【摘要】：建立電感耦合等離子體串聯(lián)質(zhì)譜(ICP-MS/MS)法在多元素分析中的應(yīng)用。高純硅微粉經(jīng)氫氟酸+硝酸微波消解后直接采用ICP-MS/MS測定其中8個(gè)常見雜質(zhì)元素(Na、Mg、Al、K、Ti、Fe、Cu、Zn)。在MS/MS模式下,通過向碰撞反應(yīng)池(CRC)中通入NH_3/He,利用目標(biāo)離子與NH_3/He發(fā)生反應(yīng)消除多原子離子質(zhì)譜干擾,其中Na、Mg、Al、K、Zn采用NH_3/He原位質(zhì)量測定,Ti、Fe、Cu采用NH_3/He質(zhì)量轉(zhuǎn)移測定,考察了NH_3/He反應(yīng)氣流速待測元素分析結(jié)果的影響,優(yōu)化并獲得了最佳NH_3/He反應(yīng)氣流速。選擇Sc為內(nèi)標(biāo)元素校正樣品傳輸、霧化效率以及信號強(qiáng)度變化時(shí)所產(chǎn)生的誤差。8個(gè)待測元素的檢出限為0.001~0.76μg/L,采用所建立的方法分析國家標(biāo)準(zhǔn)物質(zhì)石英巖(GBW07835),測定結(jié)果與標(biāo)準(zhǔn)物質(zhì)所提供的驗(yàn)證值基本一致,相對標(biāo)準(zhǔn)偏差(RSD)≤5.5%,表明方法具有準(zhǔn)確性好和精密度高的特點(diǎn),可用于高純硅微粉中多個(gè)雜質(zhì)元素的準(zhǔn)確分析。
[Abstract]:The application of inductively coupled plasma tandem mass spectrometry (ICP-MS/MS) in multielement analysis was established. Eight common impurity elements (Na,Mg,Al,K,Ti,Fe,Cu,Zn) were directly determined by ICP-MS/MS after microwave digestion of high purity silicon powder by hydrofluoric acid nitric acid. In the MS/MS mode, the polyatomic ion mass spectrometry interference is eliminated by the incorporation of NH_3/He, into the (CRC) of the collision reaction cell by the reaction of the target ions with the NH_3/He, in which the Na,Mg,Al,K,Zn is determined by NH_3/He in situ mass measurement and the Na,Mg,Al,K,Zn is determined by NH_3/He mass transfer. The influence of the element analysis results of the NH_3/He reaction flow rate to be measured was investigated, and the optimum NH_3/He reaction gas flow rate was obtained. Select Sc as the internal standard element to correct the sample transmission, The detection limit of the eight elements to be tested is 0.001 ~ 0.76 渭 g / L, and the established method is used to analyze the national standard quartzite (GBW07835). The results are in good agreement with the verification values provided by the standard materials. The relative standard deviation (RSD) 鈮，

本文編號：2235191