ASTM D7704-12
(Test Method)Standard Test Method for Total Aldehydes in Styrene Monomer by Potentiometric Titration
Standard Test Method for Total Aldehydes in Styrene Monomer by Potentiometric Titration
SIGNIFICANCE AND USE
This test method is suitable for determining the quantity of aldehydes, both for quality control and quality assurance of the product.
SCOPE
1.1 This test method covers the wet chemical determination of aldehydes in styrene monomer. Aldehydes are calculated and reported as benzaldehyde. The range of concentration for this test method is 0.001 mass % to 0.030 mass %.
1.2 In determining conformance of the test results using this method to applicable specifications, results shall be rounded off in accordance with the rounding-off method of Practice E29.
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.
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Designation: D7704 − 12
StandardTest Method for
Total Aldehydes in Styrene Monomer by Potentiometric
1
Titration
This standard is issued under the fixed designation D7704; 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 2.2 Other Documents:
OSHA Regulations, 29 CFR paragraphs 1910.1000 and
1.1 This test method covers the wet chemical determination
3
1910.1200
of aldehydes in styrene monomer. Aldehydes are calculated
and reported as benzaldehyde. The range of concentration for
3. Summary of Test Method
this test method is 0.001 mass % to 0.030 mass %.
3.1 An alcoholic solution of hydroxylamine hydrochloride
1.2 In determining conformance of the test results using this
is added to a specimen of styrene monomer. Active aldehydes
methodtoapplicablespecifications,resultsshallberoundedoff
present react in accordance with Eq 1:
in accordance with the rounding-off method of Practice E29.
RCHO1NH OH·HCl→RCHNOH1H O1HCl (1)
2 2
1.3 The values stated in SI units are to be regarded as
The amount of hydrochloric acid released, which is equiva-
standard. No other units of measurement are included in this
lent to the aldehyde present in the sample, is titrated with
standard.
standard alcoholic potassium hydroxide solution.
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 This test method is suitable for determining the quantity
priate safety and health practices and determine the applica-
of aldehydes, both for quality control and quality assurance of
bility of regulatory limitations prior to use.
the product.
2. Referenced Documents
5. Interferences
2
2.1 ASTM Standards:
5.1 Ketones, if present, interfere by partially reacting with
D1193 Specification for Reagent Water
the reagent.
D3437 Practice for Sampling and Handling Liquid Cyclic
5.2 Methanolusedinthisproceduremaypartiallyreactwith
Products
aldehydes to form (hemi)acetals.
D6809 Guide for Quality Control and Quality Assurance
Procedures for Aromatic Hydrocarbons and Related Ma-
6. Apparatus
terials
6.1 Titration Vessel, 150 mL.
E29 Practice for Using Significant Digits in Test Data to
Determine Conformance with Specifications
6.2 Combined pH – Glass Electrode, dedicated for non-
aqueous liquids.
1
This test method is under the jurisdiction of ASTM Committee D16 on 6.3 Stirring Bar, 30 mm.
Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of
6.4 Titration Stand with stirrer.
Subcommittee D16.07 on Styrene, Ethylbenzene and C9 and C10 Aromatic
Hydrocarbons.
6.5 Pipets, 25 mL.
Current edition approved March 1, 2012. Published March 2012. Originally
approved in 2011. Last previous edition approved in 2011 as D7704 - 11. DOI:
6.6 Volumetric Flasks, 100 mL.
10.1520/D7704–12.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
3
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Available from Standardization Documents Order Desk, DODSSP, Bldg. 4,
Standards volume information, refer to the standard’s Document Summary page on Section D, 700 Robbins Ave., Philadelphia, PA 19111-5098, http://
the ASTM website. dodssp.daps.dla.mil.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D7704 − 12
6.7 Burets, 5 mL. (Microburets are preferred.) 10. Procedure
6.8 Exchange Unit, 5 mL. 10.1 Prepare the pH electrode according to the manufactur-
er’s instructions.
