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GB/T 41671-2022Man-made fibers—Determination of solvent residues content (English PDF)

化学纤维 溶剂残留量的测定

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Issued by

SAMR; SAC

Level / Type

National · Recommended

Issue date

July 11, 2022

Implementation date

February 1, 2023

Scope

GB/T 41671-2022 is the English-translated version of 化学纤维 溶剂残留量的测定.

GB/T 41671-2022 tells laboratories how to measure the solvent left in man-made fibres after spinning.

It covers seven organic solvents and two inorganic ones, sodium thiocyanate and concentrated sulfuric acid, and gives four families of method: gas chromatography-mass spectrometry, high performance liquid chromatography-tandem mass spectrometry, spectrophotometry, and complexometric and acid-base titration, each with its principle, reagents, instruments, procedure, calculation, detection and quantification limits and precision.

Annexes add headspace gas chromatography for decalin in ultra-high molecular weight polyethylene fibre, a method for wet-spun fibre of the same kind, tables matching fibre types to solvents and methods, and worked detection parameters and chromatograms.

It applies to solution-spun fibres such as spandex, acrylic, polyimide, aramid, polyvinyl alcohol, lyocell and carbon fibre precursor. It was issued on 11 July 2022 and has applied since 1 February 2023.

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Document preview — GB/T 41671-2022

National Standard of the People's Republic of China

ICS
59.060.20
Classification
W 50

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

Contents

  • Preface
  • 1 Scope
  • 2 Normative references
  • 3 Terms and Definitions
  • 4 General Requirements
  • 5 Gas chromatography-mass spectrometry (GC-MS)
  • 5.1 Principle
  • 5.2 Reagents and materials
  • 5.3 Instruments and equipment
  • 5.4 Test Step
  • 5.5 Result calculation
  • 5.6 Detection limit, quantification limit
  • 5.7 Precision
  • 6 High performance liquid chromatography-tandem mass spectrometry (LC-MS/MS)
  • 6.1 Principle
  • 6.2 Reagents and materials
  • 6.3 Instruments and equipment
  • 6.4 Test Step
  • 6.5 Result calculation
  • 6.6 Detection limit, quantification limit
  • 6.7 Precision
  • 7 Spectrophotometry
  • 7.1 Principle
  • 7.2 Reagents and materials
  • 7.3 Instruments and equipment
  • 7.4 Test Step
  • 7.5 Result calculation
  • 7.6 Notes
  • 8 Titration
  • 8.1 Complexometric titration
  • 8.2 Acid-base titration
  • 9 Test report
  • Appendix A (Informative) Names of 7 Organic Solvents
  • Appendix B (normative) Determination of decalin residues in ultra-high molecular weight polyethylene fibers --- Headspace gas chromatography
  • Appendix C (normative) Determination of solvent residues in wet spinning ultra-high molecular weight polyethylene fibers
  • Appendix D (informative) Correspondence between various types of fibers, solvents and test methods
  • Appendix E (Informative) GC-MS Detection Parameter Conditions
  • Appendix F (informative) GC-MS analysis of organic solvent standard substance ion chromatogram
  • Appendix G (Informative) Statistical Results of Precision Test by GC-MS Method
  • Appendix H (Informative) Example LC-MS/MS Detection Parameters
  • Appendix I (Informative) LC-MS/MS Analysis of Organic Solvent Standard Material Gas Chromatogram

Foreword

This document is in accordance with the provisions of GB/T 1.1-2020 "Guidelines for Standardization Work Part 1: Structure and Drafting Rules of Standardization Documents" drafted.

1 Scope

This document describes the determination of the residues of 7 kinds of organic solvents (see Appendix A) and 2 kinds of inorganic solvents (sodium thiocyanate, concentrated sulfuric acid) in chemical fibers try method.

This document applies to some solution spinning chemical fibers, including spandex, acrylic, polyimide, meta-aramid, polyvinyl alcohol, super High molecular weight polyethylene fiber, lyocell fiber, polyacrylonitrile-based carbon fiber precursor, para-aramid. Other solution-spun chemical fibers can be found in according to use.

2 Normative references

The contents of the following documents constitute essential provisions of this document through normative references in the text. Among them, dated citations documents, only the version corresponding to that date applies to this document; for undated references, the latest edition (including all amendments) applies to this document.

GB/T 4146 (all parts) Textile chemical fibers

GB/T 6682 Analysis Laboratory Water Specifications and Experimental Methods

JJG 178-2007 Verification Regulations for Ultraviolet, Visible and Near Infrared Spectrophotometers

3 Terms and Definitions

The terms and definitions defined in GB/T 4146 (all parts) and the following terms and definitions apply to this document.

3.1 Solution spinning

A method of spinning a fiber-forming polymer by dissolving it into a concentrated solution of a certain concentration.

Note: According to the different coagulation methods, it is divided into dry spinning and wet spinning.

3.2 Solvent residues content

The mass of organic and inorganic compound solvents used in the spinning production process but not completely removed per unit mass of fibers.

4 General requirements

Gas chromatography-mass spectrometry (GC-MS) for N,N-dimethylacetamide (DMAC), N,N-dimethylformamide (DMF), N-methylacetamide Determination of residual amounts of pyrrolidone (NMP), dimethyl sulfoxide (DMSO), decalin and tetrahydronaphthalene. Determination of decalin residues can also be used by headspace gas chromatography. Headspace gas chromatography is carried out in accordance with the provisions of Appendix B.

High performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) for organic solvent N-methylmorpholine-N-oxide (NMMO) and its fractions Determination of residual amount of hydrolyzed products N-methylmorpholine (NMM), N-nitrosomorpholine (NNM) and morpholine (MOR).

Spectrophotometry is suitable for the determination of residues of dimethylformamide (DMF), dimethylacetamide (DMAC) and dimethyl sulfoxide (DMSO). The determination of the residual amount of N-methylpyrrolidone (NMP) can be used by reference.

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This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 25 pages — is available in the English PDF.

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