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GB/T 6150.1-2023 PDF English

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GB/T 6150.1-2023: Methods for chemical analysis of tungsten concentrates - Part 1: Determination of tungsten trioxide content - Ammonium tungstate igniting gravimetric method
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GB/T 6150.1: Evolution and historical versions

Standard IDContents [version]USDSTEP2[PDF] deliveryName of Chinese StandardStatus
GB/T 6150.1-2023English200 Add to Cart 0-9 seconds. Auto-delivery Methods for chemical analysis of tungsten concentrates - Part 1: Determination of tungsten trioxide content - Ammonium tungstate igniting gravimetric method Valid
GB/T 6150.1-2008English100 Add to Cart 0-9 seconds. Auto-delivery Methods for chemical analysis of tungsten concentrates - Determination of tungsten trioxide content - The ammonium tungstate igniting gravimetric method Obsolete
GB/T 6150.1-1985English199 Add to Cart 2 days Methods for chemical analysis of tungsten concentrates--The ammonium tungstate igniting gravimetric method for the determination of tungsten trioxide content Obsolete

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GB/T 6150.1-2023: Methods for chemical analysis of tungsten concentrates - Part 1: Determination of tungsten trioxide content - Ammonium tungstate igniting gravimetric method


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GB NATIONAL STANDARD OF THE PEOPLE'S REPUBLIC OF CHINA ICS 77.120.99 CCS H 14 Replacing GB/T 6150.1-2008 Methods for chemical analysis of tungsten concentrates - Part 1.Determination of tungsten trioxide content - Ammonium tungstate igniting gravimetric method Issued on. NOVEMBER 27, 2023 Implemented on. JUNE 1, 2024 Issued by. State Administration for Market Regulation; Standardization Administration of PRC.

Table of Contents

Foreword... 3 Introduction... 6 1 Scope... 9 2 Normative references... 9 3 Terms and definitions... 9 4 Principle... 9 5 Reagents or materials... 10 6 Instruments and equipment... 10 7 Samples... 11 8 Test steps... 11 9 Experimental data processing... 12 10 Precision... 13 11 Test report... 13 Appendix A (Informative) Raw data of the precision test... 15

