Methods for chemical analysis of copper concentrates—Part 12:Determination of fluoride and chloride contents—Ion chromatography and potentiometric titration
Foreword
Codeofchina.com is in charge of this English translation. In case of any doubt about the English translation, the Chinese original shall be considered authoritative.
This document is drafted in accordance with the rules given in GB/T 1.1-2020 Directives for standardization - Part 1: Rules for the structure and drafting of standardizing documents.
This document is Part 12 of GB/T 3884 Methods for chemical analysis of copper concentrates. The following parts of GB/T 3384 have been issued:
——Part 1: Determination of copper content - Iodine titration method;
——Part 2: Determination of gold and silver contents - Flame atomic absorption spectrometric method and fire assay method;
—— Part 3: Determination of sulfur content - Gravimetric method and Combustion-titration method;
——Part 4: Determination of magnesium oxide content - Flame atomic absorption spectrophotometry method;
——Part 5: Determination of fluoride content - Ion selective electrode method;
——Part 6: Determination of lead, zinc, cadmium and nickel content - Flame atomic absorption spectrometry method;
——Part 7: Determination of lead content - Na2EDTA titration method;
——Part 8: Determination of zinc content - Na2EDTA titration method;
——Part 9: Determination of arsenic and bismuth contents - Hydride generation-atomic fluorescence spectrometry method, the potassium bromate titration method and silver diethyl dithiocarbamate photometry method;
——Part 10: Determination of Antimony content - Hydride generation atomic fluorescence spectrometry method;
——Part 11: Determination of mercury content - Cold atomic absorption spectrometric method;
——Part 12: Determination of fluoride and chloride contents - Ion chromatography and potentiometric titration;
——Part 13: Determination of copper - Electrogravimetric method;
——Part 14: Determination of gold and silver - Fire assay gravimetric and flame atomic absorption spectrometric method;
——Part 15: Determination of iron content - Potassium dichromate titration method;
——Part 16: Determination of silicon dioxide content - K2SiF6 titrimetric method and gravimetric method;
——Part 17: Determination of aluminium oxide content - Chromazurol S spectrophotometric method and precipitation separation-fluoride salts device - Na2EDTA titrimetric method;
——Part 18: arsenic, antimony, bismuth, lead, zinc, nickel, cadmium, cobalt, magnesium oxide, calcium oxide contents - Inductively coupled plasma atomic emission spectrometry;
——Part 19: Determination of thallium content - Inductively coupled plasma mass spectrometry;
——Part 20: Determination of mercury content - Solid sampling and direct mercury analysis method;
——Part 21: Determination of copper, sulfur, lead, zinc, iron, aluminium, calcium, magnesium, manganese content - Wavelength dispersive X-ray fluorescence spectrometric method;
This document replaces GB/T 3884.12-2010 Methods for chemical analysis of copper concentrates - Part 12: Determination of fluoride content and chloride content - Ion chromatography. In addition to structural adjustments and editorial changes, the following main technical changes have been made with respect GB/T 3884.12-2010:
a) Method 2 Potentiometric method has been added for chlorine determination, the scope of which is 0.050% to 4.50% (see Clauses 1 and 5 hereof);
b) The requirements for water use in Method 1 has been changed (see 4.2.1 hereof; Clause 3 of Edition 2010);
c) The drying temperature of the baseline sodium fluoride has been changed (see 4.2.7 hereof; 3.6 of Edition 2010);
d) The regulation for the range of syringes has been changed (see 4.3.4 hereof; 4.4 of Edition 2010);
e) The specimen determination volume has been added (see Table 1 hereof);
f) The requirement for rounding off numerical values in the test data processing of Method 1 has been added (see 4.6 hereof);
g) The method for obtaining repeatability and reproducibility has been changed (see 4.7 hereof; Clause 8 of Edition 2010);
h) The content of “Test report” has been added (see Clause 6 hereof);
i) "Quality assurance and control" has been deleted (see Clause 9 of Edition 2010).
