Determination of plutonium by inductively coupled plasma mass spectrometry (ICP-MS)

Inductively coupled plasma mass spectrometry (ICP-MS) has been applied to the measurement of plutonium isotopes in soils. In the ICP-MS, a calibration curve method was conveniently utilized even in high viscosity solution using a Babington nebulizer. Plutonium concentrations in soil around the Kashiwazaki-Kariwa nuclear power station were found to be in the range of 0.054 to 1.0 Bq/kg with an average of 0.27 Bq/kg. The ratios of ²³⁹Pu/²⁴⁰Pu were also obtained with the ICP-MS to investigate the origin of Pu-isotopes. On the basis of this result, the origin of the Pu-isotopes was attributed to be fallout from the past atmospheric nuclear tests.     

Neptunium determination by inductively coupled plasma mass spectrometry (ICP-MS)

The determination of neptunium-237 (²³⁷Np) traditionally has been performed by alpha spectrometry or neutron activation analysis. These methods are labor intensive and require several days for completion. Inductively Coupled Plasma Mass Spectrometry (ICP-MS) is a possible alternative for²³⁷Np determinations. This paper describes the analytical method developed for samples that have significant levels of uranium present. The lower reporting limits achievable by ICP-MS are competitive with the counting methods, but the real advantage for this laboratory lies in the lower cost and faster turnaround time provided by ICP-MS.     

Determination of trace elements in marine plankton by inductively coupled plasma mass spectrometry (ICP-MS)

A method has been developed for the determination of 23 elements in marine plankton in which inductively coupled plasma (ICP) source mass spectrometry (MS) was used to quantify the elements in the solution after digestion in a mixture of hydrofluoric and nitric acids in sealed PTFE vessels in a microwave field. The procedure was validated by the analysis of a standard reference soil (SRM 2709 San Joaquin Soil) and a standard reference fresh water plankton (CRM 414). The method was applied to the analysis of several marine plankton samples grown under controlled conditions including several whose growth media had been enriched with selenium. Matrix induced signal suppressions and instrumental drift were corrected by internal standardization. The suitabilities of germanium, indium, rhodium, scandium and yttrium as internal standard elements were evaluated. Neither scandium nor yttrium could be used due to the presence of these elements in the samples, germanium was used for the determination of As, Co, Cu, Fe, Ni, Se, Si and Zn, indium was used for Al, Ba, Ca, Eu, Sr, and Tl, and rhodium was used for Cd, Cr, Hg, Mg, Pb, Sb, Sn, and V. For Al, Ca, Cr, Cu, Fe, Mg, Mn, Ni, Si, Sr, V, and Zn internal standardization did not completely compensate for the suppressive effect of the heavier elements and the solutions were diluted. However, for As, Ba, Cd, Co, Eu, Hg, Pb, Sb, Se, Sn and Tl, it was possible to obtain accurate results despite the 35–¶40% suppression in the signals. Isobaric overlap was only a problem in the cases of ⁴²Ca and ⁷⁸Se; ⁴⁴Ca and ⁷⁷Se, respectively, were used. Memory effects were only observed with Hg for which a nitric acid-sodium chloride solution was the most effective wash-out solution. The marine plankton samples were able to tolerate a higher concentration of Hg as the selenium concentration increased.     

电感耦合等离子体质谱法测定血液和精液中的硼

采用HNO3-H2O2和氨水-甘露醇两种方法处理样品,电感耦合等离子体质谱法（ICP-MS）测定血液和精液中的硼。Be作内标补偿基体效应,并用标准加入法验证了方法的可靠性,标准加入法与外标法测定结果相吻合。在测定B的同时,还可进行Cr、Cu、Cd、Ba、Sr、Mn、Co、Tl、Li、Pb、Zn、Sc、Ti、V、As等多元素测定。两种样品处理方法的测定值呈显著正相关（r=0.99919）。方法检出限为0．11ng／mL（氨水-甘露醇法）,0.06ng／mL（HNO3-H2O2）。已用于测定某硼矿区血液和精液样品中的硼。     

