GB/T 23513.2-2009Chemical analysis methods for germanium concentrate - Part 2: Determination of arsenic content - Ferrous ammonium sulfate titration (English PDF)
锗精矿化学分析方法 第2部分：砷量的测定 硫酸亚铁铵滴定法
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Issued by
SAMR; SAC
Level / Type
National · Recommended
Issue date
April 8, 2009
Implementation date
February 1, 2010
Scope
GB/T 23513.2-2009 is the English-translated version of 锗精矿化学分析方法 第2部分：砷量的测定 硫酸亚铁铵滴定法.
GB/T 23513.2-2009 is the second part of GB/T 23513, Chemical analysis methods for germanium concentrate, and it gives a ferrous ammonium sulfate titration method for the arsenic content of germanium concentrate.
Clause 1 states that this part specifies the determination of the arsenic content of germanium concentrate, that it applies to that determination, and that the measurement range is 0.2% to 20%; no other limitation is given on the page.
Clause 2, principle of the method, states that the sample is decomposed with nitric acid, ammonium fluoride and bromine and then with sulfuric acid and nitric acid, that in a hydrochloric acid medium with copper sulfate as catalyst hypophosphite reduces the arsenic to elemental arsenic which is filtered off, that the arsenic is then dissolved and oxidised to the pentavalent form with a standard potassium dichromate solution, and that a ferrous ammonium sulfate standard solution titrates the excess dichromate, so the arsenic is determined indirectly.
Clause 3, Reagents, specifies hypophosphite, sulfuric, nitric, hydrochloric and phosphoric acids, 3% bromine water, a 5% copper sulfate solution, a 10% ammonium fluoride solution, a 10 g/L diphenylamine sulfonate indicator, a sulfur-phosphorus mixed acid prepared from 700 mL of water with 150 mL of sulfuric acid and 150 mL of phosphoric acid, a potassium dichromate standard solution and a ferrous ammonium sulfate standard solution with its own preparation and calibration sub-clauses.
The foreword states that GB/T 23513 is divided into five parts, the other four being the determination of germanium content by potassium iodate titration, of sulfur content by the barium sulfate gravimetric method, of fluorine by the ion selective electrode method and of silicon dioxide content by a gravimetric method.
The foreword also names Yunnan Lincang Xinyuan Germanium Industry Co., Ltd. as the unit responsible for drafting this part. The draft on the page breaks off inside the calibration sub-clause of clause 3, so the apparatus, procedure and result clauses are not shown. It was issued on 8 April 2009 and has applied since 1 February 2010.
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Document preview — GB/T 23513.2-2009
National Standard of the People's Republic of China
- ICS
- 77.120.99
- Classification
- H 66
Issued by: State Administration for Market Regulation; Standardization Administration of the PRC
Contents
- Foreword
- 1 Scope
- 2 Principle of the method
- 3 Reagents
Foreword
GB/T 23513 "Chemical analysis methods for germanium concentrate" is divided into five parts.
--- Part 1. Determination of germanium content of potassium iodate titration;
--- Part 2. Determination of arsenic content ammonium ferrous sulfate titration;
--- Part 3. Determination of sulfur content of barium sulfate gravimetric method;
--- Part 4. Determination of the amount of fluorine ion selective electrode method;
--- Part 5. silicon dioxide content - Gravimetric method.
This is Part 2.
1 Scope
GB/T 23513 provisions of this part of the determination of germanium concentrate arsenic content.
This section applies to the determination of germanium concentrate arsenic content. Measurement range. 0.2% to 20%.
2 Principle of the method
Sample with nitric acid, ammonium fluoride, bromine decomposition with sulfuric acid and nitric acid decomposition and after the expulsion, in hydrochloric acid medium with copper sulfate as catalyst, Hypophosphite reduced to elemental arsenic arsenic filtration. With standard potassium dichromate solution, dissolved and oxidized to pentavalent arsenic; ferrous ammonium sulfate standard Standard solution titrate the excess potassium dichromate solution, indirect determination of arsenic.
3 Reagents
Unless otherwise stated, only confirmed in the analysis of analytical grade reagents and distilled water or equivalent purity.
3.1 Hypophosphite (NaH2PO2 . H2O).
3.2 Sulfate (rho1.83g/mL).
3.3 Nitrate (rho1.42g/mL).
3.4 Hydrochloride (rho1.19g/mL).
3.5 Phosphoric acid (rho1.68g/mL).
3.6 Sulfate (1 + 1).
3.7 HCl (1 + 1).
3.8 Bromine water (3%).
3.9 Ammonium chloride solution (50g/mL).
3.10 Copper sulfate solution (5%).
3.11 HCl (1 + 3 + 0.5% NaPO2 . H2O).
3.12 Ammonium fluoride solution (10%).
3.13 sulfur - phosphorus mixed acid. in 1000mL beaker, 700mL of water was added first, then slowly added to 150mL of sulfuric acid (3.2) and 150mL Phosphoric acid (3.5) and mix.
3.14 Diphenylamine sulfonate indicator (10g/L).
3.15 potassium dichromate standard solution. Weigh pre-drying to constant weight basis of potassium dichromate 1.6361g at 150 °C in 500mL beaker, Add 100mL of water, stirring to dissolve completely moved into 1000mL volumetric flask with water to volume, and mix. Ba (1/6K2Cr2O3) of 0.03337mol/L.
3.16 ferrous ammonium sulfate standard solution
3.16.1 Formulated
Weigh previously dried in the dryer of 6.2294g ammonium ferrous sulfate in 1000mL beaker, add 500mL of water was added slowly 100mL sulfuric acid (3.2), stirring to dissolve completely cooled and transferred to 1000mL volumetric flask with water to volume, and mix.
3.16.2 Calibration
Pipette 25mL to 300mL Erlenmeyer flask, ferrous ammonium sulfate standard solution (3.16.1) (Vp 3), then add 20mL sulfur - phosphorus
......
This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 15 pages — is available in the English PDF.
Referenced standards
Normative references
GB/T 23513
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Related Standards
GB/T 23513.1-2009 — Chemical analysis methods for germanium concentrate - Part 1: Determination of germanium content - Potassium iodate titration
GB/T 23513.3-2009 — Chemical analysis methods for germanium concentrate - Part 3: Determination of sulfur content - Barium sulfate gravimetry
GB/T 23513.4-2009 — Chemical analysis methods for germanium concentrate - Part 4: Determination of fluoride content - ISE
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