本文選題：高壓密閉消解 + 電感耦合等離子體質(zhì)譜法�。� 參考：《冶金分析》2017年09期

【摘要】：采用電感耦合等離子體質(zhì)譜法(ICP-MS)測定地球化學(xué)樣品中痕量Rh時,待測溶液的基體及分子離子干擾嚴(yán)重影響ICP-MS測定~(103)Rh的準(zhǔn)確性。實(shí)驗(yàn)以10ng/mL的~(175)Lu消除基體干擾,以數(shù)學(xué)校正方程消除多原子離子~(87)Sr~(16)O~+、~(63)Cu~(40)Ar~+、~(86)SrOH、~(206)Pb~(2+)對~(103)Rh的干擾,最終實(shí)現(xiàn)了電感耦合等離子體質(zhì)譜法測定地球化學(xué)樣品中痕量Rh。分別詳細(xì)考察了Cu、Sr、Pb對Rh測定的干擾情況,不僅有效消除了~(87)Sr~(16)O~+、~(63)Cu~(40)Ar~+、~(86)SrOH多原子離子對~(103)Rh的測定干擾,而且發(fā)現(xiàn)了雙電荷離子~(206)Pb~(2+)對~(103)Rh的測定存在嚴(yán)重的質(zhì)譜干擾。同時通過向不同濃度Rh的標(biāo)準(zhǔn)溶液中分別加入不同量的干擾元素Cu、Sr及Pb進(jìn)行試驗(yàn),得到了對~(103)Rh元素進(jìn)行校正的數(shù)學(xué)校正方程。實(shí)驗(yàn)表明,Rh在0.050~100.0ng/mL范圍內(nèi)與其對應(yīng)的信號強(qiáng)度呈良好的線性關(guān)系,線性相關(guān)系數(shù)為0.999 9,方法檢出限(3σ)為0.014ng/g。采用實(shí)驗(yàn)方法對鉑族元素地球化學(xué)一級標(biāo)準(zhǔn)物質(zhì)中Rh進(jìn)行分析,結(jié)果與認(rèn)定值的相對誤差(RE)為-7.27%~6.15%,相對標(biāo)準(zhǔn)偏差(RSD,n=12)均不大于8.6%。將實(shí)驗(yàn)方法應(yīng)用于云南、四川、新疆等地區(qū)不同含量貴金屬地球化學(xué)樣品中Rh的測定,所得結(jié)果與錫試金方法符合性較好。
[Abstract]:In the determination of trace Rh in geochemical samples by inductively coupled plasma-mass spectrometry (ICP-MS), the accuracy of ICP-MS determination of Rh is seriously affected by the matrix and molecular ion interference of the solution to be determined.In this experiment, the matrix interference was eliminated by using 10ng/mL 175H Lu, and the interference of polyatomic ion Srm7O16O ~ ~ ~ () ~ ~ ~In this paper, the interference of Cu ~ (2 +) Sr ~ (2 +) Pb to the determination of Rh is investigated in detail. It not only effectively eliminates the interference caused by the polyatomic ion of Cu ~ (87) O ~ (16) O ~ (6) C ~ (6) C ~ (60) C ~ (60) O ~ (?) ~ (?) ~ (86) S ~ (OH) on the determination of Rh, but also finds that there is a serious mass spectrometry interference in the determination of Rh by the double charge ion (206Pbbbn2), which is not only effective in the determination of Rh, but also in the determination of Rh.At the same time, by adding different amounts of interference elements Cu-Sr and Pb into the standard solution of different concentrations of Rh, the mathematical correction equation for the correction of Rh is obtained.The experimental results show that Rh has a good linear relationship with the corresponding signal intensity in the range of 0.050~100.0ng/mL, with a linear correlation coefficient of 0.999 and a detection limit of 3 蟽) of 0.014 ng / g.The Rh in the primary reference material of platinum group element geochemistry is analyzed by experimental method. The relative error between the result and the determined value is -7.276.15, and the relative standard deviation (RSDN) is not greater than 8.6%.The experimental method has been applied to the determination of Rh in precious metal geochemical samples with different contents in Yunnan, Sichuan and Xinjiang.
【作者單位】： 河南省巖石礦物測試中心國土資源部貴金屬分析技術(shù)重點(diǎn)實(shí)驗(yàn)室;河南省地質(zhì)礦產(chǎn)勘查開發(fā)局第一地質(zhì)勘查院;
【基金】：河南省“兩權(quán)價款”地質(zhì)科研項(xiàng)目(豫國土資發(fā)[2016]56號-4)
【分類號】：O657.63;P632
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本文編號：1761304