纯净真空铬铁（Pure vacuum ferrochrome）.doc

纯净真空铬铁（Pure vacuum ferrochrome） Q/SJFC. J08-017.5-2008 Malachite - benzene extraction spectrophotometric determination of antimony 1 scope This standard provides for the calculation of the method, reagent material, instrument and equipment, analysis procedure, and analysis results of the method of determination of antimony content of malachite green - benzene extraction spectrophotometry. This standard is applicable to the determination of antimony content in pure vacuum micro-carbon ferrochrome alloy, and the range (quality score) : 0.00020% - 0.0020%. 2 method feeds Sample by sulfuric acid decomposition, in hydrochloric acid medium, the possible existence of antimony with stannous chloride (Ⅳ), reduction of antimony (Ⅲ), then the antimony (Ⅲ) with sodium nitrite and antimony oxide (Ⅴ), antimony (Ⅴ) complex anion ([SbCl6]) and malachite green generate blue-green complex available benzene extraction, to perform photometric measurement points photometer wavelength of 630 nm. Three reagents 3.1 hydrochloric acid (2 + 1) 3.2 hydrochloric acid (3 + 1) 3.3 sulfuric acid (1 + 5) 3.4 sulfuric acid (1 + 8) 3.5 phosphoric acid (1 + 24) 3.6 dichloride solution (100g/L), called 10g dichloride, dissolved in 100mL hydrochloric acid (3.2), blended. 3.7 sodium nitrite solution (200g/L) 3.8 urea solution: take 50g urea, dissolve in 50mL hot water, mix well and cool to room temperature. 3.9 malachite green solution (5g/L), said to take 0.5 g of peacock green, dissolved in 100mL ethanol (3 + 1), mix well. 3.10 benzene Antimony standard solution 3.11.1 to take 0.1000g of pure antimony, dissolved in 50mL of sulfuric acid (rho 1.84 g/mL), and 50mL of sulfuric acid (rho 1.84 g/mL), cooling. In the volumetric flask with 600mL water, the water is diluted to the scale, and the solution 1mL contains 0.1 mg of antimony. 3.11.2 remove 10.00 mL antimony standard solution (3.11.1) in 500mL volumetric flask, dilute with sulphuric acid (3.4) to the scale and mix well. This solution is 1 ml contain