矿物微区Lu-Hf同位素分析技术研究进展

王浩; 杨岳衡; 杨进辉

doi:10.15898/j.cnki.11-2131/td.202202210027

矿物微区Lu-Hf同位素分析技术研究进展

王浩^{1, 2,},
杨岳衡^{1, 2},
杨进辉^{1, 2}

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.
中国科学院大学地球与行星科学学院, 北京 100049

基金项目:

国家自然科学基金面上项目 41973035

中国科学院青年创新促进会人才项目 2020068

详细信息

作者简介:
王浩，博士，副研究员，主要从事同位素地球化学与前寒武纪地质学研究。E-mail: wanghao@mail.iggcas.ac.cn

中图分类号: O657.63
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出版历程
- 收稿日期: 2022-02-20
- 修回日期: 2022-03-21
- 录用日期: 2022-03-22
- 网络出版日期: 2022-12-13
- 刊出日期: 2022-11-27

A Review of Progress in Microbeam Lu-Hf Isotopic Analysis on Minerals

WANG Hao^{1, 2,},
YANG Yueheng^{1, 2},
YANG Jinhui^{1, 2}

1.
State Key Laboratory of Lithospheric Evolution, Institute of Geology and Geophysics, Chinese Academy of Sciences, Beijing 100029, China
2.
College of Earth and Planetary Sciences, University of Chinese Academy of Sciences, Beijing 100049, China

摘要

摘要:
矿物微区Lu-Hf同位素分析技术为了解岩浆活动和变质反应的微观过程以及示踪沉积物源信息提供了重要手段，极大地促进了岩石地球化学等领域学科发展。本文评价了¹⁷⁶Yb和¹⁷⁶Lu同质异位素、稀土元素氧化物以及富Ta基体等对微区Hf同位素测量精度和准确度的影响方式、校正策略和应对方案，总结了针对锆石、斜锆石、钙钛锆石、钛锆钍矿、异性石、金红石、锡石和铌铁矿等富铪矿物的微区Lu-Hf同位素分析方法、适用对象以及相关标样特征。富镥矿物的微钻/微锯Lu-Hf同位素等时线定年具有高精度的特点，可精确限定多期造山作用和矿物生长持续时间等。利用激光剥蚀电感耦合等离子体三重四极杆串级质谱(LA-ICP-Q-MS/MS)可以实现对石榴石等富镥矿物微米尺度高空间分辨率的微区Lu-Hf单点/等时线定年。该方法依赖Hf与NH₃的碰撞反应实现Lu和Hf的在线分离，达到同步测量¹⁷⁶Lu/¹⁷⁷Hf和¹⁷⁶Hf/¹⁷⁷Hf比值的目的。新一代带碰撞/反应池的多接收串级磁式质谱具有高稳定性和高灵敏度特性，可在消除多离子(团)干扰的同时实现高精度Hf同位素分析，是未来微区Lu-Hf同位素分析发展的重要方向。
- Lu-Hf同位素 /
- LA-MC-ICPMS /
- 锆石 /
- 石榴石 /
- 微区分析
要点
(1) 评述了消除微区Lu-Hf同位素分析离子(团)干扰和基体元素拖尾效应的策略。

(2) 归纳了通过外标和稳定同位素比值监控富铪矿物微区Lu-Hf同位素分析准确性的办法。

(3) 总结了依赖碰撞反应实现富镥矿物微区Lu-Hf同位素定年的方法及改进方向。

HIGHLIGHTS
(1) The strategies to eliminate the interference of ions (clusters) and the tailing effect of matrix elements during microbeam Lu-Hf isotopic analysis are reviewed.

(2) Two ways to monitor the accuracy of microbeam Lu-Hf isotopic analysis on hafnium-rich minerals, including external standards and internal stable isotope ratios, are summarized.

(3) The collision reaction methods for microbeam Lu-Hf isotope dating on lutetium-rich minerals are introduced and new development directions are discussed.
Abstract:
BACKGROUND
Mircobeam Lu-Hf isotopic analysis on minerals provides an important means to understand the microscopic process of magmatic activity and metamorphic reaction and to trace provenance of sediment, which greatly promotes the development of petrogeochemistry. Many methods were provided to obtain accurate and precise microbeam Lu-Hf isotopic data, and many mineral standards for microbeam Lu-Hf isotopic analysis were developed.
OBJECTIVES
To review and understand the microbeam methods for Lu-Hf isotopic analysis.
METHODS
Systematic compilations of published data of standards and discussion on the different methods for microbeam Lu-Hf isotopic analysis.
RESULTS
The development history of microbeam Lu-Hf isotopic analysis in the past 30 years is reviewed, and the influence of ¹⁷⁶Yb and ¹⁷⁶Lu isobars, REE oxides, and Ta-rich matrices on the precision and accuracy of Hf isotope measurement is systematically evaluated as well as the different correction strategies and programs provided in previous studies. In addition, a comprehensive compilation of the different Yb and Lu isotopic compositions reported in references and the different methods of microbeam Lu-Hf isotopic analyses on various Hf-rich minerals such as zircon, baddeleyite, zirconolite, zirkelite, calzirtite, eudialyte, rutile, cassiterite, and columbite-group minerals is made. The micro-drill/micro-saw sampling Lu-Hf isotopic analysis of Lu-rich minerals has played an important role in revealing the multi-stage orogenic process and the duration of mineral growth. The advent of laser ablation inductively coupled plasma triple quadrupole mass spectrometry (LA-ICP-Q-MS/MS) has increased the spatial resolution of Lu-Hf single-spot/isochron dating analysis of Lu-rich minerals to the micrometer scale. This method relies on the collision reaction of Hf and NH₃ to realize the online separation of Hf from Lu, and achieves the purpose of synchronous measurement of ¹⁷⁶Lu/¹⁷⁷Hf and ¹⁷⁶Hf/¹⁷⁷Hf ratios, which is introduced in detail.
CONCLUSIONS
The new generation of tandem multi-collector sector field mass spectrometer with collision/reaction cell has high stability and sensitivity, which can be used to determine online separation of Hf from REEs, produce high-precision Hf isotope measurements for high Yb/Hf or Ta-rich minerals under high spatial resolution conditions, and significantly improve the precision and accuracy of microbeam Lu-Hf isotopic analysis. This deserves extensive attention in the future.
- Lu-Hf isotope /
- LA-MC-ICPMS /
- zircon /
- garnet /
- microbeam analysis

