GB/T 8152.15-2021Methods for chemical analysis of lead concentrates—Part 15:Determination of soluble lead content—Flame atomic absorption 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" Drafting.

This document is part 15 of GB/T 8152 "Methods for Chemical Analysis of Lead Concentrates".

GB/T 8152 has released the following parts.

---Determination of lead content by acid dissolution-EDTA titration (GB/T 8152.1);

---Determination of lead content, lead sulfate precipitation-EDTA back titration method (GB/T 8152.2);

---Determination of aluminum oxide content Chromazurol S spectrophotometric method (GB/T 8152.3);

---Determination of zinc content EDTA titration method (GB/T 8152.4);

---Quantity determination by atomic fluorescence spectrometry (GB/T 8152.5);

--- Polarographic determination of bismuth content (GB/T 8152.6);

---Determination of copper content by flame atomic absorption spectrometry (GB/T 8152.7);

---Dithiodiantipyrine methane spectrophotometric method for the determination of bismuth content (GB/T 8152.8);

---Determination of Magnesium Oxide by Flame Atomic Absorption Spectrometry (GB/T 8152.9);

---Determination of silver and gold content, lead precipitation or ash-blowing fire assay and flame atomic absorption spectrometry (GB/T 8152.10);

---Determination of mercury content by atomic fluorescence spectrometry (GB/T 8152.11);

---Determination of cadmium content by flame atomic absorption spectrometry (GB/T 8152.12);

---Part 13: Determination of thallium content inductively coupled plasma mass spectrometry and inductively coupled plasma-atomic emission spectrometry (GB/T 8152.13);

---Part 14: Determination of silicon dioxide content molybdenum blue spectrophotometric method (GB/T 8152.14);

--- Part 15: Determination of soluble lead content by flame atomic absorption spectrometry (GB/T 8152.15).

Introduction

Lead is an important raw material for storage batteries, cable sheaths, lead pipe lead plates, and radiation protection. In my country's non-ferrous metal consumption, it is second only to copper, aluminum, Zinc. GB/T 8152 "Methods for Chemical Analysis of Lead Concentrates" specifies the chemical analysis methods for the content of various elements in lead concentrates, which are designed to meet the requirements of lead concentrates. Domestic and foreign trade.

GB/T 8152 consists of 15 parts.

---Determination of lead content by acid dissolution-EDTA titration (GB/T 8152.1);

---Determination of lead content, lead sulfate precipitation-EDTA back titration method (GB/T 8152.2);

---Determination of aluminum oxide content Chromazurol S spectrophotometric method (GB/T 8152.3);

---Determination of zinc content EDTA titration method (GB/T 8152.4);

---Determination of Arsenic Atomic Fluorescence Spectrometry (GB/T 8152.5);

--- Polarographic determination of bismuth content (GB/T 8152.6);

---Determination of copper content by flame atomic absorption spectrometry (GB/T 8152.7);

---Dithiodiantipyrine methane spectrophotometric method for the determination of bismuth content (GB/T 8152.8);

---Determination of Magnesium Oxide by Flame Atomic Absorption Spectrometry (GB/T 8152.9);

---Determination of silver and gold content, lead precipitation or ash-blowing fire assay and flame atomic absorption spectrometry (GB/T 8152.10);

---Determination of mercury content by atomic fluorescence spectrometry (GB/T 8152.11);

---Determination of cadmium content by flame atomic absorption spectrometry (GB/T 8152.12);

---Part 13: Determination of thallium content inductively coupled plasma mass spectrometry and inductively coupled plasma-atomic emission spectrometry (GB/T 8152.13);

---Part 14: Determination of silicon dioxide content molybdenum blue spectrophotometric method (GB/T 8152.14);

--- Part 15: Determination of soluble lead content by flame atomic absorption spectrometry (GB/T 8152.15).

Lead concentrates mainly exist in the state of lead sulfide, and at the same time, there may be soluble lead (lead sulfate lead oxide lead carbonate), and a small amount of difficult Dissolved lead (sulfurite, tungsten, arsenic) and other forms exist. The lead concentrate produced by flotation has a low content of soluble lead, which is generally not More than 1%. In the current lead concentrate trade, there is lead-containing waste, such as lead slag, waste batteries, lead mud, imported lead-containing waste, etc., mixed into lead concentrate In the middle, shoddy good for profit. The cost of these lead-containing wastes is very low, much lower than the price of lead sulfide concentrates. Moreover, the soluble lead (sulfuric acid) in the lead concentrate The content of lead oxide, lead carbonate, and lead carbonate directly affects the temperature, desulfurization rate, and agglomeration of the sinter during the smelting process. So accurately analyze The soluble lead in lead concentrate (lead sulfate, lead oxide, lead carbonate) is of great guiding significance for the refinery production.

GB/T 8152.15 focuses on supplementing the determination of soluble lead content in lead concentrates to meet the needs of production and trade.

1 Scope

This document specifies the method for determining the soluble lead content in lead concentrates.

This document is applicable to the determination of soluble lead content in lead concentrates. Measuring range. 0.3%~10.5%.

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 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

The following terms and definitions apply to this document.

4 Method summary

The sample uses acetic acid-ammonium acetate as a solvent to selectively leaching soluble lead, and a small amount of stannous dichloride dihydrate is added to eliminate the interference of Fe3, and it is mixed with sulfur. Lead and insoluble lead salts (thioantimonite, tungsten-lead ore, arsenic ore) are effectively separated. In dilute nitric acid medium, use air-acetylene flame, The absorbance of lead was measured at the wavelength of 283.3nm in the atomic absorption spectrometer, and the content of soluble lead was calculated according to the standard working curve method.

5 Reagents

Unless otherwise specified, only use reagents confirmed to be analytically pure and secondary water that meets the requirements of GB/T 6682 in the analysis.

5.1 Stannous dichloride dihydrate.

5.2 Nitric acid (1+2).

5.3 Acetic acid-ammonium acetate solution. Weigh 150g of ammonium acetate solid and dissolve it in an appropriate amount of water, add 30mL of acetic acid, and dilute to 1000mL with water. Mix well.

5.4 Lead standard storage solution. Weigh 1.0000g metallic lead (wPb>=99.99%) into a 300mL beaker, add 40mL nitric acid (5.2), cover with a watch glass, heat at low temperature to dissolve completely, boil to drive off nitrogen oxides, remove and cool, transfer to a 1000mL volumetric flask, use […]