GB/T 41067-2021Nanotechnologies—Determination of sulfur, fluorine, chlorine and bromine content in graphene flakes—Combustion ion chromatography method (English PDF)

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.

Introduction

The sources of sulfur, fluorine, chlorine and bromine in graphene powder are wide. The production raw materials of some graphene powders contain a certain amount of the above-mentioned four Elements, chemical reagents used in the production and preparation process may also introduce the above four elements. Sulfur, fluorine, chlorine and bromine in graphene powder The content of the element has a certain influence on its application in lubricating oil, electrical and electronic products, functional coatings and other fields.

Combustion ion chromatography has the characteristics of rapidity, convenience, good reproducibility and high sensitivity.

The content of sulfur, fluorine, chlorine and bromine in graphene powder.

Warning: Persons using this document should have practical experience with formal laboratory work. This method does not specify any There are security concerns. Some of the experimental procedures specified in this document may lead to hazardous situations, and it is the responsibility of the user to take appropriate safety and health measures, and ensure compliance with the conditions stipulated by the relevant national laws and regulations.

1 Scope

This document describes a method for the determination of sulfur, fluorine, chlorine and bromine content in graphene powder by combustion ion chromatography.

This document is applicable to the determination of sulfur, fluorine, chlorine and bromine content in graphene powder.

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 6682 Analysis Laboratory Water Specifications and Test Methods

GB/T 8170 Numerical Rounding Rules and Representation and Judgment of Limit Values

GB/T 30544.13 Nanotechnology Terminology Part 13. Graphene and related two-dimensional materials

3 Terms and Definitions

The terms and definitions defined in GB/T 30544.13 and the following apply to this document.

4 Principles

Based on the principle of pyrolysis, the sample is pyrolyzed and burned in an oxygen stream, fluorine, chlorine, and bromine are converted into hydrogen halide gas, and sulfur is converted into oxidized gas. material gas. The generated gas is transported by the carrier gas to the hydrogen peroxide absorption liquid for absorption, and converted into halogenated acid and sulfuric acid solution respectively. Fluorine in the absorption liquid After the ion, chloride ion, bromide ion and sulfate ion are separated by the chromatographic column, the electrical conductivity of each anion component is determined by a conductivity detector with a suppressor.

The conductivity was qualitatively determined according to the relative retention time of each component in the standard solution, and quantified by the standard curve method. The content of sulfur, fluorine, chlorine and bromine in the sample It is calculated from the content of sulfate ion, fluoride ion, chloride ion and bromide ion in the absorption liquid respectively.

5 Reagents and Materials

5.1 Unless otherwise stated, the reagents used in this method are all analytically pure, and the water is first-grade water that meets the requirements of GB/T 6682.