Determination of Silver in Soil and Stream Sediments by ICP-MS/MS with Four Collision/Reaction Modes
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摘要:
由于受到铌、锆的质谱干扰，使用电感耦合等离子体质谱法（ICP-MS）很难准确测定土壤和水系沉积物中的银。本文采用电感耦合等离子体串联质谱法（ICP-MS/MS），通过研究93Nb16O+、91Zr16OH2+、92Zr16OH+和109Ag+在氦气、氧气和氨气中质谱信号变化，探讨不同碰撞/反应模式的干扰消除能力和消除机理。实验采用盐酸-硝酸-氢氟酸-高氯酸消解样品，选用氦气MS/MS模式、氧气MS/MS模式、氨气MS/MS模式、氨气Mass-Shift模式测定土壤和水系沉积物中的银含量。结果表明：在优化池气体流速后，四种模式下铌、锆对银的干扰程度分别降低20、1500、1500和2000多倍；方法检出限分别为0.005mg/kg、0.002mg/kg、0.003mg/kg和0.003mg/kg；准确度和精密度采用国家标准物质验证，测定值和标准值的相对误差分别在-1.4%~84.3%、-7.6%~7.2%、-15.0%~10.0%和-12.5%~8.6%之间，相对标准偏差（RSD）分别在1.5%~6.3%、1.4%~8.3%、1.4%~5.9%和0.7%~8.2%之间。氦气MS/MS模式消除干扰能力一般，仅适合测定铌、锆干扰较轻的样品；氧气MS/MS模式、氨气MS/MS模式、氨气Mass-Shift模式消除质谱干扰能力较强，可用于土壤和水系沉积物中痕量银的测定。与行业标准DZ/T 0279.11—2016相比，这三种方法检出限更低、测定范围更宽，并可实现多元素同时测定。
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关键词:
- 碰撞/反应模式 /
- 银 /
- 电感耦合等离子体串联质谱法 /
- 土壤 /
- 水系沉积物
Abstract:BACKGROUND It is difficult to accurately determine the content of Ag in soil and sediment due to the mass spectrum interference of niobium, zirconium oxide and hydroxide during inductively coupled plasma-mass spectrometry (ICP-MS) analysis.
OBJECTIVES To develop methods for the determination of trace Ag in soil and sediment samples by four collision/reaction modes.
METHODS The changes of mass spectrum signals of 93Nb16O+, 91Zr16OH2+, 92Zr16OH+ and 109Ag+ in helium, oxygen and ammonia were determined using inductively coupled plasma-tandem mass spectrometry (ICP-MS/MS). The interference elimination ability and elimination mechanism of different collision/reaction modes were investigated. The samples were digested by HCl-HNO3-HF-HClO4. The content of Ag in soil and stream sediments was determined by helium MS/MS mode, oxygen MS/MS mode, ammonia MS/MS mode and ammonia Mass-Shift mode.
RESULTS With the optimal gas flow rate in the tank of the four collision/reaction modes, the interference degree of niobium and zirconium on Ag were decreased more than 20, 1500, 1500 and 2000 times, respectively. The detection limits of the method were 0.005mg/kg, 0.002mg/kg, 0.003mg/kg and 0.003mg/kg, respectively. The accuracy and precision were verified by national reference materials of soil and sediment, while the relative errors of measured values and certified values were -1.4%-84.3%, -7.6%-7.2%, -15.0%-10.0% and -12.5%-8.6%, respectively. The relative standard deviations were 1.5%-6.3%, 1.4%-8.3%, 1.4%-5.9% and 0.7%-8.2%, respectively.
CONCLUSIONS Helium MS/MS mode has a low capacity to eliminate mass spectrometry interference, and is suitable for the determination of samples with little interference of niobium and zirconium. Oxygen MS/MS, ammonia MS/MS and ammonia Mass-Shift modes have a strong ability to eliminate mass spectrometry interference, which can be used for the determination of trace Ag in soil and stream sediments; and have the advantages of lower detection limit, wider linear range, and simultaneous determination of multiple elements, when compared with the industry standard DZ/T 0279.11—2016.
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图 2 (a) 氦气MS/MS模式、(b)氧气MS/MS模式、(c)氨气MS/MS模式、(d)氨气Mass-Shift模式下池气体流速对基体空白溶液、基体加标溶液信号强度和背景等效浓度的影响
Figure 2.