Determination of trace elements in marine plankton by inductively coupled plasma mass spectrometry (ICP-MS)

A method has been developed for the determination of 23 elements in marine plankton in which inductively coupled plasma (ICP) source mass spectrometry (MS) was used to quantify the elements in the solution after digestion in a mixture of hydrofluoric and nitric acids in sealed PTFE vessels in a microwave field. The procedure was validated by the analysis of a standard reference soil (SRM 2709 San Joaquin Soil) and a standard reference fresh water plankton (CRM 414). The method was applied to the analysis of several marine plankton samples grown under controlled conditions including several whose growth media had been enriched with selenium. Matrix induced signal suppressions and instrumental drift were corrected by internal standardization. The suitabilities of germanium, indium, rhodium, scandium and yttrium as internal standard elements were evaluated. Neither scandium nor yttrium could be used due to the presence of these elements in the samples, germanium was used for the determination of As, Co, Cu, Fe, Ni, Se, Si and Zn, indium was used for Al, Ba, Ca, Eu, Sr, and Tl, and rhodium was used for Cd, Cr, Hg, Mg, Pb, Sb, Sn, and V. For Al, Ca, Cr, Cu, Fe, Mg, Mn, Ni, Si, Sr, V, and Zn internal standardization did not completely compensate for the suppressive effect of the heavier elements and the solutions were diluted. However, for As, Ba, Cd, Co, Eu, Hg, Pb, Sb, Se, Sn and T1, it was possible to obtain accurate results despite the 35-40% suppression in the signals. Isobaric overlap was only a problem in the cases of 42Ca and 78Se; 44Ca and 77Se, respectively, were used. Memory effects were only observed with Hg for which a nitric acid-sodium chloride solution was the most effective wash-out solution. The marine plankton samples were able to tolerate a higher concentration of Hg as the selenium concentration increased.     

微波消解法-电感耦合等离子体质谱(ICP-MS)法测定韭菜中11种元素

为快速、准确测定韭菜中多元素含量,采用微波消解法对韭菜中样品进行消解处理,优化了前处理方法、ICP-MS工作条件和检测方法,利用微波消解-电感耦合等离子体质谱法测定韭菜中Pb、Cd、Se、As、Zn、Cu、Ni、Fe、Cr、Ca、K等11种元素含量。结果表明,在硝酸-双氧水(7:1)体系中,消解功率1550W,温度梯度为120℃-160℃-195℃,总时长为45min,赶酸温度选择150℃,可将韭菜完全消解,并且ICP-MS射频功率设为1550W,运用在线内标的检测方式降低非质谱干扰。11种元素回归系数R₂^{均大于0.999,方法检出限为}0.002～0.100μg/kg,方法定量限为0.006～0.300μg/kg。方法回收率88.0%～102.7%,相对标准偏差为1.8%～4.6%,可以满足韭菜中多种元素同时测定的需求。方法具有灵敏度高、线性范围宽、准确性高等特点,可为韭菜样品的多元素同时测定提供可靠的方法支撑。     

Determination of selenium in red blood cells by inductively coupled plasma mass spectrometry (ICP-MS) after microwave digestion

Selenium is an essential trace element and its levels in blood have been widely used for assessing Se status in humans. The aim of this present study is to develop a suitable method for the determination of Se in red blood cells (RBC) using ICP-MS after microwave digestion. The blood samples were obtained from patients with benign prostatic hyperplasia (BPH), who attended urology clinics at the Princess Alexandra hospital, Brisbane, Australia. No apparent polyatomic and matrix interferences were encountered when ⁸²Se isotope was used for the analysis of Se levels in RBC. Whole Blood Seronorm Trace Elements (SERO, Norway) and dogfish muscle (DORM-1, NRCC) were used as reference materials for method validation. The method was rapid and accurate, and ideal for routine analysis of Se in RBC, and in particular for assessing of Se status in humans. This revised version was published online in August 2006 with corrections to the Cover Date.     

