Study on the Causes for ICP-MS Signal Intensity Declination of Os Water Absorption Liquid

Li-min ZHOU; Chao LI; Xin-wei LI; Hong ZHAO; Wen-jun QU; An-dao DU

doi:10.15898/j.cnki.11-2131/td.201805010054

Rock and Mineral Analysis > 2018 > 37(4): 431-438. > DOI: 10.15898/j.cnki.11-2131/td.201805010054

Li-min ZHOU, Chao LI, Xin-wei LI, Hong ZHAO, Wen-jun QU, An-dao DU. Study on the Causes for ICP-MS Signal Intensity Declination of Os Water Absorption Liquid[J]. Rock and Mineral Analysis, 2018, 37(4): 431-438. DOI: 10.15898/j.cnki.11-2131/td.201805010054

Citation:

PDF (1498 KB)

Study on the Causes for ICP-MS Signal Intensity Declination of Os Water Absorption Liquid

Li-min ZHOU^1,2,,
Chao LI^1,2,
Xin-wei LI^1,2,
Hong ZHAO^1,2,
Wen-jun QU^1,2,
An-dao DU^1,2

1.
National Research Center for Geoanalysis, Beijing 100037, China
2.
Key Laboratory of Re-Os Isotope Geochemistry, Chinese Academy of Geological Sciences, Beijing 100037, China

More Information

Received Date: April 30, 2018
Revised Date: May 30, 2018
Accepted Date: June 10, 2018
Published Date: June 30, 2018

Abstract

HIGHLIGHTS
(1) The volatilization and reduction of OsO₄ cause the decline of Inductively Coupled Plasma-Mass Spectrometry (ICP-MS) signal, but the latter is the main reason.

(2) Keeping the absorbing liquid in high-acidity (about 3.5 mol/L) and freezing can suppress the signal decline.

ABSTRACT

BACKGROUNDOs can be separated from the sample matrix by distillation, and the absorbing liquid can be introduced into ICP-MS directly, which is a key step of the molybdenite Re-Os isotopic age analysis. However, the Os signal intensity declines significantly after long time storage. According to the properties of OsO₄, the possible causes may include:1) volatilization which reduces the Os content in the absorbing liquid, and 2) the reduction in which Os(Ⅷ) transforms to the low valence state without volatility and OsO₄ in the gas state decreases. Although they can both reduce the Os being introduced into ICP-MS ultimately, the extent of their effect is not clear.
OBJECTIVESTo quantify the effects of absorbing liquid storage conditions such as duration, acidity and temperature on the Os signal intensity, to identify the cause of this decline and to find out the methods for its suppression. METHODS:The experiment consists of two parts:1) using the molybdenite Re-Os dating reference materials to construct a different absorbing liquid storage condition series, including duration, acidity and temperature, and measure their Os signal intensities in terms of ¹⁸⁷Os/¹⁹³Ir relative ratios. 2) sealing the residual absorbing liquid together with the spike and oxidizing agents within the Carius tube with sequent heating and distillation. The ¹⁸⁷Os/¹⁹⁰Os ratios were determined to calculate the Os content and the retention rate.
RESULTSAfter storing, the Os signal intensities of absorbing liquids decline with time from 3.2% to 68.6%. The longer time, the lower acidity and the higher temperature for OsO₄ absorbing liquid storage, the more obvious Os signal declines. After storing at room temperature for the same time, the Os retention rate of the low-acidity series is higher than that of the high-acidity series, but the former has a lower signal intensity than the latter. This indicates that both volatilization and reduction contribute to the decline of Os signal intensity and are the main factors.
CONCLUSIONSFreezing to -18℃ can inhibit the volatilization of OsO₄, whereas increasing the acidity (about 3.5 mol/L) can reduce OsO₄ reduction. The combination of the two inhibits signal attenuation, and increases the flexibility and applicability of the distillation method.
- Re-Os isotope,
- distillation,
- ICP-MS,
- volatilization,
- reduction

FullText(HTML)

References (23)

References

Du A D, He H L, Yin N W, et al.Direct dating of moly-bdenites using the Re-Os geochronometer[J].Chinese Sciences Bulletin, 1993, 38(15):1319-1320. http://www.cqvip.com/QK/86894X/199315/4001551757.html

Stein H J, Markey R J, Morgan J W, et al.The remark-able Re-Os chronometer in molybdenite:How and why it works[J].Terra Nova, 2001, 13(6):479-486. doi: 10.1046/j.1365-3121.2001.00395.x

Hou Z Q, Zeng P S, Gao Y F, et al.Himalayan Cu-Mo-Au mineralization in the Eastern Indo-Asian collision zone:Constraints from Re-Os dating of molybdenite[J].Geological Review, 2006, 41(1):33-45. http://d.old.wanfangdata.com.cn/Periodical/OA000004921

