YS/T 953.4-2014Methods for chemical analysis of fire smelting nickel substrate material. Part 4: Determination of chrome content. Ammonium ferrous sulfate titration method (English PDF)

Foreword

YS/T 953 "pyro-metallurgical materials for chemical analysis of nickel substrate" is divided into 11 parts.

--- Part 1. Determination of the amount of nickel dimethylglyoxime spectrophotometry and dimethylglyoxime gravimetric method;

--- Part 2. Determination of the amount of silicon molybdenum blue spectrophotometric method and perchloric acid dehydration gravimetric method;

--- Part 3. Determination of phosphorus content of bismuth phosphorus molybdenum blue spectrophotometric method;

--- Part 4. Determination of chromium content ammonium ferrous sulfate titration;

--- Part 5. Determination of manganese content - Potassium periodate spectrophotometric method;

--- Part 6. Determination of cobalt content of 5-Cl-PADAB spectrophotometry and flame atomic absorption spectrometry;

--- Part 7. Determination of copper content bicyclic cyclohexanone oxalyl Spectrophotometric Method and flame atomic absorption spectrometry;

--- Part 8. Determination of iron content dichromate method;

--- Part 9. Carbon and sulfur content was measured high-frequency combustion infrared absorption method;

--- Part 10. nickel, chromium, manganese, cobalt, copper, phosphorus content - Inductively coupled plasma atomic emission spectrometry;

--- Part 11. lead, arsenic, cadmium, mercury content - Inductively Coupled Plasma Mass Spectrometry.

This section YS/T Part 4 953.

This section drafted in accordance with GB/T 1.1-2009 given rules.

The non-ferrous metal part by the National Standardization Technical Committee (SAC/TC243) centralized.

This section is responsible for drafting unit. Zhongbao Binhai Nickel Industry Co., Ltd.

This section is drafted. Northwest Nonferrous Metal Research Institute, Zhongbao Binhai Nickel Industry Co., Ltd.

Participated in the drafting of this section. Shanxi Taigang Stainless Steel Co., Ltd., Tianjin, People's Republic of China Exit Inspection and Quarantine, river Nanna Shi Technology Co., Ltd., Guangxi Science and Technology Silver billion mining and metallurgy companies.

1 Scope

YS/T of the provisions of section 953 determination pyrometallurgical nickel substrate amount of chromium compound ammonium ferrous sulfate titration.

This section applies to the determination of pyrometallurgical nickel substrate compound chromium content. Determination of the range of 0.10% to 10.00%.

2 Normative references

The following documents for the application of this document is essential. For dated references, only the dated version suitable for use herein Member. For undated references, the latest edition (including any amendments) applies to this document.

GB/T 20066 Steel and iron - Sampling and determination of the chemical composition of the sample with a sample preparation method

3 Method summary

Sample by a certain proportion of hydrochloric acid, nitric acid and hydrofluoric acid dissolution. Sulfuric acid - phosphoric acid medium with silver nitrate as a catalyst, ammonium persulfate Chromium (III) oxidized to Cr (VI), while manganese was oxidized to permanganate, sodium chloride in the boiling reducing permanganate to eliminate the interference. Then N- benzene-generation anthranilic acid as indicator, titrated with ferrous ammonium sulfate standard titration solution turns from purple to bright green as the end point.

4 Reagents

Unless otherwise indicated in the analysis using only recognized as analytical grade reagents and distilled or deionized water or equivalent purity.

4.1 Hydrofluoric acid (rho = 1.15g/mL).

4.2 hydrochloric acid (rho = 1.19g/mL).

4.3 nitric acid (rho = 1.42g/mL).

4.4 sulfate (rho = 1.84g/mL).

4.5 phosphoric acid (rho = 1.69g/mL).

4.6 sulfuric acid - phosphoric acid mixed. in 300mL of water, stirring slowly added 200mL of sulfuric acid (4.4) and 100mL phosphoric acid (4.5), Mix well.

4.7 silver nitrate solution (10g/L), stored in brown bottles.

4.8 ammonium persulfate solution (200g/L), with the preparation.

4.9 manganese sulfate solution (40g/L).

4.10 sodium chloride solution (50g/L).

4.11 Chromium standard stock solution (1mg/mL). Weigh 2.8289g pre-bake at 150 °C after 1h, placed in a desiccator to cool to room temperature Potassium dichromate (baseline), placed in a beaker, dissolved in water and transferred to 1000mL volumetric flask, dilute with water to volume, and mix.

4.12 chromium standard solution (0.25mg/mL). Pipette 25.00mL chromium standard stock solution (4.11) into 100mL volumetric flask with water Dilute to volume, and mix.