冶金分析
冶金分析
야금분석
METALLURGICAL ANALYSIS
2015年
6期
31-34
,共4页
电感耦合等离子体质谱法(ICP-MS)%标准加入法%高纯镍板%砷%锡%锑%铅%铋
電感耦閤等離子體質譜法(ICP-MS)%標準加入法%高純鎳闆%砷%錫%銻%鉛%鉍
전감우합등리자체질보법(ICP-MS)%표준가입법%고순얼판%신%석%제%연%필
inductively coupled plasma mass spectrometry( ICP-MS)%standard addition method%high-purity nick-el plate%arsenic%tin%antimony%lead%bismuth
采用10 mL硝酸(1+1)低温加热至沸溶解0.1000 g试样,在优化仪器参数的基础上,通过选择合适的同位素以避免质谱干扰和采用标准加入法绘制校准曲线以消除基体效应,建立了电感耦合等离子体质谱法( ICP-MS)测定高纯镍板中砷、锡、锑、铅、铋的方法。各元素校准曲线的相关系数为0.9992~0.9999,方法检出限为0.009~0.047μg/g。方法应用于高纯镍板实际样品分析,测得结果的相对标准偏差( RSD, n=9)为2.4%~5.4%,加标回收率为95%~106%。方法测定高纯镍板实际样品的结果与原子吸收光谱法( AAS)相吻合。
採用10 mL硝痠(1+1)低溫加熱至沸溶解0.1000 g試樣,在優化儀器參數的基礎上,通過選擇閤適的同位素以避免質譜榦擾和採用標準加入法繪製校準麯線以消除基體效應,建立瞭電感耦閤等離子體質譜法( ICP-MS)測定高純鎳闆中砷、錫、銻、鉛、鉍的方法。各元素校準麯線的相關繫數為0.9992~0.9999,方法檢齣限為0.009~0.047μg/g。方法應用于高純鎳闆實際樣品分析,測得結果的相對標準偏差( RSD, n=9)為2.4%~5.4%,加標迴收率為95%~106%。方法測定高純鎳闆實際樣品的結果與原子吸收光譜法( AAS)相吻閤。
채용10 mL초산(1+1)저온가열지비용해0.1000 g시양,재우화의기삼수적기출상,통과선택합괄적동위소이피면질보간우화채용표준가입법회제교준곡선이소제기체효응,건립료전감우합등리자체질보법( ICP-MS)측정고순얼판중신、석、제、연、필적방법。각원소교준곡선적상관계수위0.9992~0.9999,방법검출한위0.009~0.047μg/g。방법응용우고순얼판실제양품분석,측득결과적상대표준편차( RSD, n=9)위2.4%~5.4%,가표회수솔위95%~106%。방법측정고순얼판실제양품적결과여원자흡수광보법( AAS)상문합。
0. 100 0 g of sample was dissolved with 10 mL of nitric acid (1+1) by heating from low temperature to boiling. Based on the optimization of instrumental parameters, the mass spectrometry interference was avoided by selecting proper isotope, and the calibration curve was plotted by standard addition method to eliminate the matrix effect. Consequently, a determination method of arsenic, tin, antimony, lead and bismuth in high-purity nickel plate was established by inductively coupled plasma mass spectrometry ( ICP-MS ) . The correlation coefficient of calibration curve for each element was between 0. 999 2 and 0. 999 9 . The detection limit of method was 0. 009-0. 047 μg/g. The proposed method was applied to the analysis of high purity nickel plate actual sample. The rela-tive standard deviation (RSD, n=9) was 2. 4%-5. 4%, and the recoveries were between 95% and 106%. The determination results of high purity nickel plate actual sample were consistent with those obtained by atomic absorp-tion spectrometry ( AAS) .