HTML全文

中国是稀土资源大国，占世界稀土矿产资源的80%，稀土元素对岩石形成过程、元素的迁移等研究都有一定的作用，提供了有价值的信息^[1-3]。由于稀土元素的化学性质极其相似，因此采用传统化学法分析时需要冗长的分离富集过程^[4]，且只能测定稀土总量，而不能测定特定元素的含量^[5]。样品中的稀土元素含量超过0.1%，对于这种通常概念上的微量元素，其实已转变为常量组分，大多采用电感耦合等离子体发射光谱法(ICP-OES)^[6]测定，相对于应用X射线荧光光谱法(XRF)的前处理程序比较繁琐且试剂用量大。

XRF法具有制样方法简单、分析速度快、重现性好等特点^[7]，熔融制样法能消除粒度效应，降低元素间的基体效应影响，使复杂的试样也能完全熔融^[8]，适合于多种固体样品中主量、次量多元素的同时测定。目前XRF法分析稀土矿石类样品，主要的应用有：混合稀土氧化物中稀土分量的测定^[9-11]；采用同步辐射XRF法测定稀土元素的最低浓度^[12]；利用粉末压片法制备样品，通过无标定量分析软件添加与待测组分相似样品来建立标签，从而实现稀土矿物中五氧化二磷的准确测定^[13]；以及在其他地质矿化类样品中测定主次量元素开展了大量的研究^{[5, 14-17]}。但应用于测定稀土矿石、矿化样品中的主、次量元素的相关报道较少。对于稀土样品的分析，存在现有的稀土国家标准物质少、稀土元素含量较低、重稀土元素谱线重叠严重等问题，从而导致了应用XRF分析稀土矿石类样品中的主量元素和稀土元素仍存在一定的困难。

鉴于此，本文通过现有的国家稀土标准样品和高纯稀土氧化物混合均匀制得的人工标准样品绘制工作曲线，扩大了自然界丰度较大的稀土元素镧、铈、钇的线性范围，应用熔融制样-波长色散XRF法测定样品，采用理论α系数的校准方法对主量元素进行校正的同时加入稀土元素的校正系数，其余元素用经验系数法来校正元素间的基体效应，对有谱线重叠的元素进行重叠干扰校正。通过对未知样品的检测和对标准样品的反测检验方法的可行性，证明了建立的测定方法可满足稀土矿化类样品分析的可靠性，可为地质评估提供满意的数据要求。

1. 实验部分

1.1 仪器和测量条件

Axios型X射线荧光光谱仪(荷兰帕纳科公司)。主要测量参数：X光管最大电压60 kV，最大电流125 mA，满功率4.0 kW，真空光路，视野光栏直径为32 mm，试样盒面罩直径32 mm。各待测元素的谱线选择和测量条件见表 1。

表 1 仪器分析条件

Table 1. Working conditions of the elements by XRF

元素及谱线	分晶体	准直器 (μm)	探测器	电压 (kV)	电流 (mA)	2θ(°)			PHD范围
元素及谱线	分晶体	准直器 (μm)	探测器	电压 (kV)	电流 (mA)	峰值	背景1	背景2	PHD范围
Si Kα	PE 002	550	FL	32	100	109.14	-2.3160	1.7938	26~76
K Kα	LiF 200	150	FL	32	100	136.73	-1.1730	2.2190	26~74
Ti Kα	LiF 200	150	FL	40	90	86.215	-0.6320	0.8640	26~75
Mn Kα	LiF 200	150	DUP	55	66	62.998	-0.7190	0.7868	13~72
Na Kα	PX1	550	FL	32	100	27.895	-1.8910	2.1214	22~82
Mg Kα	PX1	550	FL	32	100	23.077	-1.8760	2.1788	20~78
Al Kα	PE 002	550	FL	32	100	144.98	2.9372	-1.2490	21~76
P Kα	Ge 111	550	FL	32	100	141.02	-1.3960	2.8040	23~78
S Kα	Ge 111	550	FL	32	100	110.74	-1.5160	1.4708	16~74
Ca Kα	LiF 200	150	FL	32	100	113.16	-0.8730	1.6258	28~70
Fe Kα	LiF 200	150	DUP	55	66	57.530	-0.7130	0.8854	16~69
Cr Kα	LiF 200	150	DUP	55	66	69.365	-0.6450	0.7386	12~73
Ni Kα	LiF 200	150	DUP	55	66	48.658	-0.5890	0.8294	18~70
Y Kα	LiF 200	150	SC	55	66	23.767	0.7668	-0.7400	23~78
Rb Kα	LiF 200	150	SC	55	66	26.581	0.7720	-0.5110	22~78
Sr Kα	LiF 200	150	SC	55	66	25.121	-0.5610	0.7542	22~78
Zr Kα	LiF 200	150	SC	55	66	22.470	-0.7750	0.8758	24~78
Nb Kα	LiF 200	150	SC	55	66	21.372	-0.5870	0.4690	24~78
Cu Kα	LiF 200	150	DUP	55	66	45.010	-0.6960	0.9256	20~69
Zn Kα	LiF 200	150	SC	55	66	41.796	-0.7050	0.6534	15~78
Ba Kα	LiF 200	150	FL	40	90	87.204	0.6376	-	33~71
Rh Kα_c	LiF 200	150	SC	55	66	18.447	-	-	26~78
V Kα	LiF 200	150	DUP	40	90	76.929	-0.6230	-	15~74
Br Kα	LiF 200	150	SC	55	66	29.940	-0.6830	0.9706	20~78
La Lα	LiF 200	150	FL	40	90	82.938	-0.9010		24~78
Ce Lα	LiF 200	150	DUP	40	90	79.047	-0.8740	-	26~78
Pr Lα	LiF 200	150	DUP	55	66	75.379	-0.8580	-	15~74
Nd Lα	LiF 200	150	DUP	55	66	72.141	-0.9860	-	13~74
Sm Lα	LiF 200	150	DUP	55	66	66.237	0.9598	-	15~73
Tb Lα	LiF 200	150	DUP	55	66	58.800	0.3626	-	15~72
Dy Lα	LiF 200	150	DUP	55	66	56.600	-0.8020	-	15~71
Ho Lα	LiF 200	150	DUP	55	66	54.575	-0.6550	-	16~71
Er Lα	LiF 200	150	DUP	55	66	52.605	0.7728	-	17~71
Yb Lα	LiF 200	150	DUP	55	66	49.038	0.8474	-	18~70
Lu Lα	LiF 200	150	DUP	55	66	47.417	-0.4030	-	19~70
Ta Lα	LiF 200	150	DUP	55	66	44.403	0.9066	-	20~69
Eu Lα	LiF 200	150	DUP	55	66	63.591	0.4858	-	15~73
Gd Lα	LiF 200	150	DUP	55	66	61.115	-0.8880	-	15~72
注: FL为流气式正比计数器, SC为闪烁计数器。DUP为流气式正比计数器和封闭式正比计数器串联使用，以提高探测效率。PHD为脉冲高度分析器。

