Abstract：Zinc material containing chromium carbide contained chromium carbides. These carbides had high melting point and good chemical stability, and cannot be completely dissolved with common acids. They were only decomposed by strong acid mixture at high temperature. The sample was dissolved by microwave digestion in nitric acid-hydrochloric acid-hydrofluoric acid. This method could not only fully dissolve the insoluble chromium carbides in sample, but also effectively avoid the loss of volatile arsenic under high temperature conditions. Then the contents of lead, copper, iron, cadmium, chromium and arsenic were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). The determination ranges of elements were listed as follows: 0.10%≤w (Pb,Cu)≤5.00%; 0.10%≤w(Fe)≤10.00%; 0.010%≤w(Cd,Cr)≤3.00%; 0.08%≤w(As)≤3.00%. The correlation coefficients of calibration curves of elements in linear range were all higher than 0.999. The detection limit was 0.001-0.018μg/mL. The experimental method was applied for the determination of lead, copper, iron, cadmium, chromium and arsenic in five zinc materials containing chromium carbide. The relative standard deviations (RSD, n=11) of determination results were in range of 0.75%-2.0%. The contents of lead, copper, iron, cadmium, chromium and arsenic in three zinc materials containing chromium carbide were determined according to the experimental method. The found results were consistent with those obtained by other methods (the contents of lead, copper, iron and cadmium were determined by flame atomic absorption spectrometry after alkali dissolution according to GB 6730.30-2016 Methods for chemical analysis of iron ores-The diphenyl carbazide photometric method for the determination of chromium content; the content of chromium was determined according to GB 6730.30-2016 Methods for chemical analysis of iron ores-The diphenyl carbazide photometric method for the determination of chromium content; the content of arsenic was determined according to GB/T 8151.7-2012 Methods for chemical analysis of zinc concentrate-Part 7: Determination of arsenic-Hydride generation-atomic fluorescence spectrometry).
江荆,魏雅娟,邬景荣,等.丁二酮肟沉淀分离-EDTA滴定法测定含镍锌物料中锌[J].冶金分析,2016,36(11):62-66.JIANG Jing,WEI Ya-juan,WU Jing-rong,et al.Determination of zinc in materials containing nickel and zinc by diketone oxime precipitation-edta titration[J].Metallurgical Analysis,2016,36(11):62-66.
[2]
江荆,魏雅娟,伍斯静,等.强碱性阴离子交换纤维吸附-电感耦合等离子体原子发射光谱法测定含锌物料中镉[J].冶金分析,2016,36(12):38-43.JIANG Jing,WEI Ya-juan,WU Si-jing,et al.Determination of cadmium in zinc materials by adsorption-inductively coupled plasma atomic emission spectrometry with strong alkaline anion exchange fiber[J].Metallurgical Analysis,2016,36(12):38-43.
[3]
赵晶晶.电感耦合等离子体发射光谱法测定锌精矿、锌矿石、铅锌混合矿中的锌、铜、砷、铅、镉含量[J].现代仪器与医疗,2013,19(6):55-58.ZHAO Jing-jing.Determination of zinc,copper,arsenic,lead and cadmium in zinc concentrate,zinc ore and lead-zinc mixture by inductively coupled plasma emission spectrometry[J].Modern Instruments and Medicine,2013,19(6):55-58.
[4]
魏雅娟,吴雪英,江荆,等.微波消解-电感耦合等离子体原子发射光谱法测定银精矿中铅锌铜砷锑铋镉[J].冶金分析,2018,38(5):47-53.WEI Ya-juan,WU Xue-ying,JIANG Jing,et al.Determination of Pb,Zn,Cu, Sb, Bi,Cd in silver concentrate by microwave digestion coupled with inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2018,38(5):47-53.
[5]
王云杰,王皓莹.硫氰酸钾-自动电位滴定法测定锌精矿中的银含量[J].中国资源综合利用,2018,36(6):21-23,26.WANG Yun-jie,WANG Hao-ying.Determination of silver content in zinc concentrate by potassium thiocyanate-automatic potentiometric titration[J].China Resources Comprehensive Utilization,2008,36(6):21-23,26.
