微波消解-电感耦合等离子体质谱法测定高岭土中10种微量元素

李丽君; 薛静

doi:10.15898/j.cnki.11-2131/td.202103240042

微波消解-电感耦合等离子体质谱法测定高岭土中10种微量元素

李丽君,
薛静^,

中国地质调查局沈阳地质调查中心, 自然资源部黑土地演化与生态效应重点实验室, 辽宁沈阳 110034

基金项目:
中国地质调查局地质调查项目“兴凯湖平原及松辽平原西部土地质量地球化学调查”（DD20190520）

详细信息

作者简介: 李丽君, 硕士, 高级工程师, 从事土壤、岩矿测试及地质矿产分析方法研究。E-mail: 475876904@qq.com

通讯作者: 薛静, 硕士, 高级工程师, 主要从事土壤、岩石矿物等无机元素分析方法研究。E-mail: may927@163.com

中图分类号: O657.63

收稿日期: 2021-03-24

修回日期: 2021-06-03

录用日期: 2021-07-02

刊出日期: 2022-01-28

Determination of 10 Trace Elements in Kaolin by ICP-MS with Microwave Digestion

LI Li-jun,
XUE Jing^,

Shenyang Centre of Geological Survey, China Geological Survey; Key Laboratory for Evolution and Ecological Effect in Black Soil, Ministry of Natural Resources, Shenyang 110032, China

More Information

Corresponding author: XUE Jing, may927@163.com

Received Date: 24 March 2021

Revised Date: 03 June 2021

Accepted Date: 02 July 2021

Publish Date: 28 January 2022

摘要

摘要:
高岭土作为重要的铝硅酸盐，其微量元素的含量决定着高岭土产品的性能指标。高岭土的三种国家标准物质成分GBW03121、GBW03122、GBW03122a中均未含有As、Sb等10种微量元素的标准值，在高岭土的检测中只能采用近似的岩石标准物质作为监控物质，对高岭土组分的准确分析有一定影响。本文通过微波消解技术，对比了硝酸-氢氟酸二酸及硝酸-氢氟酸-过氧化氢三酸溶样体系，讨论了微波消解的程序升温条件及消解时间等影响因素，并对电感耦合等离子体质谱法（ICP-MS）的干扰因素进行了探讨，建立了微波消解硝酸-氢氟酸-过氧化氢三酸溶样体系，ICP-MS法测定高岭土中As、Sb等10种微量元素的分析方法。方法检出限在0.01~0.09mg/kg之间，测定下限在0.03~0.30mg/kg之间。利用岩石标准物质直接验证了方法的准确度和精密度，元素回收率在90.9%~103.2%之间，相对标准偏差（RSD）在1.2%~5.8%之间。同时对方法的不确定度进行了综合评估，证实方法准确可靠。本方法酸类用量少，缩短了测定时间，减少了对环境及人体的影响，适用于高岭土样品中As、Sb等10种微量元素的批量分析，对高岭土国家标准物质成分中As、Sb等10种微量元素的标准值测定提供了参考。
- 高岭土 /
- 微量元素 /
- 硝酸-氢氟酸-过氧化氢酸溶 /
- 微波消解 /
- 电感耦合等离子体质谱法 /
- 动能歧视模式
Abstract: BACKGROUND
As an important aluminosilicate, trace element contents affect the performance of the product. The kaolin standard substances GBW03121, GBW03122, GBW03122a lack the recommended values of ten elements such as arsenic and antimony. Similar rock standard materials were used for monitoring the determination procedure, but the accurate results of the kaolin samples may be affected.
OBJECTIVES
To establish a method for accurate determination of 10 trace elements in kaolin sample such as arsenic and antimony.
METHODS
With microwave digestion technology, the nitrate-hydrofluoric acid system and nitrate-hydrofluoric-peroxide system were compared for the procedural heating conditions and dissolution time of microwave digestion. Interference factors of the inductively coupled plasma mass spectrum were also investigated.
RESULTS
The detection limits of 10 elements were 0.01-0.09mg/kg, and measurement limits were 0.03-0.30mg/kg. The accuracy and precision of the method were directly verified by using rock reference materials. The element recovery was between 90.9% and 103.2%, and the relative standard deviation (RSD) was between 1.2% and 5.8%. At the same time, a comprehensive evaluation of the uncertainty of the method was carried out, and the method was proved to be accurate and reliable.
CONCLUSIONS
This method has little acid dosage, shortens the measurement time, and reduces the damage on the environment and human, making it suitable for the batch analysis of 10 trace elements in kaolin samples. The method also provides a reference for the determination of the certified values of 10 trace elements such as As and Sb in the national standard material of kaolin.
- kaolin /
- trace elements /
- nitrate-hydrofluoric-peroxide acid dissolution /
- microwave digestion /
- inductively coupled plasma-mass spectrometry /
- kinetic energy discrimination model

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图 1 消解条件对元素回收率的影响

Figure 1.

