氧气反应模式-电感耦合等离子体串联质谱法测定土壤中的镉

赵志飞; 任小荣; 李策; 郭朝; 宋娟娥; 龚华

doi:10.15898/j.cnki.11-2131/td.202003150034

氧气反应模式-电感耦合等离子体串联质谱法测定土壤中的镉

1.
安捷伦科技(中国)有限公司, 北京 100102

2.
湖北省地质实验测试中心, 湖北武汉 430022

3.
中国科学院南京土壤研究所, 江苏南京 210000

详细信息

作者简介: 赵志飞, 硕士, 应用工程师, 从事原子光谱方法开发与研究。E-mail: zzfeel@126.com

中图分类号: S151.93;O657.63

收稿日期: 2020-03-15

修回日期: 2020-04-17

录用日期: 2020-08-24

刊出日期: 2021-01-28

Determination of Cadmium in Soil Samples by ICP-MS/MS Using Oxygen Reaction Mode

1.
Agilent Technologies(China) Co., LTD, Beijing 100102, China

2.
Hubei Geological Research Laboratory, Wuhan 430022, China

3.
Institute of Soil Science, Chinese Academy of Sciences, Nanjing 210000, China

Received Date: 15 March 2020

Revised Date: 17 April 2020

Accepted Date: 24 August 2020

Publish Date: 28 January 2021

摘要

摘要:
应用电感耦合等离子体质谱法(ICP-MS)分析土壤中的镉元素时，锆的氢氧化物、钼的氧化物、锡的同位素会对镉造成严重的干扰，导致准确测定土壤中镉的难度较大。本文采用电感耦合等离子体串接质谱法(ICP-MS/MS)，选取无同质异位素干扰的¹¹¹Cd为分析谱线，在MS/MS模式下碰撞反应池中通入的氧气可以与⁹⁴Zr¹⁶O¹H⁺、⁹⁵Mo¹⁶O⁺进行电子转移、去氢、加氧等反应，抑制这些多原子离子对¹¹¹Cd的重叠干扰。结果表明：氧气流量越大，去除多原子离子的效果越好，当氧气流量在0.45mL/min时，溶液中2000μg/L以下的锆、1000μg/L以下的钼在¹¹¹Cd处形成的多原子重叠干扰小于0.005μg/L。实验在石墨消解仪中采用氢氟酸-硝酸-高氯酸消解样品，盐酸复溶，溶液定容稀释至1000倍测定，方法检出限(3δ)达到0.003μg/g；本方法经过国家土壤一级标准物质验证，11个国家土壤一级标准物质的测量值和认定值的相对误差在±7%以内，3个国家土壤一级标准物质的精密度(RSD，n=12)小于5%。本方法可以作为土壤样品中痕量镉元素的分析方法。
- 土壤 /
- 镉 /
- 氧气反应模式 /
- 多原子离子 /
- 电感耦合等离子体串接质谱法
Abstract: BACKGROUND
When using inductively coupled plasma-mass spectrometry (ICP-MS) to analyze soil, the zirconium hydroxide, molybdenum oxide, and tin isotopes can cause serious interference on cadmium, which makes it difficult to accurately determine cadmium in soil samples.
OBJECTIVES
To develop a method for accurate determination of Cd in soil samples.
METHODS
ICP-MS/MS was used, and ¹¹¹Cd without isobaric interference was selected as the analysis line. In MS/MS mode, the oxygen introduced into the collision reaction cell can be reacted with ¹¹¹Zr¹⁶O¹H⁺, ¹¹¹Mo¹⁶O⁺, inducing electron transfer, dehydrogenation, oxygenation and other reactions to inhibit the overlapping interference of these polyatomic ions on ¹¹¹Cd.
RESULTS
Oxygen flow was the key factor in this method. 0.45mL/min oxygen flow can reduce oxide interference to less than 0.005μg/L when zirconium concentration was lower than 2000μg/L and molybdenum concentration was below 1000μg/L. The method has been verified by the national reference materials. The relative error of the measured value and recognized value of the 11 national reference materials was within ±7%, and the relative standard deviation (n=12) of three soil reference materials was less than 5%.
CONCLUSIONS
Triple quadrupole ICP-MS oxygen reaction mode can eliminate Zr and Mo polyatomic ion interference on Cd, and this method can be used for the determination of trace Cd in soil samples.
- soil /
- cadmium /
- oxygen reaction mode /
- polyatomic ion /
- triple quadrupole inductively coupled plasma-mass spectrometry

HTML全文

图 1 ICP-MS/MS氧气模式分析¹¹¹Cd示意图

Figure 1.