表 1 ICP-MS/MS仪器工作参数
Table 1. Working parameters of ICP-MS/MS instrument
工作参数 标准MS/MS模式 氦气MS/MS模式 氧气MS/MS模式 氨气MS/MS模式 氨气Mass-Shift模式 产物离子 109Ag+ 109Ag+ 109Ag+ 109Ag+ 109Ag17(NH3)2+ Q1→Q3(m/z) 109→109 109→109 109→109 109→109 109→143 质量切割参数(RPq) 0.25 0.25 0.45 0.45 0.45 池气体 - He O2 NH3 NH3 气体流速(mL/min) - 7.0 2.6 1.8 1.8 
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表 2 不同浓度的锆、铌溶液在不同测量模式下对109Ag干扰情况
Table 2. Interference effects of different concentrations of Zr and Nb solutions on 109Ag in different measurement modes
溶液类型 锆或铌溶液浓度
(mg/L)109Ag测定值(μg/L) 氦气MS/MS模式 氧气MS/MS模式 氨气MS/MS模式 氨气Mass-Shift模式 锆溶液 10.0 0.013 0.006 0.006 0.005 50.0 0.061 0.008 0.007 0.007 100 0.140 0.019 0.022 0.020 500 1.047 0.035 0.030 0.030 1000 2.432 0.050 0.047 0.046 铌溶液 1.00 0.441 0.000 0.000 0.000 5.00 2.630 0.005 0.007 0.003 10.0 4.960 0.009 0.011 0.005 50.0 26.542 0.036 0.037 0.013 100 43.441 0.077 0.074 0.026 500 411.726 0.472 0.356 0.128 1000 978.826 1.006 0.780 0.261
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表 3 不同测量模式下方法准确度和精密度
Table 3. Accuracy and precision tests of the method by different measurement modes
标准物质编号 银标准值
(mg/kg)Nb/Ag Zr/Ag 氦气MS/MS模式 氧气MS/MS模式 氨气MS/MS模式 氨气Mass-Shift模式 银测定平均值
(mg/kg)RSD
(%)相对误差
(%)银测定平均值
(mg/kg)RSD
(%)相对误差
(%)银测定平均值
(mg/kg)RSD
(%)相对误差
(%)银测定平均值
(mg/kg)RSD
(%)相对误差
(%)GBW07403 0.091±0.007 102 2703 0.096 2.4 5.5 0.094 2.2 3.3 0.095 3.1 4.4 0.093 2.6 2.2 GBW07404 0.070±0.011 543 7143 0.115 3.0 64.3 0.075 4.0 7.2 0.077 3.8 10.0 0.076 4.6 8.6 GBW07405 4.4±0.4 5 62 4.42 1.5 0.5 4.41 1.4 0.3 4.31 2.8 -2.1 4.40 2.4 0 GBW07407 0.057±0.011 1123 5579 0.105 4.9 84.3 0.053 4.2 -7.1 0.051 5.1 -10.6 0.055 5.6 -3.6 GBW07451 0.074±0.006 208 3446 0.073 5.0 -1.4 0.074 2.7 0 0.072 4.2 -2.8 0.070 2.8 -5.5 GBW07302a 0.040±0.011 1000 3550 0.072 4.7 80.0 0.038 8.3 -5.0 0.034 5.9 -15.0 0.035 7.5 -12.5 GBW07305a 0.63±0.06 27 437 0.652 3.3 3.5 0.629 1.8 -0.2 0.626 1.4 -0.7 0.628 0.7 -0.4 GBW07309 0.089±0.010 202 4157 0.088 3.1 -1.2 0.086 1.8 -3.4 0.083 2.9 -6.8 0.087 3.6 -2.3 GBW07311 3.2±0.4 8 48 3.20 2.0 0 3.21 1.4 0.4 3.18 1.6 -0.7 3.28 2.2 2.5 GBW07375 0.040±0.004 155 2190 0.043 6.3 7.5 0.037 4.5 -7.6 0.038 5.6 -5.0 0.037 8.2 -7.5 注：Nb/Ag和Zr/Ag分别为标准样品中铌和锆的含量与银含量的比值。
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