碱熔-电感耦合等离子体质谱法测定铍矿石中的铍和锡

常学东; 杜晶; 孙文明; 徐国强; 阿米娜·胡吉; 董瑞瑞

doi:10.15898/j.ykcs.202403310073

碱熔-电感耦合等离子体质谱法测定铍矿石中的铍和锡

1.
中国地质调查局乌鲁木齐自然资源综合调查中心，新疆乌鲁木齐 830057

基金项目: 中国地质调查局地质调查项目“战略性矿产勘查岩矿测试技术支撑（乌鲁木齐中心）”(DD20243023)，“康西瓦一带稀有金属矿重点调查区调查评价”(DD20242747)

详细信息

作者简介: 常学东，高级工程师，主要从事地球化学样品分析测试方法研究。E-mail：155054377@qq.com

通讯作者: 杜晶，高级工程师，主要从事地球化学样品分析测试方法研究。E-mail：584409782@qq.com。

中图分类号: O657.63

收稿日期: 2024-03-31

修回日期: 2024-07-10

录用日期: 2024-07-17

刊出日期: 2024-09-30

Determination of Beryllium and Tin in Beryllium Ore by Inductively Coupled Plasma-Mass Spectrometry with Alkali Fusion

1.
Urumqi Comprehensive Survey Center of Natural Resources, China Geological Survey, Urumqi 830057, China

More Information

Corresponding author: DU Jing, 584409782@qq.com

Received Date: 31 March 2024

Revised Date: 10 July 2024

Accepted Date: 17 July 2024

Publish Date: 30 September 2024

摘要

摘要:
稀有金属矿物组成复杂，且矿物成分多样化，现有质谱方法对铍的测定以地质样品中或矿石样品中的低含量铍分析为主，也很少应用于分析铍矿石中伴生的难溶锡元素。本文以新疆大红柳滩高品位铍矿石并伴生较高含量锡元素的样品为研究对象，建立了铍矿石中难溶元素铍和锡同时测定的方法。利用高温熔融态过氧化钠强的复分解能力，将矿物中的坚固晶格破坏，使目标物转换为易溶盐被提取，通过10倍稀释降低样品基体盐分含量，保证长期测量的稳定性RSD低于5%，并对校准曲线进行基体匹配，以电感耦合等离子体质谱(ICP-MS)测定，铍和锡在5～2000ng/mL浓度范围内线性关系良好，相关系数均大于0.999，检出限为铍0.20μg/g、锡0.17μg/g；测量精密度高(RSD≤5%)，测量上限为氧化铍5.6%，锡2%。本文方法线性范围宽，适合各种高品位铍矿石中铍和锡的分析。将建立的方法应用于分析新疆大红柳滩高品位铍矿等多金属稀有金属矿，氧化铍含量达到0.85%、锡含量达到0.078%的样品测量精密度良好；还适用于分析铍矿石中其他稀有元素锂铷铯铌钽和稀土元素。
- 碱熔 /
- 铍矿石 /
- 铍 /
- 锡 /
- 电感耦合等离子体质谱法
Abstract:
Due to the complex composition of rare metal minerals and the diversity of mineral components, the existing mass spectrometry methods for the determination of beryllium mainly focus on the analysis of low content beryllium in geological samples or ore samples, and rarely study and analyze the associated insoluble tin element in beryllium ores. A method for simultaneous determination of insoluble elements beryllium and tin in beryllium ores with high grade beryllium ore and associated high tin content in Dahongliutan, Xinjiang was established. The strong complex decomposition ability of molten sodium peroxide at high temperature was used to destroy the solid crystal lattice in the mineral, so that the target object was converted into soluble salt and extracted. The salt content of the sample matrix was reduced by 10 times dilution to ensure the long-term measurement stability of RSD below 5%. The matrix matching of the calibration curve was performed and determined by inductively coupled plasma-mass spectrometry. The linear relationship between beryllium and tin was good in the concentration range of 5−2000ng/mL, and the correlation coefficients were greater than 0.999. The detection limits of beryllium and tin were 0.20μg/g and 0.17μg/g respectively. High measurement stability (RSD)≤5%, the upper limit of measurement of beryllium oxide was 5.6%, tin was 2%. Compared with the existing methods, this method has a wide linear range and is suitable for the analysis of beryllium and tin in various high grade beryllium ores. The established method was applied to polymetallic rare metals such as high-grade beryllium ore in Dahongliutan, Xinjiang, and it was found that the precision of the samples with beryllium oxide content above 0.85% and tin content above 0.078% was good. This method is also suitable for the determination of other rare elements such as lithium, rubidium, cesium, niobium, tantalum and rare earth in beryllium ores.
- alkali fusion /
- beryllium ore /
- beryllium /
- tin /
- inductively coupled plasma-mass spectrometry

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图 1 铍(a)和锡(b)测定的校准曲线

Figure 1.