6.9 Thermometers, capable of differentiating 1°C at ambi-
ent. 10.2 Pipet 25.0 mL of the sample ( Warning—see 8.2) and
25 mL of methanol (7.4) into a 150-mL titration vessel with
7. Reagents and Materials
stirringbar.Add0.2mLofwater.Add25mLoftheneutralized
hydroxylamine hydrochloride solution and allow to stand 0.5 h
7.1 Purity of Reagents—Reagent grade chemicals shall be
while stirring. Titrate with the 0.02 N KOH/methanol solution,
used in all tests. Unless otherwise indicated, it is intended that
dispensed from a 5-mL buret, until the first equivalence point,
all reagents conform to the specifications of the Committee on
and record the volume used.
Analytical Reagents of the American Chemical Society where
4
such specifications are available. Other grades may be used,
10.3 Since methanol may contain aldehydes, run a blank
provided it is first ascertained that the reagent is of sufficiently
determination on 25 mL of methanol (7.4), record the volume
high purity to p
...
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:D7704–11 Designation:D7704–12
Standard Test Method for
Total Aldehydes in Styrene Monomer by Potentiometric
1
Titration
This standard is issued under the fixed designation D7704; 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 test method covers the wet chemical determination of aldehydes in styrene monomer. Aldehydes are calculated and
reported as benzaldehyde. The range of concentration for this test method is 0.001 mass % to 0.030 mass %.
1.2 In determining conformance of the test results using this method to applicable specifications, results shall be rounded off
in accordance with the rounding-off method of Practice E29.
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.
2. Referenced Documents
2
2.1 ASTM Standards:
D1193 Specification for Reagent Water
D3437 Practice for Sampling and Handling Liquid Cyclic Products
D6809 Guide for Quality Control and Quality Assurance Procedures for Aromatic Hydrocarbons and Related Materials
E29 Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
2.2 Other Documents:
3
OSHA Regulations, 29 CFR paragraphs 1910.1000 and 1910.1200
3. Summary of Test Method
3.1 Analcoholicsolutionofhydroxylaminehydrochlorideisaddedtoaspecimenofstyrenemonomer.Activealdehydespresent
react in accordance with Eq 1:
RCHO 1 NH OH·HCl→ RCHNOH 1 H O 1 HCl (1)
2 2
D7704-12_1
The amount of hydrochloric acid released, which is equivalent to the aldehyde present in the sample, is titrated with standard
alcoholic potassium hydroxide solution.
4. Significance and Use
4.1 This test method is suitable for determining the quantity of aldehydes, both for quality control and quality assurance of the
product.
5. Interferences
5.1 Ketones, if present, interfere by partially reacting with the reagent.
5.2 Methanol used in this procedure may partially react with aldehydes to form (hemi)acetals.
6. Apparatus
6.1 Titration Vessel, 150 mL.
1
This test method is under the jurisdiction ofASTM Committee D16 onAromatic Hydrocarbons and Related Chemicals and is the direct responsibility of Subcommittee
D16.07 on Styrene, Ethylbenzene and C and C Aromatic Hydrocarbons.
9 10
Current edition approved March 1, 2011. Published March 2011. DOI: 10.1520/D7704–11.on Styrene, Ethylbenzene and C9 and C10 Aromatic Hydrocarbons.
Current edition approved March 1, 2012. Published March 2012. Originally approved in 2011. Last previous edition approved in 2011 as D7704 - 11. DOI:
10.1520/D7704–12.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM 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.
3
Available from Standardization Documents Order Desk, DODSSP, Bldg. 4, Section D, 700 Robbins Ave., Philadelphia, PA 19111-5098, http://dodssp.daps.dla.mil.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1
---------------------- Page: 1 ----------------------
D7704–12
6.2 Combined pH – Glass Electrode, dedicated for non-aqueous liquids.
6.3 Stirring Bar,30mm.
6.4 Titration Stand with stirrer.
6.5 Pipets,25mL.
6.6 Volumetric Flasks, 100 mL.
6.7 Burets, 5 mL. (Microburets are preferred.)
6.8 Exchange Unit, 5 mL.
6.9 Thermometers, capable of differentiating 1°C at ambient.
7. Reagents and Materials
7.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society where such
4
specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity
to permit its use without lessening the accuracy of the determination.
7.2 Purity of Water—Unless otherwise indicated, references to water shall be unders
...
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