电感耦合等离子体串联质谱法分析凹凸棒黏土中的微量元素

李坦平; 李爱阳

doi:10.15898/j.cnki.11-2131/td.202004090043

电感耦合等离子体串联质谱法分析凹凸棒黏土中的微量元素

湖南工学院新型建筑材料研究院, 湖南衡阳 421002

基金项目:
国家自然科学基金项目（81603400）；湖南省自然科学基金项目（2019JJ60026）；湖南省教育厅重点项目（18A428）；湖南省应用特色学科材料科学与工程学科资助项目（湘教通[2018]469号）；湖南省工程研究中心资助项目（湘发改委高技[2019]853号）

详细信息

作者简介: 李坦平, 教授, 主要从事固体工业废弃物建材资源化利用研究。E-mail: hwl0466@163.com

中图分类号: O657.63

收稿日期: 2020-04-09

修回日期: 2020-07-30

录用日期: 2021-01-12

刊出日期: 2021-03-28

Determination of Trace Elements in Attapulgite Clay by Inductively Coupled Plasma-Tandem Mass Spectrometry

Academy of New Building Materials, Hunan Institute of Technology, Hengyang 421002, China

Received Date: 09 April 2020

Revised Date: 30 July 2020

Accepted Date: 12 January 2021

Publish Date: 28 March 2021

摘要

摘要:
凹凸棒黏土是具有层链状结构的含水富镁铝硅酸盐矿物，矿床成因不同导致凹凸棒黏土中微量元素的组成存在差异，其中Be、Cr、Ni、As、Cd、Sb、Hg、Pb会对健康和环境产生不利影响，而V、Mn、Co、Cu、Zn、Mo、Sn、Ba作为凹凸棒黏土的重要微量元素影响其性能和应用范围，因此，对凹凸棒黏土中微量元素进行精准分析可为凹凸棒黏土的高效增值深加工提供理论依据。采用电感耦合等离子体质谱法（ICP-MS）测定岩矿中微量元素具有检出限低和灵敏度高的特点，但因存在复杂质谱干扰，即使采用碰撞反应池（CRC）技术也很难完全消除。本文应用电感耦合等离子体串联质谱法（ICP-MS/MS）来消除质谱干扰，建立了准确测定凹凸棒黏土中微量元素Be、V、Cr、Mn、Co、Ni、Cu、Zn、As、Mo、Cd、Sn、Sb、Ba、Hg、Pb含量的分析方法。实验中采用由硝酸、盐酸、氢氟酸组成的混合酸对凹凸棒黏土样品进行微波消解，不仅加快了样品的消解速度，而且保持了消解溶液中分析元素的稳定。针对分析过程中所面临的质谱干扰，在MS/MS模式下，通过向CRC内加入O₂和NH₃/He为反应气，利用质量转移反应生成相应的氧化物离子和团簇离子消除干扰，选择质量数相近且质谱行为相似的内标元素校正基体效应，稳定了分析信号。应用本方法对国家标准参考物质玄武岩（GBW07105）中16种微量元素进行测定，分析元素的相对误差在-9.60%~8.21%之间，相对标准偏差（RSD）≤6.0%。在选定的分析条件下，各元素的检出限为0.13~51.6ng/L。本方法有效减少了质谱干扰，提高了某些特定同位素在复杂介质中的准确性和灵敏度，适合凹凸棒黏土中16种微量元素的快速测定。
- 凹凸棒黏土 /
- 电感耦合等离子体串联质谱法 /
- 微量元素 /
- 质谱干扰 /
- 反应气
Abstract: BACKGROUND
Attapulgite clay is a water-rich magnesium aluminosilicate mineral with a layered chain structure. The different genesis of the deposit results in a different composition of trace elements in attapulgite clay. Elements Be, Cr, Ni, As, Cd, Sb, Hg, and Pb have adverse effects to health and environment, while V, Mn, Co, Cu, Zn, Mo, Sn and Ba can affect the performance and application of attapulgite clay. Therefore, accurate analysis of trace elements in attapulgite clay can provide a theoretical basis for the high-efficiency value-added deep processing of attapulgite clay. Determination of trace elements in rocks and minerals by inductively coupled plasma-mass spectrometry (ICP-MS) has the characteristics of low limit of detection (LOD) and high sensitivity. Complex spectral interference during the analysis is difficult to completely eliminate, even if collision reaction cell (CRC) technology is used.
OBJECTIVES
To establish an analytical method for the accurate determination of trace elements in attapulgite clay by ICP-MS/MS.
METHODS
In view of the spectral interference in the analysis process, in the MS/MS mode, O₂ and NH₃/He were added into CRC as reaction gases, and the corresponding oxide ions and cluster ions were generated by mass shift reaction to eliminate the interference. Internal standard elements with similar mass number and similar mass spectrometry behavior were selected to correct the matrix effect and stabilize the analysis signal.
RESULTS
The microwave digestion of attapulgite samples with mixed nitric acid, hydrochloric acid and hydrofluoric acid can not only accelerate the digestion speed of the sample, but also maintain the stability of the analytical elements in the digestion solution. The method was used to determine 16 trace elements in national standard reference material basalt (GBW07105). The relative errors of analytes were -9.60%-8.21%, and the relative standard deviation (RSD) was less than 6.0%. Under the selected analytical conditions, the LOD of analyte was 0.13-51.6ng/L.
CONCLUSIONS
ICP-MS/MS can effectively reduce the interference of mass spectrometry and improve the accuracy and sensitivity of some specific isotopes in complex media. The method is suitable for the rapid determination of trace elements in attapulgite clay.
- attapulgite clay /
- inductively coupled plasma-tandem mass spectrometry /
- trace elements /
- mass spectral interference /
- reaction gas

