氨水沉淀分离EDTA络合滴定法测定镧镍合金废渣中的镍
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摘要
实验了镧镍合金废渣中镍的分析方法及测定镍的最佳条件。试样用盐酸、硝酸溶解,加高氯酸冒烟使其完全溶解后,在氯化铵存在下经氨水沉淀分离镧,在p H9.0~10.0氯化铵-氨水缓冲溶液中,以紫脲酸铵为指示剂,用EDTA标准溶液滴定镍。考察了试样的溶解、氨水沉淀分离镧的实验、p H值、紫脲酸铵用量、共存物质对实验的影响。方法的回收率为98.0%~102.0%,相对标准偏差小于5%(n=8)。结果表明,该方法步骤简单,操作简便,经济实用,准确度高,结果可靠,能满足镧镍合金废渣中镍含量的分析需要。
The analytical method of nickel in waste lanthanum-nickel alloy and the optimum condition for determining nickel were obtained by experiments. The samples were dissolved by hydrochloric acid and nitric acid,then spiked with perchloric acid and heated to nearly dry. In the ammonia chloride medium,La( Ⅲ) is precipitated by adding ammonia,while nickel can react with ammonia to form complexes of Ni( NH3)2+6 and remain in the titrate. In p H9. 0 ~ 10. 0 NH4 Cl-NH3·H2 O buffer solution,nickel was titrated with EDTA standard solution using murexide as indicator. The effects of sample decomposition,separation of lanthanum by ammonia precipitant,p H,murexide concentration and coexisting substances on the dertermination of nickel were studied. The labeled recovery is 98. 0% ~ 102. 0% and the relative deviation is under 5%( n = 8).Owing to simple steps,reproducibility,controllable reaction,low-cost reagents and satisfactory results,the method has been applied to the determination of nickel in waste lanthanum-nickel alloy.
The analytical method of nickel in waste lanthanum-nickel alloy and the optimum condition for determining nickel were obtained by experiments. The samples were dissolved by hydrochloric acid and nitric acid,then spiked with perchloric acid and heated to nearly dry. In the ammonia chloride medium,La( Ⅲ) is precipitated by adding ammonia,while nickel can react with ammonia to form complexes of Ni( NH3)2+6 and remain in the titrate. In p H9. 0 ~ 10. 0 NH4 Cl-NH3·H2 O buffer solution,nickel was titrated with EDTA standard solution using murexide as indicator. The effects of sample decomposition,separation of lanthanum by ammonia precipitant,p H,murexide concentration and coexisting substances on the dertermination of nickel were studied. The labeled recovery is 98. 0% ~ 102. 0% and the relative deviation is under 5%( n = 8).Owing to simple steps,reproducibility,controllable reaction,low-cost reagents and satisfactory results,the method has been applied to the determination of nickel in waste lanthanum-nickel alloy.
引文
[1]冶金工业信息标准研究院标准化研究所,中国标准出版社第二编辑室.GB/T223.25-94钢铁及铁合金化学分析方法标准汇编(下)[M].北京:中国标准出版社,2002.109-113.China metallurgical information and standardization institute,Standards Press of China(the second editorial room).Chemical Analysis Methods Standard Compilation for iron,Steel and Alloy(GB/T223.25-94)[M].Beijing:Standards Press of China,2002.109-113.
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[14]苏梦晓,陆安军.电感耦合等离子体原子发射光谱法、X射线荧光光谱法和摄谱法测定地球化学样品中铜、铅、锌、镍的比较[J].冶金分析,2015,35(5):48-53.Su M X,Lu A J.Comparison of inductively coupled plasma atomic emission spectrometry,X-ray fluorescence spectrometry and spectrographic method for the determination of copper,lead,zinc and nickel in geochemical samples[J].Metallurgical Analysis,2015,35(5):48-53.
[15]邵从和.电感耦合等离子体原子发射光谱法测定铜电积液中锑、铋、钴、镍和砷的含量[J].理化检验:化学分册,2016,52(6):691-694.Shao C H.ICP-AES Determination of stibium,bismuth,cobalt,nickel and arsenic in copper electrowinning solution[J].PTCA(Part B:Chem Anal),2016,52(6):691-694.
