用电感耦合等离子体质谱法测定中草药中重金属元素

建立了用电感耦合等离子体质谱法(ICP-MS)测定中草药中重金属元素(砷、铅、镉、铬、汞、镍)的方法.中草药样品用硝酸和过氧化氢经微波消解后,消化液直接用ICP-MS同时测定6种重金属元素.以钪、钇、铟和铋作为内标物质,补偿了基体效应;选择适当的待测元素同位素克服了质谱干扰;6种重金属元素的检出限在0.001～0.006 μg·L-1之间,回收率在90%～107%之间,相对标准偏差小于3.2%.     

微波消解-电感耦合等离子体质谱法测定人面果树中的重金属元素

建立了微波消解-电感耦合等离子体质谱(ICP-MS)法测定人面果树中As,Cr,Cd,Pb,Ni,Se,Hg 7种重金属元素含量的方法。样品采用HNO3-H2O2消解体系,避免了赶酸的操作,经微波消解后,用电感耦合等离子体质谱(ICP-MS)测定样品中As,Cr,Cd,Pb,Ni,Se,Hg 7种重金属元素的含量。方法对7种元素的校准曲线的相关系数r>0.9997,检出限在0.0098～0.0874μg/L之间,回收率在93%～115%之间,RSD在0.41%～4.9%。     

电感耦合等离子体质谱测定地质样品中多种元素

用电感耦合等离子体质谱(ICP-MS)测定了地质样品中多种元素。考察了测量过程中的基体效应及质谱干扰,利用In内标,补偿由于基体效应的影响所引起的测量偏差,建立校正公式校正质谱干扰。方法的检出限为0.06~250ng/L,精密度为1.7%~3.2%,加标回收率为91%~108%,方法适于批量地质样品分析。     

电感耦合等离子体发射光谱(ICP-OES)法同时测定高纯钼中多种痕量元素

建立了电感耦合等离子体发射光谱(ICP-OES)法测定钼中Co、Cu、Fe、Mg、Mn、W、Zr元素含量的方法。确定了溶样方法和分析谱线,采用基体匹配消除干扰。对方法精密度和准确度进行实验,实验结果表明,各元素的相对标准偏差均小于3%,加标回收率在81.0%~110%。所建方法快速、准确,适用于钼中多元素同时测定。     

KED碰撞模式-电感耦合等离子体质谱（ICP-MS） 法测定血液、尿液中8种重金属和准金属元素

在金属中毒与死亡案件中,实验室常用的标准曲线法对人体内重金属和准金属元素的定量分析的准确性易受不同人群血液、尿液基质差异以及基质效应的影响,为此建立了直接稀释-电感耦合等离子体质谱结合标准加入法测定人体血液和尿液中Cr、Co、Ni、As、Cd、Sb、Pb、Tl等8种重金属和准金属元素含量的方法。优化了碰撞气流量和载气流速,提高了对8种目标元素定性定量的灵敏度;探究了不同体积分数下ICP-MS增敏剂Triton X-100和乙醇对元素响应值的影响,采用0.1% HNO3-0.05% Triton X-100混合溶液作为血液稀释剂稀释检材50倍,0.1% HNO3-1%乙醇混合溶液作为尿液稀释剂稀释检材10倍,提高样品溶液中元素的响应值的同时避免了未消解有机物对仪器信号的影响。标准加入法的应用避免引入其他空白样品定量目标元素,保持定量过程中基质的一致性从而克服了样品中的基质效应,采用动能歧视（KED）模式对直接稀释后的目标元素进行测定,干扰离子与He碰撞裂解有效降低了多原子离子干扰,并选择60 s的清洗时间降低了元素的记忆效应。该方法各元素检出限（LOD）为0.0060~0.0630 μg/L,定量限（LOQ）为0.0200~0.2100 μg/L,血液和尿液中的回收率为78.85%~117.88%,日内和日间精密度均小于8.7%。建立的方法快速准确、灵敏度高、操作安全,方法及相关数据可以为相关案件中血液、尿液检材中重金属和准金属元素的检验鉴定提供方法参考和数据支撑。。     

