GB/T 7717.16-2022Acrylonitrile for industrial use—Part 16: Determination of iron and copper content—Graphite furnace atomic absorption spectrometry and inductively coupled plasma mass spectrometry (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.

This document is Part 16 of GB/T 7717 "Acrylonitrile for Industrial Use". GB/T 7717 has released the following parts.

--- Part 1: Specifications;

--- Part 5: Determination of acidity, pH value and titration value;

--- Part 8: Spectrophotometric method for the determination of total aldehyde content;

--- Part 9: Determination of total cyanide content by titration;

--- Part 10: Spectrophotometric method for the determination of peroxide content;

--- Part 11: Spectrophotometric method for the determination of iron and copper content;

--- Part 12: Determination of purity and impurity content by gas chromatography;

--- Part 15: Determination of p-hydroxyanisole content;

--- Part 16: Determination of iron and copper content by graphite furnace atomic absorption spectrometry and inductively coupled plasma mass spectrometry.

This document replaces GB/T 7717.16-2009 "Industrial Acrylonitrile Part 16: Determination of Iron Content Graphite Furnace Atomic Absorption Law" and GB/T 7717.17-2009 "Industrial Acrylonitrile Part 17: Determination of Copper Content Graphite Furnace Atomic Absorption Method", and Compared with GB/T 7717.17-2009, in addition to structural adjustment and editorial changes, the main technical changes are as follows.

a) Changed the scope (see Chapter 1, Chapter 1 of GB/T 7717.16-2009 and GB/T 7717.17-2009);

b) Added Inductively Coupled Plasma Mass Spectrometry (see Chapter 5);

c) Added quality assurance and control (see Chapter 6).

Introduction

GB/T 7717 "Industrial Acrylonitrile" includes product standards and supporting method standards for industrial acrylonitrile. In order to facilitate management and use, It consists of the following parts.

--- Part 1: Specifications. It specifies the product classification, technical requirements and test methods, sampling, inspection rules and standards of acrylonitrile for industrial use. signs, labels and accompanying documents, packaging, transport and storage.

--- Part 5: Determination of acidity, pH value and titration value. Determination of acidity by chemical titration; pH measurement by pH meter; Potentiometric drop Determine the titer value.

--- Part 8: Determination of total aldehyde content Spectrophotometric method. It is the reaction of total aldehydes and derivatizing reagents to produce colored anionic dyes.

The absorbance value was measured, and the total aldehyde content was calculated.

--- Part 9: Determination of total cyanide content by titration. The cyanide in the sample is extracted with an alkaline solution of potassium iodide to make it soluble The total cyanide content was calculated by titration with silver nitrate standard titration solution.

--- Part 10: Spectrophotometric method for the determination of peroxide content. Under the action of acetic anhydride, peroxide reacts with potassium iodide Yellow iodide ions should be generated, and the content of peroxide is calculated by measuring the absorbance value of the solution.

--- Part 11: Determination of iron and copper content by spectrophotometry. Evaporate the sample to dryness and digest with mixed acid to remove organic matter, and iron After the ion and copper ions react with the derivatizing reagent respectively, a colored complex is formed, which is measured with a spectrophotometer, and the iron and copper are calculated. content.

--- Part 12: Determination of purity and impurity content by gas chromatography. is the determination of the purity of acrylonitrile samples by gas chromatography and impurity content.

--- Part 15: Determination of p-hydroxyanisole content. Including spectrophotometry and gas chromatography, where spectrophotometry uses The absorbance of the sample was directly measured at 295 nm by an ultraviolet spectrophotometer, and the content of p-hydroxyanisole was calculated; gas chromatography method The content of p-hydroxyanisole was separated and determined by gas chromatography.

--- Part 16: Determination of iron and copper content by graphite furnace atomic absorption spectrometry and inductively coupled plasma mass spectrometry. of which stone Ink furnace atomic absorption spectrometry is to measure the absorbance at the characteristic wavelengths of iron and copper after diluting the sample with ethanol.

Calculate the iron and copper content; inductively coupled plasma mass spectrometry is to dilute the sample with ethanol, add the internal standard solution, and use iron and copper.

The characteristic mass of the mass spectrometer was collected, and the iron and copper contents were calculated.

Industrial Acrylonitrile Part 16: Determination of iron and copper content Graphite Furnace Atomic Absorption Spectrometry and Inductive Coupling plasma mass spectrometry Caution - This document is not intended to address all safety issues related to its use. It is the user's responsibility to take appropriate safety and Health measures to ensure compliance with the relevant state regulations.

1 Scope

This document specifies the graphite furnace atomic absorption spectrometry, inductively coupled plasma mass spectrometry for the determination of iron and copper content in industrial acrylonitrile Spectrum.

Graphite furnace atomic absorption spectrometry in this document is suitable for 0.010mg/kg~1.000mg/kg iron and copper content in industrial acrylonitrile Determination; Inductively coupled plasma mass spectrometry is suitable for the determination of 0.005mg/kg~1.000mg/kg iron and copper content in industrial acrylonitrile.

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 602 Preparation of standard solutions for the determination of impurities in chemical reagents

GB/T 3723 General Rules for Sampling Safety of Chemical Products for Industrial Use

GB/T 6678 General Rules for Sampling of Chemical Products

GB/T 6680 General Rules for Sampling of Liquid Chemical Products

GB/T 6682 Analysis Laboratory Water Specifications and Test Methods

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

3 Terms and Definitions

There are no terms and definitions that need to be defined in this document.

4 Graphite Furnace Atomic Absorption Spectrometry