高压密闭消解-电感耦合等离子体质谱法测定和田玉中15种稀土元素

周安丽; 武志远; 宁海龙; 王东; 杨丽; 吕新明

doi:10.15898/j.cnki.11-2131/td.201907170106

高压密闭消解-电感耦合等离子体质谱法测定和田玉中15种稀土元素

1.
石河子大学化学化工学院, 新疆石河子 832003

2.
阿拉山口海关技术中心, 新疆阿拉山口 833418

3.
乌鲁木齐海关技术中心阿勒泰分中心, 新疆阿勒泰 836500

基金项目:
国家重点研发计划项目“国家质量基础的共性技术研究与应用”(2018YFF0215400)

详细信息

作者简介: 周安丽, 硕士研究生, 从事岩石矿产品分析检测。E-mail:zhouanli1210@163.com

通讯作者: 吕新明, 高级工程师, 从事岩石矿产品分析检测。E-mail:ciqlxm@163.com

中图分类号: O657.63

收稿日期: 2019-07-17

修回日期: 2019-09-04

录用日期: 2019-10-21

Determination of 15 Rare Earth Elements in Hetian Jade by Inductively Coupled Plasma-Mass Spectrometry with High-pressure Closed Digestion

1.
College of Chemistry and Chemical Engineering, Shihezi University, Shihezi 832003, China

2.
Alashankou Customs Technology Center, Alashankou 833418, China

3.
Altay Branch of Urumqi Customs Technical Center, Altay 836500, China

More Information

Corresponding author: Xin-ming LÜ, ciqlxm@163.com

Received Date: 17 July 2019

Revised Date: 04 September 2019

Accepted Date: 21 October 2019

摘要

摘要: 和田玉的稀土元素丰富，准确测定稀土元素含量对于揭示和田玉成矿物质来源、成矿流体的性质和矿床成因具有重要的意义。本文通过比较硝酸-氢氟酸、四硼酸锂-偏硼酸锂碱熔两种前处理方法，确定了使用硝酸-氢氟酸溶样，再采用电感耦合等离子体质谱法(ICP-MS)测定和田玉中钇镧铈镨钕钐铕钆铽镝钬铒铥镱镥15种稀土元素的含量。为降低基体效应，以¹⁰³Rh和⁴⁹In作内标补偿基体效应和校正灵敏度漂移，样品检出限为0.0008~0.0091μg/L，回收率为101.0%~120.0%，精密度(RSD)为0.55%~1.83%(n=11)。本方法的用酸量少，空白值低，应用于不同地区和田玉的分析，其稀土元素的配分模式特征为右倾型轻稀土富集，初步探讨的稀土元素丰度特征可为研究主产区宝玉石的矿床成因提供依据。
- 和田玉 /
- 稀土元素 /
- 硝酸-氢氟酸 /
- 酸溶 /
- 电感耦合等离子体质谱法
Abstract: BACKGROUNDThere are abundant rare earth elements in Hetian jade. The accurate determination of the content of rare earth elements is of great significance for revealing the source of ore-forming materials, the nature of ore-forming fluids and the genesis of the deposit. OBJECTIVESTo compare the different acid systems in microware digestion and investigate the elimination test of polyatomic interferences, so as to develop a method for the determination of REE in Hetian jade by inductively coupled plasma-mass spectrometry (ICP-MS) with microwave digestion. METHODSAfter comparing the efficiency of HNO₃-HF acid dissolution and Li₂B₄O₇-LiBO₂ fusion, the Hetian jade samples were digested by HNO₃-HF. Fifteen rare earth elements were determined by ICP-MS. ¹⁰³Rh and ⁴⁹In are used as internal isotopes to complement matrix effect and correct sensitivity drift, in order to reduce matrix effect. RESULTSThe detection limits of the method were 0.0008-0.0091μg/L, whereas the recoveries were 101.0%-120.0%. The relative standard deviation was 0.55%-1.83%(n=11). CONCLUSIONSThis method uses less acid and has a low blank value. It is applied to the analysis of Hetian jade in different regions. The distribution pattern of rare earth elements is characterized by right-inclined light rare earth enrichment, which provides constraints on the genesis of the jade deposit.
- Hetian jade /
- Trace elements /
- rare earth elements /
- inductively coupled plasma-mass spectrometry /

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图 1 和田玉稀土元素配分型式

Figure 1.

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表 1 ICP-MS仪器工作条件

Table 1. Working parameters of the ICP-MS instrument

工作参数	设定条件
功率	1100W
冷却气流量	18.0L/min
辅助气流量	1.2L/min
雾化气流量	0.93L/min
采样锥孔径	1.0mm
截取锥孔径	0.5mm
测定方式	跳峰
扫描次数	30
停留时间/通道	15ms
每个质量通道数	3
总采集时间	20s