车载电感耦合等离子体质谱法现场快速测定水中22种重金属元素

近年来,我国发生了多起水质重金属污染事件,有2010年7月紫金矿业酮酸水渗漏事件、2010年10月广东省北江流域铊污染事件、2012年1月广西龙江镉污染事件、2013年7月广西贺江镉/铊污染事件、2015年甘肃陇南锑污染事件、2017年5月四川广元铊污染事件等。上述重金属污染事件对我国水环境带来了非常严重的影响并产生了巨大的经济损失,因此现场快速有效地开展应急监测,经筛查后准确获取重金属污染信息,为应急决策提供技术支撑,最大程度地降低经济损失、充分保障水质安全具有非常重要的意义。     

电感耦合等离子体质谱法同时测定枇杷叶中多种无机元素

枇杷叶试样于聚四氟烯消解罐中加入硝酸及过氧化氢置于微波炉中加热消解,对所得试样溶液中的14种无机元素用电感耦合等离子体质谱法同时测定.在测定钙、锰、镁、磷及铁的试验中,测得其线性范围在0～200μg·L-1之间,用标准加入法对所测定的14种无机元素作了回收试验,所得回收率在90%～110%之间.按规定要求测定14种无机元素的检出限,测得结果在0.002～0.4μg·L-1之间.     

微波消解/ICP-MS同时测定粮食、蔬菜中的11种重金属元素

建立了微波消解/电感耦合等离子体质谱法同时测定粮食和蔬菜中11种重金属元素(Cu、Mn、Cr、Pb、Cd、Ni、Sb、Hg、Co、Ag、As)的方法,优化了微波消解条件和仪器测定条件,采用HNO_3-HF-H_2O_2和HNO_3-H_2O_2两种混酸体系,将样品进行完全消解。结果显示,11种金属元素的线性系数不小于0.999 5,方法的检出限为0.001~10.00μg/L,测定的相对标准偏差(RSD,n=5)不大于5.0%。该方法具有快速、简便、灵敏度高、稳定性好、准确度高等优点。     

ICP-MS测定醋酸酯淀粉中7种元素含量

建立了醋酸酯淀粉中7种元素含量微波消解-电感耦合等离子体质谱(ICP-MS)测定方法。通过比较干法、湿法、微波消解三种醋酸酯淀粉前处理方法,选用耗时短、回收率高、操作稳定的微波消解法对醋酸酯淀粉进行消解,利用ICP-MS法测定硼、铝、铬、镍、砷、镉、铅7种元素含量。该方法线性范围广,线性相关系数r0.999 7,回收率92.0%~100.3%,RSD3.8%。具有操作简单、快速、准确、可靠等优点,在醋酸酯淀粉分析中,取得了令人满意的结果。检测结果表明,醋酸酯淀粉中铝含量在4 mg/kg~7 mg/kg,其余元素均小于0.2 mg/kg。     

正交试验在原油重金属元素测定中的应用

采用微波消解技术,以ICP-AES同时测定原油中V、Ni、Mn、Pb重金属元素的含量。该方法回收率在94.73%～107.2%之间,相对标准偏差小于2.12%,适用于原油中各种重金属元素的测定。采用正交设计法安排实验,可以以少量的实验次数获得大量信息,既节省时间又节约药品。同时利用原油样品中的V/Ni的比值作为参数,可判断原油油源的特征及地质特点。     

Determination of heavy metals in groundwater samples — ICP-MS analysis and evaluation

An analytical programme which permits the direct, simultaneous determination of Al, As, Cd, Cr, Cu, Mn, Ni, Pb and Zn in groundwater samples was developed for ICP-MS. Spectral mass interferences, attributable to great differences in groundwater matrices, precision and accuracy have been discussed. The evaluation of analytical results was demonstrated for selected sampling points of the groundwater observation network of Thuringia.     