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. The issuing body of this document shall not be held responsible for identifying any or all such patent rights.
This document was proposed by China Nonferrous Metals Industry Association.
This document is under the jurisdiction of National Technical Committee on Nonferrous Metals of Standardization Administration of China (SAC/TC 243).
All the editions of this document are as follows:
——It was firstly issued as GB/T 3884.12-2003 in 2010;
——This is the first revision.
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Introduction
Copper concentrate is the main raw material for producing cathode copper. In the standard system of nonferrous metals field, the standard of chemical composition determination method of copper concentrate plays an important role in ensuring the quality of copper concentrate products. This series of method standards serve the production, trade and application of copper concentrate and provide technical support for the high-quality development of China's nonferrous metals industry. The purpose of GB/T 3884 Methods for chemical analysis of copper concentrates is to describe the determination methods of copper, gold, silver, lead, zinc and other chemical elements in copper concentrates. Because copper concentrate contains a certain amount of fluorine and chlorine, the high content of fluorine and chlorine causes the content of hydrogen fluoride and hydrogen chloride in smelting flue gas to increase, and the flue gas with high hydrogen fluoride and hydrogen chloride enters the acid-making process, which is easy to corrode and damage the acid-making equipment and is unfavorable to smelting. The control of fluorine and chlorine content in copper concentrate is a very important technical index in copper refining process. Therefore, it is of great significance to determine the content of fluorine and chlorine in copper concentrate.
GB/T 3884 Methods for chemical analysis of copper concentrates consists of 21 parts:
——Part 1: Determination of copper content - Iodine titration method;
——Part 2: Determination of gold and silver contents - Flame atomic absorption spectrometric method and fire assay method;
—— Part 3: Determination of sulfur content - Gravimetric method and Combustion-titration method;
——Part 4: Determination of magnesium oxide content - Flame atomic absorption spectrophotometry method;
——Part 5: Determination of fluoride content - Ion selective electrode method;
——Part 6: Determination of lead, zinc, cadmium and nickel content - Flame atomic absorption spectrometry method;
——Part 7: Determination of lead content - Na2EDTA titration method;
——Part 8: Determination of zinc content - Na2EDTA titration method;
——Part 9: Determination of arsenic and bismuth contents - Hydride generation-atomic fluorescence spectrometry method, the potassium bromate titration method and silver diethyl dithiocarbamate photometry method;
——Part 10: Determination of Antimony content - Hydride generation atomic fluorescence spectrometry method;
——Part 11: Determination of mercury content - Cold atomic absorption spectrometric method;
——Part 12: Determination of fluoride and chloride contents - Ion chromatography and potentiometric titration;
——Part 13: Determination of copper - Electrogravimetric method;
——Part 14: Determination of gold and silver - Fire assay gravimetric and flame atomic absorption spectrometric method;
——Part 15: Determination of iron content - Potassium dichromate titration method;
——Part 16: Determination of silicon dioxide content - K2SiF6 titrimetric method and gravimetric method;
——Part 17: Determination of aluminium oxide content - Chromazurol S spectrophotometric method and precipitation separation-fluoride salts device-Na2EDTA titrimetric method;
——Part 18: arsenic, antimony, bismuth, lead, zinc, nickel, cadmium, cobalt, magnesium oxide, calcium oxide contents - Inductively coupled plasma atomic emission spectrometry;
——Part 19: Determination of thallium content - Inductively coupled plasma mass spectrometry;
——Part 20: Determination of mercury content - Solid sampling and direct mercury analysis method;
——Part 21: Determination of copper, sulfur, lead, zinc, iron, aluminium, calcium, magnesium, manganese content - Wavelength dispersive X-ray fluorescence spectrometric method.