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Front-1型电热式熔样机(国家地质实验测试中心研制)。

铂金坩埚(95%铂+5%金)。石英表面皿:直径20 cm。

1.2 主要试剂

偏硼酸锂+四硼酸锂混合熔剂^[8](质量比22：12，购自张家港火炬仪器厂):将混合溶剂置于大表面皿中，于马弗炉中650℃灼烧2 h，待冷却转入试剂瓶，置于干燥器中保存备。

碘化锂^[18](脱模剂)：优级纯，浓度为40 g/L。配制方法：称取40.0 g碘化锂溶于100 mL棕色试剂瓶中，待用。

硝酸铵(氧化剂):分析纯。

氧化镧、氧化钇、氧化铈:均为分析纯, 纯度99.99%。

1.3 样片制备

样品及熔剂的称量：精确称取灼烧后的混合溶剂5.8500±0.0002 g于30 mL瓷坩埚中，精确称取0.6500±0.0002 g样品置于瓷坩埚中^[16]，用玻璃棒充分搅匀(样品的要求:样品的粒径需小于200目，分取样品于纸质样品袋置于烘箱中，在105℃温度下烘样2 h。于干燥器内保存^[16])。

熔样机条件设定：熔样温度1150℃，预熔2 min，上举1.5 min，摆平0.5 min，往复4次，熔样时间约为10 min；先粗略称取0.100 g硝酸铵^[8]试剂平铺于铂金坩埚中，将称量好的试剂及样品倒入铂金坩埚中，滴两滴碘化锂溶液^[18]，当熔样机温度到达1150℃后，用坩埚钳将装有试样的铂金坩埚放入熔样机，启动熔样机开始熔样。待熔样机提示熔样完成后，将铂金坩埚取出，此时样品为玻璃熔融状态。观察试样底部是否有气泡，如有气泡可手动将气泡摇出^[16]，将铂金坩埚置于水平冷却台待样品底部与铂金坩埚分离后吹风冷却约3 min, 此时在玻璃样片上贴上标签，倒出样片置于干燥器中保存, 待测。

制备样片时，将稀土矿石标准物质(GBW07187、GBW07158、GBW07159、GBW07160、GBW07161)和人工配制标准样品(HC-XT-1~HC-XT-8)分别制备两套重复样片，一套用于建立标准曲线，另一套用作样品测量，检测方法的可行性。GBW07188、HC-XT-8分别重复制备10个，用于精密度的分析。岩石国家一级标准物质(GBW07122、GBW07123、GBW07124、GBW07125、GBW07104~GBW07106)，碳酸盐岩石标准物质(GBW07127~GBW07136)和超基性岩石样品(DZΣ1、DZΣ2)各制备一个用于建立标准曲线。

1.4 样品配制及制备标准曲线的范围

在自然界中，镧、铈、钇的丰度较大，日常样品检测中这三个元素矿化的样品最为常见，因此本文重点通过人工标准物质来解决镧、铈、钇高含量样品的定量问题。在不同的稀土矿石国家标准物质(GBW07187、GBW07188、GBW07158、GBW07159、GBW07160、GBW07161)中加入不等量高纯的稀土氧化物(La₂O₃、CeO₂、Y₂O₃)扩大稀土的含量范围，既使各人工标准基体存在差异，镧、铈、钇含量又有一定梯度。制备人工标准样片时，各高纯稀土氧化物成分的质量和各标准物质称样量见表 2所示。

表 2 人工标准样品的配制

Table 2. Preparation of artificial standard samples

人工标准样品编号	La₂O₃加入量 (g)	CeO₂加入量 (g)	Y₂O₃加入量 (g)	国家标准物质编号	标准物质称样量 (g)
HC-XT-1	0.0400	0.0500	-	GBW07159	0.5600
HC-XT-2	0.0300	0.0400	-	GBW07160	0.5800
HC-XT-3	0.0200	0.0300	-	GBW07187	0.6000
HC-XT-4	0.0100	0.0200	-	GBW07158	0.6200
HC-XT-5	-	0.0100	-	GBW07188	0.6400
HC-XT-6	-	-	-	GBW07187	0.3250
HC-XT-7	-	-	0.0200	GBW07188	0.3250
HC-XT-8	0.0050	0.0050	-	GBW07161	0.6300
				GBW07188	0.6400

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为满足不同类型稀土样品的测试要求，又要满足日常普通硅酸盐、碳酸盐样品的测试要求，本实验采用稀土矿石标准物质(GBW07187、GBW07188、GBW07158、GBW07159、GBW07160、GBW07161)，岩石国家一级标准物质(GBW07122、GBW07123、GBW07124、GBW07125、GBW07104~GBW07106)，碳酸盐岩石标准物质(GBW07127~GBW07136)，DZΣ1、DZΣ2和人工配制标准样品(HC-XT-1~HC-XT-8)共33个样片作为标准样品制备标准曲线。

各元素工作曲线范围列于表 3。

表 3 各元素工作曲线浓度范围

Table 3. Working range of elements concentration

主量元素	含量范围(%)	稀土元素	含量范围(μg/g)
SiO₂	0.3~74.55	Pr₆O₁₁	5.43~890
Al₂O₃	0.1~19.04	Sm₂O₃	13.53~2000
TFe₂O₃	0.07~3.49	Eu₂O₃	0.31~75
FeO	0.007~0.49	Gd₂O₃	27.91~2500
TiO₂	0.003~0.537	Tb₄O₇	5.15~550
CaO	0.0224~55.49	Dy₂O₃	26.04~3700
Na₂O	0.014~0.66	Tm₂O₃	2.29~310
MnO	0.004~0.1	Yb₂O₃	13.45~2100
P₂O₅	0.0022~0.124	La₂O₃^*	0.002~6.16
MgO	0.066~20.15	CeO₂^*	0.0022~7.69
K₂O	0.01~5.52	Y₂O₃^*	0.017~3.2
		Nd₂O₃^*	0.0024~0.4
		Lu₂O₃	1.91~300
		Ho₂O₃	5.44~640
		Er₂O₃	15.26~2000
		Σ RE_xO_y^*	0.085~13.92
注：标记“*”的元素含量单位为%。

