实时在线氧校正205Pb-233U-236U稀释剂单颗粒锆石ID-TIMS U-Pb高精度年龄测定方法

储著银; 许俊杰; 凌潇潇; 张普; 程海; 郭敬辉; 周新华

doi:10.18654/1000-0569/2022.12.09

实时在线氧校正²⁰⁵Pb-²³³U-²³⁶U稀释剂单颗粒锆石ID-TIMS U-Pb高精度年龄测定方法

- 1.
  中国科学院地质与地球物理研究所, 岩石圈演化国家重点实验室, 北京 100029
- 2.
  中国科学院地球科学研究院, 北京 100029
- 3.
  西安交通大学全球环境变化研究院, 西安 712000
基金项目:
本文受国家自然科学基金项目（42073050、41673061）和国家重点研发计划项目（2020YFA0714803）联合资助

详细信息

作者简介:
储著银, 男, 1970年生, 研究员, 主要从事同位素地球化学研究工作, E-mail: zhychu@mail.iggcas.ac.cn

中图分类号: P597

收稿日期: 2022-06-10

修回日期: 2022-08-14

刊出日期: 2022-12-01

Precise ID-TIMS U-Pb dating of single zircons using ²⁰⁵Pb-²³³U-²³⁶U tracers: Isobaric oxide corrections for UO₂⁺ with in-run measured ¹⁸O/¹⁶O

- 1.
  State Key Laboratory of Lithospheric Evolution, Institute of Geology and Geophysics, Chinese Academy of Sciences, Beijing 100029, China
- 2.
  Innovation Academy for Earth Science, Chinese Academy of Sciences, Beijing 100029, China
- 3.
  Institute of Global Environmental Change, Xi'an Jiaotong University, Xi'an 712000, China

Received Date: 10 June 2022

Revised Date: 14 August 2022

Publish Date: 01 December 2022

摘要

摘要:
单颗粒锆石化学溶蚀同位素稀释热电离质谱（CA-ID-TIMS）U-Pb法是目前精度最高的同位素地质年代学方法，由于存在²³⁶U¹⁶O¹⁸O⁺和²³⁶U¹⁸O¹⁶O⁺对²³⁸U¹⁶O₂⁺的干扰问题，目前国际上通用的U-Pb定年稀释剂是²⁰⁵Pb-²³³U-²³⁵U而不采用²⁰⁵Pb-²³³U-²³⁶U。针对该问题，本文详细探讨了热电离质谱法（TIMS）测定U同位素过程中，²³⁶U¹⁶O¹⁸O⁺和²³⁶U¹⁸O¹⁶O⁺对²³⁸U¹⁶O₂⁺的干扰对U-Pb年龄测定结果的影响程度，指出ID-TIMS U-Pb分析过程中控制²³³U-²³⁶U稀释剂的加入量，保证样品-稀释剂²³⁸U/²³⁶U混合比>0.5，²³⁶U¹⁶O¹⁸O⁺和²³⁶U¹⁸O¹⁶O⁺对²³⁸U¹⁶O₂⁺的干扰对定年结果的影响并不显著。此外，详细探讨了热电离质谱（TIMS）U、Pb同位素测定过程中二次电子倍增器（SEM）死时间的准确设定对高精度CA-ID-TIMS U-Pb定年的重要性。在此基础上，建立了在线氧校正²⁰⁵Pb-²³³U-²³⁶U稀释剂CA-ID-TIMS单颗粒锆石U-Pb年龄高精度测定方法。最后，采用所建立方法对标准锆石ZS进行了测定，获得的²⁰⁶Pb/²³⁸U年龄加权平均值为559.91±0.25Ma（2σ，仅分析误差），与文献报道值在误差范围内一致。由于采用了²³³U-²³⁶U双稀释剂内部校正U同位素分馏效应，该标样年龄测定精度达到0.05%，优于其²⁰⁵Pb-²³⁵U单稀释剂法年龄测定结果的精度。
- 同位素稀释热电离质谱法 /
- 铀-铅定年 /
- 锆石 /
- 双稀释剂
Abstract:
Due to the interferences of ²³⁶U¹⁶O¹⁸O⁺ and ²³⁶U¹⁸O¹⁶O⁺ on ²³⁸U¹⁶O₂⁺, a ²⁰⁵Pb-²³³U-²³⁵U spike rather than a ²⁰⁵Pb-²³³U-²³⁶U spike is usually used for the single grain zircon CA-ID-TIMS U-Pb dating worldwide. In order to use the ²⁰⁵Pb-²³³U-²³⁶U spike for correcting the U isotope fractionation effect by the ²³³U-²³⁶U double spike, in this study, the impact of isobaric interferences of ²³⁶U¹⁶O¹⁸O⁺ and ²³⁶U¹⁸O¹⁶O⁺ on ²³⁸U¹⁶O₂⁺ for the TIMS U isotope analysis is thoroughly addressed. We found that it is critical to ensure the sample is not over-spiked using the ²⁰⁵Pb-²³³U-²³⁶U spike by controlling the amount of the spike to be added into the sample during the CA-ID-TIMS U-Pb analysis. Actually, when the ²³⁸U/²³⁶U ratio in the sample-spike mixture is not < 0.5, the effect of the interferences of ²³⁶U¹⁶O¹⁸O⁺ and ²³⁶U¹⁸O¹⁶O⁺ on ²³⁸U¹⁶O₂⁺ on the final U-Pb dating result is not significant. In addition, the importance of the correct setting of the dead-time of SEM (secondary electron multiplier) for the U and Pb isotope analyses for the CA-ID-TIMS U-Pb dating has also been fully addressed. Accordingly, a high precision CA-ID-TIMS U-Pb geochronology method for single zircons using ²⁰⁵Pb-²³³U-²³⁶U tracers with in-run measured ¹⁸O/¹⁶O for UO₂⁺ isobaric oxide corrections has been developed. Finally, a standard zircon-ZS was analyzed using the method, yielding a weighted mean ²⁰⁶Pb/²³⁸U age of 559.91±0.25Ma (2σ, analytical error), which is consistent with the previously reported date within analytical error. Due to the use of ²³³U-²³⁶U double spike for internal correction of U isotope fractionation effect, the analytical precision for this standard zircon is better than 0.05% (2RSE), which is significantly better than that obtained by using the single ²⁰⁵Pb-²³⁵U tracer.
- CA-ID-TIMS /
- U-Pb dating /
- Zircon /
- Double spike