Gannoun A, Burton K W, Day J, et al.Highly siderophile element and Os isotope systematics of volcanic rocks at divergent and convergent plate boundaries and in intraplate settings[J].Reviews in Mineralogy & Geochemistry, 2016, 81(1):651-724. http://eprints.whiterose.ac.uk/102470/

Kendall B, Creaser R A, Gordon G W, et al.Re-Os and Mo isotope systematics of black shales from the Middle Proterozoic Velkerri and Wollogorang Formations, McArthur Basin, Northern Australia[J].Geochimica et Cosmochimica Acta, 2009, 73(9):2534-2558. doi: 10.1016/j.gca.2009.02.013

Carius L.Vber die Elementaranalyse organischer Verbin-dungen[J].Justus Liebigs Annalen der Chemie, 1860, 116(1):1-30. doi: 10.1002/(ISSN)1099-0690

Sun Y L, Xu P, Li J, et al.A practical method for determination of molybdenite Re-Os age by inductively coupled plasma-mass spectrometry combined with Carius tube-HNO₃ digestion[J].Analytical Methods, 2010, 2(5):575-581. doi: 10.1039/b9ay00258h

Chu Z Y, Yan Y, Chen Z, et al.A comprehensive method for precise determination of Re, Os, Ir, Ru, Pt, Pd concentrations and Os isotopic compositions in geological samples[J].Geostandards & Geoanalytical Research, 2015, 39(2):151-169. http://www.wanfangdata.com.cn/details/detail.do?_type=perio&id=HYC201604180000017481

Reisberg L, Meisel T.The Re-Os isotopic system:A review of analytical techniques[J].Geostandards & Geoanalytical Research, 2010, 26(3):249-267. doi: 10.1111-j.1751-908X.2002.tb00633.x/

Qi L, Zhou M F, Gao J F, et al.An improved Carius tube technique for determination of low concentrations of Re and Os in pyrites[J].Journal of Analytical Atomic Spectrometry, 2010, 25(4):585-589. doi: 10.1039/b919016c

屈文俊, 杜安道.高温密闭溶样电感耦合等离子体质谱准确测定辉钼矿铼-锇地质年龄[J].岩矿测试, 2003, 22(4):254-262. doi: 10.3969/j.issn.0254-5357.2003.04.003

Qu W J, Du A D.Highly precise Re-Os dating of molybdenite by ICP-MS with Carius tube sample digestion[J].Rock and Mineral Analysis, 2003, 22(4):254-262. doi: 10.3969/j.issn.0254-5357.2003.04.003

Puchtel I S, Humayun M, Walker R J.Os-Pb-Nd isotope and highly siderophile and lithophile trace element systematics of komatiitic rocks from the Volotsk suite, SE Baltic 217 Shield[J].Precambrian Research, 2007, 158(1-2):119-137. doi: 10.1016/j.precamres.2007.04.004

Luck J M, Birck J L, Allegre C J.¹⁸⁷Re-¹⁸⁷Os systema-tics in meteorites:Early chronology of the solar system and the age of the galaxy[J].Nature, 1980, 283:256-259. doi: 10.1038/283256a0

王淑贤, 王守业, 杜安道, 等.CCl₄萃取Os用于ICP-MS测定Re-Os年龄的初步研究[J].质谱学报, 2000, 21(3-4):141-142. http://d.old.wanfangdata.com.cn/Periodical/zpxb200003072

Wang S X, Wang S Y, Du A D, et al.Primary study on extraction CCl₄ of Os for Re-Os dating by ICP-MS[J].Journal of Chinese Mass Spectrometry Society, 2000, 21(3-4):141-142. http://d.old.wanfangdata.com.cn/Periodical/zpxb200003072

Birck J L, Barman M R, Campas F.Re-Os isotopic mea-surements at the femtomole level in natural samples[J].Geostandards Newsletter, 1997, 21(1):19-27. doi: 10.1111/ggr.1997.21.issue-1

Morgan J W, Walker R J.Isotopic determinations of rhe-nium and osmium in meteorites by using fusion, distillation and ion-exchange separations[J].Analytical Chimica Acta, 1989, 222(1):291-300. doi: 10.1016/S0003-2670(00)81904-2

杜安道, 何红蓼, 殷宁万, 等.辉钼矿的铼-锇同位素地质年龄测定方法研究[J].地质学报, 1994, 68(4):339-347. doi: 10.3321/j.issn:0001-5717.1994.04.005

Du A D, He H L, Yin N W, et al.A study on the rhenium-osmium geochronometry of molybdenites[J].Acta Geologica Sinica, 1994, 68(4):339-347. doi: 10.3321/j.issn:0001-5717.1994.04.005

Brauns C M.A rapid, low-blank technique for the extra-ction of osmium from geological samples[J].Chemical Geology, 2001, 176(1-4):379-384. doi: 10.1016/S0009-2541(00)00371-5

李超, 屈文俊, 周利敏, 等.Carius管直接蒸馏快速分离锇方法研究[J].岩矿测试, 2010, 29(1):14-16. doi: 10.3969/j.issn.0254-5357.2010.01.004

