Determination of chlorine in sponge titanium by silver nitrate turbidmetry with ultrasonic accelerated dissolution
LIU Lin, GONG Hou-liang, ZHONG Li, WANG Yong
Product Quality Supervision and Testing Institute of Panzhihua,National Center for Quality Supervision and Inspection of Vanadium and Titanium Products,Panzhihua 617000,China
Abstract：The titanium sponge sample was dissolved with hydrofluoric acid by ultrasonic. The low-valence titanium was oxidized by adding nitric acid. The excessive fluorine ions were complexed with boric acid. The stability of silver chloride colloid was improved through ultrasonic with glycerol as dispersant. The solution was diluted with nitric acid (1+19) and determined at 420 nm. Thus, a determination method of chlorine in titanium sponge by silver nitrate turbidimetry was established. The results indicated that about 1 g of sample could be digested completely with 20 mL of hydrofluoric acid(1+5) by ultrasonic at 80 kHz for 5 min. 30 mL of nitric acid (1+19), 2.5 mL of glycerol and 3.0 mL of silver nitrate solution were added into certain volume of sample solution. After dilution to the mark with nitric acid (1+19), the solution was shaken up by ultrasonic for 40 s, kept in darkness for 10 min and followed by determination. The results indicated that the mass concentration of chlorine ions in range of 0.05-2.4 μg/mL showed linear relationship with its corresponding absorbance. The linear correlation coefficient was 0.999 7. The detection limit of chlorine was 0.05 μg/mL. The content of chlorine in two titanium sponge samples was determined according to the experimental method. The results were basically consistent with those obtained by national standard method GB/T 4698.25-1996. The relative standard deviation (RSD, n=11) was less than 5%. The recoveries were between 96% and 103%.
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LIU Lin, GONG Hou-liang, ZHONG Li, WANG Yong. Determination of chlorine in sponge titanium by silver nitrate turbidmetry with ultrasonic accelerated dissolution. , 2017, 37(3): 78-82.
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