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GB/T 7731.1-2021Ferrotungsten—Determination of tungsten content—Cinchonine gravimetric method and ammonium nitrate gravimetric method (English PDF)

钨铁 钨含量的测定 辛可宁重量法和硝酸铵重量法

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Issued by

SAMR; SAC

Level / Type

National · Recommended

Issue date

August 20, 2021

Implementation date

March 1, 2022

Scope

GB/T 7731.1-2021 is the English-translated version of 钨铁 钨含量的测定 辛可宁重量法和硝酸铵重量法.

GB/T 7731.1-2021 is part of the Chinese series of methods for the chemical analysis of ferrotungsten, and specifies two gravimetric methods for its tungsten content, over a range of 50.00% to 90.00%.

In the first, the sample is dissolved in nitric and hydrofluoric acids, tungstic acid is precipitated with cinchonine and alpha-benzoin oxime and ignited to impure tungsten trioxide, whose impurities are then separated by sodium carbonate fusion, with a spectrophotometric correction for molybdenum.

The second, added in this edition, is an ammonium nitrate gravimetric method. The document gives reagents, calculation formulas, permissible differences between laboratories, a molybdenum determination annex and a flow chart for accepting test results.

Ferroalloy producers and testing laboratories use it. It replaces GB/T 7731.1-1987, was issued on 20 August 2021 and has applied since 1 March 2022.

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Document preview — GB/T 7731.1-2021

National Standard of the People's Republic of China

ICS
77.100
Classification
H 11
Replacing
GB/T 7731.1-1987

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

Contents

  • Foreword
  • Introduction
  • 1 Scope
  • 2 Normative references
  • 3 Terms and definitions
  • 4 Method 1. Cinchonine weight method

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" Drafting.

This document is Part 1 of GB/T 7731. GB/T 7731 currently publishes the following parts.

---Determination of tungsten iron tungsten content Cinchonine gravimetric method and ammonium nitrate gravimetric method;

---Determination of tungsten, ferromanganese, periodate spectrophotometry and flame atomic absorption spectrometry;

---Determination of tungsten iron copper content dicyclohexanone oxalyl dihydrazone photometry and flame atomic absorption spectrometry;

---Determination of ferrotungsten and phosphorus content Phosphomolybdenum blue spectrophotometric method;

---Determination of tungsten iron silicon content silicon molybdenum blue spectrophotometric method;

---Determination of tungsten, iron, arsenic content, molybdenum blue photometry and inductively coupled plasma atomic emission spectrometry;

---Determination of tungsten iron tin content phenylfluorone photometric method and inductively coupled plasma atomic emission spectrometry;

---Determination of iron tungsten and antimony content Rhodamine B photometric method and inductively coupled plasma atomic emission spectrometry;

---Determination of bismuth tungsten iron bismuth iodide photometric method and inductively coupled plasma atomic emission spectrometry;

---Determination of tungsten iron carbon content infrared absorption method;

---Determination of ferro-tungsten and sulfur content infrared absorption method and combustion neutralization titration method;

---Determination of tungsten, iron and lead content by polarography and inductively coupled plasma atomic emission spectrometry.

This document replaces GB/T 7731.1-1987 "Methods for Chemical Analysis of Ferrotungsten Cinchonine Gravimetric Method for the Determination of Tungsten Content". With GB/T 7731.1- Compared with 1987, in addition to structural adjustments and editorial changes, the main technical changes are as follows.

a) Modified the measurement range from "greater than 65%" to "50.00%~90.00%" (see Chapter 1, Chapter 1 of the 1987 edition);

b) Modified the flux used to melt insoluble residue, from "0.5g sodium carbonate and 0.5g diboron trioxide" to "5g anhydrous carbonic acid Sodium" (see 4.4.3.3, 4.3.3 of the 1987 edition);

c) Modified the temperature of burning impure tungsten trioxide, from "not exceeding 750°C" to "750°C~800°C" (see 4.4.3.6, 1987 edition) 4.3.6);

d) Modified the calculation formula of Method 1, and added "[]" in the numerator of the formula (see 4.5.1, Chapter 5 of the 1987 edition);

e) Modified the allowable difference section of Method 1, and increased the allowable difference between laboratories (see 4.6, Chapter 6 of the 1987 edition);

f) Added method two. ammonium nitrate gravimetric method (see Chapter 5);

g) Modified the concentration of molybdenum standard solution in Appendix A, from "0.5µgMO/mL" to "20µg/mL" (see A.2.8, 1987 Version of A3);

h) Modified the calculation formula in Appendix A, deleting "m0'" in the denominator (see A.4, A4 in the 1987 edition);

i) Added "Test Results Acceptance Flow Chart" (see Appendix B).

Introduction

As there are many elements involved in the detection process of ferrotungsten, the applicable scope and applicable methods of the elements are different. to ensure that The convenience and accuracy of ferrotungsten testing standards. We have established national standards to support ferrotungsten testing based on the analysis methods for different elements of ferrotungsten. system. The GB/T 7731 series of analysis methods for ferro-tungsten are the basic standards for the detection of ferro-tungsten in my country. It is planned to consist of the following fourteen parts. But some The points have been abolished, and you need to pay attention to it during use.

---GB/T 7731.1 Determination of tungsten iron tungsten content Cinchonine gravimetric method and ammonium nitrate gravimetric method. The purpose is to measure the tungsten iron For the tungsten content, the cinchonine gravimetric method and the ammonium nitrate gravimetric method are used.

---GB/T 7731.2 Determination of Tungsten Ferromanganese Content Periodate Spectrophotometry and Flame Atomic Absorption Spectrometry. Aim at To measure the manganese content in ferrotungsten, periodate spectrophotometry and flame atomic absorption spectrometry were used.