The development of this document is based on the demand of copper concentrate trade at home and abroad. The establishment of this standard can better adapt to the determination of fluorine and chlorine content in copper concentrates from different producing places at home and abroad, and provide an accurate and scientific basis for the determination of fluorine and chlorine content in copper concentrates. Therefore, the addition of "Determination method 2 for chlorine content" fills the blank in determination of higher chlorine content in copper concentrates. It is convenient to adopt a unified analysis method in trade transactions, which is beneficial to reduce commercial disputes caused by differences in detection methods, and has good economic and social benefits.
Methods for chemical analysis of copper concentrates - Part 12: Determination of fluoride and chloride contents - Ion chromatography and potentiometric titration
WARNING - Persons using this document shall be familiar with normal laboratory practice. This document does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user to establish appropriate safety and health practices and to ensure compliance with any national regulatory conditions.
1 Scope
This document describes methods for the determination of fluorine and chlorine 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. The determination range of Method 1: fluorine content (mass fraction) is 0.005% to 0.50%, chlorine content (mass fraction) is 0.010% to 0.50%; determination range of Method 2: chlorine content (mass fraction) is 0.050% to 4.50%. Method 2 is used as arbitration method for chlorine content greater than 0.05%.
Note: The chlorine determined in Method 1 of this document refers to acid leaching chlorine.
2 Normative references
The following normative documents contain provisions which, through reference in this text, constitute provisions of this standard. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.
GB/T 6682 Water for analytical laboratory use - Specification and test methods
GB/T 8170 Rules of rounding off for numerical values & expression and judgment of limiting values
3 Terms and Definitions
No terms and definitions are listed in this document.
4 Method 1: Ion chromatography
4.1 Principle
The test portion is decomposed by sulfuric acid, and fluorine and chlorine escaped with water vapor and separated from the sample, which is absorbed by absorption solution and determined by ion chromatography. The retention time is used qualitatively, and the fluorine and chlorine contents are calculated by working curve method.
4.2 Reagents
Unless otherwise specified, only reagents confirmed as guarantee reagent shall be used in the analysis.
4.2.1 Water, in accordance with GB/T 6682, Grade I water.
4.2.2 Sodium hydroxide.
4.2.3 Sulfuric acid (ρ=1.84g/mL).
4.2.4 Sulfuric acid solution (2+1): Take 200 mL of sulfuric acid (4.2.3) and slowly pour it into 100 mL of water, mix well.
4.2.5 Sodium hydroxide solution, cNaOH=0.2mol/L: Weigh 8.0 g of sodium hydroxide (4.2.2) and dissolve it in 1000 mL of water, mix well.
4.2.6 Sodium hydroxide solution, cNaOH=0.02 mol/L: Weigh 0.8 g of sodium hydroxide (4.2.2) and dissolve it in 1000 mL of water, mix well, or prepare using an automatic eluent generator of OH-type.
4.2.7 Standard storage solution of fluorine: Weigh 2.2110 g of reference sodium fluoride dried at 120°C for 2 h in advance, dissolve it in water, move it into a 1000 mL volumetric flask, dilute it with water to scale, and mix well. Transfer the solution into dry plastic bottles for storage. 1 mL of this solution contains 1000 μg of fluorine.
4.2.8 Chlorine standard storage solution: Weigh 1.6485 g of reference sodium chloride burned to constant weight at 500°C to 600°C in advance, dissolve it in water, move it into a 1000 mL volumetric flask, dilute it with water to scale, and mix well. This solution contains 100 μg of chloride per 1 mL.
4.2.9 Mixed standard solution of fluorine and chlorine: Take 5.00 ml of fluorine standard storage solution (4.2.7) and chlorine standard storage solution (4.2.8) in 50 mL of volumetric flask respectively, and dilute it to scale with water. One mL of this solution contains 100 μg of fluorine and 100 μg of chlorine respectively.
Foreword i
Introduction iv
1 Scope
2 Normative references
3 Terms and Definitions
4 Method 1: Ion chromatography
5 Methods 2 Potentiometric titration
6 Test report
Annex A (Informative) Steam distillation unit
Annex B (Informative) Original data of precision test in Method 2