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2. 结果与讨论

2.1 基体效应及谱线重叠干扰的校正

对主量元素采用消去烧失量的理论α系数法, 其余元素用经验系数法来校正元素间的基体效应，其中NiO、Rb₂O、SrO、Y₂O₃、ZrO₂、Nb₂O₅、Sm₂O₃、CeO₂、Tb₄O₇、Ho₂O₃、Er₂O₃、Lu₂O₃采用Rh Kα线康普顿散射强度作内标校正基体效应^[19]。采用帕纳科公司SuperQ3.0软件所用的综合数学校正公式(1)，通过回归，同时求出校准曲线的基体校正系数和谱线重叠干扰校正系数。

$ \begin{align} &{{C}_{\text{i}}}=\text{ }{{D}_{\text{i}}}-\sum {{L}_{\text{im}}}{{Z}_{\text{m}}}+{{E}_{\text{i}}}{{R}_{\text{i}}}(1+\sum\limits_{j\ne 1}^{N}{{{\alpha }_{\text{ij}}}\cdot {{Z}_{\text{j}}}+} \\ &\ \ \ \ \ \sum\limits_{j=1}^{N}{\frac{{{\beta }_{\text{ij}}}}{1+{{\delta }_{\text{ij}}}\cdot {{C}_{\text{j}}}}\cdot {{Z}_{\text{j}}}+\sum\limits_{j=1}^{N}{\sum\limits_{k=1}^{N}{{{\gamma }_{\text{ij}}}\cdot {{Z}_{\text{j}}}\cdot {{Z}_{\text{k}}}}})} \\ \end{align} $

式中：C_i为校准样品中分析元素i的含量(在未知样品分析中，C_i为基体校正后分析元素i的含量；D_i为分析元素i的校准曲线的截距；L_im为干扰元素m对分析元素i的谱线重叠干扰校正系数；Z_m为干扰元素m的含量或计数率；E_i为分析元素i校准曲线的斜率；R_i为分析元素i的计数率(或与内标线的强度比值)；Z_j、Z_k为共存元素的含量；C_j为共存元素j的含量；N为共存元素的数目；α、β、δ、γ为校正基体效应的因子。

根据快速扫描的结果，对有谱线重叠干扰的元素进行谱线重叠干扰校正，表 4列出了各稀土元素所校正的元素。

表 4 稀土元素的重叠谱线和影响元素

Table 4. Overlapping spectral lines and influencing elements of rare earth elements

待测元素	重叠谱线	校正基体元素
Y	Rb Kβ₁	Al，Si，Ba，Sr，Ni，Cr，Fe，Ca
La	Cs Lβ₁	Si，Fe，Nd
Nd	Ce Lβ₁	La，Sm，Al
Ce	Ba Lβ₂	-
Sm	Ce Lβ₂	-
Tb	Sm Lβ₁	La，Ce
Ho	Gd Lβ₁	Er，Yb
Er	Tb Lβ₁，Co Kα	La，Ce，Fe
Yb	Ni Kα	Y
Lu	Dy Lβ₂，Ni Kβ₁	La
Pr	La Lβ₁	La，Ce
Eu	-	La，Ce
Gd	Ce Lγ₁	La，Nd，Dy
P	Y Lβ₁	-

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2.2 方法检出限

按照检出限的公式计算出各元素的检出限：

$ \text{LOD}=\frac{3\sqrt{2}}{m}\sqrt{\frac{{{I}_{\text{b}}}}{t}} $

式中：m为计数率；I_b为背景计数率；t为峰值及背景的测量时间。

采用较低的标准物质重复测定12次计算的检出限结果见表 5。因本方法考虑测定的是稀土矿化类样品中的主量元素，而稀土元素检出限均在60 μg/g以下，因此对于高含量稀土元素能够满足定量分析要求。

表 5 分析元素的检出限

Table 5. Detection limits of elements

元素	方法检出限 (μg/g)
Na₂O	56.44
MgO	44.34
Al₂O₃	15.82
SiO₂	96.03
P₂O₅	18.59
K₂O	25.36
CaO	30.37
TiO₂	20.04
MnO	8.32
Fe₂O₃	6.69
Y₂O₃	4.52
La₂O₃	42.6
Nd₂O₃	52.85
Sm₂O₃	42.74
CeO₂	38.11
Tb₄O₇	44.83
Dy₂O₃	39.23
Ho₂O₃	8.86
Er₂O₃	27.19
Yb₂O₃	30.10
Lu₂O₃	13.41
Pr₆O₁₁	58.19
Eu₂O₃	6.14
Gd₂O₃	29.25

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2.3 方法精密度和准确度

按照所建立的方法对国家标准物质GBW07188和人工标准样品HC-XT-8分别重复制作13个样片，以表 1所选测量条件测定，计算的相对标准偏差(RSD)和相对误差等测量结果列于表 6，其中绝大多数主量元素的RSD均小于1.5%，稀土元素的RSD在7%以下，个别含量较低元素的精密度较差，例如HC-XT-8号样品的CaO标准值为0.026%，测定平均值为0.021%，RSD为16.3%。而对于其他高含量CaO样品能够实现准确定量，例如GBW07188的CaO标准值为0.29，测定平均值同样为0.29，RSD为1.4%。对于Tb₄O₇、Lu₂O₃、Pr₆O₁₁等存在相同情况。表 6中的低含量结果仅作为参考数据，在此不作讨论。