电感耦合等离子体质谱法(ICP-MS)测定废水中有害元素银的含量

为了寻求一种更加适合废水中低含量银的测定方法,本文采用石墨电热板消解-电感耦合等离子体质谱法测定废水中的低含量银离子。通过仪器工作条件最优化、测定线性回归方程、检出限、准确度、精密度、实际样品加标回收率,并与电感耦合等离子体发射光谱法（ICP-AES）的实际样品测定结果进行比对来评价该方法的实用性。石墨电热板消解-电感耦合等离子体质谱法前处理方法简便,分析速度快且该方法检出限较低,为0.03ug/L,标准样品测定的相对误差为-0.7%～1.7%,相对标准偏差为1.1%～2.5%,实际样品加标回收率在97.0%～103%之间,回收率高,能够满足废水中低含量银的测定。     

Coupling of inductively coupled plasma mass spectrometry (ICP-MS) with electrothermal vaporisation (ETV)

An inductively coupled plasma mass spectrometer (ICP-MS) was coupled on-line with an electrothermal vaporisation (ETV). The influence of aerosol gas flow as well as the variation of the coupling distance on the signal intensity was investigated and compared with the results of hydraulic high-pressure nebulizer (HHPN) measurements. Furthermore, temperature programs known from graphite furnace atomic absorption spectroscopy (GFAAS) were applied to ETV-ICP-MS. After optimisation of temperature programs, calibration series based on mono-element and multi-element solutions were carried out. The dynamic range and the detection limits of the method were determined. By use of internal standardisation it was tried to improve linearity and reproducibility. According to the results, internal standardisation does not have a great impact on linearity, but may be a useful tool to improve reproducibility. However, the latter is still low.     

电感耦合等离子体原子发射光谱法测定自来水中的8种元素

采用电感耦合等离子体原子发射光谱法(ICP-AES)测定了化学实验室自来水中铝、钾、锶、钡、锰、钴、钼、硒8种元素的含量;对仪器的工作条件进行了优化,确定了各元素的分析波长和检出限.结果表明,所述方法可以方便地用于测定化学实验室自来水样品中的8种元素,相对标准偏差为0.08%～6.90%.     

Accurate determination of lead in wines by inductively coupled plasma mass spectrometry

Summary The capability of inductively coupled plasma mass spectrometry (ICP-MS) for Pb determinations in wine samples is studied. An evaluation is made of the signal behaviour in aqueous ethanolic medium. The effect of preliminary sample preparation on signal suppression or enhancement is investigated in conjunction with the ability of internal standardization to correct for it. As a result, an accurate and precise method of analysis is described in which the sample preparation is limited to a 10-fold dilution and external calibration is applied for quantitation. A detection limit of 0.2 g 1^–1 Pb in wine is achieved. The Pb content of ten different wines was found to range around 40 g 1^–1 with extreme values of 1.63 and 58.8 g 1^–1.     

湿法消解-电感耦合等离子体质谱(ICP-MS)法测定大气降尘中7种重金属

为精准防控大气降尘污染,提供其重金属检测方法。重点考察了样品前处理中混合酸体系选择和最佳酸用量比对实验。在最优条件下建立了混合酸（硝酸、氢氟酸、盐酸和高氯酸）湿法消解大气降尘样品和电感耦合等离子体质谱仪进行7种重金属（铊、铅、镉、铬、铜、锌和镍）含量测试的实验方法。实验结果显示7种重金属在一定的浓度范围内线性关系好,线性系数均大于0.999,7种重金属方法检出限为0.02 mg/kg～2.0 mg/kg,实际样品6次测定相对标准偏差为1.1 %～5.7 %,加标回收回收率为87.7 %～108.9 %。该方法经济环保、准确快捷,可作为大气沉降重金属检测参考方法。     

Determination of trace and platinum-group elements in high ionic-strength volcanic fluids by sector-field inductively coupled plasma mass spectrometry (ICP-MS)

