Designation: D 2119 – 03

Standard Test Method for

Aldehydes in Styrene Monomer1
This standard is issued under the fixed designation D 2119; 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 (e) indicates an editorial change since the last revision or reapproval.

1. Scope* RCHO 1 NH2OH·HCl → RCHNOH 1 H 2O 1 HCl

1.1 This laboratory test method covers the wet chemical The hydrochloric acid, which is equivalent to the aldehyde
determination of aldehydes in styrene monomer. Aldehydes are present in the sample, is titrated with standard sodium hydrox-
calculated and reported as benzaldehyde. The range of concen- ide solution.
tration for this test method is 0.001 % to 0.030 %.
1.2 For purposes of determining conformance with this test 4. Significance and Use
method, an observed value or a calculated value shall be 4.1 This test method is suitable for determining the quantity
rounded off “to the nearest unit” in the last right-hand digit of aldehydes, both for quality control and quality assurance of
used in expressing the specification limit, in accordance with the product.
the rounding-off method of Practice E 29.
1.3 This standard does not purport to address all of the 5. Interferences
safety concerns, if any, associated with its use. It is the 5.1 Ketones, if present, interfere by partially reacting with
responsibility of the user of this standard to establish appro- the reagent.
priate safety and health practices and determine the applica-
6. Apparatus
bility of regulatory limitations prior to use. For specific hazard
statements, see Section 8. 6.1 Erlenmeyer Flasks, glass-stoppered, 250-mL.
6.2 Pipets, 25-mL.
2. Referenced Documents 6.3 Volumetric Flasks, 100-mL.
2.1 ASTM Standards: 6.4 Burets, 10-mL. (Microburets are preferred.)
D 1193 Specification for Reagent Water2 6.5 Thermometers, capable of differentiating 1°C at ambi-
D 3437 Practice for Sampling and Handling Liquid Cyclic ent.
Products3
E 29 Practice for Using Significant Digits in Test Data to 7. Reagents
Determine Conformance with Specifications4 7.1 Purity of Reagents—Reagent grade chemicals shall be
2.2 Other Documents: used in all tests. Unless otherwise indicated, it is intended that
OSHA Regulations, 29 CFR, paragraphs 1910.1000 and all reagents conform to the specifications of the Committee on
1910.12005 Analytical Reagents of the American Chemical Society where
such specifications are available.6 Other grades may be used,
3. Summary of Test Method provided it is first ascertained that the reagent is of sufficiently
3.1 An alcoholic solution of hydroxylamine hydrochloride high purity to permit its use without lessening the accuracy of
is added to a specimen of styrene monomer. Active aldehydes the determination.
present react in accordance with the following equation: 7.2 Purity of Water—Unless otherwise indicated, references
to water shall be understood to mean reagent water as defined
by Type III of Specification D 1193.
1
This test method is under the jurisdiction of ASTM Committee D16 on
Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of
Subcommittee D16.07 on Styrene, Ethylbenzene, and C9 and C10 Aromatic
Hydrocarbons.
Current edition approved Aug. 10, 2003. Published August 2003. Originally
6
approved in 1962. Last previous edition approved in 1996 as D 2119 – 96. Reagent Chemicals, American Chemical Society Specifications, American
2
Annual Book of ASTM Standards, Vol 11.01. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
3
Annual Book of ASTM Standards, Vol 06.04. listed by the American Chemical Society, see Analar Standards for Laboratory
4
Annual Book of ASTM Standards, Vol 14.02. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
5
Available from Standardization Documents Order Desk, DODSSP, Bldg. 4, and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
Section D, 700 Robbins Ave., Philadelphia, PA 19111-5098 MD.

*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
 D 2119 – 03
7.3 Hydrochloric Acid, Standard (0.05 N)—Prepare a 0.05 10.2 Since methanol may contain aldehydes, run a blank
N solution of hydrochloric acid (HCl) by diluting 4.15 mL of determination on 25 mL of methanol.
concentrated HCl (density 1.19 g/mL) to 1 L with water.
7.4 Hydroxylamine Hydrochloride Solution—Dissolve 20 g 11. Calculation
of hydroxylamine hydrochloride (NH2OH·HCl) in 1 L of 11.1 Calculate the percentage of aldehydes as benzaldehyde
methanol and neutralize to the red-yellow end point of thymol as follows:
blue indicator.
Aldehydes, % 5 @~~A 2 B!N 3 0.106!/25C# 3 100
7.5 Methanol.
7.6 Sodium Hydroxide, Standard Solution (0.05 N)— where:
Dissolve 2.00 g of low-carbonate sodium hydroxide (NaOH) in A = NaOH solution required for titration of the specimen,
water and dilute to 1 L. Standardize against primary standard mL,
benzoic acid. B = NaOH solution required for titration of the methanol
7.7 Thymol Blue Indicator Solution— Dissolve 0.1 g of blank, mL,
thymol sulfonphthalein, sodium salt, in water and dilute to 100 N = normality of NaOH solution used, and
mL. C = density of styrene monomer.

8. Hazards 12. Report

8.1 Consult the latest OSHA regulations, supplier’s Material 12.1 Report the aldehydes content to the nearest 0.001 %.
Safety Data Sheets, and local regulations regarding all mate-
rials used in this test method. 13. Precision and Bias
8.2 Styrene monomer is flammable and polymerizes exo- 13.1 Intermediate Precision (formerly called
thermally on contact with peroxides, mineral acids, and AlCl3. Repeatability)—Duplicate results by the same operator should
9. Sampling not be considered suspect (95 % confidence limit) unless they
differ by more than the following:
9.1 Collect the sample as directed in Practice D 3437. Aldehyde Content, % Repeatability, %
0.004 0.0006
10. Procedure
10.1 Pipet 25.0 mL of the sample ( Warning—see 8.2) into 13.2 Reproducibility—The averages of duplicate results
a 250-mL glass-stoppered Erlenmeyer flask containing 25 mL submitted by each of two laboratories should not be considered
of methanol. Record the temperature of the sample. Add 0.2 suspect (95 % confidence limit) unless they differ by more than
mL of thymol blue indicator and, if necessary, neutralize with the following:
0.05 N NaOH solution or 0.05 N HCl to the red-yellow end Aldehyde Content, % Reproducibility, %
0.004 0.0016
point (do not record). Add 25 mL of the neutralized hydroxy-
lamine hydrochloride solution and allow to stand 1 h, shaking 13.3 Bias—Since there is no accepted reference material
the flask occasionally. Titrate to the original red-yellow end suitable for determining the bias in this test method for
point with 0.05 N NaOH solution, dispensed from a 10-mL measuring aldehydes, bias has not been determined.
buret, and record the volume used. Let stand 1 h and again
titrate any acid that may have been liberated. Record the total 14. Keywords
volume of NaOH used. 14.1 aldehyde content; aldehydes in styrene; styrene

SUMMARY OF CHANGES

Committee D16 has identified the location of selected changes to this standard since the last issue
(D 2119 – 96) that may impact the use of this standard.

(1) A concentration range for the method was added to the (2) Section 5 Interferences was added.
Scope paragraph 1.1. The value was calculated based on the (3) Editorial changes made to conform to D16 Editorial
theoretical abilities of the method and typical range. Guidelines.

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.

2
 D 2119 – 03

This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
address or at 610-832-9585 (phone), 610-832-9555 (fax), or service@astm.org (e-mail); or through the ASTM website
(www.astm.org).