表 6 方法准确度和精密度

Table 6. Accuracy and precision tests of the method

元素	GBW07188				HC-XT-8
元素	测定平均值 (%)	标准值 (%)	相对误差 (%)	RSD (%)	测定平均值 (%)	标准值 (%)	相对误差 (%)	RSD (%)
Na₂O	0.62	0.66	5.30	2.35	0.121	0.156	3.54	5.45
MgO	0.13	0.11	11.82	4.07	0.074	0.076	25.0	4.37
Al₂O₃	13.8	14.26	2.52	0.27	14.51	14.47	2.14	0.213
SiO₂	66.8	66.9	0.01	0.19	73.5	73.4	0.15	0.17
K₂O	5.56	5.52	1.09	0.32	4.861	4.9	0.86	0.27
CaO	0.29	0.29	0.69	1.40	0.021	0.026	2.80	16.3
TiO₂	0.18	0.17	4.12	1.09	0.034	0.022	3.59	7.07
MnO	0.05	0.052	7.69	1.40	0.017	0.017	7.84	2.89
Fe₂O₃	2.28	2.24	2.05	0.30	1.13	1.13	1.90	0.14
Y₂O₃	2.14	2.16	0.93	0.71	0.054	0.056	1.78	0.98
La₂O₃	0.21	0.23	7.83	1.64	0.768	0.771	8.85	0.49
Nd₂O₃	0.41	0.4	2.50	0.88	0.003	0.003	5.57	69.5
Sm₂O₃^*	2006	2000	0.05	2.92	30	15.5	3.40	34.7
CeO₂	0.0619	0.053	26.42	5.39	0.728	0.771	2.26	2.30
Tb₄O₇^*	652	550	16.55	6.94	7.93	8.07	24.17	46.2
Dy₂O₃^*	3645	3700	2.38	0.69	未检出	55.4	6.64	-
Ho₂O₃^*	655	640	5.16	2.05	10.8	11.8	7.30	26.9
Er₂O₃^*	1989	2000	1.95	1.94	25.45	35.8	13.71	38.8
Lu₂O₃^*	306	300	5.60	4.13	2.57	5.4	1.02	48.1
Pr₆O₁₁^*	863	890	8.58	5.40	99.5	6.2	18.49	55.2
Yb₂O₃^*	2063	2100	2.72	0.79	13.55	36	8.95	33.0
Gd₂O₃^*	2536	2500	0.80	1.16	111.9	31.9	7.47	13.4
加和	99.8	-	-	0.12	99.6	-	-	0.14
注：标记“*”的元素含量单位为μg/g。

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2.4 全分析加和结果

以本文所建立的方法测量6个国家一级稀土标准物质、8个人工标准样品及8个未知的稀土样品，分析结果列于表 7，样品中主量元素、稀土元素和烧失量的加和结果均在99.41%~100.63%之间，所建分析方法能够满足全分析加和的要求，符合DZ/T0130—2006《地质矿产实验室测试质量管理规范》规定的一级标准。

表 7 全分析加和结果

Table 7. Analytical results of sam additivity

标准物质和样品编号	烧失量	主量元素和稀土元素测定值(%)	加和 (%)
GBW07187	5.42	94.51	99.93
GBW07188	5.53	94.36	99.89
GBW07158	6.73	93.00	99.73
GBW07159	3.70	96.39	100.09
GBW07160	3.77	96.08	99.85
GBW07161	6.80	92.61	99.41
HC-XT-1	3.19	96.58	99.77
HC-XT-2	3.36	96.18	99.55
HC-XT-3	5.00	94.90	99.90
HC-XT-4	6.42	93.21	99.63
HC-XT-5	5.35	94.52	99.87
HC-XT-6	5.43	94.70	100.13
HC-XT-7	6.59	93.00	99.59
HC-XT-8	3.64	95.93	99.57
GX-TC-F2	7.48	93.15	100.63
GX-TC-F4	5.38	94.76	100.14
GX-DB-F1	5.85	94.27	100.12
GX-DB-F2	6.02	94.59	100.61
GX-DB-F3	3.55	96.55	100.10
GX-DB-F4	3.57	96.29	99.86
GX-DB-F5	3.65	96.53	100.18
XF-WX-F3	7.13	93.28	100.41

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3. 结论

通过配制人工标准样品，解决了现有国家标准物质不能满足稀土矿样品等复杂类型样品中主量元素和稀土元素的定量问题。通过加入高纯氧化镧、氧化铈和氧化钇与碳酸盐标准样品混合，配制人工标准样品扩大了La、Ce和Y的定量范围。对稀土标准物质、人工标准样品和未知稀土样品进行反测，测定结果未采用归一化处理，元素的精密度和全分析加和结果都比较理想。本方法有效地扩大了XRF方法的适用范围。

图 1 文献报道的自然界Yb同位素组成(数据见表 1)

(a) ¹⁷⁶Yb/¹⁷¹Yb-¹⁷²Yb/¹⁷¹Yb; (b) ¹⁷⁶Yb/¹⁷¹Yb-¹⁷³Yb/¹⁷¹Yb; (c) ¹⁷⁶Yb/¹⁷²Yb-¹⁷²Yb/¹⁷¹Yb; (d) ¹⁷⁶Yb/¹⁷²Yb-¹⁷³Yb/¹⁷²Yb; (e) ¹⁷⁶Yb/¹⁷³Yb-¹⁷³Yb/¹⁷¹Yb; (f) ¹⁷⁶Yb/¹⁷³Yb-¹⁷³Yb/¹⁷²Yb。

Figure 1. Natural Yb isotopic compositions reported in references (The data are shown in Table 1)

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图 2 (a) 主要富铪矿物标样¹⁷⁶Hf/¹⁷⁷Hf-年龄相关图；(b)主要富铪矿物标样¹⁷⁶Yb/¹⁷⁷Hf-¹⁷⁶Lu/¹⁷⁷Hf相关图(数据来源见表 2)

Figure 2. (a) Plot of ¹⁷⁶Hf/¹⁷⁷Hf vs. age for Hf-rich mineral standards; (b) Plot of ¹⁷⁶Yb/¹⁷⁷Hf vs. ¹⁷⁶Lu/¹⁷⁷Hf for Hf-rich mineral standards (The data is from Table 2)

