LA-ICPMS技術(shù)優(yōu)化及應(yīng)用
發(fā)布時(shí)間：2018-07-29 20:28
【摘要】：激光剝蝕-電感耦合等離子體質(zhì)譜是由激光剝蝕系統(tǒng)和電感耦合等離子體質(zhì)譜儀聯(lián)用的新型儀器(英文縮寫為L(zhǎng)A-ICPMS),該分析技術(shù)具有原位、實(shí)時(shí)、快速的分析優(yōu)勢(shì)和靈敏度高、空間分辨率較好等優(yōu)點(diǎn)。盡管LA-ICPMS固體微區(qū)原位分析應(yīng)用廣泛,但對(duì)地質(zhì)樣品中元素含量的準(zhǔn)確分析仍舊受到多種因素的制約,諸如儀器條件、分餾效應(yīng)隨樣品基體組成的變化、基體匹配標(biāo)準(zhǔn)物質(zhì)的不足、定量化計(jì)算策略和有效的靈敏度漂移校正等。在開(kāi)展LA-ICPMS鋯石U-Pb測(cè)年正常運(yùn)行了數(shù)年的基礎(chǔ)上,本文通過(guò)對(duì)LA-ICPMS分析技術(shù)優(yōu)化改進(jìn),包括將儀器自帶的常規(guī)剝蝕池更換為旋轉(zhuǎn)式雙通道剝蝕池、增加信號(hào)勻化器、在等離子體中心氣流(Ar+He)中加入少量氮?dú)?氣體流量為2.5 ml/min)等措施,實(shí)現(xiàn)了提高儀器靈敏度、降低檢出限和改善分析精密度。利用優(yōu)化后的LA-ICPMS分析技術(shù),開(kāi)展了激光束斑為24μm和16μm的鋯石U-Pb測(cè)年。以NIST SRM 610為標(biāo)樣校正元素含量,以鋯石91500為國(guó)際標(biāo)準(zhǔn)校正年齡值,以Zr91為內(nèi)標(biāo)元素,獲得了激光束斑為24μm條件下三個(gè)鋯石標(biāo)準(zhǔn)Plesovice、Mud Tank和Qinghu 206Pb/238U年齡加權(quán)平均值分別為337.0±3.1 Ma、732.0±6.8 Ma、158.2±1.6 Ma,激光束斑為16μm三個(gè)鋯石標(biāo)準(zhǔn)Plesovice、Mud Tank和Qinghu 206Pb/238U年齡加權(quán)平均值分別為339.6±4.1 Ma、732.9±8.1 Ma、159.8±1.8 Ma,上述結(jié)果與推薦值吻合較好。說(shuō)明本實(shí)驗(yàn)室開(kāi)展的小激光束斑鋯石U-Pb測(cè)年方法是可行的,該鋯石U-Pb測(cè)年方法適用于顆粒較小和成因復(fù)雜的鋯石,對(duì)于獲得更精細(xì)的年齡有著重要意義。本實(shí)驗(yàn)室還開(kāi)展了硅酸鹽主微量元素的測(cè)試工作。利用優(yōu)化后的LA-ICPMS分析技術(shù),在激光束斑為44μm、頻率為5 Hz的條件下,對(duì)BCR-2G、BIR-1G、ATHO-G、GOR132-G、T1-G和St Hs6/80-G這六個(gè)國(guó)際標(biāo)準(zhǔn)物質(zhì)的熔融玻璃進(jìn)行了LA-ICPMS的10種主量元素和47種微量元素分析,對(duì)同一套數(shù)據(jù)分別以NIST SRM 610、GSE-1G和MPI-DING國(guó)際標(biāo)準(zhǔn)物質(zhì)做外標(biāo),采用Ca為歸一化元素,分別采用無(wú)內(nèi)標(biāo)法和以Ca為內(nèi)標(biāo)法的校正策略,對(duì)每一個(gè)樣品所獲得的6組結(jié)果進(jìn)行對(duì)比,結(jié)果表明本實(shí)驗(yàn)室建立的硅酸鹽單礦物L(fēng)A-ICPMS主微量元素測(cè)試方法是可行的,并且對(duì)比了不同校正策略所獲的結(jié)果之間的差別,并初步探討了其可能的原因。此外,還嘗試了碳酸鹽的主微量元素的測(cè)試工作。以NIST SRM 610、GSE-1G和MPI-DING國(guó)際標(biāo)準(zhǔn)物質(zhì)做外標(biāo),采用44μm、60μm的激光束斑,5 Hz的激光頻率,以無(wú)內(nèi)標(biāo)法和以Ca為內(nèi)標(biāo)的校正策略,對(duì)碳酸鹽國(guó)際標(biāo)準(zhǔn)物質(zhì)MACS-3進(jìn)行了主量和微量元素的分析測(cè)試。分析結(jié)果表明,大部分元素測(cè)試值與推薦值的相對(duì)誤差(RE)在20%以內(nèi),相對(duì)標(biāo)準(zhǔn)偏差(RSD)基本都在10%以內(nèi),同時(shí)我們用無(wú)內(nèi)標(biāo)法能夠準(zhǔn)確地測(cè)定出碳酸鹽的主微量元素,說(shuō)明本實(shí)驗(yàn)室嘗試建立的碳酸鹽主微量元素LA-ICPMS微區(qū)原位測(cè)試方法設(shè)計(jì)可行性。
[Abstract]:Laser denudation-inductively coupled plasma mass spectrometry (ICP-MS) is a new type of instrument (abbreviated LA-ICPMS), which is used by laser denudation system and inductively coupled plasma mass spectrometer (LA-ICPMS). It has the advantages of in-situ, real-time, rapid analysis and high sensitivity. Good spatial resolution and other advantages. Although LA-ICPMS solid microanalysis is widely used in situ analysis, the accurate analysis of element content in geological samples is still restricted by many factors, such as instrumental conditions, fractionation effect and changes of sample matrix composition. The deficiency of matrix matching standard material, quantitative calculation strategy and effective sensitivity drift correction etc. Based on the normal operation of LA-ICPMS zircon U-Pb dating for several years, this paper optimizes and improves the LA-ICPMS analysis technology, including replacing the conventional denudation tank with the instrument into a rotary two-channel denudation