[16]张瑞霖,樊鑫,曹吉祥,等.电感耦合等离子体原子发射光谱法测定精炼镍中10种杂质元素[J].冶金分析,2017,37(1):66-70.Zhang R L,Fan X,Cao J X,et al.Determination of ten impurity elements in refined nickel by inductively coupled plasma atomic emission spectrometer[J].Metallurgical Analysis,2017,37(1):66-70.
[17]李占波.ICP-MS测定土壤样品中的铜、镍、铬、铅镉[J].工业技术,2015,(5):26-27.Li Z B.Simultaneous determiation of copper,nickel,chromium,lead and cadmium in soil samples by Inductively coupled plasma-mass spectrometry[J].China Science and Technology Rev,2015,(5):26-27.
[18]许涛,王东杰,郝茜,等.钐钴合金中稀土总量的测定[J].稀土,2014,35(3):72-76Xu T,Wang D J,Hao Q,et al.Determination of total rare earth contents in Sm Co alloy[J].Chinese Rare Earths,2014,35(3):72-76
[19]王东杰,许涛,王素梅,等.钐钴合金中钴的测定方法研究[J].稀土,2015,36(1):89-92.Wang D J,Xu T,Wang S M,et al.Study on determination of Co in Sm Co alloy[J].Chinese Rare Earths,2015,36(1):89-92.
[20]刘惠婉,袁竹青,乔桂芳,等.重量法测定氧化镍中的镍含量[J].河南化工,2013,30(1):59-60.Liu H W,Yuan Z Q,Qiao G F,et al.Determination of nickel content in nickel oxide by gravimetric method[J].Henan Chemical Industry,2013,30(1):59-60.
[2]阮代锬,覃光举,周骏宏.EDTA直接滴定法测量镍磷铁中镍的测定条件研究[J].硫磷设计与粉体工程,2013,(6):42-45.Ruan D Y,Qin G J,Zhou J H.Study on determination of the amount of nickel in nickel-phosphorus-iron alloy by using EDTA direct titration method[J].S P&BMH Related Engineering,2013,(6):42-45.
[3]中国标准出版社第二编辑室.有色金属工业标准汇编-重金属及其合金化学分析方法[M].北京:中国标准出版社,2001.704-707.Standards Press of China(the second editorial room).Nonferrous Metals Industry Standard Compilation-chemical Analysis Methods of Heavy Metals and Their Alloys[M].Beijing:Standards Press of China,2001.704-707.
[4]张智宏,王玉峰,张少瑜.氧化镍中三价镍含量的测定.冶金分析,2009,29(10):47-51.Zhang Z H,Wang Y F,Zhang S Y.Determination of nickelic content in nickel oxide[J].Metallurgical Analysis,2009,29(10):47-51.
[5]常照荣,李云平,李苞,等.氢氧化镍中3价镍含量的测定[J].电源技术,2004,28(6):376-378.Chang Z R,Li Y P,Li B,et al.Determination of nickelic content in Ni(OH)2[J].Chinese Journal of Power Sources,2004,28(6):376-378.
[6]菅豫梅,王培.EDTA滴定法测定铬基焊粉中的镍含量[J].湖南有色金属,2006,22(3):58-60.Jian Y M,Wang P.Determination of nickel in chromium base weld powder by EDTA titration[J].Hunan Nonferrous Metals,2006,22(3):58-60.
[7]唐华应.氯化钡沉淀分离EDTA滴定法测定钒钼镍催化剂中镍[J].冶金分析,2004,24(1):48-49.Tang H Y.Determination of nickel in V-Mo-Ni catalyst by EDTA titrimetry after separation with barium chloride[J].Metallurgical Analysis,2004,24(1):48-49.
[8]中华人民共和国国家标准委员会.GB/T 223.23-2008,钢铁及合金镍含量的测定-丁二酮肟分光光度法[S].北京:中国标准出版社,2008.The national standard committee of the People's Republic of China.Iron steel and alloy-Determination of nickel content-The dimethylglyoxime spectrophotometric method(GB/T 223.23-2008)[S].Beijing:Standards Press of China,2008.