The accurate measurement of ultra-trace concentrations of rare metals and platinum group elements in volcanic fluids is complicated by interferences, complex matrices, and preferential element partitioning. We analyzed condensed, high-temperature magmatic fluids collected from Kudryavy volcano (Kurile Islands, Russia) for Be, B, Rb, Sr, Mo, Ru, Rh, Pd, Cd, W, Re, Pt, Pb, Bi, and U using ICP-MS. The samples had three different matrices: 5 mol L^–1 sodium hydroxide (NaOH, pH = 11), gas condensates of sulfuric acid (H₂SO₄, pH = 0), and solid elemental sulfur. Interferences and suppression/enhancement effects were investigated using standards in concentrated NaOH and H₂SO₄ solutions to determine adequate dilution for sample analyses, which then required very low levels of element detection (< 1 μg L^–1 for most elements). Depending on the field sampling technique of volcanic gas vents, our results show significant differences in concentrations of some trace elements due to the precipitation of solid sulfur during gas condensation and variations in element volatility as a function of temperature. Received: 1 March 1998 / Revised: 1 July 1998 / Accepted: 7 July 1998     

Determination of trace and platinum-group elements in high ionic-strength volcanic fluids by sector-field inductively coupled plasma mass spectrometry (ICP-MS)

The accurate measurement of ultra-trace concentrations of rare metals and platinum group elements in volcanic fluids is complicated by interferences, complex matrices, and preferential element partitioning. We analyzed condensed, high-temperature magmatic fluids collected from Kudryavy volcano (Kurile Islands, Russia) for Be, B, Rb, Sr, Mo, Ru, Rh, Pd, Cd, W, Re, Pt, Pb, Bi, and U using ICP-MS. The samples had three different matrices: 5 mol L^–1 sodium hydroxide (NaOH, pH = 11), gas condensates of sulfuric acid (H₂SO₄, pH = 0), and solid elemental sulfur. Interferences and suppression/enhancement effects were investigated using standards in concentrated NaOH and H₂SO₄ solutions to determine adequate dilution for sample analyses, which then required very low levels of element detection (< 1 μg L^–1 for most elements). Depending on the field sampling technique of volcanic gas vents, our results show significant differences in concentrations of some trace elements due to the precipitation of solid sulfur during gas condensation and variations in element volatility as a function of temperature.     

微波消解-电感耦合等离子体质谱法(ICP-MS)测定板栗中的矿物元素及稀土元素[ ]

采用微波消解前处理方法,结合电感耦合等离子体质谱技术,建立了板栗中钠（Na）、钾（K）、镁（Mg）、锰（Mn）、铁（Fe）、钒（V）、钴（Co）等19种矿物元素及镧（La）、铈（Ce）、镨（Pr）、钕（Nd）、钐（Sm）、铕（Eu）、钆（Gd）、铽（Tb）、镝（Dy）、钬（Ho）、铒（Er）、铥（Tm）、镱（Yb）、镥（Lu）、钇（Y）等15种稀土元素的同时分析测定方法。该方法检出限为0.0027~0.78μg?L-1,相对标准偏差为1.4%~6.3%。通过国家标准物质GBW10019苹果的准确率实验验证,测定结果均在标准证书值范围内。实验结果表明,该方法适用于板栗中矿物元素及稀土元素的同时测定。     