pool, and increasing the signal leveller. A small amount of nitrogen (gas flow rate 2.5 ml/min) was added to the plasma central gas flow (Ar He) to improve the instrument sensitivity, reduce the detection limit and improve the analytical precision. Zircon U-Pb dating with laser beam spot of 24 渭 m and 16 渭 m was carried out by using the optimized LA-ICPMS analysis technique. Using NIST SRM 610 as standard sample to calibrate element content, zircon 91500 as international standard correction age value, Zr91 as internal standard element, The three zircon standard plesovicem Tank and Qinghu 206Pb/238U age weighted mean values of 337.0 鹵3.1 Mai 732.0 鹵6.8 Ma 158.2 鹵1.6 Ma were obtained under the laser beam spot condition of 24 渭 m. The average age weighted values of the three zircon standard plesovicege Mud Tank and Qinghu 206Pb/238U were 339.6 鹵4.1 Ma 73 2.9 鹵8.1 Mai 159.8 鹵1.8 Ma, respectively, for the laser beam spot of 16 渭 m. The results show that the average age weighted values of the three zircon standard plesovicege Mud Tank and Qinghu 206Pb/238U are 339.6 鹵4.1 Ma, 732.9 鹵8.1 Ma, 159.8 鹵1.8 Ma, respectively. The results are in good agreement with the recommended values. The results show that the U-Pb dating method of small laser beam zircon developed in our laboratory is feasible, and the U-Pb dating method is suitable for zircon with small grain size and complex genesis, which is of great significance for obtaining a more precise age. The test of silicate main trace elements was also carried out in our laboratory. Under the condition of laser beam spot of 44 渭 m and frequency of 5 Hz, the melting glass of six international standard materials, BCR-2GN, BIR-1G, ATHO-G, GOR132-G, T1-G and St Hs6/80-G, was analyzed by using the optimized LA-ICPMS analysis technique. Ten major elements and 47 trace elements of LA-ICPMS were analyzed. For the same set of data, NIST SRM 610G and MPI-DING were used as external standard, Ca as normalized element, no internal standard method and Ca as internal standard method respectively. The results obtained from each sample were compared. The results show that the test method of silicate single mineral LA-ICPMS is feasible, and the differences between the results obtained by different correction strategies are compared, and the possible reasons are discussed. In addition, the main trace elements of carbonate were tested. Using NIST SRM 610G and MPI-DING as the external standard, using the laser frequency of 44 渭 m or 60 渭 m, the method of no internal standard and the correction strategy of Ca as the internal standard, the main quantity and trace element of MACS-3, the international standard material of carbonate, were analyzed and tested by using the laser frequency of 44 渭 m or 60 渭 m. The results show that the relative error between the test value and the recommended value of most elements is within 20%, and the relative standard deviation (RSD) is less than 10%. At the same time, we can accurately determine the main trace elements of carbonate by using no internal standard method. The results show that the in-situ test method of carbonate main trace element LA-ICPMS is feasible.
