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GB/T 3884.12-2023Methods for chemical analysis of copper concentrates—Part 12:Determination of fluoride and chloride contents—Ion chromatography and potentiometric titration (English PDF)

铜精矿化学分析方法 第12部分:氟和氯含量的测定 离子色谱法和电位滴定法

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Issued by

SAMR; SAC

Level / Type

National · Recommended

Issue date

August 6, 2023

Implementation date

March 1, 2024

Scope

GB/T 3884.12-2023 is the English-translated version of 铜精矿化学分析方法 第12部分:氟和氯含量的测定 离子色谱法和电位滴定法.

GB/T 3884.12-2023 is Part 12 of GB/T 3884 and gives two methods for the fluorine and chlorine content of copper concentrates.

In method 1 the sample is decomposed with sulfuric acid, the fluorine and chlorine escape with the water vapour into an absorbing solution and are measured by ion chromatography against a working curve; the ranges are 0.005% to 0.50% fluorine and 0.010% to 0.50% chlorine, and the chlorine so measured is acid-leached chlorine.

Method 2 measures chlorine by potentiometric titration from 0.050% to 4.50%, and is the arbitration method above 0.05% chlorine. The document also covers the reagents, the treatment of test data, the determination of repeatability and reproducibility, and the test report.

It replaces GB/T 3884.12-2010, was issued on 6 August 2023 and has applied since 1 March 2024.

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Document preview — GB/T 3884.12-2023

National Standard of the People's Republic of China

ICS
77.120.30
Classification
H 13
Replacing
GB/T 3884.12-2010

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

Contents

  • Foreword
  • Introduction
  • 1 Scope
  • 2 Normative reference documents
  • 3 Terms and definitions
  • 4 Method 1 Ion chromatography

Foreword

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

This document is Part 12 of GB/T 3884 "Chemical Analysis Methods for Copper Concentrates". GB/T 3884 has released the following parts.

---Part 1: Determination of copper amount by iodometric method;

---Part 2: Determination of the amount of gold and silver by flame atomic absorption spectrometry and fire assay;

---Part 3: Determination of sulfur content by gravimetric method and combustion-titration method;

---Part 4: Determination of magnesium oxide content by flame atomic absorption spectrometry;

---Part 5: Determination of fluorine content by ion selective electrode method;

---Part 6: Determination of lead, zinc, cadmium and nickel amounts by flame atomic absorption spectrometry;

---Part 7: Determination of lead content by Na2EDTA titration method;

---Part 8: Determination of zinc content by Na2EDTA titration method;

---Part 9: Determination of the amount of arsenic and bismuth hydride generation - atomic fluorescence spectrometry, potassium bromate titration and diethyldithioamide Silver formate spectrophotometry;

---Part 10: Determination of antimony amount hydride generation-atomic fluorescence spectrometry;

---Part 11: Determination of mercury content by cold atomic absorption spectrometry;

---Part 12: Determination of fluorine and chlorine content by ion chromatography and potentiometric titration;

---Part 13: Determination of copper content by electrolytic method;

---Part 14: Determination of the amount of gold and silver by fire assay gravimetric method and atomic absorption spectrometry;

---Part 15: Determination of iron content by potassium dichromate titration method;

---Part 16: Determination of silica content by potassium fluosilicate titration and gravimetric method;

---Part 17: Determination of the amount of aluminum oxide chromium azure S micelle solubilization photometric method and precipitation separation - fluorine salt replacement - Na2EDTA titration;

---Part 18: Determination of arsenic, antimony, bismuth, lead, zinc, nickel, cadmium, cobalt, chromium, aluminum oxide, magnesium oxide, calcium oxide content, inductive coupling, etc. Ion plasma atomic emission spectrometry;

---Part 19: Determination of thallium content by inductively coupled plasma mass spectrometry;

---Part 20: Determination of mercury content by solid injection direct method;

---Part 21: Determination of copper, sulfur, lead, zinc, iron, aluminum, calcium, magnesium and manganese by wavelength dispersive X-ray fluorescence spectrometry.

This document replaces GB/T 3884.12-2010 "Methods for chemical analysis of copper concentrates - Part 12: Determination of fluorine and chlorine content. Ion chromatography Spectrum Method", compared with GB/T 3884.12-2010, in addition to structural adjustments and editorial changes, the main technical changes are as follows.

a) Added method 2, measuring chlorine by potentiometric titration, with a measuring range of 0.050%~4.50% (see Chapter 1 and Chapter 5);

b) Changed the water requirements for Method 1 (see 4.2.1, Chapter 3 of the 2010 edition);

c) Changed the drying temperature of the reference sodium fluoride (see 4.2.7, 3.6 of the 2010 edition);

d) Changed the regulations on syringe range (see 4.3.4, 2010 version of 4.4);

e) Increased sample measurement volume (see Table 1);

f) Added requirements for numerical rounding in method 1 test data processing (see 4.6);

g) Changed the method of determining repeatability and reproducibility (see 4.7, see Chapter 8 of the 2010 edition);

h) Added the content of "Test Report" (see Chapter 6);

i) Delete "Quality Assurance and Control" (see Chapter 9 of the 2010 edition).

Introduction

Copper concentrate is the main raw material for the production of cathode copper. In the non-ferrous field standard system, the determination method standards for the chemical composition of copper concentrate are important in ensuring the copper Concentrate product quality plays an important role. This series of method standards serve the production, trade and application of copper concentrate and provide a solid foundation for my country's non-ferrous gold industry.