---GB/T 7731.3 Determination of tungsten-iron-copper content. Dicyclohexanone oxalyl dihydrazone spectrophotometry and flame atomic absorption spectrometry. Item The method is to measure the copper content in ferro tungsten, using dicyclohexanone oxalyl dihydrazone spectrophotometry and flame atomic absorption spectrometry.

---GB/T 7731.4 Determination of Tungsten Ferrophosphorus Content Phosphomolybdenum Blue Spectrophotometric Method. The purpose is to measure the phosphorus content in ferro tungsten, Using phosphomolybdenum blue spectrophotometry.

---GB/T 7731.5 Determination of tungsten ferrosilicon content Silicon molybdenum blue spectrophotometric method. The purpose is to measure the silicon content in ferro tungsten, Using silicon molybdenum blue spectrophotometry.

---GB/T 7731.6 Determination of tungsten, iron, arsenic content, molybdenum blue photometry and inductively coupled plasma atomic emission spectrometry. Item The purpose is to measure the arsenic content in ferro-tungsten, using molybdenum blue photometry and inductively coupled plasma atomic emission spectrometry.

---GB/T 7731.7 Determination of tungsten-iron-tin content-Phenylfluorone photometric method and inductively coupled plasma atomic emission spectrometry Law. The purpose is to measure the tin content in ferro tungsten, using phenylfluorone photometry and inductively coupled plasma atomic emission light Spectrum method.

---GB/T 7731.8 Determination of tungsten iron antimony content Rhodamine B photometric method and inductively coupled plasma atomic emission spectrometry Law. The purpose is to measure the antimony content in ferro tungsten, using rhodamine B photometry and inductively coupled plasma atomic emission light Spectrum method.

---GB/T 7731.9 Determination of bismuth tungsten iron bismuth iodide photometric method and inductively coupled plasma atomic emission spectrometry.

The purpose is to measure the bismuth content in ferro-tungsten, using bismuth iodide photometry and inductively coupled plasma atomic emission spectrometry.

---GB/T 7731.10 Determination of tungsten iron carbon content infrared absorption method. The purpose is to measure the carbon content in ferro tungsten, using Infrared absorption method.

---GB/T 7731.11 Ferrotungsten Chemical Analysis Method Coulometric Method for the Determination of Carbon Content. The purpose is to measure the carbon content in ferro tungsten, using Coulomb method. This part has been abolished.

---GB/T 7731.12 Determination of tungsten iron and sulfur content infrared absorption method and combustion neutralization titration method. The purpose is to measure tungsten The sulfur content in iron uses infrared absorption method and combustion neutralization titration method.

---GB/T 7731.13 Methods for chemical analysis of ferrotungsten. Combustion neutralization titration method for the determination of sulfur content. The purpose is to measure the sulfur in ferro tungsten For the content, use the combustion neutralization titration method. This part has been abolished.

---GB/T 7731.14 Determination of tungsten, iron and lead content by polarography and inductively coupled plasma atomic emission spectrometry. Purpose To measure the lead content in ferro-tungsten, polarography and inductively coupled plasma atomic emission spectrometry are used.

Warning---Personnel using this document should have formal laboratory work experience. This document does not indicate all possible safety issues question. The user is responsible for taking appropriate safety and health measures and ensuring compliance with the conditions stipulated by relevant national laws and regulations.

1 Scope

This document specifies the cinchonine gravimetric method and the ammonium nitrate gravimetric method for the determination of tungsten content in ferrotungsten.

This document is applicable to the determination of tungsten content in ferro-tungsten. Measuring range (mass fraction). 50.00%~90.00%.

2 Normative references

The contents of the following documents constitute the indispensable clauses of this document through normative references in the text. Among them, dated quotations Only the version corresponding to that date is applicable to this document; for undated reference documents, the latest version (including all amendments) is applicable to this document.

GB/T 4010 Collection and preparation of samples for chemical analysis of ferroalloys

GB/T 6682 Analytical laboratory water specifications and test methods

GB/T 8170 Numerical rounding rules and the expression and determination of limit values

3 Terms and definitions

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

4 Method 1. Cinchonine weight method

4.1 Principle

The sample is dissolved with nitric acid and hydrofluoric acid, and sulfuric acid emits a large amount of white smoke to drive fluorine. Add water and hydrochloric acid to dissolve the soluble salts, and the insoluble residue will be carbon Sodium melts. In the hydrochloric acid solution, cinchonine and alpha-benzoin oxime were used to completely precipitate tungstic acid. Filter and burn to get impure trioxide Tungsten, weighed. The impure tungsten trioxide is melted with sodium carbonate, and sodium tungstate is dissolved in water after being dissolved in hot water. Other insoluble impurities are filtered, burned, Weigh, and calculate the mass fraction of tungsten from the two mass differences. If the sample contains molybdenum, the spectrophotometric determination of molybdenum is carried out, and then the amount of tungsten is corrected.

4.2 Reagents

Unless otherwise specified, only use analytical reagents.

4.2.1 Water, GB/T 6682, level three.

4.2.2 Anhydrous sodium carbonate, solid.

4.2.3 Nitric acid, rho=1.42g/mL.

4.2.4 Hydrofluoric acid, rho=1.15g/mL.

4.2.5 Hydrochloric acid, rho=1.19g/mL.

4.2.6 Absolute ethanol. […]

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

Referenced standards

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Editions of GB/T 7731.1

EditionTitleRevisionStatus
GB/T 7731.1-2021Ferrotungsten—Determination of tungsten content—Cinchonine gravimetric method and ammonium nitrate gravimetric methodcurrent editionCurrent
GB/T 7731.1-1987Ferrotungsten—Determination of tungsten content—Cinchonine gravimetric method and ammonium nitrate gravimetric methodprevious editionSuperseded

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