HTML全文

图 1 不同反应模式下消除质谱干扰的工作原理

Figure 1.

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图 2 样品溶液中16种分析元素2h的稳定性情况

Figure 2.

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图 3 不同反应气流速下分析元素的加标回收率

Figure 3.

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表 1 不同消解酸对分析元素的提取率

Table 1. Extraction rate of analytes by different digestion acids

元素	分析元素的提取率(%)			元素	分析元素的提取率(%)
元素	硝酸	硝酸-氢氟酸	硝酸-盐酸-氢氟酸	元素	硝酸	硝酸-氢氟酸	硝酸-盐酸-氢氟酸
Be	55.3	97.2	98.6	As	48.4	101.0	98.1
V	68.3	101.0	97.5	Mo	73.5	97.4	102.0
Cr	76.5	96.9	101.0	Cd	81.2	96.6	98.2
Mn	90.3	101.0	102.0	Sn	89.7	98.1	97.0
Co	71.8	98.5	99.3	Sb	63.0	102.0	101.0
Ni	75.8	96.6	101.0	Ba	80.3	97.7	98.3
Cu	57.6	100.0	102.0	Hg	72.8	83.6	98.0
Zn	74.0	97.5	98.4	Pb	40.6	103.0	97.5

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表 2 在MS/MS模式下分析元素的背景等效浓度

Table 2. Background equivalent concentrations (BECs) of analytes in the MS/MS mode