微波消解-电感耦合等离子体质谱(ICP-MS)法测定黑土地地表基质调查样品中碘

碘是活跃元素,价态多,各价态间易相互转化,使其具有熔点低、易挥发,严重记忆效应的独特性质,其分析一直是个挑战。传统方法如半熔法、高压密闭法等存在操作难度大、消解时间长、工作效率低等问题。通过采用硝酸-氢氟酸微波消解处理样品,并利用电感耦合等离子体质谱（ICP-MS）法测定碘含量,克服了传统碘分析方法的一列问题。研究了不同酸体系和赶酸时间对样品分解效率和挥发损失的影响,同时验证了不同冲洗液对降低碘记忆效应的效果。在此基础上,确定了最佳反应条件为7 mL硝酸 +1 mL氢氟酸混合酸比例,180 ℃赶酸控温程序,并采用2% NH3·H2O充当冲洗液,降低了ICP-MS测定过程中的记忆效应,提高测试的稳定性。为验证该方法的准确性和精密度,使用国家一级标准物质进行方法验证。结果表明,方法的准确度(?lgc)为0.001～0.004,相对标准偏差(RSD)为1.2%～3.4%,相关系数为0.999 8,检出限为0.17 mg/kg,定量限为0.54 mg/kg,表现出较好的准确度和精密度,满足规范要求。通过实际样品测试,进一步验证了该方法的可行性,实验结果表明相对偏差在1.6%～4.1%。该方法操作方便、试剂用量少、工作效率高,适用于测定黑土地地表基质调查样品,同时也为碘的快速、准确分析提供了一种可行的解决方案。     

Determination of vanadium by reaction cell inductively coupled plasma mass spectrometry

Recent advances in inductively coupled plasma mass spectrometry (ICP-MS) have included the addition of interference reduction technologies, such as collision and reaction cells, to improve its detection capability for certain elements that suffer from polyatomic interferences. The principle behind reaction cell (RC)-ICP-MS is to remove a particular polyatomic interference by dissociation or formation of a different polyatomic species that no longer interferes with the analyte of interest. However, some interferences cannot be removed by commonly reported reaction gases, such as hydrogen, oxygen, or methane, necessitating using more reactive and hazardous gases, such as ammonia. The current study investigates oxygen as a reaction gas in RC-ICP-MS to specifically react with vanadium analyte ions, rather than the interferents, to produce a polyatomic analyte species and thereby provide a way to analyze for vanadium in complex environmental matrices. The technique has been tested on a series of river water, tap water, and synthetic laboratory samples, and shown to be successful in vanadium analyses in high chloride and sulfate matrices. The zinc isobaric interference on the new vanadium oxide analyte at m/z 67 is also investigated, and can be corrected by using a standard mathematical correction equation. The results of this study further increase the utility of RC-ICP-MS analytical techniques for complex environmental matrices.     

茶叶和蔬菜中铅的同位素稀释电感耦合等离子体质谱的测定

采用同位素稀释电感耦合等离子体质谱(ID-ICP-MS)法测定了铅的含量,通过对茶叶标准物质(GBW-07605)中铅的测定,考察了方法的准确度和精密度,比较了同位素稀释法与普通外标定量法的测定结果。在5mLHNO3～0.5mLHF～1mLH2O2的消解体系中,ID-ICP-MS法测量茶叶中铅的回收率可达97.7%,相对标准偏差(RSD)小于1.2%。实验对市售的12种茶叶和10种蔬菜中Pb进行测定,铅含量符合相应国家标准的样品分别占总样品数的83%和90%。该法适合于植物样品中微量铅的测定。     

Determination of trace elements in granites by inductively coupled plasma mass spectrometry

Proposed is a simple and reliable method for the dissolution of granite and the determination of 38 elements by inductively coupled plasma mass spectrometry. One hundred milligrams of sample are digested with 1 ml of HF and 0.5 ml of HNO(3) in screw top PTFE-lined stainless steel bombs at 190 degrees C for 12 h. Insoluble residues are dissolved using 8 ml of 40% HNO(3) (v/v) heated to 110 degrees C for 3 h. Six granite standard reference materials (GSR-1, JG-2, G-2, NIM-G, SG-3, SG-1a) were studied. Analytical calibration was accomplished using aqueous standard solutions. Rhodium was used as an internal standard to correct for matrix effects and instrument drift. We report data for: Li, Be, Sc, V, Cr, Co, Ni, Cu, Zn, Ga, Rb, Sr, Y, Zr, Nb, Mo, Cs, Ba, Hf, Ta, W, Pb, Th, U and 14 of the rare earth elements. The recoveries for most of these elements in granite ranged from 90 to 110%.