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GB/T 24153-2009Rubber and elastomer materials - Determination of N-nitrosamines (English PDF)

橡胶及弹性体材料 N-亚硝基胺的测定

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Issued by

SAMR; SAC

Level / Type

National · Recommended

Issue date

June 15, 2009

Implementation date

February 1, 2010

Scope

GB/T 24153-2009 is the English-translated version of 橡胶及弹性体材料 N-亚硝基胺的测定.

GB/T 24153-2009 is the Chinese standard "Rubber and Elastomer Materials - Determination of N-nitrosaminess". Its scope clause reads: This Standard specifies adopting gas chromatography - mass selective detector (GC- MSD) to determine 12 types of N-nitrosamines (see Appendix A) contents in the rubber and elastomer.

This Standard is applicable to the rubber, elastomer materials and their products. Its clauses include principle; reagents and materials; apparatus; analytical procedures; result calculation; determination lower limit; test report.

It was issued by the General Administration of Quality Supervision, Inspection and Quarantine on JUNE 15, 2009 and took effect on FEBRUARY 1, 2010.

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Document preview — GB/T 24153-2009

National Standard of the People's Republic of China

ICS
83.060
Classification
G 40

Issued by: State Administration for Market Regulation; Standardization Administration of the PRC

Contents

  • Foreword3
  • 1 Scope4
  • 2 Principle4
  • 3 Reagents and Materials4
  • 4 Apparatus5
  • 5 Analytical Procedures5
  • 6 Result calculation7
  • 7 Determination Lower Limit7
  • 8 Test Report7
  • Appendix A (Normative) 12 Types of N-Nitrosamines Names and their GC/MS Selective Quantitative Ions9
  • Appendix B (Informative) N-Nitrosamines Standard Products' GC/MS Total Ion Flow Diagram10

Foreword

This Standard's Appendix A is normative; while Appendix B is informative.

1 Scope

This Standard specifies adopting gas chromatography - mass selective detector (GC- MSD) to determine 12 types of N-nitrosamines (see Appendix A) contents in the rubber and elastomer.

This Standard is applicable to the rubber, elastomer materials and their products.

2 Principle

The sample was extracted by methanol; after concentrating, the extracting solution passes through C18 solid-phase extraction column to purify; the sample solution enters into the gas chromatography - mass selective detector (GC-MSD) to be measured; qualified by full-scanning detection; select ions to quantify by external standard method.

3 Reagents and Materials

Unless otherwise is specified, all the reagents used are chromatographic pure.

3.1 Methanol, the blank test check there are no interfering substances.

3.2 C18 solid-phase extraction column. 500mg/3mL.

3.3 Standard stock solution. separately and accurately weigh the appropriate amount of each N-nitrosamines standard products; use methanol to prepare the standard stock solution with concentration of 200mg/L; inject into the brown reagent bottle; store in the refrigerator at 5°C below; and valid for 3 months.

4 Apparatus

4.1 Gas chromatograph. equipped with mass selective detector (MSD).

4.2 Ultrasonic generator. operating frequency of 40kHz.

4.5 Vortex mixer.

4.6 Conical flask. brown, with ground stopper, 100mL.

4.7 Concentrated bottle. brown, 150mL.

4.8 Centrifuge tube. brown, 10mL.

5 Analytical Procedures

5.1 Specimen preparation and extraction

Take the representative sample, use appropriate tool to cut it into particles with edges of 3mm below, mix evenly.

5.2 Purification

Place C18 solid-phase extraction column (3.2) onto the solid-phase extraction apparatus (4.4), use 5mL of methanol to pre-leach C18 column; discard the effluent.

5.3 Determination

5.3.1 Determination condition of gas chromatography-mass spectrometry

Since the test results depend on the apparatus used, the general parameters for chromatographic analysis can't be given. The operating parameters given below have been shown to be feasible, which only serve as reference for measurement.

5.3.2 Qualitative and quantitative analysis of gas chromatography-mass

spectrometry Separately take 1µL standard working solution (3.4) and sample solution (5.2), inject into the chromatograph for determination. If there is a chromatogram peak at the same retention time in the total ion flow diagram of sample solution and standard working solution, qualify through comparing the characteristic ions of sample and standard products; use the selective ion monitoring method to perform the external standard method.

6 Result calculation

Each N-nitrosamines content in the sample shall be calculate as per Formula (1).

7 Determination Lower Limit

The determination lower limit of this method is 0.5mg/kg.

8 Test Report

The test report shall give the following contents at least. […]

......
This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 15 pages — is available in the English PDF.

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