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ASTM E1863-18

(Test Method)

Standard Test Method for Analysis of Acrylonitrile by Gas Chromatography

Standard Test Method for Analysis of Acrylonitrile by Gas Chromatography

SIGNIFICANCE AND USE
4.1 This test method is designed to obtain acrylonitrile purity on the basis of impurities normally present in acrylonitrile and may be useful for final product inspection and process control.  
4.2 This test method will measure the following impurities: acetone, acrolein, acetonitrile, and acetaldehyde. It also will allow calibration of other impurities including benzene, methacrylonitrile, oxazole, propionitrile, cis-crotononitrile, trans-crotononitrile, and others where specific impurity standards are available.
SCOPE
1.1 This test method covers the determination of the impurities in, and the purity of, acrylonitrile by flame ionization detector gas chromatography. It is applicable to acrylonitrile in the range of 99 to 100 % purity.  
1.2 The values stated in SI units are to be regarded as standard. The values given in parentheses are for information only.  
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. Specific hazard statements are given in Sections 6 and 7.  
1.4 Review the current MSDS for detailed information concerning toxicity, first aid procedures, and safety precautions.  
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.

General Information

Status
Published
Publication Date
30-Sep-2018
ICS
71.040.40 - Chemical analysis
Technical Committee
D20 - Plastics
Drafting Committee
D20.15 - Thermoplastic Materials
Current Stage
Ref Project

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ASTM E1863-18 - Standard Test Method for Analysis of Acrylonitrile by Gas ChromatographyASTM E1863-18 - Standard Test Method for Analysis of Acrylonitrile by Gas Chromatography
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ASTM E1863-18 - Standard Test Method for Analysis of Acrylonitrile by Gas Chromatography
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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
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: E1863 − 18
Standard Test Method for
1
Analysis of Acrylonitrile by Gas Chromatography
This standard is issued under the fixed designation E1863; 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. Summary of Test Method
1.1 This test method covers the determination of the impu- 3.1 In this test method, a representative sample of acrylo-
rities in, and the purity of, acrylonitrile by flame ionization nitrile is introduced in a gas chromatograph equipped with a
detector gas chromatography. It is applicable to acrylonitrile in flameionizationdetectorandacapillarycolumnwherespecific
the range of 99 to 100% purity. impurities are separated from the acrylonitrile. The chromato-
graphic area for each impurity is compared to the area of the
1.2 The values stated in SI units are to be regarded as
internalstandard,tolueneorothersuitableknown,addedtothe
standard. The values given in parentheses are for information
sample. From response factors of these impurities relative to
only.
that of the internal standard and the amount of the standard
1.3 This standard does not purport to address all of the
added,theconcentrationoftheimpuritiesarecalculated.Other
safety concerns, if any, associated with its use. It is the
impurities, such as water, are obtained by use of Test Methods
responsibility of the user of this standard to establish appro-
E1178. The acrylonitrile content is obtained by subtracting the
priate safety, health, and environmental practices and deter-
total amount of all impurities from 100.0.
mine the applicability of regulatory limitations prior to use.
Specific hazard statements are given in Sections 6 and 7.
4. Significance and Use
1.4 Review the current MSDS for detailed information
4.1 This test method is designed to obtain acrylonitrile
concerning toxicity, first aid procedures, and safety precau-
purity on the basis of impurities normally present in acryloni-
tions.
trileandmaybeusefulforfinalproductinspectionandprocess
1.5 This international standard was developed in accor-
control.
dance with internationally recognized principles on standard-
4.2 This test method will measure the following impurities:
ization established in the Decision on Principles for the
acetone, acrolein, acetonitrile, and acetaldehyde. It also will
Development of International Standards, Guides and Recom-
allow calibration of other impurities including benzene,
mendations issued by the World Trade Organization Technical
methacrylonitrile, oxazole, propionitrile, cis-crotononitrile,
Barriers to Trade (TBT) Committee.
trans-crotononitrile, and others where specific impurity stan-
dards are available.
2. Referenced Documents
2
2.1 ASTM Standards:
5. Apparatus
E180Practice for Determining the Precision of ASTM
5.1 Capillary Gas Chromatograph—Any gas chromato-
Methods for Analysis and Testing of Industrial and Spe-
3
graph equipped with a flame ionization detector and a split
cialty Chemicals (Withdrawn 2009)
injection system for use with capillary columns that can be
E1178Test Methods for Analysis of Acrylonitrile (With-
3
operated at the conditions given in Table 1.
drawn 2016)
4
5.2 Column—The column, such as Supelcowax 10, must
give satisfactory resolution and proper peak shapes for the
1
ThistestmethodisunderthejurisdictionofASTMCommitteeD20onPlastics
components listed in Fig. 1.
and is the direct responsibility of Subcommittee D20.15 on Thermoplastic Materi-
5.3 Recorder/Integrator—Electronic integration is recom-
als.
Current edition approved Oct. 1, 2018. Published October 2018. Originally
mended for this analysis.
approvedin1997.Lastpreviouseditionapprovedin2007asE1863–07,whichwas
5.4 Syringe, 10 µL capacity.
withdrawn January 2016 and reinstated in October 2018. DOI: 10.1520/E1863-18.
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
4
the ASTM website. ASupelcowax 10 fused silica capillary column (60 m by 0.32 mm ID by 1 µm
3
The last approved version of this historical standard is referenced on film thickness), has been found to be suitable, but similar polar wax columns from
www.astm.org. other vendors may be used after shown to be suitable.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

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Salts of organic and inorganic acids (Note 6)  
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5.2 As stated in 1.2, this test method uses a weaker acid to titrate the base than Test Method D2896, and the titration solvents are also different. Test Method D2896 uses a stronger acid and a more polar solvent system than Test Method D4739. As a result, Test Method D2896 will titrate salts of weak acids (soaps), basic salts of polyacidic bases, and weak alkaline salts of some metals. They do not protect the oil from acidic components due to the degradation of the oil. This test method may produce a falsely exaggerated base number. Test Method D4739 will probably not titrate these weak bases but, if so, will titrate them to a lesser degree of completion. It measures only the basic components of the additive package that neutralizes acids. On the other hand, if the additive package contains weak basic components that do not play a role in neutralizing the acidic components of the degrading oil, then the Test Method D4739 result may be falsely understated.  
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SCOPE
1.1 This test method covers a procedure for the determination of basic constituents in petroleum products and new and used lubricants. This test method resolves these constituents into groups having weak-base and strong-base ionization properties, provided the dissociation constants of the more strongly basic compounds are at least 1000 times than that of the next weaker groups. This test method covers base numbers up to 250.  
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