低温乙醇分离-电感耦合等离子体原子发射光谱法测定粗铅中金  

Determination of Gold in Crude Lead by ICP-AES after Separation with Low Temperature Ethanol

作　　者：齐白羽[1] 王丁[1] 王卓 卢昌祥 刘静静 QI Baiyu;WANG Ding;WANG Zhuo;LU Changxiang;LIU Jingjing(Northwest Research Institute of Mining and Metallurgy,Baiyin 730900,China)

机构地区：[1]西北矿冶研究院,白银730900

出　　处：《理化检验（化学分册）》2021年第11期977-980,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：建立了低温乙醇分离-电感耦合等离子体原子发射光谱法(ICP-AES)测定粗铅中金含量的方法。取2.0~10.0 g粗铅样品,先用33%(体积分数)硝酸溶液溶解,再用盐酸溶解完全。加入液溴(氯金酸保护剂)1~3 mL,微沸赶酸至体积约为20 mL后,再加入液溴2 mL和水50 mL,进行重复赶酸,以降低体系酸度。在上述体系中加入60 mL乙醇,0℃放置2 h后过滤。弃去沉淀,在滤液中加入1~3 mL液溴,加热除去乙醇至体积约为10 mL,用5%(体积分数)盐酸溶液定容至10~50 mL,供ICP-AES分析。结果显示:金的质量浓度在0.5~8.0 mg·L^(-1)内与其对应的光谱强度呈线性关系,检出限(3.143s)为0.026 g·t^(-1);对纯铅样品进行加标回收试验,回收率大于96.0%;方法用于实际样品分析,并与YS/T 248.6-2007进行比对,所得测定值基本一致,标准偏差(0.085 g·t^(-1))低于依据YS/T 248.6-2007中内插法计算所得的重复性限(0.5 g·t^(-1))。A method for determination of gold in crude lead by ICP-AES after separation with low temperature ethanol was established.Crude lead sample(2.0-10.0 g)was taken and dissolved with 33%(volume fraction)nitric acid solution,and then completely dissolved with hydrochloric acid.1-3 mL of liquid bromine(chloroauric acid protector)was added,and the acid in the solution was driven out by boiling slightly,and the volume of the solution was concentrated to about 20 mL.Liquid bromine(2 mL)and water(50 mL)were added to drive out the acid repeatedly,thus to reduce the acidity of the system.Ethanol(60 mL)was added to the above system,and the solution was placed at 0℃for 2 h and filtered.The precipitation was discarded,liquid bromine(1-3 mL)was added into the filtrate,and the solution was heated to remove ethanol until the volume reached about 10 mL and then diluted to 10-50 mL with 5%(volume fraction)hydrochloric acid solution for ICP-AES analysis.The results showed that linear relationship between mass concentration of gold and its respective spectral intensity was kept in the range of 0.5-8.0 mg·L^(-1),with detection limit(3.143s)of 0.026 g·t^(-1).The spiked recovery test was made on pure lead,giving values of recovery more than 96.0%.The prescribed method was applied to the analysis of actual sample and compared with YS/T 248.6-2007,the determined value was basically consistent,and the standard deviation(0.085 g·g-1)was lower than the repeatability limit(0.5 g·t-1)calculated by the interpolation method in YS/T 248.6-2007.

关 键 词：乙醇 低温分离 电感耦合等离子体原子发射光谱法 金 粗铅 

分 类 号：O657.31[理学—分析化学]