[9]程建聪.碱锰电池用KOH中镍含量的测定[J].电池,2000,30(6):273-273.Cheng J C.The determination of the nickel content in potassium hydroxide[J].Battery Bimonthly,2000,30(6):273-273.
[10]张皓.不锈钢中镍的快速测定[J].有色矿冶,2009,25(3):52-53.Zhang G.Rapid determination of nickel in stainless steel[J].Non-ferrous Mining and Metallurgy,2009,25(3):52-53.
[11]王茹.废催化剂中金属镍含量的测定[J].辽宁化工,2004,33(8):492-493.Wang R.Determination of nickel in waste catalyst[J].Liaoning Chemical Indust Iy,2004,33(8):492-493.
[12]钟晕波,邢天海.高含量镍的原子吸收分光光度法测定[J].化工科技,1996,(3):54-57.Zhong Y B,Xing T H.Determination of the high content nickel by atomic absorption spectrophotometry[J].Science&Technology in Chemical Industry,1996,(3):54-57.
[13]刘志新.高含量铷化探样品中镍的XRF法测定[J].光谱实验室,2002,19(1):8-10.Liu Z X.Determination of nickel in high rubidium content samples by X-ray fluorescence spectrometry[J].Chinese Journal of Spectroscopy Laboratory,2002,19(1):8-10.
[14]苏梦晓,陆安军.电感耦合等离子体原子发射光谱法、X射线荧光光谱法和摄谱法测定地球化学样品中铜、铅、锌、镍的比较[J].冶金分析,2015,35(5):48-53.Su M X,Lu A J.Comparison of inductively coupled plasma atomic emission spectrometry,X-ray fluorescence spectrometry and spectrographic method for the determination of copper,lead,zinc and nickel in geochemical samples[J].Metallurgical Analysis,2015,35(5):48-53.
[15]邵从和.电感耦合等离子体原子发射光谱法测定铜电积液中锑、铋、钴、镍和砷的含量[J].理化检验:化学分册,2016,52(6):691-694.Shao C H.ICP-AES Determination of stibium,bismuth,cobalt,nickel and arsenic in copper electrowinning solution[J].PTCA(Part B:Chem Anal),2016,52(6):691-694.
[16]张瑞霖,樊鑫,曹吉祥,等.电感耦合等离子体原子发射光谱法测定精炼镍中10种杂质元素[J].冶金分析,2017,37(1):66-70.Zhang R L,Fan X,Cao J X,et al.Determination of ten impurity elements in refined nickel by inductively coupled plasma atomic emission spectrometer[J].Metallurgical Analysis,2017,37(1):66-70.
[17]李占波.ICP-MS测定土壤样品中的铜、镍、铬、铅镉[J].工业技术,2015,(5):26-27.Li Z B.Simultaneous determiation of copper,nickel,chromium,lead and cadmium in soil samples by Inductively coupled plasma-mass spectrometry[J].China Science and Technology Rev,2015,(5):26-27.
[18]许涛,王东杰,郝茜,等.钐钴合金中稀土总量的测定[J].稀土,2014,35(3):72-76Xu T,Wang D J,Hao Q,et al.Determination of total rare earth contents in Sm Co alloy[J].Chinese Rare Earths,2014,35(3):72-76
[19]王东杰,许涛,王素梅,等.钐钴合金中钴的测定方法研究[J].稀土,2015,36(1):89-92.Wang D J,Xu T,Wang S M,et al.Study on determination of Co in Sm Co alloy[J].Chinese Rare Earths,2015,36(1):89-92.
[20]刘惠婉,袁竹青,乔桂芳,等.重量法测定氧化镍中的镍含量[J].河南化工,2013,30(1):59-60.Liu H W,Yuan Z Q,Qiao G F,et al.Determination of nickel content in nickel oxide by gravimetric method[J].Henan Chemical Industry,2013,30(1):59-60.