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表 1 不同文献报道的自然界Yb-Lu同位素组成

Table 1 Natural Yb and Lu isotopic compositions reported in different references

测量方式	¹⁷²Yb/¹⁷¹Yb	¹⁷³Yb/¹⁷¹Yb	¹⁷⁴Yb/¹⁷¹Yb	¹⁷⁶Yb/¹⁷¹Yb	¹⁷⁶Yb/¹⁷²Yb	¹⁷⁶Yb/¹⁷³Yb	¹⁷³Yb/¹⁷²Yb	¹⁷⁴Yb/¹⁷²Yb	¹⁷⁶Lu/¹⁷⁵Lu	文献来源
TIMS	1.526374	1.124778	2.216312	0.885860	0.580369	0.787586	0.736896	1.452011	-	[67]
TIMS+MC-ICPMS	1.526400	1.124800	2.216300	0.885900	0.580385	0.787607	0.736897	1.451979	0.02656	[6]
TIMS	1.532075	1.132685	2.242466	0.901821	0.588627	0.796180	0.739314	1.463679	0.02655	[61]
MC-ICPMS	1.532227	1.132685	2.242716	0.901864	0.588597	0.796218	0.739241	1.463697	-	[61]
MC-ICPMS	1.530570	1.130172	2.235486	0.897145	0.586151	0.793813	0.738400	1.460558	-	[66]
TIMS	-	-	-	-	-	0.795200	-	-	0.02656	[68]
TIMS	1.525914	1.123456	2.215594	0.884110	0.579397	0.786956	0.736251	1.451979	0.02645	[63]
MC-ICPMS	1.526049	1.123575	2.215790	0.884081	0.579327	0.786847	0.736264	1.451979	0.02645	[63]
TIMS	1.529607	1.129197	2.232678	0.895504	0.585447	0.793045	0.738227	1.459642	0.02655	[65]
TIMS	1.531736	1.132338	2.241970	0.901691	0.588673	0.796310	0.739251	1.463679	0.02655	[65]
TIMS	1.532105	1.132554	2.242509	0.901976	0.588717	0.796409	0.739215	1.463679	-	[69]
MC-ICPMS	1.530245	1.131999	2.238963	0.900121	0.588220	0.795161	0.739750	1.463140	-	[70]
MC-ICPMS	-	-	-	-	0.587150	-	-	1.461820	-	[62]
MC-ICPMS	-	1.132685	-	-	-	0.796390	-	-	-	[71]
注：“-”代表无数据。

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表 2 主要富铪矿物标样的REE-Hf同位素组成特征

Table 2 REE-Hf isotopic compositions of Hf-rich mineral standards

标准溶液	年龄(Ma)	年龄类型	¹⁶⁰Gd/¹⁷⁷Hf	¹⁶¹Dy/¹⁷⁷Hf	¹⁷⁶Yb/¹⁷⁷Hf	¹⁷⁶Lu/¹⁷⁷Hf	¹⁷⁶Hf/¹⁷⁷Hf	Hf (μg/g)	σ	参考文献
JMC475	-	-	-	-	-	-	0.282160	-	-	[4, 83-84]