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表 1 微波消解仪的工作参数

Table 1. Working parameters of microwave digestion apparatus

实验条件	步骤	功率(W)	升温时间(min)	温度(℃)	保持时间(min)
条件一(阶梯升温模式)	1	1600	3	100	3
	2	1600	7	150	3
	3	1600	5	170	3
	4	1600	5	190	15
条件二(阶梯升温模式)	1	1600	7	150	3
	2	1600	5	170	3
	3	1600	5	190	15
条件三(直接升温模式)	1	1600	5	190	15

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表 2 方法准确度和精密度(n=5)

Table 2. Accuracy and precision tests of the method (n=5)

标准物质编号	元素	标准值(mg/kg)	平均值(mg/kg)	相对误差(%)	回收率(%)	相对标准偏差(%)	相对误差允许限(%)
	As	6.27	6.26	-0.2	99.8	1.7	20.4
	Sb	0.15	0.14	-6.7	93.3	4.3	35.9
	Bi	0.37	0.35	-5.4	94.6	3.4	31.5
	Cd	0.07	0.064	-8.6	91.4	4.5	40.1
	Cr	3.6	3.7	2.8	102.8	2.2	22.2
GBW07109	Cu	11.8	11.7	-0.8	99.2	1.8	18.4
	Mo	0.26	0.251	-3.5	96.5	3.5	33.1
	Ni	1.75	1.73	-1.1	98.9	1.8	24.9
	Pb	196	195	-0.5	99.5	1.6	11.3
	Zn	112	111	-0.9	99.1	3.6	12.5
	As	5.96	6.021	1.0	101.0	1.2	20.5
	Sb	1.34	1.26	-6.0	94.0	4.8	25.9
	Bi	0.09	0.087	-3.3	96.7	2.3	38.7
	Cd	0.61	0.59	-3.3	96.7	2.8	29.2
	Cr	7.7	7.0	-9.1	90.9	5.8	19.7
GBW07110	Cu	9.1	9.01	-1.0	99.0	4.5	19.2
	Mo	0.95	0.98	3.2	103.2	4.2	27.3
	Ni	12.6	12.3	-2.4	97.6	4.0	18.2
	Pb	97.7	97.4	-0.3	99.7	1.9	12.8
	Zn	164	161	-1.8	98.2	2.5	11.7
	As	0.4	0.37	-7.5	92.5	3.9	31.1
	Sb	1.34	1.31	-2.2	97.8	2.9	25.9
	Bi	0.05	0.048	-4.0	96.0	2.7	42.1
	Cd	0.08	0.078	-2.5	97.5	3.7	39.3
	Cr	37.6	37.5	-0.3	99.7	2.9	15.2
GBW07111	Cu	8.8	8.74	-0.7	99.3	2.7	19.3
	Mo	0.47	0.45	-4.3	95.7	3.6	30.4
	Ni	24.4	24.14	-1.1	98.9	3.2	16.3
	Pb	19.8	18.97	-4.2	95.8	3.0	16.9
	Zn	85.4	85.0	-0.4	99.6	4.9	13.1
	As	0.7	0.72	2.9	102.9	1.3	28.6
	Sb	0.38	0.37	-2.6	97.4	2.1	31.3
	Bi	0.06	0.056	-6.7	93.3	5.4	41.0
	Cd	0.14	0.13	-7.1	92.9	3.9	36.3
	Cr	7.3	7.21	-1.2	98.8	2.9	19.9
GBW07113	Cu	10.9	10.18	-6.6	93.4	4.6	18.6
	Mo	2.46	2.37	-3.7	96.3	4.3	23.6
	Ni	64.5	62.78	-2.7	97.3	4.1	13.8
	Pb	33.3	31.5	-5.4	94.6	3.2	15.5
	Zn	86.3	85.4	-1.0	99.0	2.6	13.1

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表 3 方法的方法检出限及测定下限(n=12)

Table 3. Detection limits and lower limit of the method (n=12)