[6]
李悦.原子吸收光谱法测定锌矿石中的锌硅酸盐[J].化工管理,2017(8):145.LI Yue.Determination of zinc silicate in zinc ores by atomic absorption spectrometry[J].Chemical Industry Management,2017(8):145.
[7]
闵国华,张庆建,刘稚,等.电感耦合等离子体原子发射光谱法测定铅矿、锌矿和铅锌矿中杂质元素[J].冶金分析,2014,34(5):51-55.MIN Guo-hua,ZHANG Qing-jian,LIU Zhi,et al.Determination of impurity elements in lead ore,zinc ore and lead zinc ore by ICP-AES[J].Metallurgical Analysis,2014,34(5):51-55.
[8]
罗继锋,王莹,祁雨凡,等.电感耦合等离子体发射光谱法快速测定铜铅锌矿石中的硫[J].世界有色金属,2016(10):160-161,163.LUO Ji-feng,WANG Ying,QI Yu-fan,et al.Rapid determination of sulfur in copper,lead and zinc ores by inductively coupled plasma emission spectrometry[J].World Nonferrous Metals,2016(10):160-161,163.
[9]
张小军,师世龙.ICP-MS法测定铅精矿、锌精矿、混合铅锌矿中的铊[J].化学分析计量,2017,26(2):82-85.ZHANG Xiao-jun,SHI Shi-long.Determination of thallium in lead concentrate,zinc concentrate and mixed lead-zinc ore by ICP-MS method[J].Chemical Analysis and Measurement,2017,26(2):82-85.
[10]
邱丽,唐碧玉,古行乾,等.电感耦合等离子体质谱法测定铅锌矿尾矿渣中铜、铅、锌和镉[J].理化检验:化学分册,2015,51(7):943-946.QIU Li,TANG Bi-yu,GU Xing-qian,et al.Determination of copper, lead,zinc and cadmium in lead-zinc mine tailings by inductively coupled plasma mass spectrometry[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2015,51(7):943-946.
[11]
杨挺.X-荧光光谱法分析锌精矿中的硅铁铜铅[J].世界有色金属,2018(17):148-149.YANG Ting. Analysis of Si,Fe,Cu,Pb in zinc concentrate by X-ray fluorescence spectrometry[J].World Nonferrous Metals,2018(17):148-149.
[12]
王松君,常平,王璞珺,等.电感耦合等离子体发射光谱法直接测定黄铜矿中多元素[J].岩矿测试,2004,23(3),228-230.WANG Song-jun,CHANG Ping,WANG Pu-jun,et al.Direct determination of multiple elements in chalcopyrite by inductively coupled plasma emission spectrometry[J].Rock and Mineral Analysis,2004,23(3),228-230.
[13]
闫月娥.微波消解-电感耦合等离子体原子发射光谱法测定钒钛铁精矿中10种主次元素的含量[J].理化检验:化学分册,2018,54(9):1044-1048.YAN Yue-e.Determination of the content of 10 primary and secondary elements in vanadium titanium iron concentrate by microwave digestion coupled with inductively coupled plasma atomic emission spectrometry[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2008,54(9):1044-1048.
[14]
倪文山,张萍,姚明星,等.微波消解-电感耦合等离子体原子发射光谱法测定矿石样品中铌钽[J].冶金分析,2010,30(8):50-53.NI Wen-shan,ZHANG Ping,YAO Ming-xing,et al.Determination of niobium and tantalum in ore samples by microwave digestion and inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2010,30(8):50-53.
[15]
胡述戈.微波消解-电感耦合等离子体原子发射光谱法测定铁矿石中8种成分[J].冶金分析,2006(6):40-43.HU Shu-ge.Determination of eight components in iron ore by microwave digestion coupled with inductively coupled plasma atomic emission spectrometry[J]. Metallurgical Analysis,2006(6):40-43.
[16]
孟时贤,邓飞跃,杨远,等.电感耦合等离子体发射光谱法测定铅锌矿中15个主次量元素[J].岩矿测试,2015,34(1):48-54.MENG Shi-xian,DENG Fei-yue,YANG Yuan,et al.Determination of fifteen primary and secondary elements in lead-zinc ore by inductively coupled plasma emission spectrometry [J].Rock and Mineral Analysis,2015,34(1):48-54.
