D 2119 - 96 - Rdixmtktukve
D 2119 - 96 - Rdixmtktukve
D 2119 - 96 - Rdixmtktukve
1. Scope*
1.1 This laboratory test method covers the wet chemical determination of aldehydes in styrene monomer. Aldehydes are
calculated and reported as benzaldehyde.
1.2 The following applies to all specified limits in benzaldehyde. The range of concentration for this test method: f is 0.001 %
to 0.030 %.
1.2 For purposes of determining conformance with this test method, an observed value or a calculated value shall be rounded
off “to the nearest unit” in the last right-hand digit used in expressing the specification limit, in accordance with the rounding-off
method of Practice E 29.
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 and health practices and determine the applicability of regulatory
limitations prior to use. For specific hazard statements, see Section 7. 8.
2. Referenced Documents
2.1 ASTM Standards:
D 1193 Specification for Reagent Water2
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 C 10 Aromatic Hydrocarbons.
Current edition approved June Aug. 10, 1996. 2003. Published August 1996. 2003. Originally published as D 2119 – 62 T. approved in 1962. Last previous edition
e1
D 2119 – 87 (1992) . approved in 1996 as D 2119 – 96.
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D 2119 – 9603
D 3437 Practice for Sampling and Handling Liquid Cyclic Products3
E 29 Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications4
2.2 Other Documents:
OSHA Regulations, 29 CFR, paragraphs 1910.1000 and
1910.12005
3. Summary of Test Method
3.1 An alcoholic solution of hydroxylamine hydrochloride is added to a specimen of styrene monomer. Active aldehydes present
react in accordance with the following equation:
RCHO 1 NH2OH·HCl → RCHNOH 1 H 2O 1 HCl
The hydrochloric acid, which is equivalent to the aldehyde present in the sample, is titrated with standard sodium hydroxide
solution. Ketones, if present, interfere by partially reacting with the reagent. 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.
6. Apparatus
56.1 Erlenmeyer Flasks, glass-stoppered, 250-mL.
56.2 Pipets, 25-mL.
56.3 Volumetric Flasks, 100-mL.
56.4 Burets, 10-mL. (Microburets are preferred.)
56.5 Thermometers, capable of differentiating 1°C at ambient.
67. Reagents
67.1 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
specifications are available.6 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.
67.2 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.
67.3 Hydrochloric Acid, Standard (0.05 N)—Prepare a 0.05 N solution of hydrochloric acid (HCl) by diluting 4.15 mL of
concentrated HCl (density 1.19 g/mL) to 1 L with water.
67.4 Hydroxylamine Hydrochloride Solution—Dissolve 20 g of hydroxylamine hydrochloride (NH2OH·HCl) in 1 L of methanol
and neutralize to the red-yellow end point of thymol blue indicator.
67.5 Methanol.
67.6 Sodium Hydroxide, Standard Solution (0.05 N) —Dissolve 2.00 g of low-carbonate sodium hydroxide (NaOH) in water
and dilute to 1 L. Standardize against primary standard benzoic acid.
67.7 Thymol Blue Indicator Solution— Dissolve 0.1 g of thymol sulfonphthalein, sodium salt, in water and dilute to 100 mL.
78. Hazards
78.1 Consult the latest OSHA regulations, supplier’s Material Safety Data Sheets, and local regulations regarding all materials
used in this test method.
78.2 Styrene monomer is flammable and polymerizes exothermally on contact with peroxides, mineral acids, and AlCl3.
8. Sampling
8.1 Collect the sample as directed in Practice D 3437.
2
Annual Book of ASTM Standards, Vol 11.01.
3
Annual Book of ASTM Standards, Vol 06.04.
4
Annual Book of ASTM Standards, Vol 14.02.
5
Available from Superintendent of Documents, U.S. Government Printing Office, Washington, DC 20402. Standardization Documents Order Desk, DODSSP, Bldg. 4,
Section D, 700 Robbins Ave., Philadelphia, PA 19111-5098
6
Reagent Chemicals, American Chemical Society Specifications , American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed by
the American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and National
Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville, MD.
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D 2119 – 9603
9. Sampling
9.1 Collect the sample as directed in Practice D 3437.
10. Procedure
910.1 Pipet 25.0 mL of the sample ( Warning—see 7 8.2) into a 250-mL glass-stoppered Erlenmeyer flask containing 25 mL
of methanol. Record the temperature of the sample. Add 0.2 mL of thymol blue indicator and, if necessary, neutralize with 0.05
N NaOH solution or 0.05 N HCl to the red-yellow end point (do not record). Add 25 mL of the neutralized hydroxylamine
hydrochloride solution and allow to stand 1 h, shaking the flask occasionally. Titrate to the original red-yellow end point with 0.05
N NaOH solution, dispensed from a 10-mL buret, and record the volume used. Let stand 1 h and again titrate any acid that may
have been liberated. Record the total volume of NaOH used.
910.2 Since methanol may contain aldehydes, run a blank determination on 25 mL of methanol.
101. Calculation
101.1 Calculate the percentage of aldehydes as benzaldehyde as follows:
Aldehydes, % 5 @~~A 2 B!N 3 0.106!/25C# 3 100
where:
A = NaOH solution required for titration of the specimen, mL,
B = NaOH solution required for titration of the methanol blank, mL,
N = normality of NaOH solution used, and
C = density of styrene monomer.
11. Report
11.1 Report the aldehydes content to the nearest 0.001 %.
12. Report
12.1 Report the aldehydes content to the nearest 0.001 %.
123.2 Reproducibility—The averages of duplicate results submitted by each of two laboratories should not be considered
suspect (95 % confidence limit) unless they differ by more than the following:
Aldehyde Content, % Reproducibility, %
0.004 0.0016
13.3 Bias—Since there is no accepted reference material suitable for determining the bias in this test method for measuring
aldehydes, bias has not been determined.
14. Keywords
134.1 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 Scope paragraph 1.1. The value was calculated based on the theoretical
abilities of the method and typical range.
(2) Section 5 Interferences was added.
(3) Editorial changes made to conform to D16 Editorial Guidelines.
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D 2119 – 9603
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