ICP-MS determination of heavy metals in submerged cultures of wood-rotting fungi

Accumulation of five heavy metal ions by five species of wood-rotting basidiomycetes during a 9-day cultivation was studied. Contents of Cd, Cu, Pb, and Zn were measured using ICP-MS; the amount of mercury was determined directly in solid samples using the Advanced Mercury Analyser. A standard operation procedure for the sample preparation and determination of metal content was developed and validated. Presence of Cd, Cu, Hg, and Pb decreased the accumulation of zinc by the fungi. The basidiomycete Pycnoporus cinnabarinus exhibited the highest metal binding capacity of all fungi tested.     

尿样中铀同位素的ICP-MS快速测量技术研究

核事故状态下的应急处理,要求对环境介质中的放射性核素进行快速分析。尿样中铀同位素测量作为内照射剂量评价的主要手段,其分析效率越高,则对核事故中涉铀人员的安全救治越及时、有效。而尿样中其它无机离子是铀含量的106倍,导致ICP-MS测量过程中尿盐堵塞进样毛细管。为降低样品的含盐量并获得较好的检测结果,本文对样品预处理过程进行优化。采用先加热氧化去除有机物,再进行1～10倍稀释后测试样品的铀同位素丰度及浓度。结果表明：将25 mL样品稀释至100 mL后效果最佳,分析方法不确定度为5.4 %,回收率95 %~105 %。     

Liquid chromatographic determination of quinolones in water and human urine samples after microextraction by packed sorbent

A method for the simultaneous determination of quinolones in water and urine samples by microextraction in a sorbent-packed syringe (MEPS) with LC is described. MEPS is a new miniaturized SPE technique that can be used with chromatographic instruments without any modifications. In MEPS, approximately 1 mg of the solid packing material is inserted into a syringe (100-250 microL) as a plug. Sample preparation takes place on the packed bed. The new method is promising, easy to use, economical, and rapid. The determination of quinolones in groundwater and urine was performed using MEPS as a sample preparation method with LC-UV determination. Four quinolone antibiotics--enrofloxacin, enoxacin, danofloxacin, and nalidixic acid--in groundwater and urine samples were used as analytes. The extraction recovery was found to be between 64.9 and 98.9%. The results showed high correlation coefficients (R2 > 0.992) for all of the analytes within the calibration range. The LOQ was between 0.091 and 0.315 ng/mL.     

Determination of metals and metalloids in light and heavy crude oil by ICP-MS after digestion by microwave-induced combustion

A method for light and heavy crude oil digestion using microwave-induced combustion (MIC) in closed vessels is described for further determination of Ag, As, Ba, Bi, Ca, Cd, Cr, Fe, K, Mg, Li, Mn, Mo, Ni, Pb, Rb, Se, Sr, Tl, V, and Zn by inductively coupled plasma mass spectrometry (ICP-MS). Conventional microwave-assisted acid digestion (MW-AD) in pressurized vessels and analyte determination by inductively coupled plasma optical emission spectrometry (ICP OES) were also used for results comparison. For MIC procedure, samples were wrapped in polyethylene films and combusted using 20 bar of oxygen and 50 µl of 6 mol l^− 1 ammonium nitrate as aid for ignition. The concentration of nitric acid used as absorbing solution was evaluated (1, 2, 4, 7, 10 and 14 mol l^− 1) using an additional reflux step after combustion. Accuracy was evaluated for As, Ba, Ni, Se V, and Zn using certified reference material (CRM) with similar matrix composition and for Cr, Fe, K, Mg, Mn, and Mo by neutron activation analysis (NAA). Recovery tests were also performed for all the analytes by MIC and they were better than 97% using 2 mol l^− 1 nitric acid as absorbing solution (with reflux step). Agreement with certified values and NAA results was better than 95%. Using MIC it was possible to obtain lower limits of detection (LODs) by ICP-MS and also by ICP OES in comparison with those obtained by MW-AD. In spite of both sample preparation techniques were apparently suitable for crude oil digestion, MIC was preferable in view of the possibility of using diluted nitric acid as absorbing solution that is an important aspect to minimize interferences by ICP-MS and ICP OES. In order to avoid polyatomic interferences on ⁵²Cr and ⁵⁶Fe determinations by ICP-MS, a dynamic reaction cell with ammonia gas was used. Residual carbon content in digests obtained by MW-AD and MIC was 15% and < 1%, respectively. Using MIC the simultaneous digestion of 8 samples was possible in less than 30 min.     