Provide technical support for the high-quality development of the industry. GB/T 3884 "Chemical Analysis Methods for Copper Concentrates" aims to describe the contents of copper, gold, and Methods for determining the composition of different chemical elements such as silver, lead, zinc, etc. Because copper concentrate contains a certain amount of fluorine and chlorine; high levels of fluorine and chlorine cause The content of hydrogen fluoride and hydrogen chloride in the smelting flue gas increases, and the flue gas with high levels of hydrogen fluoride and hydrogen chloride enters the acid-making process, which is prone to corrosion and damage to the acid-making equipment, which is harmful to the smelting industry.

Refining causes disadvantages. The control of fluorine and chlorine content in copper concentrate is a very important technical indicator in the copper refining step. Therefore, for copper essence The determination of fluorine and chlorine content in mines is of great significance.

GB/T 3884 "Chemical Analysis Methods for Copper Concentrates" consists of 21 parts.

---Part 1: Determination of copper amount by iodometric method;

---Part 2: Determination of the amount of gold and silver by flame atomic absorption spectrometry and fire assay;

---Part 3: Determination of sulfur content by gravimetric method and combustion-titration method;

---Part 4: Determination of magnesium oxide content by flame atomic absorption spectrometry;

---Part 5: Determination of fluorine content by ion selective electrode method;

---Part 6: Determination of lead, zinc, cadmium and nickel amounts by flame atomic absorption spectrometry;

---Part 7: Determination of lead content by Na2EDTA titration method;

---Part 8: Determination of zinc content by Na2EDTA titration method;

---Part 9: Determination of the amount of arsenic and bismuth hydride generation - atomic fluorescence spectrometry, potassium bromate titration and diethyldithioamide Silver formate spectrophotometry;

---Part 10: Determination of antimony amount hydride generation-atomic fluorescence spectrometry;

---Part 11: Determination of mercury content by cold atomic absorption spectrometry;

---Part 12: Determination of fluorine and chlorine content by ion chromatography and potentiometric titration;

---Part 13: Determination of copper content by electrolytic method;

---Part 14: Determination of the amount of gold and silver by fire assay gravimetric method and atomic absorption spectrometry;

---Part 15: Determination of iron content by potassium dichromate titration method;

---Part 16: Determination of silica content by potassium fluosilicate titration and gravimetric method;

---Part 17: Determination of the amount of aluminum oxide chromium azure S micelle solubilization photometric method and precipitation separation - fluorine salt replacement - Na2EDTA titration;

---Part 18: Determination of arsenic, antimony, bismuth, lead, zinc, nickel, cadmium, cobalt, chromium, aluminum oxide, magnesium oxide, calcium oxide content, inductive coupling, etc. Ion plasma atomic emission spectrometry;

---Part 19: Determination of thallium content by inductively coupled plasma mass spectrometry;

---Part 20: Determination of mercury content by solid injection direct method;

---Part 21: Determination of copper, sulfur, lead, zinc, iron, aluminum, calcium, magnesium and manganese by wavelength dispersive X-ray fluorescence spectrometry.

The formulation of this document is based on the needs of domestic and foreign copper concentrate trade. The establishment of this standard can better adapt to the requirements of different origins at home and abroad.

The determination of fluorine and chlorine content in copper concentrate provides an accurate and scientific basis for the determination of fluorine and chlorine content in copper concentrate. Therefore, the determination of chlorine content The addition of determination method 2 fills the gap in the determination of higher chlorine content in copper concentrates. Facilitates the use of unified analysis methods in trade transactions, and It is conducive to reducing commercial disputes caused by differences in detection methods, and has good economic and social benefits.

Warning---Personnel using this document should have practical experience in regular laboratory work. This document does not address all possible safety question. Users are responsible for taking appropriate safety and health measures and ensuring compliance with the conditions stipulated in relevant national regulations.

1 Scope

This document describes methods for the determination of fluorine and chlorine content in copper concentrates, including ion chromatography (Method 1) and potentiometric titration (Method 2).

This document is applicable to the determination of fluorine and chlorine content in copper concentrate. Method 1 measurement range. fluorine content (mass fraction) is 0.005%~0.50%, chlorine (mass fraction) is 0.010%~0.50%; method 2 measurement range. chlorine content (mass fraction) is 0.050%~4.50%. chlorine If the content is greater than 0.05%, use method 2 as the arbitration method.

Note: The chlorine measured in Method 1 of this document refers to acid leached chlorine.

2 Normative reference documents

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

GB/T 6682 Specifications and test methods for water used in analytical laboratories

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

3 Terms and definitions

There are no terms or definitions to be defined in this document.

4 Method 1 Ion chromatography

4.1 Principle

The sample is decomposed by sulfuric acid, and the fluorine and chlorine in it escape with water vapor and are separated from the sample. They are absorbed by the absorbing liquid and measured by ion chromatography. to protect The retention time was determined qualitatively, and the fluorine and chlorine content were calculated using the working curve method.

4.2 Reagents

Unless otherwise stated, only reagents confirmed to be of high purity are used in the analysis.

4.2.1 Water, in line with GB/T 6682, first-class water.

4.2.2 Sodium hydroxide.

4.2.3 Sulfuric acid (rho=1.84g/mL).

4.2.4 Sulfuric acid solution (2 1). Measure 200mL of sulfuric acid (4.2.3) and slowly pour it into 100mL of water and mix well.

4.2.5 Sodium hydroxide solution, cNaOH=0.2mol/L. Weigh 8.0g of sodium hydroxide (4.2.2) and dissolve it in 1000mL of water, and mix well.

......
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 3884.12

EditionTitleRevisionStatus
GB/T 3884.12-2023Methods for chemical analysis of copper concentrates—Part 12:Determination of fluoride and chloride contents—Ion chromatography and potentiometric titrationcurrent editionCurrent
GB/T 3884.12-2010Methods for chemical analysis of copper concentrates—Part 12:Determination of fluoride and chloride contents—Ion chromatography and potentiometric titrationprevious editionSuperseded

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