锆石	年龄(Ma)	年龄类型	¹⁶⁰Gd/¹⁷⁷Hf	¹⁶¹Dy/¹⁷⁷Hf	¹⁷⁶Yb/¹⁷⁷Hf	¹⁷⁶Lu/¹⁷⁷Hf	¹⁷⁶Hf/¹⁷⁷Hf	Hf (μg/g)	σ	参考文献
Zr 2-1	0	-	0.000001	0.000005	0.000002	0.000000	0.282209±9	6105	330	[85]
Zr 3-1	0	-	0.000001	0.000006	0.001997	0.000504	0.282213±8	6819	382	[85]
Zr 3-2	0	-	0.000001	0.000005	0.002283	0.000568	0.282210±10	7598	304	[85]
Zr 4-1	0	-	0.000012	0.000003	0.001426	0.000356	0.282230±7	10011	300	[85]
Zr 4-2	0	-	0.000010	0.000004	0.002033	0.000524	0.282234±8	8648	796	[85]
MUNZirc 0	0	-	-	-	0.000130±65	0.000007±4	0.282135±7	-	-	[58]
MUNZirc 1	0	-	0.000534	0.004097	0.029±13	0.00147±67	0.282135±7	8933	-	[58]
MUNZirc 2	0	-	0.000282	0.002999	0.078±37	0.0029±12	0.282135±7	10415	-	[58]
MUNZirc 3	0	-	0.001090	0.010273	0.109±29	0.0044±15	0.282135±7	9232	751	[58]
MUNZirc 4	0	-	0.005968	0.037853	0.321±64	0.0127±24	0.282135±7	11790	601	[58]
FM0411	1.2±0.1^L	²⁰⁶Pb/²³⁸U	0.0006	0.0027	0.0058±13	0.00017±2	0.282983±4	9323	422	[20, 86-87]
61.308A	2.488±0.004	²⁰⁶Pb/²³⁸U	-	-	0.030697	0.00186	0.282977±14	5780	-	[88]
61.308B	2.508±0.002	²⁰⁶Pb/²³⁸U	-	-	0.030772	0.00228	0.282977±6	5537	-	[88]
Penglai	4.4±0.1	²⁰⁶Pb/²³⁸U	0.0019	0.0059	0.0140±80	0.00038±20	0.282906±10	5152	355	[86, 89-90]
FCT	28.402±0.023	²⁰⁶Pb/²³⁸U	0.0036	0.0109	0.055±11	0.00210±43	0.282538±16	10773	1055	[91-92]
SK10-2	32.10±0.49^L	²⁰⁶Pb/²³⁸U	-	-	-	-	0.282752±53	-	-	[44, 93-94]
GHR1	48.106±0.023	²⁰⁶Pb/²³⁸U	-	-	0.048±30	0.0019±12	0.283050±17	-	-	[95]
Monastery	90.1±0.5	²⁰⁶Pb/²³⁸U	-	-	0.00061±16	0.000009	0.282738±8	-	-	[45, 96-99]
KIM-5	90±3^S	²⁰⁶Pb/²³⁸U	0.0001	0.0004	0.000430	0.000015±4	0.282660±24	9114	192	[100-102]
Jilin	117.63±0.04	²⁰⁶Pb/²³⁸U	0.0054	0.0140	0.0310±14	0.00082±35	0.282926±14	9135	510	[103]
Qinghu	159.38±0.12	²⁰⁶Pb/²³⁸U	0.0019	0.0063	0.026±13	0.00068±21	0.283002±4	11750	802	[104-105]
LV-11	~290	²⁰⁶Pb/²³⁸U	-	-	0.166±11	0.0026±2	0.282837±28	-	-	[106]
Plesovice	337.13±0.37	²⁰⁶Pb/²³⁸U	0.0018	0.0061	0.005107	0.000125	0.282482±12	11167	-	[98-99, 107]
TEMORA-1	416.75±0.24	²⁰⁶Pb/²³⁸U	0.0039	0.0173	0.032±15	0.00110±30	0.282685±11	7801	-	[20, 38, 51, 108-110]
TEMORA-2	418.37±0.14 416.78±0.33	²⁰⁶Pb/²³⁸U	0.0020	0.0078	0.035±14	0.00109	0.282686±8	9362	239	[97-98, 109, 111-112]
R33	419.26±0.39 420.53±0.16	²⁰⁶Pb/²³⁸U	0.0047	0.0184	0.070±29	0.001990±87	0.282764±14	9764	1373	[50-51, 98, 109, 111]
M127	524.36±0.16	²⁰⁶Pb/²³⁸U	0.0017	0.0060	0.0177±14	0.000654±64	0.282396±4	12400	500	[113]
GZ7	530.26±0.05	²⁰⁶Pb/²³⁸U	0.0020	0.0059	0.012528	0.00049	0.281666±4	10060	290	[114]
SA01	535.08±0.32	²⁰⁶Pb/²³⁸U	0.0031	0.0055	0.0127±87	0.00045±28	0.282293±7	9797	563	[115]
SA02	535.10±0.24	²⁰⁶Pb/²³⁸U	0.0148	0.0205	0.0203±62	0.00064±17	0.282287±16	8976	507	[116]
GZ8	543.92±0.06	²⁰⁶Pb/²³⁸U	0.0010	0.0036	0.006325	0.00024	0.281662±5	11600	240	[114]
BB12	557.4±6.8	²⁰⁶Pb/²³⁸U	0.0005	0.0011	0.007068	0.000062	0.281677±11	6177	-	[117]
BR266 Z6266	559.0±0.2 559.27±0.11	²⁰⁶Pb/²³⁸U	0.0007	0.0025	0.004910	0.000217	0.281630±10	8778	258	[97, 118-121]
BB17	559.2±6.0	²⁰⁶Pb/²³⁸U	0.0013	0.0032	0.010624	0.000141	0.281677±6	8085.5	-	[117]
BB9	560.2±4.7	²⁰⁶Pb/²³⁸U	0.0005	0.0011	0.006797	0.000052	0.281675±14	6008	-	[117]
M257	561.3±0.3	²⁰⁶Pb/²³⁸U	0.0005	0.0013	0.002986	0.000096	0.281518±11 0.281544±18	10610	-	[35, 49, 110, 122]
BB16	562±3^L	²⁰⁶Pb/²³⁸U	0.0002	0.0006	0.00134±47	0.000050±17	0.281669±12	8807	-	[123-124]
CZ3	563.9±1.3	²⁰⁶Pb/²³⁸U	0.0001	0.0004	0.00098±1	0.000034±1	0.281732±7	12980	250	[20, 34, 121, 125-126]
Peixe	564±4	²⁰⁶Pb/²³⁸U	0.0016	0.0069	0.022229	0.000835	0.281944±29	4958	201	[50, 127-128]
Tanz	566.16±0.78	²⁰⁶Pb/²³⁸U	-	-	-	-	0.281820±7	-	-	[129]
SL7	569±3^S	²⁰⁶Pb/²³⁸U	-	-	-	-	0.281620±30	-	-	[13]
LKZ-1	570.0±2.5	²⁰⁶Pb/²³⁸U	0.0003	0.0011	0.00358±35	0.000104±1	0.281794±16	7740	310	[130]
GJ-1	601.86±0.37	²⁰⁶Pb/²³⁸U	0.0013	0.0033	0.00590±42	0.000238±5	0.282000±5	6681	57	[51, 131-134]
Mud tank	731.65±0.49	²⁰⁶Pb/²³⁸U	0.0011	0.0034	0.003204	0.000093	0.282507±6	11800	-	[97-98, 100, 132, 135]
WJS810	816.88±0.49	²⁰⁶Pb/²³⁸U	-	-	0.017655	0.000779	0.282534±6	9671	-	[136]
91500	1065.4±0.3 1066.4±0.3 1066.01±0.61	²⁰⁷Pb/²⁰⁶Pb	0.0005	0.0023	0.00739±45	0.00031±14	0.282308±6	5900	300	[20, 38, 51, 88, 119, 132, 137-138]
FC-1 AS3 AS57	1099±0.6 1099.1±0.5 1098.6±0.3 1098.47±0.16 1098.70±0.16 1099.96±0.58	²⁰⁷Pb/²⁰⁶Pb	0.0054	0.0201	0.0450±19	0.001262	0.282184±16	11031	1222	[97-99, 111, 119, 139-144]
CN92-1UQ-Z1	1142.8±0.8	²⁰⁷Pb/²⁰⁶Pb	-	-	0.020±10	0.00080±12	0.282172±16	-	-	[20, 145]
LH94-15	1830.3±1.9	²⁰⁷Pb/²⁰⁶Pb	-	-	-	-	0.281730±6	-	-	[146-147]
QGNG	1851.6±0.6 1851.5±0.3	²⁰⁷Pb/²⁰⁶Pb	-	-	0.0181±48	0.000731	0.281612±4	-	-	[51, 97-99, 119, 148]
Phalaborwa	2052.2±0.8	²⁰⁷Pb/²⁰⁶Pb	-	-	0.014±11	0.0004±3	0.281234±11	-	-	[20, 149]
KV01 EKC02-51	3227.2±0.2	²⁰⁷Pb/²⁰⁶Pb	0.0019	0.0066	0.0149±42	0.00068±17	0.280810±13	10410	675	[119, 150]
OG1	3465.4±0.6 3466.09±0.33	²⁰⁷Pb/²⁰⁶Pb	0.0037	0.0096	0.033±13	0.00119±26	0.280633±34	9346	641	[99, 151-153]

