膜去溶-电感耦合等离子体质谱法测定环境地质样品中的镉
国家核安保技术中心, 北京 102401 |
Determination of Cd in Environmental Geological Samples by Inductively Coupled Plasma-Mass Spectrometry with Membrane Desolvation
State Nuclear Security Technology Center, Beijing 102401, China |
摘要：应用电感耦合等离子体质谱法（ICP-MS）分析环境地质样品中的Cd时，Zr、Mo元素的氧化物和氢氧化物会对Cd造成严重干扰，导致结果有明显的偏差。针对此问题，本文建立了膜去溶-ICP-MS直接测定环境地质样品中微量Cd的分析方法，该方法可有效地消除Zr、Mo氧化物和氢氧化物对Cd的干扰，保证结果准确、可靠。膜去溶-ICP-MS相比于常规ICP-MS测定Cd的方法，可将Zr、Mo氧化物和氢氧化物对Cd的干扰降低到0.001%，检测灵敏度提高3.5倍左右。在给定条件下，Cd的检出限为0.28 ng/L，测定下限为2.2 ng/L，精密度（RSD，n=12）为2.2%。利用该方法分析20种岩石、土壤和沉积物国家标准物质的测定值与标准值相符，表明膜去溶-ICP-MS法直接测定环境地质样品中痕量或超痕量Cd时具有一定的应用潜力。同时，用该方法对2016年中核集团组织的实验室间两个比对样品中的Cd进行测定，稳健Z比分数分别为0.500和-0.964，Z的绝对值都小于2。
Determination of Cd in Environmental Geological Samples by Inductively Coupled Plasma-Mass Spectrometry with Membrane Desolvation
ABSTRACT Cadmium suffers from significant Zr and Mo based oxide/hydroxide interferences during Inductively Coupled Plasma-Mass Spectrometry (ICP-MS) analysis of environmental samples, which can result in a significant deviation of the results. Direct determination method of Cd in environmental geological samples by ICP-MS with membrane desolvation has been developed in this study. This method can effectively eliminate the interference of Zr, Mo oxides and hydroxides, and ensure the results are accurate and reliable. Compared with the conventional method of ICP-MS, the interference of Zr and Mo oxides and hydroxides can be reduced to 0.001% when membrane desolvation is used. Meanwhile, the sensitivity of Cd can be increased 3.5 times. Under the given conditions, the detection limit of Cd was 0.28 ng/L, the lower limit of determination was 2.2 ng/L, and the precision (RSD, n=12) was 2.2%. The method was applied to analyze 20 Chinese environmental geological reference materials. The analytical results are consistent with the certificated values. It indicates that the proposed method has a great potential for the direct determination of trace or ultra-trace levels of cadmium in environmental geological samples. At the same time, the method was used to determine Cd in two comparison samples between two laboratories in 2016. This comparison was organized by the China National Nuclear Corporation. The Z-scores were 0.500 and -0.964, respectively for the two laboratories, and the absolute values of Z were less than 2.
本文参考文献
| [1] |
Balmuri S R, Selvaraj U, Kumar V V, et al. Effect of surfactant in mitigating cadmium oxide nanoparticle toxicity:Implications for mitigating cadmium toxicity in environment[J].Environmental Research, 2017, 152: 141-149. doi: 10.1016/j.envres.2016.10.005 |
| [2] |
Eichler A, Tobler L, Eyrikh S, et al. Icecore based assessment of historical anthropogenic heavy metal (Cd, Cu, Sb, Zn) emissions in the Soviet Union[J]. Environmental Science & Technology, 2014, 48(5): 2635-2642. |
| [3] |
Moritz B, Ulrich A, Rehmus A, et al. Accumulation of cadmium and uranium in arable soils in Switzerland[J].Environmental Pollution, 2017, 221: 85-93. doi: 10.1016/j.envpol.2016.11.035 |
| [4] |
Oliveira F M, Marchioni C A, Barros J A V, et al. Assessment of cadmium and iron adsorption in sediment, employing a flow injection analysis system with on line filtration and detection by flame atomic absorption spectrometry and thermospray flame furnace atomic absorption spectrometry[J].Analytica Chimica Acta, 2014, 809: 82-87. doi: 10.1016/j.aca.2013.11.048 |
| [5] |
Fırat M, Bakırdere S, Fındıkoglu S M, et al. Deter-mination of trace amount of cadmium using dispersive liquid-liquid microextraction-slotted quartz tube-flame atomic absorption spectrometry[J]. Spectrochimica Acta Part B:Atomic Spectroscopy, 2017, 129(1): 37-41. |
| [6] |
徐子优. 固体直接进样-石墨炉原子吸收光谱法测定土壤中镉元素[J]. 中国无机分析化学, 2013, 3(3): 8-12. Xu Z Y. Determination of cadmium in soil by direct solid sample introduction-graphite furnace atomic absorption spectrometry[J]. Chinese Journal of Inorganic Analytical Chemistry, 2013, 3(3): 8-12. |
| [7] |
Wu Q H, Wu C X, Wang C, et al. Sensitive determination of cadmium in water, beverage and cereal samples by a novel liquid-phase microextraction coupled with flame atomic absorption spectrometry[J].Analytical Methods, 2011, 3: 210-216. doi: 10.1039/C0AY00524J |