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图 1

SEM Pb死时间

Figure 1.

SEM deadtime for Pb

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图 2

SEM U死时间

Figure 2.

SEM deadtime for U

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图 3

ZS锆石U-Pb谐和图(a)和²⁰⁶Pb/²³⁸U年龄加权平均值(b)

Figure 3.

Concordia and Weighted mean ²⁰⁶Pb/²³⁸U ages for ZS zircon

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表 1

U同位素测定数据采集参数

Table 1.

Data acquisition parameters for U isotope ratio measurement

质量数(amu)	265	267	268	270	272
主同位素	²³³U¹⁶O₂	²³⁵U¹⁶O₂	²³⁶U¹⁶O₂	²³⁸U¹⁶O₂	²³⁸U¹⁶O¹⁸O、²³⁸U¹⁸O¹⁶O
积分时间(s)	4	4	4	4	8
跳扫等待时间(s)	2	1	1	1	1

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表 2

²⁰⁵Pb-²³³U-²³⁶U稀释剂Pb、U同位素比值

Table 2.

Pb, U isotope compositions for the ²⁰⁵Pb-²³³U-²³⁶U spike

同位素比值	²⁰⁵Pb/²⁰⁶Pb	²⁰⁴Pb/²⁰⁶Pb	²⁰⁷Pb/²⁰⁶Pb	²⁰⁸Pb/²⁰⁶Pb	²³⁵U/²³⁶U	²³⁸U/²³⁶U
平均值(n=5)	2456	0.151	1.053	2.011	0.0000637	0.0002768
标准差	33	0.008	0.068	0.009	0.0000086	0.0000079

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表 3

²⁰⁵Pb-²³³U-²³⁶U稀释剂²⁰⁵Pb、²³³U和²³⁶U浓度

Table 3.

²⁰⁵Pb, ²³³U and ²³⁶U concentration for the ²⁰⁵Pb-²³³U-²³⁶U spike

分析次数	²³³U	²³⁶U	²⁰⁵Pb	²³⁶U/²⁰⁵Pb
分析次数	(pmol/g)			²³⁶U/²⁰⁵Pb
1	361.70	354.94	10.540	33.71
2	361.81	355.04	10.541	33.72
3	361.95	355.18	10.540	33.73
4	361.67	354.90	10.552	33.67
5	362.25	355.48	10.548	33.73
平均值	361.88	355.11	10.544	33.71
相对误差(%)	0.058	0.058	0.048	0.073

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表 4

全流程Pb、U本底

Table 4.