The determination of nitrogen in metals by isotope dilution

A wet chemical procedure for determining the amount of nitrogen in a metal or alloy has been developed which utilizes the isotope dilution technique. Ammonium sulfate, either enriched or depleted in ¹⁵N, is added to the metal sample during solution procedures. Ammonium ions resulting from the hydrolysis of bound nitrogen in the metals mix with that of the tracer and the total is then oxidized to N₂ in which form the element is analyzed in the mass spectrometer. The method has been tested on a variety of metals and alloys including thorium, lanthanum, yttrium, titanium, chromium, manganese, various steels, nickel-chromium, ferrotitaniuin, ferromanganese and ferrochromium. The range of nitrogen in these materials was from -2 ppm to almost 6%. Average precision was generally better than ± 5%.     

ICP-MS multielement determination in fly ash after microwave-assisted digestion of samples

A microwave assisted digestion procedure has been developed for dissolution of fly ash samples prior to the inductively coupled plasma-mass spectrometric determination of their elemental composition. The developed methodology was validated by carrying out the analysis of two high-silicate containing reference materials (CRM 134R sewage amended soil and NIES JR 1 rock) and by means of the comparison between results found by microwave-assisted digestion and ICP-MS of fly ash samples with those found by neutron activation analysis (NAA) for Sb, Cs, Cr, Co, Fe, U and Zn determination. The method developed can be recommended for routine multielement analysis of fly ash.     

Direct analysis of solid samples by GFAAS – determination of trace heavy metals in barytes

Solid sampling graphite furnace atomic absorption spectroscopy (SS-GFAAS) has been used for the determination of traces of heavy metals (Cd, Pb, Cu, Cr, Ni, V and As) in barytes over a wide concentration range, e.g. Cd from 0.023 to 27.0 μg/g and Pb from 1.54 to 3509 μg/g.The necessity of determining heavy metals in commercial barytes (naturally occurring barium sulfate), a mineral important to the oil industry because of its use in drilling muds, is discussed. The problems presented by the analysis of this difficult matrix are elegantly solved by using SS-GFAAS for the direct determination of heavy metals. A high-performance graphite furnace AAS with D₂-background correction system and a transversely heated graphite atomizer was used for the investigations. The spectrometer was combined with a mechanical sampling module and an ultramicrobalance. The transfer of solid samples (sample weights 0.031–0.686 mg) into the atomizer was carried out by using an optimized graphite platform as the sample carrier. Calibration curve techniques and standard addition methods were employed using external standards (CRMs). Problems associated with signal deformations like multiple peaks, tailing or shoulders are also discussed and possibilities to solve the problems are given. The influence of the homogeneity of solid samples on the precision and accuracy are shown in a real example. The results obtained by SS-GFAAS were compared with results by other methods like X-ray fluorescence spectroscopy (XRF) and flame AAS after aqua regia microwave extraction. This study has demonstrated that SS-GFAAS is a very powerful and easy-to-use method for quick and accurate analysis of barytes. Received: 9 November 1998 / Revised: 29 January 1999 / Accepted: 2 February 1999     

ICP-MS 法直接测定冰芯样品中超痕量镉

采用 ICP- MS法对冰芯样品中超痕量 Cd的直接测定进行了研究。确定了直接测定浓度为 pg/m L 级的 Cd的最佳仪器参数、载气流速、进样速度等与灵敏度之间的关系以及浓度和扫描参数对分析精度的影响。本方法对浓度 5～2 0 0 pg/m L Cd的分析 ,RSD<1 0 % ,回收率在 88%～ 1 0 5%之间 ,检测限为0 .1 5pg/m L     

Substoichiometric extraction of metals and its application to the determination of heavy metals in environmental samples by neutron activation analysis

Solvent extraction as a technique for the separation of ionic solutes and the advantages and application of substoichiometric extraction in neutron activation analysis have been discussed. The application of this technique has been elucidated with reference to the determination of Zn, Cd and Hg in environmental samples. The decontamination factor, accuracy, precision, sensitivity and radiochemical purity of the separated fraction have been discussed.