發(fā)布時(shí)間：2018-06-06 08:10

  本文選題：多接收電感耦合等離子體質(zhì)譜 + 飛秒激光剝蝕　； 參考：《西北大學(xué)》2015年碩士論文

【摘要】：本文建立了以溶液霧化(SN)和飛秒激光剝蝕(fsLA)的進(jìn)樣方式,應(yīng)用多接收等離子體質(zhì)譜(MC-ICPMS)分析硫化物中S與Pb同位素組成的方法。研究內(nèi)容如下：建立硫化物樣品化學(xué)消解方法與溶液樣品中S同位素分離純化流程；研究SN與膜去溶霧化進(jìn)樣方式(DSN)的MC-ICPMS分析測(cè)試方法；利用266nm飛秒激光剝蝕與多接收等離子體質(zhì)譜聯(lián)用(fsLA-MC-ICPMS)原位微區(qū)分析測(cè)試硫化物中Pb同位素；本文應(yīng)用不同類型MC-ICPMS儀器(小型Nu Plasma II與大型Nu Plasma 1700)初步建立S同位素分析測(cè)試方法,結(jié)果表明經(jīng)化學(xué)消解、分離后測(cè)試結(jié)果的精密度和準(zhǔn)確度均與國際現(xiàn)有報(bào)道值一致,可用于實(shí)際硫化物中S同位素研究。1.建立硫化物化學(xué)消解方法,用濃HNO3與濃HCl可將樣品溶解并氧化至最高價(jià)態(tài),利用AG 50-X8陽離子交換樹脂分離純化,S回收率大于97%。2.建立S同位素分析測(cè)試方法,采用標(biāo)準(zhǔn)-樣品交叉(SSB)法,校正儀器的質(zhì)量歧視效應(yīng)及空間電荷效應(yīng)；通過對(duì)比實(shí)驗(yàn)研究進(jìn)樣方式即溶液進(jìn)樣(濕法進(jìn)樣,wet plasma)與膜去溶進(jìn)樣(干法進(jìn)樣,dry plasma);S同位素分析采用TRA (Time Resolved Analysis)模式進(jìn)行On-Peak-Zero方式扣除背景干擾；采用高純水(MQ-H2O)比常用的2%HN03具有更快速背景清洗能力,并可擴(kuò)大濃度匹配范圍；對(duì)比不同分辨率(中分辨與高分辨模式)對(duì)分析測(cè)試結(jié)果影響,儀器分析所需分辨率與進(jìn)樣方式相關(guān),DSN干法進(jìn)樣可消除多原子離子(O2+離子)干擾,采用中分辨率分析以提高靈敏度,而濕法進(jìn)樣中O2+離子干擾無法消除,采用高分辨模式分開干擾峰以獲得準(zhǔn)確結(jié)果；加入內(nèi)標(biāo)元素(C1元素)校正S同位素分析測(cè)試中存在的分餾效應(yīng), Cl同位素與S同位素在MC-ICPMS中的分餾效應(yīng)不同無法有效校正S同位素；分析測(cè)試國際標(biāo)準(zhǔn)樣品：IAEA-S-1, NBS-123及標(biāo)準(zhǔn)溶液Alfa-S,結(jié)果與文獻(xiàn)報(bào)道值誤差范圍內(nèi)完全一致,表明研究建立的分析方法可行,可用于實(shí)際硫化物樣品中S同位素研究。3.通過Nu Plasma 1700大型高分辨多接收等離子體質(zhì)譜(MC-ICPMS),采用高分辨率可消除S同位素分析測(cè)試中存在的多原子離子干擾,測(cè)試不同進(jìn)樣方式、濃度效應(yīng)影響,分析測(cè)試國際標(biāo)準(zhǔn)樣品(IAEA-S-2, IAEA-S-3與NBS.123)及標(biāo)準(zhǔn)溶液樣品(Spex-S和Alfa-S) S同位素組成,實(shí)驗(yàn)結(jié)果與文獻(xiàn)報(bào)道值誤差范圍內(nèi)一致。4.建立fsLA-MC-ICPMS研究硫化物中Pb同位素組成原位微區(qū)分析技術(shù),分餾效應(yīng)及質(zhì)量歧視效應(yīng)采用內(nèi)標(biāo)TI (NIS TNBS 997)和外標(biāo)(NIST SRM 610)相結(jié)合方式進(jìn)行校正。利用研究建立的方法分析了都龍錫鋅銦多金屬礦帶中的黃銅礦、黃鐵礦和閃鋅礦中Pb同位素組成。結(jié)果表明,不同礦物間及相同礦物不同顆粒間Pb含量差異大,Pb含量高于10μg/g的黃銅礦和閃鋅礦顆粒顯示了一致的Pb同位素分布,而Pb含量高于100μg/g的所有硫化物顆粒均具有誤差范圍內(nèi)一致的Pb同位素組成,且與化學(xué)法得到的結(jié)果誤差范圍內(nèi)吻合,表明本研究方法結(jié)果可靠。
[Abstract]:In this paper, a method for the determination of S and Pb isotopic compositions in sulfides by multi-receiver plasma mass spectrometry (MC-ICPMSs) has been established by using the injection method of solution atomization (SNN) and femtosecond laser denudation (fsla). The main contents of the study are as follows: to establish the chemical digestion method of sulfide sample and the separation and purification process of S isotope in solution sample, to study the MC-ICPMS analysis and test method of SN and membrane desolvent atomization injection method; 266nm femtosecond laser denudation and multi-receiver plasma-mass spectrometry were used to analyze the Pb isotopes of sulfides in situ, and different types of MC-ICPMS instruments (small Nu Plasma II and large Nu Plasma 1700) were used to establish a S-isotope analysis method. The results show that the precision and accuracy of the test results after chemical digestion are consistent with those reported in the world and can be used for the study of S isotopes in actual sulfides. The sulphide chemical digestion method was established. The sample could be dissolved and oxidized to the highest valence state by using concentrated HNO3 and concentrated HCl. The recovery of S was more than 97. 