| [8] |
Wysocka I, Vassileva E. Determination of cadmium, copper, mercury, lead and zinc mass fractions in marine sediment by isotope dilution inductively coupled plasma mass spectrometry applied as a reference method[J]. Microchemical Journal, 2016, 18: 198-207. |
| [9] |
Inagaki K, Takatsu A, Uchiumi A, et al. Determination of cadmium in sediment by isotope dilution inductively coupled plasma mass spectrometry using a co-precipitation separation technique[J].Journal of Analytical Atomic Spectrometry, 2001, 16: 1370-1374. doi: 10.1039/b106974h |
| [10] |
Suzuki Y, Endo Y, Ogawa M, et al. Determination of sub-ppb cadmium in urine by solid-phase extraction and inductively coupled plasma-mass spectrometry[J].Analytical Sciences, 2008, 24(8): 1049-1052. doi: 10.2116/analsci.24.1049 |
| [11] |
何红蓼, 胡明月, 巩爱华, 等. 碘化物升华分离-电感耦合等离子体光谱法测定土壤和沉积物中砷、锑、铋、镉、锡[J]. 光谱学与光谱分析, 2008, 28(3): 663-666. He H L, Hu M Y, Gong A H, et al. Determination of As, Sb, Bi, Cd and Sn in soils and sediments by inductively coupled plasma atomic emission spectrometry after sublimation separation as iodides[J]. Spectroscopy and Spectral Analysis, 2008, 28(3): 663-666. |
| [12] |
Bagheri A, Behbahani M, Amini M M, et al. Simultane-ous separation and determination of trace amounts of Cd(Ⅱ) and Cu(Ⅱ) in environmental samples using novel diphenylcarbazide modified nanoporous silica[J].Talanta, 2012, 89: 455-461. doi: 10.1016/j.talanta.2011.12.062 |
| [13] |
周丽萍, 李中玺. 王水提取-电感耦合等离子体质谱法同时测定地质样品中微量银、镉、铋[J]. 分析试验室, 2005, 24(9): 20-25. Zhou L P, Li Z X. Determination of silver, cadmium and bismuth in geological samples by inductively coupled plasma mass spectrometry with aqua regia treatment[J]. Chinese Journal of Analysis Laboratory, 2005, 24(9): 20-25. |
| [14] |
徐娟, 胡兆初, 刘勇胜, 等. 膜去溶-电感耦合等离子质谱测定21种国际地质标样中的银[J]. 分析化学, 2008, 31(11): 1493-1498. doi: 10.3321/j.issn:0253-3820.2008.11.008 Xu J, Hu Z C, Liu Y S, et al. Direct determination of Ag in 21 international geological reference materials by membrane desolvation-inductively coupled plasma-mass spectrometry[J].Chinese Journal of Analytical Chemistry, 2008, 31(11): 1493-1498. doi: 10.3321/j.issn:0253-3820.2008.11.008 |
| [15] |
韩国军, 伍星, 童坚, 等. 膜去溶-ICP-MS测定高纯CeO2中14种痕量稀土杂质分析方法研究[J]. 中国稀土学报, 2009, 27(1): 137-144. Han G J, Wu X, Tong J, et al. Determination of 14 trace rare earth impurities in high-purity CeO2 by inductively coupled plasma mass spectrometry with membrane desolvation[J]. Journal of the Chinese Rare Earth Society, 2009, 27(1): 137-144. |
| [16] |
刘妹, 程志中, 顾铁新, 等. 矿石与钼精矿成分分析标准物质研制[J]. 岩矿测试, 2013, 32(6): 944-951. Liu M, Cheng Z Z, Gu T X, et al. Preparation of molybdenum ore and molybdenum concentrate reference materials[J]. Rock and Mineral Analysis, 2013, 32(6): 944-951. |
| [17] |
李自强, 李小英, 钟琦, 等. 电感耦合等离子体质谱法测定土壤重金属普查样品中铬铜镉铅的关键环节研究[J]. 岩矿测试, 2016, 35(1): 37-41. Li Z Q, Li X Y, Zhong Q, et al. Determination of Cr, Cu, Cd and Pb in soil samples by inductively coupled plasma-mass spectrometry for an investigation of heavy metal pollution[J]. Rock and Mineral Analysis, 2016, 35(1): 37-41. |
| [18] |
李力争, 韩张雄, 王龙山, 等. 电感耦合等离子体质谱法测定地球化学样品中镉[J]. 分析试验室, 2016, 31(12): 69-72. Li L Z, Han Z X, Wang L S, et al. Determination of Cd in geochemical samples by inductively coupled plasma-mass spectrometry[J]. Chinese Journal of Analysis Laboratory, 2016, 31(12): 69-72. |
| [19] |
Guo W, Hu S H, Xie Y F, et al. Direct determination of trace cadmium in environmental samples by dynamic reaction cell inductively coupled mass spectrometry[J].Chemosphere, 2010, 81(11): 1463-1468. doi: 10.1016/j.chemosphere.2010.08.056 |
| [20] |
孙朝阳, 董利明, 贺颖婷, 等. 电感耦合等离子体质谱法测定地质样品中钪镓锗铟镉铊时的干扰及其消除方法[J]. 理化检验(化学分册), 2016, 52(9): 1026-1030. Sun C Y, Dong L M, He Y T, et al. Elimination of interferences in ICP-MS determination of Sc, Ga, Ge, In, Cd and Tl in geological sample[J]. Physical Testing and Chemical Analysis (Part B:Chemical Analysis), 2016, 52(9): 1026-1030. |
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