Foreword

This document was drafted in accordance with the provisions of GB/T 1.1-2020 Directives for standardization - Part 1.Rules for the structure and drafting of standardizing documents. This document is part 1 of GB/T 6150 Methods for chemical analysis of tungsten concentrates. GB/T 6150 has published the following parts. -- Part 1.Determination of tungsten trioxide content - Ammonium tungstate igniting gravimetric method; -- Part 2.Determination of tin content - Potassium iodate titrimetry and inductively coupled plasma atomic emission spectrometry; -- Part 3.Determination of phosphorus content - The phosphorus molybdenum yellow spectrophotometry and inductively coupled plasma atomic emission spectrometry; -- Part 4.Determination of sulfur content - High frequency-infrared absorption method and combustion-iodometric method; -- Determination of calcium content - EDTA volumetric method and flame atomic absorption spectrometric method; -- Part 6.Determination of moisture content - Gravimetric method; -- Determination of tantalum content and niobium content - Inductively coupled plasma emission spectrometry and spectrophotometry; -- Part 8.Determination of molybdenum content - Thiocyanate spectrophotometry method; -- Determination of copper content - Flame atomic absorption spectrometry; -- Part 10.Determination of lead content - Hydride generation atomic fluorescence spectrometry and flame atomic absorption spectrometry; -- Determination of zinc content - Flame atomic absorption spectrometric method; -- Part 12.Determination of silicon dioxide content - Silicomolybdenum blue spectrophotometry and gravimetry; -- Part 13.Determination of arsenic content - Atomic fluorescence spectrometry and the silver diethyldithiocarbamate (DDTC-Ag) spectrophotometry; -- Determination of manganese content - The ammonium ferrous sulfate volumetric method and flame atomic absorption spectrometric method; -- Part 15.Determination of bismuth content - Hydride generation atomic fluorescence spectrometry and flame atomic absorption spectrometry; -- Determination of iron content - The sulfosalicylic acid spectrophotometry; -- Part 17.Determination of antimony content - Atomic fluorescence spectrometry; -- Part 18.Determination of barium content - Inductively coupled plasma atomic emission spectrometry. This document replaces GB/T 6150.1-2008 Methods for chemical analysis of tungsten concentrates - Determination of tungsten trioxide content - The ammonium tungstate igniting gravimetric method. Compared with GB/T 6150.1-2008, in addition to structural adjustments and editorial changes, the main technical changes are as follows. a) The scope of application and measurement range of the method have been changed (see Chapter 1; see Chapter 1 of the 2008 edition); b) The chapter "Terms and definitions" has been added (see Chapter 3); c) The chapter "Instruments and equipment" has been added (see Chapter 6); d) The amount of hydrochloric acid used for sample decomposition and the types of samples that require EDTA addition in the method have been changed (see 8.3.1; see 5.3.1 of the 2008 edition); e) The metered volume for residue colorimetry in the method has been changed [see 8.3.6a); see 5.3.6.1 of the 2008 edition]; f) The chapter "Precision" has been changed (see Chapter 10; see Chapter 7 of the 2008 edition); g) The chapter "Quality assurance and control" has been deleted (see Chapter 8 of the 2008 edition); h) The chapter "Test report" has been added (see Chapter 11). Please note that some of the contents of this document may involve patents. The issuing organization of this document does not assume the responsibility for identifying patents. This document was proposed by China Non-Ferrous Metals Industry Association. This document is under the jurisdiction of the National Technical Committee on Nonferrous Metals of Standardization Administration of China (SAC/TC243). Drafting organizations of this document. Ganzhou Non-ferrous Metallurgy Research Institute Co., Ltd., Hunan Shizhuyuan Non-ferrous Metal Co., Ltd., Nonferrous Metals Technology and Economic Research Institute Co., Ltd., Jiangxi Institute of Tungsten and Rare Earth, Chenzhou Tungsten Products Branch of Hunan Shizhuyuan Nonferrous Metals Co., Ltd., Ganzhou Huaxing Tungsten Products Co., Ltd., China Nonferrous Metals (Guilin) Geology and Mining Co., Ltd., Shenzhen Zhongjin Lingnan Non- ferrous Metal Co., Ltd., Jiangxi Piaotang Tungsten Industry Co., Ltd., Jiangxi College of Applied Technology, Daye Nonferrous Design and Research Institute Co., Ltd., Zijin Mining Group Co., Ltd., and Center for Industrial Analysis and Testing of Guangdong Academy of Sciences. Main drafters of this document. Zhang Wenxing, Xie Lingjun, Liu Hong, Bai Zhihui, Zhang Bilan, Luo Yansheng, Wang Changji, Ouyang Zijing, Xie Lu, Zhang Dongmei, Wen Shiwei, Hu Zhenzhen, He Xiaofeng, Wen Zhimin, Deng Zhihui, Luo Zhaoming, Zhang Wenjuan, Chen Lan, Chen Zhuhai, Huang Puying, Du Cuijuan, Yuan Qi, Yuan Dongmei. This document was first published in 1985, revised for the first time in 2008, and this is the second revision.

1 Scope

This document describes the method for the determination of tungsten trioxide content in tungsten concentrates. This document is applicable to the determination of tungsten trioxide content in tungsten concentrate with a molybdenum content of less than 0.3% and a phosphorus content of less than 0.3%. The determination range of tungsten trioxide (mass fraction). not less than 20%.

2 Normative references

The provisions of the following documents constitute the essential clauses of this document through normative references in this text. Among them, for referenced documents with dates, only the versions corresponding to the dates are applicable to this document; for referenced documents without dates, the latest versions (including all amendments) are applicable to this document. GB/T 8170 Rules of rounding off for numerical values & expression and judgment of limiting values GB/T 17433 Foundation terms for chemical analysis of metallurgical products

3 Terms and definitions

The terms and definitions defined in GB/T 17433 apply to this document.

4 Principle

The sample is dissolved in hydrochloric acid, nitric acid, and perchloric acid in the presence of a small amount of ammonium fluoride, and concentrated until white smoke is emitted to drive off fluoride ions and nitrate ions. Tungsten is precipitated as tungstic acid, filtered to separate it from most of the coexisting elements, and then tungstic acid is dissolved in ammonia water. The filtrate is evaporated and burned, and then desiliconized with hydrofluoric acid and burned again, and the mass of tungsten trioxide is weighed. The mass of tungsten trioxide in the residue is determined by spectrophotometry, and the result is corrected.

5 Reagents or materials

Unless otherwise stated, only confirmed analytical reagents and distilled water are used in the analyses. 5.1 Ammonium fluoride. 5.2 Sodium peroxide. 5.3 Disodium ethylenediaminetetraacetate (Disodium EDTA). 5.4 Hydrochloric acid (ρ=1.19 g/mL). 5.5 Perchloric acid (ρ=1.67 g/mL). 5.6 Nitric acid (ρ=1.42 g/mL). 5.7 Anhydrous ethanol. 5.8 Hydrofluoric acid (ρ=1.15 g/mL). 5.9 Perchloric acid cleaning solution (1+199). 5.10 Ammonia water (1+4). 5.11 Sodium hydroxide solution (48 g/L). 5.12 Potassium thiocyanate solution (350 g/L). 5.13 Titanium trichloride-hydrochloric acid mixed solution. Pipette 0.5 mL titanium trichloride solution (150 g/L), dilute to 100 mL with hydrochloric acid (2+3), and mix well.