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表 1 ZrOH/MoO和氧气主要产物的质量数及信号强度

Table 1. Main reaction products and signal intensity of ZrOH/MoO and oxygen

标准溶液	Q1和Q2分析的质量数 m/z	信号强度 (cps)
锆单标溶液	111 → 32	39817
	111 → 127	4073
	111 → 110	868
	111 → 126	813
钼单标溶液	111 → 32	36109
钼单标溶液	111 → 127	1750

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表 2 氧气流速的优化

Table 2. Optimization of oxygen flow

氧气流速 (mL/min)	Zr单标m/z=111处信号强度(cps)	Cd单标m/z=111处信号强度(cps)
0.000	623.35	6288.14
0.075	670.02	6024.69
0.150	593.35	8971.34
0.225	335.50	12464.13
0.300	138.00	16208.14
0.375	45.00	18299.17
0.450	21.00	18905.01
0.525	4.50	18352.57
0.600	2.00	17020.81
0.675	2.00	16071.31
0.750	2.50	14624.65

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表 3 不同模式下¹¹¹Cd干扰情况对比

Table 3. Interference elimination effects in different modes

标准溶液	浓度 (μg/L)	氦气模式下¹¹¹Cd测定结果		干扰系数	氧气模式下¹¹¹Cd测定结果
标准溶液	浓度 (μg/L)	浓度(μg/L)	信号强度(cps)	干扰系数	浓度(μg/L)	信号强度(cps)
锆单标溶液	100	0.014	87	0.00014	0.000	3
	200	0.028	173	0.00014	0.000	3
	400	0.040	247	0.00010	0.001	10
	800	0.095	580	0.00012	0.001	20
	2000	0.171	1047	0.00009	0.004	60
钼单标溶液	20	0.006	37	0.0003	0.000	3
	50	0.014	87	0.0003	0.000	3
	100	0.020	120	0.0002	0.000	7
	200	0.049	303	0.0002	0.001	13
	1000	0.172	1053	0.0002	0.005	70
	2000	0.353	2167	0.0002	0.018	237
注：表中分析的是Zr单标溶液和Mo单标溶液，镉的预测浓度都为0。

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表 4 土壤一级标准物质镉分析结果

Table 4. Analytical results of Cd in soil national standard substances

标准物质编号	认定值 (μg/g)	测定值 (μg/g)	相对误差 (%)
GBW07385	0.28 ± 0.02	0.285	1.8
GBW07385	0.28 ± 0.02	0.282	0.7
GBW07388	0.066 ± 0.007	0.067	1.5
GBW07388	0.066 ± 0.007	0.068	3.0
GBW07389	0.14 ± 0.01	0.143	2.1
GBW07389	0.14 ± 0.01	0.141	0.7
GBW07407	0.08 ±0.02	0.079	-1.3
GBW07407	0.08 ±0.02	0.079	-1.3
GBW07408	0.13 ±0.02	0.131	0.8
GBW07408	0.13 ±0.02	0.132	1.5
GBW07426	0.15 ±0.02	0.149	-0.7
GBW07426	0.15 ±0.02	0.154	2.7
GBW07427	0.13 ±0.01	0.131	0.8
GBW07427	0.13 ±0.01	0.127	-2.3
GBW07449	0.108 ± 0.011	0.105	-2.8
GBW07449	0.108 ± 0.011	0.108	0.0
GBW07451	0.065 ±0.012	0.061	-6.2
GBW07451	0.065 ±0.012	0.062	-4.6
GBW07452	0.15 ± 0.02	0.148	-1.3
GBW07452	0.15 ± 0.02	0.152	1.3
GBW07453	0.106 ±0.007	0.103	-2.8
GBW07453	0.106 ±0.007	0.105	-0.9

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表 5 方法检出限和精密度

Table 5. Detection limit and precision tests of the method

项目	Cd空白值 (μg/L)			Cd测定值(μg/g)
项目	Cd空白值 (μg/L)			GBW07408			GBW07451			GBW7389
12次测定值	-0.0004	0.0018	0.0007	0.131	0.127	0.132	0.061	0.062	0.065	0.134	0.143	0.142
	0.0021	-0.0012	0.0019	0.130	0.130	0.132	0.065	0.069	0.070	0.139	0.139	0.145
	0.0011	0.0013	0.0015	0.133	0.132	0.126	0.067	0.071	0.066	0.146	0.138	0.141
	0.0014	-0.0002	0.0010	0.127	0.130	0.132	0.068	0.065	0.064	0.136	0.142	0.140
标准偏差	0.0010			0.0024			0.0029			0.0034

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氧气反应模式-电感耦合等离子体串联质谱法测定土壤中的镉

1. 安捷伦科技(中国)有限公司, 北京 100102 2. 湖北省地质实验测试中心, 湖北 武汉 430022 3. 中国科学院南京土壤研究所, 江苏 南京 210000

作者简介: 赵志飞, 硕士, 应用工程师, 从事原子光谱方法开发与研究。E-mail: zzfeel@126.com

Determination of Cadmium in Soil Samples by ICP-MS/MS Using Oxygen Reaction Mode

1. Agilent Technologies(China) Co., LTD, Beijing 100102, China 2. Hubei Geological Research Laboratory, Wuhan 430022, China 3. Institute of Soil Science, Chinese Academy of Sciences, Nanjing 210000, China

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1.
安捷伦科技(中国)有限公司, 北京 100102

2.
湖北省地质实验测试中心, 湖北武汉 430022

3.
中国科学院南京土壤研究所, 江苏南京 210000

1.
Agilent Technologies(China) Co., LTD, Beijing 100102, China

2.
Hubei Geological Research Laboratory, Wuhan 430022, China

3.
Institute of Soil Science, Chinese Academy of Sciences, Nanjing 210000, China