斜锆石	年龄(Ma)	年龄类型	¹⁶⁰Gd/¹⁷⁷Hf	¹⁶¹Dy/¹⁷⁷Hf	¹⁷⁶Yb/¹⁷⁷Hf	¹⁷⁶Lu/¹⁷⁷Hf	¹⁷⁶Hf/¹⁷⁷Hf	Hf (μg/g)	σ	参考文献
SK10-2	32.9±0.5^S	²⁰⁶Pb/²³⁸U	-	-	0.0063±13 0.0206±95	0.00023±4	0.282739±13	-	-	[20, 64, 154]
Kovdor	378.54±0.23 378.5±1.4	²⁰⁶Pb/²³⁸U	0.0003	0.0005	0.000772	0.000025	0.282767±5	7806	319	[64, 155-157]
OG-1	411.91±0.25	²⁰⁶Pb/²³⁸U	-	-	0.0036±13	0.000067±11	0.282694±7	-	-	[64]
Karlshamn	954.2±1.1	²⁰⁷Pb/²⁰⁶Pb	-	-	-	0.000113	0.282228±5	-	-	[1]
FC-1 FC-4b	1101.41±0.50 1099.6±1.5	²⁰⁷Pb/²⁰⁶Pb	-	-	0.0073±23	0.000109±28	0.282167±5	-	-	[64, 144, 156]
SA003	1256.2±1.4	²⁰⁷Pb/²⁰⁶Pb	-	-	0.049±17	0.00067±14	0.282167±5	-	-	[64]
Sorkka	1256.2±1.4	²⁰⁷Pb/²⁰⁶Pb	-	-	0.056±36	0.00066	0.282149±10	-	-	[1, 64]
Phalaborwa	2059.60±0.35	²⁰⁷Pb/²⁰⁶Pb	0.0002	0.0002	0.000078±33 0.000102±12	0.0000027±8 0.00000467±1 0.0000033±6	0.281229±11 0.281206±19 0.281187±14	13224	450	[2, 20, 158]

钛锆钍矿	年龄(Ma)	年龄类型	¹⁶⁰Gd/¹⁷⁷Hf	¹⁶¹Dy/¹⁷⁷Hf	¹⁷⁶Yb/¹⁷⁷Hf	¹⁷⁶Lu/¹⁷⁷Hf	¹⁷⁶Hf/¹⁷⁷Hf	Hf (μg/g)	σ	参考文献
Phala-ZrkA	1937±32^S	²⁰⁷Pb/²⁰⁶Pb	0.5824	0.3145	0.024362	0.000424±9	0.281296±5	4364	-	[159]

异性石	年龄(Ma)	年龄类型	¹⁶⁰Gd/¹⁷⁷Hf	¹⁶¹Dy/¹⁷⁷Hf	¹⁷⁶Yb/¹⁷⁷Hf	¹⁷⁶Lu/¹⁷⁷Hf	¹⁷⁶Hf/¹⁷⁷Hf	Hf (μg/g)	σ	参考文献
LV01	376±6^L	²⁰⁶Pb/²³⁸U	-	-	0.092430	0.00277	0.282761±18	2986	-	[160]

金红石	年龄(Ma)	年龄类型	¹⁶⁰Gd/¹⁷⁷Hf	¹⁶¹Dy/¹⁷⁷Hf	¹⁷⁶Yb/¹⁷⁷Hf	¹⁷⁶Lu/¹⁷⁷Hf	¹⁷⁶Hf/¹⁷⁷Hf	Hf (μg/g)	σ	参考文献
SR-1	0	-	-	-	-	-	0.281879±8	42500	710	[161]
SR-2	0	-	-	-	-	-	0.281888±7	3990	280	[161]
SR-2B	0	-	-	-	-	-	0.281874±9	2790	81	[161]
SR-3	0	-	-	-	-	-	0.281877±23	388	45	[161]
SR-3A	0	-	-	-	-	-	0.281882±26	416	45	[161]
R19	489.4±3.3	²⁰⁶Pb/²³⁸U	-	-	-	0.002089	0.282163±17	8.645	-	[162-163]
JDX	509±8^S	²⁰⁶Pb/²³⁸U	-	-	0.00020±15	0.000018±4	0.281795±15	50.1	0.7	[164-165]
R10/R10b	1090±5 1089.23±0.96	²⁰⁷Pb/²⁰⁶Pb	-	-	0.00038±48	0.000026±81	0.282178±12	38.8	1.5	[162, 165-166]
Sugluk-4	1720.8±4.7	²⁰⁷Pb/²⁰⁶Pb	-	-	0.00008±39	0.000003±16	0.281172±107	51.3	9.3	[165-166]
RMJG	1751.5±4.3	²⁰⁷Pb/²⁰⁶Pb	-	-	0.000017	0.000001	0.281652±6	103	17	[167]
PCA-S207	1865.0±7.5	²⁰⁷Pb/²⁰⁶Pb	-	-	0.0006±17	0.000019±49	0.281246±146	37	13	[165-166]
Diss	-	-	-	-	-	-	0.283258±17	5.081	0.049	[162]
R1	-	-	-	-	-	0.000013	0.283097±8	49	9	[161]

铌铁矿族矿物	年龄(Ma)	年龄类型	¹⁶⁰Gd/¹⁷⁷Hf	¹⁶¹Dy/¹⁷⁷Hf	¹⁷⁶Yb/¹⁷⁷Hf	¹⁷⁶Lu/¹⁷⁷Hf	¹⁷⁶Hf/¹⁷⁷Hf	Hf (μg/g)	σ	参考文献
713-79	218±2^L	²⁰⁶Pb/²³⁸U	-	-	0.000017	0.000001	0.282749±28	712	-	[74, 168]
NP-2	380.3±2.4	²⁰⁶Pb/²³⁸U	-	-	0.005372	0.000239	0.282169±32	211	-	[74, 169]
Coltan139	505.4±1.0	²⁰⁶Pb/²³⁸U	-	-	0.147949	0.003503	0.281991±3	454	-	[74, 170]
U-3	966±12^L	²⁰⁶Pb/²³⁸U	-	-	0.000040	0.000002	0.281703±26	1430	-	[74]
U-1	971±12^L	²⁰⁶Pb/²³⁸U	-	-	0.000725	0.000021	0.281845±38	469	-	[74]
注：上标L代表LA-ICPMS，上标S代表SIMS，“-”代表暂无数据。

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1. 实验部分
1.1 仪器和测量条件
1.2 主要试剂
1.3 样片制备
1.4 样品配制及制备标准曲线的范围
2. 结果与讨论
2.1 基体效应及谱线重叠干扰的校正
2.2 方法检出限
2.3 方法精密度和准确度
2.4 全分析加和结果
3. 结论

矿物微区Lu-Hf同位素分析技术研究进展

作者简介: 王浩，博士，副研究员，主要从事同位素地球化学与前寒武纪地质学研究。E-mail: wanghao@mail.iggcas.ac.cn

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