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表 1 电感耦合等离子体质谱仪主要工作参数

Table 1. Main working parameters of ICP-MS instrument

工作参数	设定值	工作参数	设定值
等离子体气体流速	13L/min	测量模式	标准
辅助气流速	0.8L/min	测量间隔	0.2s
雾化器气体流速	0.84L/min	泵速	40r/min
分辨率模式	Normal	驻留时间	0.001s
测量方式	单点跳峰	扫描次数	50

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表 2 稀释倍数对铑内标信号的抑制程度对比

Table 2. Comparison of inhibition degree of Rh internal standard signal by different dilution ratios

稀释倍数	不同分析时间内标回收率(%)
稀释倍数	10min	20min	30min	40min	50min	60min
5.0倍	21.2	20.1	18.7	17.2	15.4	12.9
7.5倍	35.9	34.5	32.0	29.9	27.8	25.7
10倍	39.4	40.3	38.8	41.1	39.5	39.0
15倍	53.9	52.5	50.4	51.8	49.7	50.2
20倍	68.4	66.7	65.9	67.2	68.3	66.8

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表 3 连续高盐基体进样对铍和锡元素的测定准确度影响

Table 3. Effect of continuous high salt matrix injection on accuracy of Be and Sn determination

测量时间间隔	混合标准溶液校验点30ng/mL				混合标准溶液校验点800ng/mL
测量时间间隔	Be含量 (ng/mL)	相对误差 (%)	Sn含量 (ng/mL)	相对误差 (%)	Be含量 (ng/mL)	相对误差 (%)	Sn含量 (ng/mL)	相对误差 (%)
10min	29.3	−2.3	30.1	0.33	807	0.88	787	−1.6
20min	30.4	1.3	30.3	1.0	799	−0.13	793	−0.88
30min	31.2	4.0	30.0	0.0	791	−1.1	806	0.75
40min	29.7	−1.0	30.2	0.67	810	1.3	794	−0.75
50min	29.5	−1.7	31.0	3.3	819	2.4	791	−1.1
60min	30.8	2.7	31.2	4.0	809	1.1	790	−1.3
RSD（%）	2.54	‒	1.66	‒	1.20	‒	0.83	‒

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表 4 盐酸加入量对铍和锡检测结果的稳定性影响

Table 4. Effect of adding amount of hydrochloric acid on stability of Be and Sn determination

组分	测定项目	盐酸加入量
组分	测定项目	5.0mL	10.0mL	15.0mL	20.0mL	25.0mL
BeO	测定平均值(%)	0.84	0.87	0.86	0.85	0.86
BeO	RSD(%)	7.2	3.3	2.0	1.9	2.2
Sn	测定平均值(%)	0.078	0.079	0.079	0.078	0.077
Sn	RSD(%)	8.3	4.1	2.4	2.5	2.6
注：为符合标准物质中铍和锡的结果表示形式和矿石类样品实际工作中报出要求，本文对样品测定结果铍均以BeO、锡以单质形式展示。

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表 5 国家一级标准物质中铍和锡的测定结果误差

Table 5. Determination error of Be and Sn in national first-class standard materials

标准物质编号	BeO				Sn
标准物质编号	标准值（%）	测定值(%)	RSD（%）	相对误差（%）	标准值(%)	测定值(%)	RSD（%）	相对误差（%）
GBW07150	0.060±0.006	0.060	4.1	0.0	−	−	−	−
GBW07151	0.365±0.026	0.359	2.3	−2.6	−	−	−	−
GBW07152	0.018±0.001	0.019	4.7	5.6	0.0036	0.0034	4.9	−5.6
GBW07153	0.026±0.003	0.026	3.5	0.0	0.0097±0.0005	0.0093	4.4	−4.1
GBW07154	0.033±0.002	0.033	3.9	0.0	0.0052	0.0055	3.6	5.8
GBW07155	0.033（0.032～0.009）	0.035	4.0	6.1	0.0063	0.0066	4.1	4.8
GBW07311	0.0026±0.005	0.0025	4.8	−3.8	0.037±0.0068	0.037	3.8	0.0
GBW07282	−	−	−	−	1.27±0.001	1.22	1.3	−3.9
注：“−”表示没有定值；GBW07311中铍结果为单质。

