, unless specific responses versus thickness formulae have been established for the material.  
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5.1 This test method provides a simple means of characterizing the thermomechanical behavior of plastic compositions using very small amounts of material. The data obtained can be used for quality control and/or research and development purposes. For some classes of materials, such as thermosets, it can also be used to establish optimum processing conditions.  
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5.1 This test method provides a simple means of characterizing the thermomechanical behavior of plastic materials using very small amounts of material. The data obtained is used for quality control, research and development, as well as the establishment of optimum processing conditions.  
5.2 Dynamic mechanical testing provides a sensitive method for determining thermomechanical characteristics by measuring the elastic and loss moduli as a function of frequency, temperature, or time. Plots of moduli and tan delta of a material versus these variables can be used to provide graphical representation indicative of functional properties, effectiveness of cure (thermosetting resin system), and damping behavior under specified conditions.  
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5.3.8 The effect of aspect ratio on the modulus of fiber reinforcements, and  
5.3.9 The effect of fillers, additives on modulus and glass transition temperature.  
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1.3 This test method is valid for a wide range of frequencies, typically from 0.01 Hz to 100 Hz.  
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1.5 Test data obtained by this test method are relevant and appropriate for use in engineering design.  
1.6 The values stated in SI units are to be regarded as standard. The values given in parentheses are for information only.  
1.7 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
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1.5 This test method also provides for testing flexible sheet or film materials, while supported vertically.  
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1.7 This test method measures and describes the response of materials, products, or assemblies to heat and flame under controlled conditions, but does not by itself incorporate all factors required for fire hazard or fire risk assessment of the materials, products, or assemblies under actual fire conditions.  
1.8 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.9 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific hazards statement are given in Section 10.  
1.10 Fire testing is inherently hazardous. Adequate safeguards for personnel and property shall be employed in conducting these tests.
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Standard Test Method for Compressive Properties of Rigid Plastics

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4.2 Compressive properties include modulus of elasticity, yield stress, deformation beyond yield point, and compressive strength (unless the material merely flattens but does not fracture). Materials possessing a low order of ductility may not exhibit a yield point. In the case of a material that fails in compression by a shattering fracture, the compressive strength has a very definite value. In the case of a material that does not fail in compression by a shattering fracture, the compressive strength is an arbitrary one depending upon the degree of distortion that is regarded as indicating complete failure of the material. Many plastic materials will continue to deform in compression until a flat disk is produced, the compressive stress (nominal) rising steadily in the process, without any well-defined fracture occurring. Compressive strength can have no real meaning in such cases.  
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4.4 Before proceeding with this test method, reference should be made to the ASTM specification for the material being tested. Any test specimen preparation, conditioning, dimensions, and testing parameters covered in the materials specification shall take precedence over those mentioned in this test method. If there is no material specification, then the default conditions apply. Table 1 in Classification D4000 lists the ASTM materials standards that currently exist.
SCOPE
1.1 This test method covers the determination of the mechanical properties of unreinforced and reinforced rigid plastics, including high-modulus composites, when loaded in compression at relatively low uniform rates of straining or loading. Test specimens of standard shape are employed. This procedure is applicable for a composite modulus up to and including 41,370 MPa (6,000,000 psi).  
1.2 The values stated in SI units are to be regarded as the standard. The values in parentheses are for information only.
Note 1: For compressive properties of resin-matrix composites reinforced with oriented continuous, discontinuous, or cross-ply reinforcements, tests may be made in accordance with Test Method D3410/D3410M or D6641/D6641M.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. A specific precautionary statement is given in 13.1.
Note 2: This standard is equivalent to ISO 604.  
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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  • Standard
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ASTM
ASTM D1929-23(Test Method)
Standard Test Method for Determining Ignition Temperature of Plastics

SIGNIFICANCE AND USE
4.1 Tests made under conditions herein prescribed can be of considerable value in comparing the relative ignition characteristics of different materials. Values obtained represent the lowest ambient air temperature that will cause ignition of the material under the conditions of this test. Test values are expected to rank materials according to ignition susceptibility under actual use conditions.  
4.2 This test is not intended to be the sole criterion for fire hazard. In addition to ignition temperatures, fire hazards include other factors such as burning rate or flame spread, intensity of burning, fuel contribution, products of combustion, and others.
SCOPE
1.1 This fire test response test method2 covers a laboratory determination of the flash ignition temperature and spontaneous ignition temperature of plastics using a hot-air furnace.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 Caution—During the course of combustion, gases or vapors, or both, are evolved that have the potential to be hazardous to personnel.  
1.4 This standard is used to measure and describe the response of materials, products, or assemblies to heat and flame under controlled conditions, but does not by itself incorporate all factors required for fire-hazard or fire-risk assessment of the materials, products, or assemblies under actual fire conditions.  
1.5 Fire testing is inherently hazardous. Adequate safeguards for personnel and property shall be employed in conducting these tests.  
1.6 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific precautionary statements are given in 1.3 and 1.4.
Note 1: This test method and ISO 871-2022 (Option 1) are similar in all technical details.  
1.7 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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  • Standard
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