同位素	主要干扰	O₂反应模式			NH₃/He反应模式
同位素	主要干扰	产物离子	产率(%)	BEC(ng/L)	产物离子	产率(%)	BEC(ng/L)
⁵¹V	³⁵Cl¹⁶O, ³⁶Ar¹⁵N, ³⁶Ar¹⁴NH, ³⁷Cl¹⁴N	⁵¹V¹⁶O⁺	63.3	3.70	⁵¹V⁺	53.2	0.34
⁵²Cr	⁴⁰Ar¹²C, ³⁵Cl¹⁶OH, ³⁶Ar¹⁶O, ³⁸Ar¹⁴N	⁵²Cr¹⁶O⁺	17.5	20.2	⁵²Cr(¹⁴NH₃)₂⁺	0.63	19.7
⁵⁵Mn	⁴⁰Ar¹⁴NH, ⁴⁰Ar¹⁵N, ³⁶Ar¹⁹F, ²³Na¹⁶O₂	⁵⁵Mn¹⁶O⁺	16.0	9.15	⁵⁵Mn(¹⁴NH₃)⁺	0.34	26.4
⁵⁹Co	²⁴Mg³⁵Cl, ⁴⁰Ar¹⁹F, ⁴⁰Ca¹⁹F, ⁴⁰Ar¹⁸OH	⁵⁹Co¹⁶O⁺	23.0	2.88	⁵⁹Co(¹⁴NH₃)₂⁺	5.02	3.52
⁶⁰Ni	²³Na³⁶ArH, ²³Na³⁷Cl, ⁴⁴Ca¹⁶O, ⁵⁹CoH	⁶⁰Ni¹⁶O⁺	13.0	7.12	⁶⁰Ni(¹⁴NH₃)₃⁺	3.91	3.84
⁶³Cu	²⁸Si³⁵Cl, ²³Na⁴⁰Ar, ¹²C¹⁶O³⁵Cl	⁶³Cu¹⁶O⁺	0.85	46.1	⁶³Cu(¹⁴NH₃)₂⁺	5.38	40.9
⁶⁶Zn	²⁹Si³⁷Cl, ³⁴S¹⁶O₂, ⁴⁸Ca¹⁸O, ⁴⁰Ar²⁶Mg	⁶⁶Zn¹⁶O⁺	2.68	155	⁶⁶Zn(¹⁴NH₃)⁺	2.05	82.0
⁷⁵As	⁴⁰Ar³⁵Cl, ³⁶Ar³⁹K, ³⁶Ar³⁸ArH, ⁵⁹Co¹⁶O	⁷⁵As¹⁶O⁺	56.7	8.63	⁷⁵As(¹⁴NH₃)⁺	15.1	41.5

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表 3 分析元素的线性范围、检出限与定量限

Table 3. Linearity, limits of detection (LODs), and limits of quantification (LOQs) for analytes

元素	线性范围(μg/L)	相关系数(R)	LOD (ng/L)	LOQ (ng/L)	元素	线性范围(μg/L)	相关系数(R)	LOD (ng/L)	LOQ (ng/L)
Be	0.002~50	0.9999	0.71	2.38	As	0.006~5.0	1.0000	1.90	6.34
V	0.001~500	1.0000	0.13	0.43	Mo	0.015~50	1.0000	4.22	14.1
Cr	0.010~500	0.9998	2.86	9.52	Cd	0.003~5.0	0.9998	0.94	3.12
Mn	0.011~500	1.0000	3.25	10.8	Sn	0.022~50	1.0000	6.75	22.5
Co	0.001~500	0.9999	0.44	1.46	Sb	0.020~5.0	0.9999	6.10	23.3
Ni	0.017~500	0.9999	4.95	16.5	Ba	0.017~500	0.9997	5.21	17.4
Cu	0.022~500	0.9997	6.32	21.1	Hg	0.004~5.0	1.0000	1.33	4.43
Zn	0.17~500	0.9998	51.6	172	Pb	0.006~50	0.9999	1.84	6.12

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表 4 玄武岩国家标准参考物质(GBW07105)的分析结果(n=6)

Table 4. Analysis results of basalt national standard reference material (GBW07105)