元素	标准曲线设置点的浓度(mg/kg)					检出限(mg/kg)	测定下限(mg/kg)	土壤样品方法检出限(mg/kg)
元素	样品空白	GBW07103	GBW07104	GBW07106	GBW07107	检出限(mg/kg)	测定下限(mg/kg)	土壤样品方法检出限(mg/kg)
As	0	2.1	9.1	1.4	2.1	0.08	0.27	0.2
Sb	0	0.21	0.6	0.17	0.12	0.04	0.13	0.05
Bi	0	0.53	0.18	0.23	0.081	0.04	0.13	0.05
Cd	0	0.029	0.06	0.033	0.061	0.01	0.03	0.021
Cr	0	3.6	20	99	32	0.06	0.20	0.2
Cu	0	3.2	19	42	55	0.09	0.30	0.5
Mo	0	3.5	0.76	0.35	0.54	0.08	0.27	0.1
Ni	0	2.3	16.6	37	17	0.06	0.20	0.2
Pb	0	31	7.6	8.7	11.3	0.08	0.27	0.7
Zn	0	28	20	55	71	0.02	0.07	0.03
注：“土壤样品方法检出限”为DZ/T 0279—2016中数据。

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表 4 分析方法的不确定度计算结果

Table 4. Calculation results of uncertainty of the method

标准物质编号	元素	标准值(mg/kg)	标准值的不确定度(mg/kg)	A类不确定度Δ_x(mg/kg)	扩展不确定度U_Δ(mg/kg)	测定平均值和标准值的绝对差Δ_m(mg/kg)
	As	6.27	0.9	0.1	0.2	0.01
	Bi	0.37	0.07	0.02	0.04	0.02
	Cd	0.07	0.02	0.004	0.008	0.01
	Cr	3.6	1.6	0.1	0.2	0.1
GBW07109	Cu	11.8	1.7	0.3	0.6	0.1
	Mo	0.26	0.09	0.01	0.02	0.01
	Ni	1.75	0.72	0.04	0.08	0.02
	Pb	196	20	4	8	1
	Sb	0.15	0.06	0.01	0.02	0.01
	Zn	112	7	3	6	1
	As	5.96	0.89	0.09	0.18	0.061
	Bi	0.09	0.04	0.002	0.004	0.003
	Cd	0.61	0.13	0.02	0.04	0.02
	Cr	7.7	2.2	0.5	1.0	0.7
GBW07110	Cu	9.1	1.5	0.5	1.0	0.1
	Mo	0.95	0.13	0.05	0.10	0.03
	Ni	12.6	1.9	0.6	1.2	0.3
	Pb	97.7	9.3	2.3	4.6	0.3
	Sb	1.34	0.21	0.08	0.16	0.08
	Zn	164	10	5	10	3
	As	0.4	0.3	0.02	0.04	0.03
	Bi	0.05	0.03	0.002	0.004	0.002
	Cd	0.08	0.03	0.004	0.008	0.002
	Cr	37.6	3.4	1.4	2.8	0.1
GBW07111	Cu	8.8	1.5	0.3	0.6	0.1
	Mo	0.47	0.4	0.02	0.04	0.02
	Ni	24.4	2.3	0.9	1.8	0.3
	Pb	19.8	2.3	0.7	1.4	0.8
	Sb	1.34	0.21	0.05	0.10	0.03
	Zn	85.4	9.4	4.2	8.4	0.4
	As	0.7	0.3	0.01	0.02	0.02
	Bi	0.06	0.02	0.004	0.008	0.004
	Cd	0.14	0.03	0.006	0.012	0.01
	Cr	7.3	3.3	0.3	0.6	0.1
GBW07113	Cu	10.9	1.6	0.6	1.2	0.7
	Mo	2.46	0.26	0.13	0.26	0.09
	Ni	64.5	8	3	6	1.7
	Pb	33.3	3.1	1.2	2.4	1.8
	Sb	0.38	0.05	0.01	0.02	0.01
	Zn	86.3	7.8	2.8	5.6	0.9

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表 5 高岭土实际样品的测定结果(n=3)

Table 5. Analytical results of the real kaolin samples (n=3)

元素	样品1				样品2
元素	测定值(mg/kg)	加标后测定值(mg/kg)	平均回收率(%)	相对标准偏差(%)	测定值(mg/kg)	加标后测定值(mg/kg)	平均回收率(%)	相对标准偏差(%)
As	51.24	100.2	98.0	5.2	41.4	90.6	98.5	4.2
Sb	5.81	54.7	97.8	5.4	8.0	57.1	98.3	4.2
Bi	1.54	50.5	97.9	4.6	1.5	50.7	98.5	3.8
Cd	2.20	51.2	97.9	3.8	3.6	52.8	98.4	3.5
Cr	8.70	57.5	97.7	6.8	9.7	58.8	98.2	4.6
Cu	30.0	78.4	96.8	5.1	36.1	84.8	97.4	4.1
Mo	5.23	54.1	97.8	4.9	6.9	56.0	98.3	3.7
Ni	1.05	50.0	98.0	3.8	1.2	50.4	98.5	2.9
Pb	75.1	122.6	95.0	6.2	55.1	103.5	96.8	5.1
Zn	85.12	132.4	94.6	7.1	95.5	143.3	95.6	3.9

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