GB/T 42276-2022Determination of fluorine ion and chloride ion in silicon nitride powder—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 for Standardization Documents" drafting.

1 Scope

This document describes an ion chromatographic method for the determination of fluoride and chloride ions in silicon nitride powders.

This document is applicable to the determination of fluoride ion and chloride ion content in silicon nitride powder, and the test range is 0.0500mg/g~0.600mg/g.

2 Normative references

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

GB/T 602 Preparation of Standard Solution for Determination of Impurities in Chemical Reagents

GB/T 6682 Analytical laboratory water specifications and test methods

GB/T 14666 Analytical Chemistry Terminology

3 Terms and Definitions

The terms and definitions defined in GB/T 14666 apply to this document.

4 Principles of the method

The silicon nitride powder sample is burned and hydrolyzed in the mixed flow of oxygen and water vapor, and the fluorine and chlorine in the silicon nitride are converted into volatile fluorides respectively. and chloride, and dissolved in water in the form of ions, and the content of fluoride and chloride ions in silicon nitride powder was determined by ion chromatography.

5 Interfering factors

5.1 If the sample weight is too large, it will cause insufficient combustion, which will affect the test results. It is recommended to weigh 0.100g sample.

5.2 The sample and quartz sand should be mixed evenly and laid flat in the porcelain ark, otherwise the test results will be affected.

5.3 If the oxygen flow rate is too large or too small, it will affect the combustion result. It is recommended to adjust the oxygen flow rate to 400mL/min.

5.4 The sealing of the combustion hydrolysis device should be good enough, otherwise the detection result will be low.

6 Test conditions

The temperature range is 20°C~25°C, and the relative humidity is not more than 55%.

7 Reagents and Materials

7.1 Water. Class II specified in GB/T 6682