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表 2 标准曲线及相关指标

Table 2. Standard curves and related indexes

稀土元素	回归方程	相关系数	方法检出限(μg/L)	浓度范围(μg/L)	RSD (%)	重复性实验(%)
⁸⁹Y	y=11273.6x+34.3358	0.9999	0.0008	0~10	0.68	1.32
¹³⁹La	y=21295.6x+34.3538	0.9999	0.0036	0~10	0.72	1.58
¹⁴⁰Ce	y=22152.2x+49.7987	0.9999	0.0078	0~10	0.78	0.61
¹⁴¹Pr	y=41075x+100.858	0.9999	0.0029	0~10	1.76	0.58
¹⁴²Nd	y=12737.1x+10.0332	0.9999	0.0010	0~10	1.83	0.72
¹⁵²Sm	y=14301.6x+48.3617	0.9999	0.0015	0~10	0.93	0.84
¹⁵³Eu	y=1.844771x+0.11593	0.9999	0.0027	0~10	0.72	0.79
¹⁵⁸Gd	y=1.471487x+0.19631	0.9998	0.0058	0~10	1.80	2.82
¹⁵⁹Tb	y=47088x+305.9453	0.9999	0.0022	0~10	1.72	3.98
¹⁶⁴Dy	y=13553.3x+106.294	0.9999	0.0091	0~10	0.62	0.99
¹⁶⁵Ho	y=46616.3x+243.263	0.9999	0.0014	0~10	0.61	0.41
¹⁶⁶ Er	y=15467.7x+83.3893	0.9999	0.0029	0~10	0.69	2.76
¹⁶⁹Tm	y=47700x+250.002	0.9999	0.0009	0~10	0.80	1.08
¹⁷⁴Yb	y=16328x+144.771	0.9999	0.0067	0~10	0.79	0.68
¹⁷⁵Lu	y=44003x+405.547	0.9998	0.0013	0~10	0.55	1.65

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表 3 稳定性和加标回收率试验结果

Table 3. Results of the stability and recovery tests

稀土元素	RSD (%)	加标量(μg/L)	初始值(μg/L)	检测值(μg/L)	回收率(%)
⁸⁹Y	2.05	0.010	0.007	0.018	110.0
¹³⁹La	1.56	0.2	0.141	0.344	101.5
¹⁴⁰Ce	0.76	0.4	0.380	0.785	101.3
¹⁴¹Pr	0.74	0.1	0.043	0.153	110.0
¹⁴²Nd	0.45	0.1	0.183	0.285	102.0
¹⁵²Sm	2.82	0.05	0.047	0.098	102.0
¹⁵³Eu	0.63	0.02	0.016	0.038	110.0
¹⁵⁸Gd	0.82	0.1	0.088	0.190	102.0
¹⁵⁹Tb	1.62	0.01	0.008	0.020	120.0
¹⁶⁴Dy	1.36	0.05	0.045	0.098	106.0
¹⁶⁵Ho	0.52	0.1	0.009	0.110	101.0
¹⁶⁶ Er	2.70	0.03	0.028	0.060	106.7
¹⁶⁹Tm	0.61	0.005	0.004	0.010	120.0
¹⁷⁴Yb	1.52	0.03	0.025	0.058	110.0
¹⁷⁵Lu	3.08	0.005	0.003	0.009	120.0

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表 4 不同地区和田玉的稀土元素含量测试结果

Table 4. Determination of rare earth elements in Hetian jade in different regions

样品编号	稀土元素测定值(μg/kg)
样品编号	Y	La	Ce	Pr	Nd	Sm	Eu	Gd	Tb	Dy	Ho	Er	Tm	Yb	Lu
RQ-1	0.007	0.141	0.308	0.041	0.180	0.041	0.014	0.081	0.008	0.046	0.009	0.026	0.004	0.022	0.003
RQ-2	0.006	0.143	0.326	0.042	0.185	0.043	0.014	0.086	0.008	0.049	0.010	0.028	0.004	0.023	0.004
QM-1	0.015	0.235	0.149	0.043	0.185	0.032	0.009	0.056	0.006	0.032	0.007	0.021	0.002	0.015	0.002
QM-2	0.195	0.220	0.198	0.044	0.187	0.033	0.009	0.062	0.006	0.034	0.007	0.023	0.003	0.019	0.003
YT-1	0.157	0.070	0.114	0.018	0.083	0.018	0.003	0.033	0.004	0.022	0.005	0.015	0.002	0.013	0.002
YT-2	0.010	0.107	0.244	0.033	0.152	0.036	0.006	0.074	0.007	0.045	0.010	0.032	0.004	0.028	0.004
YC-1	0.001	0.026	0.094	0.007	0.031	0.009	0.004	0.021	0.001	0.009	0.002	0.006	0.001	0.006	0.001
YC-2	0.137	0.107	0.260	0.028	0.111	0.021	0.005	0.050	0.003	0.020	0.004	0.015	0.002	0.015	0.003

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高压密闭消解-电感耦合等离子体质谱法测定和田玉中15种稀土元素

1. 石河子大学化学化工学院, 新疆 石河子 832003 2. 阿拉山口海关技术中心, 新疆 阿拉山口 833418 3. 乌鲁木齐海关技术中心阿勒泰分中心, 新疆 阿勒泰 836500

作者简介: 周安丽, 硕士研究生, 从事岩石矿产品分析检测。E-mail:zhouanli1210@163.com

通讯作者: 吕新明, 高级工程师, 从事岩石矿产品分析检测。E-mail:ciqlxm@163.com

Determination of 15 Rare Earth Elements in Hetian Jade by Inductively Coupled Plasma-Mass Spectrometry with High-pressure Closed Digestion

1. College of Chemistry and Chemical Engineering, Shihezi University, Shihezi 832003, China 2. Alashankou Customs Technology Center, Alashankou 833418, China 3. Altay Branch of Urumqi Customs Technical Center, Altay 836500, China

Corresponding author: Xin-ming LÜ, ciqlxm@163.com

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1.
石河子大学化学化工学院, 新疆石河子 832003

2.
阿拉山口海关技术中心, 新疆阿拉山口 833418

3.
乌鲁木齐海关技术中心阿勒泰分中心, 新疆阿勒泰 836500

1.
College of Chemistry and Chemical Engineering, Shihezi University, Shihezi 832003, China

2.
Alashankou Customs Technology Center, Alashankou 833418, China

3.
Altay Branch of Urumqi Customs Technical Center, Altay 836500, China