Abstract:According to the principle of metallurgical refining of rhodium, a method for the determination of rhodium in rhodium nitrate products by hydrogen reduction gravimetry was established. The conditions for the determination of rhodium were investigated and optimized. The effect of impurities on the determination results of rhodium was also tested. It was found that, in the medium of 0.3-0.9 mol/L HNO3, rhodium nitrate and ammonium chloride formed a red (NH4)3RhCl6 crystal complex in which rhodium could be determined by gravimetry after a series of treatment: firstly, it was dried at 100 ℃; then, ammonium salt in it was decomposed at 350 ℃; lastly, the obtained matter was reduced into rhodium sponge by hydrogen at 750 ℃ and dried at 105 ℃. The method was employed to determine rhodium of 6.55%, 7.36%, 8.05%, 9.99% and 20.05%, in rhodium nitrate with the range (R) of ±0.01 %, the standard deviation (SD) of 0.004 1% and the relative standard deviation(RSD,n=22) of 0.02%-0.06%. The accuracy and precision of this method were higher than YS/T 594-2006 standard method.
刘文, 李勇, 朱武勋, 贺小塘, 韩守礼, 谭文进, 林波, 罗仙, 朱利亚. 氢还原重量法测定硝酸铑产品中铑含量[J]. 冶金分析, 2014, 34(8): 11-15.
LIU Wen, LI Yong, ZHU Wu-xun, HE Xiao-tang, HAN Shou-li, TAN Wen-jin, LIN Bo, LUO Xian, ZHU Li-ya. Determination of rhodium in rhodium nitrate products by hydrogen reduction gravimetry. , 2014, 34(8): 11-15.