2 by using AG 50-X8 cation exchange resin. The S isotope analysis and measurement method was established, and the quality discrimination effect and space charge effect of the instrument were corrected by the standard sample crossover SSBs method. The contrast experiment was carried out to study the methods of injection, that is, wet injection (wet injection) and dry injection (dry water Resolved analysis) to deduct background interference by using TRA time Resolved analysis model. The use of high purity water MQ-H2O has faster background cleaning ability than conventional 2%HN03, and can expand the range of concentration matching, and compare the effect of different resolution (medium resolution and high resolution mode) on the analysis and test results. The resolution required by instrument analysis is related to the way of injection. The interference of polyatomic ion O 2 ion can be eliminated by dry sampling with DSN. The medium resolution analysis is used to improve the sensitivity, but the interference of O 2 ion in wet method can not be eliminated. The interference peaks are separated by high resolution mode to obtain accurate results. The fractionation effect in the analysis and testing of S isotopes is corrected by adding the internal standard element C 1. The fractionation effect of Cl isotope and S isotope in MC-ICPMS can not be corrected effectively by adding the fractionation effect of Cl isotope and S isotope in MC-ICPMS. The analytical results of the international standard sample: 1 IAEA-S-1, NBS-123 and standard solution Alfa-Sare in full agreement with the reported error range, which indicates that the established analytical method is feasible and can be used in the study of S isotopes in actual sulphide samples .3. By means of Nu Plasma 1700 large scale high resolution multi-receiver plasma mass spectrometry (MC-ICPMS), the interference of polyatomic ions in S isotope analysis can be eliminated by using high resolution, and the influence of different sampling methods and concentration effect can be tested. The isotopic compositions of IAEA-S-2, IAEA-S-3 and NBS.123 and standard solution samples were analyzed and tested. The experimental results were in agreement with the reported error range of .4. An in situ microanalysis technique for Pb isotopic composition in sulfides was established by fsLA-MC-ICPMS. The fractionation effect and mass discrimination effect were corrected by the combination of internal standard TI NIS TNBS 997) and external standard NIST SRM 610). The Pb isotopic compositions of chalcopyrite, pyrite and sphalerite in the Dulong tin, zinc and indium polymetallic ore belt were analyzed by the established method. The results show that the Pb contents of chalcopyrite and sphalerite with Pb content higher than 10 渭 g / g show consistent Pb isotopic distribution among different minerals and different particles of the same mineral. All sulphide particles with Pb content above 100 渭 g / g have the same Pb isotopic composition in the error range, which is consistent with that obtained by the chemical method, which indicates that this method is reliable.
【學(xué)位授予單位】：西北大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2015
【分類號(hào)】：P575;O657.63

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本文編號(hào)：1985856