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GB/T 23513.1-2009: Chemical analysis methods for germanium concentrate -- Part 1: Determination of germanium content -- Potassium iodate titration Delivery: 9 seconds. True-PDF full-copy in English & invoice will be downloaded + auto-delivered via email. See step-by-step procedure Status: Valid
Similar standardsGB/T 23513.1-2009: Chemical analysis methods for germanium concentrate -- Part 1: Determination of germanium content -- Potassium iodate titration---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/GBT23513.1-2009 GB/T23513.1-2009 GB ICS 77.120.99 H 66 NATIONAL STANDARD Chemical analysis methods for germanium concentrate - Part 1.Determination of germanium content - Potassium iodate titration Issued on: APRIL 08, 2009 Implemented on: FEBRUARY 01, 2010 Issued by. General Administration of Quality Supervision, Inspection and Quarantine of the People’s Republic of China; Standardization Administration of the People’s Republic of China. Table of ContentsForeword... 3 1 Scope... 4 2 Methods and principles... 4 3 Reagents... 4 4 Analysis steps... 5 5 Determinations... 6 6 Calculation of analysis result... 7 7 Precision... 8 8 Quality assurance and control... 8ForewordGB/T 23513 Chemical analysis methods for germanium concentrate is consisted of five parts as follows. — Part 1.Determination of germanium content - Potassium iodate titration; — Part 2.Determination of arsenic content - Ferrous ammonium sulfate titration; — Part 3.Determination of sulfur content - Barium sulfate gravimetry; — Part 4.Determination of fluoride content - ISE; — Part 5.Determination of silica content – Gravimetry. This part is part 1. This part was proposed by China Nonferrous Metals Industry Association. This part shall be under the jurisdiction of National Technical Committee on Nonferrous Metals of Standardization Administration of China. The responsible drafting organization of this par. Yunnan Lincang Xinyuan Germanium Co., Ltd. The participating drafting organizations of this part. Zhongjin Lingnan Shaoguan Melting Factory, Hunan Huaihua Hongjiang Hengchang Germanium Co., Ltd., Nanjing Germanium Co., Ltd., and Beijing Guojinghui Infrared Optics Technology Co., Ltd. The chief drafting staffs of this Standard. Bao Wendong, Li Hecheng, Pu Shikun, Zheng Hong, Gao Mengchao, Wang Jian, and Sun Yan. Chemical analysis methods for germanium concentrate - Part 1.Determination of germanium content - Potassium iodate titration1 ScopeThis part of GB/T 23513 specifies the determination method of germanium content in germanium concentrate. This part applies to the determination of germanium content in germanium concentrate. Determination range. 1.0%-70%.2 Methods and principlesMelt the sample with sodium hydroxide. Use phosphoric acid and potassium permanganate to suppress the distillation escape of arsenic, antimony, tin and others. In 3 mol/L of phosphoric acid and 4.5 mol/L of hydrochloric acid, use hypophosphite to reduce the tetravalent germanium to divalent germanium; use starch as an indicator, and titrate it with standard potassium iodate solution at below 20 °C.3 ReagentsUnless otherwise stated, only analytical reagents AND distilled water or water with equivalent purity can be used in the analysis. 3.1 Potassium iodide (KI). 3.2 Anhydrous sodium carbonate (Na2CO3). 3.3 Sodium hydroxide (NaOH). 3.4 Hypophosphite (NaH2PO2·H2O). 3.5 Potassium permanganate (KMnO4). 3.6 Ammonium fluoride (NH4F). 3.7 Hydrochloric acid (ρ 1.19 g/mL-1). 3.8 Phosphate (ρ 1.69 g/mL). 3.9 Sulfate (ρ 1.83 g/mL). Weigh samples (4.1) according to Table 1.Place into a 300 mL conical flask. Add 10 ml of water and shake it well. Add 10 ml of phosphoric acid (3.8), 2 g of potassium permanganate (3.5), and 0.2 g of ammonium fluoride (3.6). Heat it at low temperature to decompose. Maintain at purple color. If the purple fades away, supplement it with a little of potassium permanganate (3.5) until it is completely decomposed; and until the white smoke decomposed by fine phosphoric acid occurs. Take down and cool it. Add 120 ml of hydrochloric acid (3.10) in a conical flask. The following operation is the same as 5.1.1.4~5.1.1.6. 5.1.3 Method III It applies to determine germanium in samples such as crude germanium dioxide with lower-impurity. Weigh sample (4.1) according to Table 1.Place into a 300 mL conical flask. Add 10 ml of water and shake it well. Add 1 g of sodium hydroxide (3.3) to heat to completely dissolve. Take down. Add 80 ml of water, 35 mL of phosphoric acid (3.8), and 7 g of hypophosphite (3.4). Shake to dissolve. Then cover the Geiger funnel. The following operation is the same as 5.1.1.6. 5.2 The determination of hydrochloric acid soluble germanium Weigh samples (4.1) according to Table 1.Place into a 300 mL conical flask. Add 0.1 g of potassium permanganate (3.5) and 80 ml of hydrochloric acid (1+1). The following operation is the same as 5.1.1.5 ~ 5.1.1.6.6 Calculation of analysis result6.1 Mass fraction of germanium Calculate the mass fraction of germanium according to Formula (1). Where w (Ge) - The mass fraction of germanium, %; c - The concentration of standard solution (1/6KIO3), the unit is moles per liter (mol/L); V - The amount of standard potassium iodate solution, the unit is milliliters (mL); V0 - The amount of standard potassium iodate solution in blank test, the unit is milliliters (mL); m – Mass analysis sample, the unit is gram (g). control, the root cause reason shall be found out; and re-verify it after correcting the error. ......Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al. 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