YS/T 1050.2-2015
(Lead-antimony concentrates - Part 2. Determination of antimony content cerium sulfate titration)
ICS 73.060
D42
People's Republic of China Nonferrous Metals Industry Standard
Methods for chemical analysis of lead-antimony concentrate
Part 2. Determination of antimony content
Cerium sulfate titration
Part 2. Determinationofantimonycontent-
Issued on. 2015-04-30
2015-10-01 implementation
Ministry of Industry and Information Technology of the People's Republic of China released
Foreword
YS/T 1050-2015 "Methods for chemical analysis of lead-antimony concentrate" is divided into the following nine sections.
--- Part 1. Determination of lead content Na2EDTA titration;
--- Part 2. Determination of antimony content cerium sulfate titration;
--- Part 3. Determination of arsenic content potassium bromate titration;
--- Part 4. Determination of zinc contents Na2EDTA titration;
--- Part 5. Determination of sulfur content - Gravimetric method;
--- Part 6. Determination of iron content cerium sulfate titration;
--- Part 7. Determination of the amount of bismuth and copper - Flame atomic absorption spectrometry amount;
--- Part 8. gold and silver content determination fire assay;
--- Part 9. Determination of the amount of silver by flame atomic absorption spectrometry.
This is Part 2.
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. Guangxi Metallurgical Product Quality Supervision and Inspection Station.
Participated in the drafting of this section. Tin Mine Twinkling Star Antimony Industry Co., Ltd., Liuzhou one hundred tough special Advanced Materials Co., Ltd., Guangxi Zhuang
Analysis and Testing Center Autonomous Region, Guizhou Province Analysis and Testing Institute.
The main drafters of this section. Lvmin Li, Huang Xusheng, Wuxiang Wu, Cuide Hai, Huangzhao Min, Xie Tao, Song should ball, Lung Chi Xiang Rui Cheng Shuai Deng Hankin,
Ren Liming, Du cold spell.
Methods for chemical analysis of lead-antimony concentrate
Part 2. Determination of antimony content
Cerium sulfate titration
1 Scope
This section YS/T 1050 specifies the method for determination of lead-antimony concentrates antimony content.
This section applies to the determination of antimony content lead-antimony concentrate in the measurement range (mass fraction) was 10.00% ~ 30.00%.
2 Method summary
Sample with sulfuric acid, potassium sulfate decomposition filter paper (after carbonization) as a reducing agent to pentavalent antimony reduced to trivalent. In hydrochloric acid medium, add phosphoric acid
High iron mask, methyl orange, methylene blue as indicator, at 80 ℃ ~ 90 ℃ titration with cerium sulfate standard solution to the red
Faded, mutation was bright green (yellow-green high iron) as the end point.
3 Reagents
Unless otherwise indicated, this part of the reagents were analytical reagent, the water for the two water.
3.1 potassium sulfate.
3.2 filter.
3.3 metal antimony (Sb mass fraction ≥99.99%).
3.4 sulfate (ρ = 1.84g/mL).
3.5 nitric acid (ρ = 1.42g/mL).
3.6 phosphoric acid (ρ = 1.70g/mL).
3.7 ethanol.
3.8 hydrochloride (11).
3.9 sulfate (11).
3.10 cerium sulfate standard titration solution.
3.10.1 formulated
Weigh 12.12g cerium sulfate [Ce (SO4) 2 · 4H2O], placed in 1000mL beaker, add 30mL sulfuric acid (3.4), are stirred
Uniform, gradually warming up in the furnace heating dissolved into a paste, and oleum take about 20min, remove cooling, 280mL sulfuric acid (3.9), and then slowly
Was added 400mL of water, stirring to dissolve the clear, cool to room temperature and transferred to 1000mL volumetric flask, dilute with water to volume, and mix.
3.10.2 Calibration
Weigh 0.0650g metal antimony (3.3), placed in 300mL conical flask, 5 ~ 10 glass beads, sulfuric acid was added 15mL
(3.4), heated to dissolve clear, and heating was continued to take oleum 5min ~ 10min, remove the cooled walls with a little water bottle blowing, slowly along the wall of the bottle