Procedural blanks for Pb and U

分析次数	1	2	3	4	5	6	7	8	9	10	平均值	标准差
Pb (pg)	3.7	2.4	4.0	3.4	2.2	3.1	1.3	2.6	1.9	2.1	2.7	0.8
U (pg)	0.66	0.47	0.59	0.90	0.57	0.60	0.41	0.56	0.68	0.56	0.60	0.13

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表 5

不同²³⁸U/²³⁶U混合比条件下²³⁶U¹⁶O¹⁸O和²³⁶U¹⁸O¹⁶O对²³⁸U¹⁶O₂干扰程度及氧校正误差

Table 5.

The interferences of ²³⁶U¹⁶O¹⁸O and ²³⁶U¹⁸O¹⁶O on ²³⁸U¹⁶O₂ and oxide correction errors for different ²³⁸U/²³⁶U mixed ratios

²³⁸U/²³⁶U	干扰	¹⁸O/¹⁶O误差	氧校正误差
2	0.20%	5%	0.010%
1	0.41%	5%	0.020%
0.5	0.82%	5%	0.041%
0.4	1.0%	5%	0.051%
0.1	4.1%	5%	0.20%

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表 6

标准锆石ZS U-Pb年龄测定结果

Table 6.

Analytical results for ZS standard zircon

测点号	同位素比值											相关系数	年龄(Ma)
			Th/U				2RSE (%)		2RSE (%)		2RSE (%)			2SE		2SE		2SE
	(a)	(a)	(b)	(c)	(d)	(d)		(d)		(d)			(e)		(e)		(e)
ZS-1	63	2.70	0.217	4121	0.0678	0.05891	0.23	0.7368	0.32	0.09070	0.18	0.72	563.9	5.0	560.5	1.4	559.70	0.94
ZS-2	69	3.04	0.221	4500	0.0689	0.05876	0.19	0.7351	0.26	0.09072	0.11	0.74	558.3	4.2	559.5	1.1	559.82	0.61
ZS-3	117	3.71	0.307	7423	0.0959	0.058910	0.12	0.7378	0.22	0.09084	0.14	0.87	563.8	2.6	561.13	0.94	560.48	0.72
ZS-4	46	5.15	0.212	3030	0.0664	0.05891	0.19	0.7367	0.32	0.09070	0.22	0.81	563.7	4.2	560.5	1.4	559.7	1.2
ZS-5	102	3.45	0.199	6708	0.0622	0.058926	0.13	0.7371	0.22	0.09072	0.13	0.86	564.4	2.8	560.7	1.0	559.79	0.71
ZS-6	60	4.36	0.311	3801	0.0970	0.05876	0.19	0.7352	0.26	0.09075	0.12	0.73	558.0	4.2	559.6	1.1	559.97	0.63
ZS-7	47	5.68	0.206	3061	0.0644	0.058920	0.15	0.7369	0.25	0.09071	0.15	0.84	564.2	3.3	560.6	1.1	559.71	0.82
ZS-8	101	6.01	0.204	6588	0.0638	0.05894	0.22	0.7373	0.28	0.09074	0.14	0.65	564.8	4.7	560.9	1.2	559.89	0.75
ZS-9	128	3.72	0.300	8156	0.0938	0.058976	0.083	0.7380	0.30	0.09075	0.26	0.97	566.2	1.8	561.2	1.3	560.0	1.4
ZS-10	50	4.38	0.292	3235	0.0913	0.058931	0.16	0.7372	0.32	0.09073	0.24	0.88	564.5	3.4	560.8	1.4	559.8	1.3
注：(a) Pb^和Pb_c分别代表放射成因铅和普通铅；(b)根据²⁰⁸Pb^/²⁰⁶Pb^和²⁰⁷Pb/²³⁵U年龄计算得到Th/U比值；(c)扣除稀释剂和分馏后²⁰⁶Pb/²⁰⁴Pb比值；(d)扣除稀释剂、分馏和本底贡献后同位素比值；普通铅被认为全部来自流程本底: ²⁰⁶Pb/²⁰⁴Pb=18.46±1.4% (RSD), ²⁰⁷Pb/²⁰⁴Pb=15.53±1.1% (RSD); ²⁰⁸Pb/²⁰⁴Pb=38.21±0.74% (RSD)；U本底，0.60±0.30pg (SD)；(e)衰变常数采用Jaffey et al*. (1971)；²⁰⁶Pb/²³⁸U和²⁰⁷Pb/²⁰⁶Pb年龄经过²³⁰Th校正(假定岩浆Th/U=3)

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