Li C, Qu W J, Zhou L M, et al.Rapid separation of osmium by direct distillation with Carius tube[J].Rock and Mineral Analysis, 2010, 29(1):14-16. doi: 10.3969/j.issn.0254-5357.2010.01.004

Jin X D, Du A D, Li W J, et al.A new modification of the sample introduction system for Os isotope ratio measurements[J].Journal of Analytical Atomic Spectrometry, 2011, 26(6):1245-1252. doi: 10.1039/c1ja00004g

周利敏, 高炳宇, 王礼兵, 等.Carius管直接蒸馏快速分离锇方法的改进[J].岩矿测试, 2012, 31(3):413-418. doi: 10.3969/j.issn.0254-5357.2012.03.005

Zhou L M, Gao B Y, Wang L B, et al.Improvements on the separation method of osmium by direct distillation in Carius tube[J].Rock and Mineral Analysis, 2012, 31(3):413-418. doi: 10.3969/j.issn.0254-5357.2012.03.005

何红蓼, 杜安道, 邹晓秋, 等.铼-锇测年法中锇的化学行为的研究[J].分析化学, 1994, 22(2):109-114. doi: 10.3321/j.issn:0253-3820.1994.02.031

He H L, Du A D, Zou X Q, et al.A study on the chemical behavior of osmium in rhenium-osmium isotope dating[J].Chinese Journal of Analytical Chemistry, 1994, 22(2):109-114. doi: 10.3321/j.issn:0253-3820.1994.02.031

Du A D, Wu S Q, Sun D Z, et al.Preparation and certification of Re-Os dating reference materials:Molybdenites HLP and JDC[J].Geostandards & Geoanalytical Research, 2004, 28(1):41-52. doi: 10.1111-j.1751-908X.2004.tb01042.x/

[1]	REN Dong, ZHOU Xiao-lin, ZONG You-yin, ZHANG Ting-zhong. Determination of Trace Iodine in Soils, Sediments and Rocks by ICP-MS after Pressurized Acid Digestion-Hydroxylamine Hydrochloride Reduction[J]. Rock and Mineral Analysis, 2019, 38(6): 734-740. DOI: 10.15898/j.cnki.11-2131/td.201901170009
[2]	Bi ZHU, Zhi-yong ZHU, Miao LÜ, Tao YANG. Application of Iolite in Data Reduction of Laser Ablation-Inductively Coupled Plasma-Mass Spectrometry Line-scan Analysis[J]. Rock and Mineral Analysis, 2017, 36(1): 14-21. DOI: 10.15898/j.cnki.11-2131/td.2017.01.003
[4]	Hui-yan GAO. Determination Systems of Nb and Ta in Geochemical Samples and Rare Earth ores by ICP-MS and ICP-AES[J]. Rock and Mineral Analysis, 2014, 33(3): 312-320.
[7]	ZHOU Li-min, GAO Bing-yu, WANG Li-bing, LI Chao, QU Wen-jun, HOU Zeng-qian, DU An-dao. Improvements on the Separation Method of Osmium by Direct Distillation in Carius Tube[J]. Rock and Mineral Analysis, 2012, 31(3): 413-418.
[8]	YANG Hongxia, LIU Wei, LI Bing, WEI Wei, ZHANG Huijuan, CHEN Dengyun. Speciation Analysis of Cadmium, Copper and Zinc in Indian Mustard (Brassica Juncea) by Size ExclusionHigh Performance Liquid ChromatographyInductively Coupled Plasma-Mass Spectrometry[J]. Rock and Mineral Analysis, 2010, 29(1): 9-13.
[9]	SHI Xian-yi, LIAO Jing-ting, WANG Shi-bin. Improvement on the method for Determination of Iron in Pyrites by Potassium Dichromate Titrimetry with Aluminium Tablet Reduction[J]. Rock and Mineral Analysis, 2009, 28(2): 197-198.
[10]	Precise Determination of Iodine in Soil Samples by ICP-MS with Carius Tube and Standard Addition Method[J]. Rock and Mineral Analysis, 2006, 25(1): 19-21.

Cited By

Cited by

Periodical cited type(2)

1.	鲍厚银，李杰. Pt-Re-Os同位素体系分析技术研究进展. 地球化学. 2024(04): 595-610 .
2.	孙胜玲，李杰，许继峰，王桂琴. 金属硫化物Re-Os同位素定年技术进展. 岩石学报. 2022(06): 1605-1620 .

Other cited types(0)

An-dao DU

1.
National Research Center for Geoanalysis, Beijing 100037, China
2.
Key Laboratory of Re-Os Isotope Geochemistry, Chinese Academy of Geological Sciences, Beijing 100037, China

Get Citation

PDF

XML

Article views (1474) PDF downloads (33) Cited by(2)

Turn off MathJax

Article Contents

ABSTRACT

References

Study on the Causes for ICP-MS Signal Intensity Declination of Os Water Absorption Liquid