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表 6 实际样品中氧化铍和锡的测定精密度

Table 6. Precision of BeO and Sn in actual samples

铍矿石实际样品编号	BeO		Sn
铍矿石实际样品编号	测定值 (%)	RSD (%)	测定值 (%)	RSD (%)
样品1	0.052	5.0	0.021	4.3
样品2	0.171	2.5	0.029	2.6
样品3	0.350	3.4	0.040	3.7
样品4	0.549	3.1	0.054	2.5
样品5	0.850	3.0	0.078	1.2

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表 7 国家一级标准物质中伴生的稀有金属测定准确度和精密度

Table 7. Determination accuracy and precision of associated rare metals in national first-class standard materials

元素	GBW07151				GBW07152
元素	标准值 (μg/g)	测定值 (μg/g)	RSD (%)	相对误差 (%)	标准值 (μg/g)	测定值 (μg/g)	RSD (%)	相对误差 (%)
Li₂O	−	−	−	−	0.46±0.01^*	0.47	0.7	2.17
Rb₂O₃	−	−	−	−	0.145±0.011^*	0.147	1.1	1.38
Cs₂O₃	−	−	−	−	0.037±0.003^*	0.038	2.3	2.70
Nb₂O₅	−	−	−	−	27.0±2.1	27.0	4.2	0.00
Ta₂O₅	−	−	−	−	49.4±4.7	46.6	5.1	−5.67
Y₂O₃	28.9±2.9	30.8	4.2	6.6	16.9±1.8	16.4	2.8	−2.96
La₂O₃	7.7±0.7	7.2	5.0	−6.5	5.1±0.5	5.4	5.5	5.88
CeO₂	14.8±1.4	14.4	4.7	−2.7	9.0±0.7	8.6	5.5	−4.44
Pr₆O₁₁	2.0±0.2	2.0	4.1	0.0	1.3±0.3	1.4	3.9	7.69
Nd₂O₃	7.6±0.7	7.8	5.4	2.6	5.0±0.6	5.1	4.1	2.00
Sm₂O₃	2.7±0.2	2.9	4.8	7.4	1.6±0.2	1.4	6.8	−12.50
Eu₂O₃	0.15	0.12	10.2	−20.0	0.14	0.12	13.2	−14.29
Gd₂O₃	3.8±0.4	4.1	5.2	7.9	2.1±0.3	2.3	5.7	9.52
Tb₄O₇	0.8±0.1	0.84	3.7	5.0	0.43±0.05	0.46	3.8	6.98
Dy₂O₃	4.6±0.5	4.9	1.9	6.5	2.5±0.3	2.5	3.3	0.00
Ho₂O₃	0.87±0.16	0.92	3.4	5.7	0.45±0.10	0.45	5.3	0.00
Er₂O₃	2.2±0.4	2.5	0.9	13.6	1.2±0.2	1.3	4.3	8.33
Tm₂O₃	0.36±0.06	0.36	3.9	0.0	0.18±0.03	0.19	6.8	5.56
Yb₂O₃	2.5±0.5	2.4	0.3	−4.0	1.3±0.03	1.4	2.2	7.69
Lu₂O₃	0.31±0.05	0.34	2.5	9.7	0.18±0.04	0.20	4.4	11.11
注：标注“*”数据单位为百分含量(%)。

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表 8 实际样品中伴生的稀有金属测定精密度

Table 8. Determination precision of associated rare metals in actual samples

铍矿石实际样品编号	Li₂O		Rb₂0₃		Cs₂O₃		Nb₂O₅		Ta₂O₅
铍矿石实际样品编号	测定值 (%)	RSD (%)	测定值 (%)	RSD (%)	测定值 (%)	RSD (%)	测定值 (μg/g)	RSD (%)	测定值 (μg/g)	RSD (%)
样品1	0.53	2.3	0.133	1.1	0.013	1.7	92.9	2.0	42.8	3.4
样品2	1.04	0.9	0.114	2.5	0.014	3.0	107	4.9	47.5	4.5
样品3	1.76	1.9	0.088	1.9	0.013	1.4	117	4.9	56.7	4.1
样品4	2.83	2.3	0.074	1.2	0.012	2	129	3.6	63.2	5.0
样品5	4.30	2.0	0.045	3.5	0.007	1.2	152	3.6	79.6	2.2

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