【學(xué)位授予單位】：合肥工業(yè)大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2017
【分類號(hào)】：P597.3;P575
本文編號(hào)：2153920
[Abstract]:Laser denudation-inductively coupled plasma mass spectrometry (ICP-MS) is a new type of instrument (abbreviated LA-ICPMS), which is used by laser denudation system and inductively coupled plasma mass spectrometer (LA-ICPMS). It has the advantages of in-situ, real-time, rapid analysis and high sensitivity. Good spatial resolution and other advantages. Although LA-ICPMS solid microanalysis is widely used in situ analysis, the accurate analysis of element content in geological samples is still restricted by many factors, such as instrumental conditions, fractionation effect and changes of sample matrix composition. The deficiency of matrix matching standard material, quantitative calculation strategy and effective sensitivity drift correction etc. Based on the normal operation of LA-ICPMS zircon U-Pb dating for several years, this paper optimizes and improves the LA-ICPMS analysis technology, including replacing the conventional denudation tank with the instrument into a rotary two-channel denudation pool, and increasing the signal leveller. A small amount of nitrogen (gas flow rate 2.5 ml/min) was added to the plasma central gas flow (Ar He) to improve the instrument sensitivity, reduce the detection limit and improve the analytical precision. Zircon U-Pb dating with laser beam spot of 24 渭 m and 16 渭 m was carried out by using the optimized LA-ICPMS analysis technique. Using NIST SRM 610 as standard sample to calibrate element content, zircon 91500 as international standard correction age value, Zr91 as internal standard element, The three zircon standard plesovicem Tank and Qinghu 206Pb/238U age weighted mean values of 337.0 鹵3.1 Mai 732.0 鹵6.8 Ma 158.2 鹵1.6 Ma were obtained under the laser beam spot condition of 24 渭 m. The average age weighted values of the three zircon standard plesovicege Mud Tank and Qinghu 206Pb/238U were 339.6 鹵4.1 Ma 73 2.9 鹵8.1 Mai 159.8 鹵1.8 Ma, respectively, for the laser beam spot of 16 渭 m. The results show that the average age weighted values of the three zircon standard plesovicege Mud Tank and Qinghu 206Pb/238U are 339.6 鹵4.1 Ma, 732.9 鹵8.1 Ma, 159.8 鹵1.8 Ma, respectively. The results are in good agreement with the recommended values. The results show that the U-Pb dating method of small laser beam zircon developed in our laboratory is feasible, and the U-Pb dating method is suitable for zircon with small grain size and complex genesis, which is of great significance for obtaining a more precise age. The test of silicate main trace elements was also carried out in our laboratory. Under the condition of laser beam spot of 44 渭 m and frequency of 5 Hz, the melting glass of six international standard materials, BCR-2GN, BIR-1G, ATHO-G, GOR132-G, T1-G and St Hs6/80-G, was analyzed by using the optimized LA-ICPMS analysis technique. Ten major elements and 47 trace elements of LA-ICPMS were analyzed. For the same set of data, NIST SRM 610G and MPI-DING were used as external standard, Ca as normalized element, no internal standard method and Ca as internal standard method respectively. The results obtained from each sample were compared. The results show that the test method of silicate single mineral LA-ICPMS is feasible, and the differences between the results obtained by different correction strategies are compared, and the possible reasons are discussed. In addition, the main trace elements of carbonate were tested. Using NIST SRM 610G and MPI-DING as the external standard, using the laser frequency of 44 渭 m or 60 渭 m, the method of no internal standard and the correction strategy of Ca as the internal standard, the main quantity and trace element of MACS-3, the international standard material of carbonate, were analyzed and tested by using the laser frequency of 44 渭 m or 60 渭 m. The results show that the relative error between the test value and the recommended value of most elements is within 20%, and the relative standard deviation (RSD) is less than 10%. At the same time, we can accurately determine the main trace elements of carbonate by using no internal standard method. The results show that the in-situ test method of carbonate main trace element LA-ICPMS is feasible.
【學(xué)位授予單位】：合肥工業(yè)大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2017
【分類號(hào)】：P597.3;P575
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