元素	认定值(μg/g)	测定值(μg/g)	相对误差(%)	RSD (%)	元素	认定值(μg/g)	测定值(μg/g)	相对误差(%)	RSD (%)
Be	2.50±0.40	2.26±0.10	-9.60	4.42	As	9.10±1.20	8.73±0.49	-4.07	5.61
V	167±11.0	174±6.44	4.19	3.70	Mo	2.60±0.20	2.53±0.15	-2.69	5.93
Cr	134±11.0	139±3.78	3.73	2.72	Cd	67.0±16.0^*	72.5±3.01^*	8.21	4.15
Mn	1310±61.0	1330±51.0	1.53	3.83	Sn	2.00±0.40	1.97±0.11	-1.50	5.58
Co	46.5±3.40	47.2±2.30	1.51	4.87	Sb	80.0^*	82.3±4.70^*	2.88	5.71
Ni	140±7.00	143±5.92	2.14	3.70	Ba	527±26.0	538±19.6	2.09	3.64
Cu	49.0±3.00	51.6±2.83	5.31	5.48	Hg	6.00±2.00^*	5.51±0.28^*	-8.17	5.08
Zn	150±10.0	158±5.07	5.33	3.21	Pb	7.00	7.23±0.34	3.29	4.70
注：标注“*”的元素含量单位为ng/g。

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表 5 凹凸棒黏土样品的分析结果(n=6)

Table 5. Analysis results of attapulgite samples (n=6)

元素	样品1			样品2
元素	本方法(μg/g)	标准加入法(μg/g)	t检验	本方法(μg/g)	标准加入法(μg/g)	t检验
Be	1.85±0.08	1.79±0.10	p=0.14	3.21±0.14	3.15±0.20	p=0.28
V	13.6±0.57	13.8±0.43	p=0.25	28.2±1.06	29.1±1.11	p=0.09
Cr	31.9±1.55	32.5±1.26	p=0.24	25.6±0.78	26.2±0.84	p=0.11
Mn	72.3±2.80	71.1±2.49	p=0.23	5.79±0.21	6.02±0.43	p=0.13
Co	3.84±0.16	3.90±0.21	p=0.29	2.02±0.11	1.97±0.15	p=0.26
Ni	28.6±1.14	27.7±1.30	p=0.12	37.0±1.27	35.4±1.39	p=0.03
Cu	10.5±0.30	10.7± 0.14	p=0.08	9.56±0.39	9.71±0.45	p=0.28
Zn	34.4±1.25	35.0±1.23	p=0.21	46.3±1.80	44.8±2.03	p=0.10
As	24.9±1.10^*	25.3±1.37^*	p=0.29	18.3±0.76^*	17.6±0.80^*	p=0.08
Mo	4.78±0.12	4.85±0.10	p=0.15	2.05±0.09	2.12±0.13	p=0.15
Cd	18.3±0.66^*	18.0±0.72^*	p=0.23	31.9±1.15^*	33.0±1.28^*	p=0.07
Sn	2.45±0.13	2.52±0.16	p=0.21	1.74±0.08	1.80±0.09	p=0.13
Sb	62.1±2.09^*	61.0±1.85^*	p=0.18	91.0±3.32^*	93.1±4.05^*	p=0.17
Ba	20.8±0.73	21.2±0.53	p=0.15	16.7±0.50	17.2±0.58	p=0.07
Hg	4.56±0.15^*	4.60±0.18^*	p=0.34	7.88±0.31^*	7.64±0.40^*	p=0.14
Pb	2.27±0.10	2.33±0.12	p=0.18	3.06±0.12	3.16±0.15	p=0.11
注：标注“*”的元素含量单位为ng/g。

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电感耦合等离子体串联质谱法分析凹凸棒黏土中的微量元素

湖南工学院新型建筑材料研究院, 湖南 衡阳 421002

作者简介: 李坦平, 教授, 主要从事固体工业废弃物建材资源化利用研究。E-mail: hwl0466@163.com

Determination of Trace Elements in Attapulgite Clay by Inductively Coupled Plasma-Tandem Mass Spectrometry

Academy of New Building Materials, Hunan Institute of Technology, Hengyang 421002, China

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湖南工学院新型建筑材料研究院, 湖南衡阳 421002