6 Instruments and equipment

6.1 Spectrophotometer. 6.2 High temperature furnace.

7 Samples

7.1 The sample particle size shall not be greater than 0.074 mm.

8 Test steps

8.1 Test specimen 8.2 Parallel tests Perform two experiments in parallel and take the average value. 8.3 Determination 8.3.1 Place the test specimen (8.1) in a 250 mL beaker, add 50 mL of hydrochloric acid (5.4) [if it is wolframite concentrate, add 100 mL of hydrochloric acid (5.4)], and place it in a boiling water bath to dissolve for 30 min~40 min; add 0.3 g of ammonium fluoride (5.1), shake, continue to dissolve for 10 min, and remove it; place it on an electric stove to concentrate the volume to 30 mL, add 3 mL of perchloric acid (5.5) and 2 mL of nitric acid (5.6), continue to heat at low temperature until white smoke appears for 1 min, remove it, and cool it slightly; blow water to clean the watch glass and the wall of the cup and dilute it to 30 mL, boil it, remove it, and let it stand for a while. 8.3.2 Filter the mixture into a 200 mL volumetric flask using medium-speed quantitative filter paper. Wash the beaker and filter paper four times each with perchloric acid solution (5.9) and once with water using the pouring method. 8.3.3 Remove the volumetric flask, add 0.5 mL of anhydrous ethanol (5.7), and dilute with water to about 150 mL (after the tungstic acid has dissolved in the platinum dish and washed, pour the solution into the original beaker for leaching the residue). 8.3.4 Place a platinum dish of constant weight under the funnel, purge the beaker and filter paper with hot ammonia water (5.10) to dissolve the tungstic acid, transfer the residue in the beaker into the funnel, and clean the beaker with a cleaning stick. 8.3.5 Place the platinum dish on a boiling water bath and evaporate to dryness, then transfer it to an electric furnace to heat and drive out all the ammonium salts; transfer it to a high-temperature furnace at 780 °C~800 °C and burn it for 10 min, remove it, and cool it. Add 5 mL of hydrofluoric acid (5.8), place it on a boiling water bath and evaporate to dryness, then transfer it to a high-temperature furnace at 780 °C~800 °C and burn it for 10 min, remove it, cool it to room temperature in a desiccator, and weigh it. Repeat the burning until the weight is constant. 8.3.6 The steps for determining the tungsten trioxide content in the residue are as follows. a) Transfer the residue obtained in 8.3.4 together with the filter paper into a 30 mL iron crucible, place it on an electric furnace to dry, ash it, and cooling; then add about 6 g of sodium peroxide (5.2), melt it in a high-temperature furnace at 700 °C~750 °C until the contents are cherry red and transparent, take it out, cool it slightly, and place it in the filtrate obtained in 8.3.3 [if it is scheelite concentrate or mixed tungsten concentrate, add 1 g of disodium EDTA (5.3)]. After leaching is complete, wash out the crucible with water, cool it, transfer it to a 200 mL volumetric flask, dilute it to the mark with water, mix it, and let it stand to clarify. Transfer 2.00 mL~10.00 mL of the supernatant [if less than 10 mL, use sodium hydroxide solution (5.11) to make up] into a 50 mL colorimetric tube. b) Add 2 mL of potassium thiocyanate solution (5.12) and dilute to the mark with titanium trichloride-hydrochloric acid mixture (5.13), mix well, and let stand for 10 min.

9 Experimental data processing

The tungsten trioxide content is expressed as the mass fraction w of tungsten trioxide and is calculated according to formula (1).

10 Precision

10.1 Repeatability The measured values of two independent test results are obtained under repeatability conditions; within the range of the average values given in Table 1, the absolute difference between the two test results is not greater than the repeatability limit (r), and the probability of exceeding the repeatability limit (r) does not exceed 5%. The repeatability limit (r) is obtained by a linear interpolation or extrapolation method according to the data in Table 1.The statistical results of precision data are shown in

11 Test report

The test report shall at least include the following contents.

Appendix A

(Informative) Raw data of the precision test The precision data in this appendix were determined by 12 laboratories conducting joint tests on 8 samples with different levels of tungsten trioxide content in 2022.Each laboratory independently measured the tungsten trioxide content at each level 11 times under repeatability conditions. The statistical results are shown in Table A.1. ......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.


      

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