ICP-MS法测定罐装鱼中5种元素含量的国际比对及其结果分析

在英国食品分析水平评估计划(FAPAS) 组织的罐装鱼残留无机元素的能力测试项目中,采用微波消解前处理方法,电感耦合等离子体质谱(ICP-MS)法同时测定,标准加入法定量分析罐装鱼中砷、镉、汞、铜、铅的含量,方法可靠,结果令人满意。通过对FAPAS能力验证结果统计报告的研究,从测定结果、样品前处理、检测方法等方面对统计结果进行了综合分析。     

微波消解-原子荧光光谱法四通道同时测定中草药中砷、锑、铋和汞元素含量

研究了一种微波消解-原子荧光光谱法四通道同时测定中草药中砷、锑、铋和汞元素含量的方法。实验对仪器条件进行了优化,对方法进行了验证,并对中草药样品进行了砷、锑、铋和汞元素含量的测定。实验结果表明:相关系数R2均在0.9988以上,相对标准偏差均小于1.54%,砷、锑、铋和汞检出限分别为0.019ng/mL、0.015ng/mL、0.008ng/mL和0.005ng/mL;测定柑橘叶标准物质和黄芪标准物质的结果与标称值相符;样品加标回收率为90.8%~114.1%。采用该方法可以准确地测定中草药中砷、锑、铋和汞元素含量,四通道同时测定4种元素,减少了试剂消耗,提高了分析效率,该方法值得推广。     

固体进样-原子荧光法测定煤中的汞

建立了一种固体直接进样-原子荧光快速测定煤中汞含量的方法 ,无需进行样品的消解前处理,提高了检测效率。实验对仪器条件进行了优化,对方法进行了验证,并对煤样品进行了汞含量的测定。实验结果表明:用汞标准溶液和煤标准物质建立标准曲线对测量结果无明显差异,可以用汞标准溶液代替煤标准物质建立标准曲线;相关系数均在0.9980以上,线性关系良好,相对标准偏差小于5.0%,检出限为13pg;测定煤标准物质和土标准物质的结果与标称值相符;样品加标回收率为85.3%~99.6%。利用固体进样原子荧光测煤中的汞,方法准确、快速、灵敏、可靠。     

全自动热解测汞仪测定粮食中汞及干扰分析

介绍了一种快速测定粮食中总汞的分析方法,本方法基于"燃烧-催化燃烧-冷原子吸收(C-CAAS)"原理,可准确测定汞含量较低粮食样品如大米、小麦、玉米等。将本方法与国标GB/T 5009.17—2014中"化学蒸汽发生-原子荧光法(HG-AFS)"进行对比,结果表明:本方法准确度、重复性均优于国标推荐方法,是一种高效、环保的汞分析技术。以进样量0.20g计算,方法检出限为0.02μg/kg,定量限为0.08μg/kg,相对标准偏差1.2%(@1ng Hg),样品加标回收率为90.2%～102.7%。这种快速、准确的汞分析方法,是粮食质量安全监管的利器,可指导超标粮食收购与储存,严防不符合食品安全标准的粮食流入口粮市场。     

直接测汞仪测定食品中的总汞

运用DMA-80型直接测汞仪,对不同类型的膳食样品(主要是谷类、奶粉、鱼类、蔬菜水果等)进行汞含量的分析测定。通过实验建立食品中总汞的测定方法。采用直接测汞仪,样品无需做任何消解以及前处理,无论固体样品还是液体样品均可用汞原子蒸气在253165nm处的共振线具有强烈的特征吸收进行测定。通过测定得到方法的检出限,线性范围,精密度和准确度。     

蒸气发生—原子荧光法测定中药材中的砷、汞、铅

研究了测定五种中药材中痕量的砷、汞、铅，建立了一种聚四氟乙烯消化罐梯度升温消解样品的方法，采用蒸气发生与原子荧光法联用技术进行测定。测得砷、汞、铅的回收率分别为94．5％、106．6％、106．0％。该方法完全可以用于中药材中砷、汞、铅的含量测定。     

直接测汞法快速测定酵母中微量总汞

利用直接测汞法对酵母中微量总汞进行快速分析测定。样品无需消解处理,直接进样,采用金质媒介吸附,形成金汞齐,高温加热释放汞单质,由冷原子吸收光谱法进行测试。总汞含量在0~10ng范围内,二次线性相关系数好(R2=1),样品加标回收率(n=6)为96.7%~100.8%,相对标准偏差(RSD)为1.2%~2.6%,方法检出限为0.063μg·kg-1。同时与原子荧光光谱法测试结果进行对比,分析结果一致。本方法准确度高、稳定性好、分析速度快,可用于酵母中总汞含量的检测。     

氢化物发生原子荧光光度法测定内墙涂料中可溶性汞含量的不确定度评定

对氢化物发生原子荧光光谱法测定内墙涂料中可溶性汞含量的测量不确定度进行评定。分析测量过程中引入的不确定度来源,对各不确定度分量进行量化和分析。结果表明,样品测量的重复性、标准曲线拟合、仪器引入是影响不确定度的主要因素。通过合成评定得到相对不确定度及测试结果,原子荧光法测定内墙涂料中的可溶性汞为0.036±0.003mg/kg。     

微波消解－氢化物原子荧光法测定洪泽湖水产品中的汞

建立了微波消解样品,原子荧光法测定水产品中汞的方法。对样品的消解条件、仪器条件、酸度、还原剂等影响进行了实验并测定了水产品中汞含量。结果表明：汞含量在0～1.0ng／mL的范围内线性良好,线性方程Y ＝24.12＋217.01 X ,r＝0.9999。方法检出限为0.031 ng／mL。样品加标浓度为0.1～0.4 ng／mL时,方法回收率为96.4％～98.7％。方法操作简便、定量准确可靠,重现性好,可以满足水产品中汞检测的要求。     

同位素稀释-电感耦合等离子体质谱法测定沉积物中铬和汞

采用同位素稀释-电感耦合等离子体质谱法（ID-ICP-MS）测定沉积物中铬和汞,分别以铬、汞单元素溶液标准物质标定⁵³Cr和²⁰²Hg浓缩同位素,将稀释剂与样品混合均匀后,加酸进行消解。对质谱测定过程的数据采集参数进行优化,探究基体效应以及H2和He两种模式对铬测定的影响。为防止汞的记忆效应干扰比值的测定,采用5 mg/L EDTA、2.5 mg/L Au溶液和3%硝酸交替冲洗管路系统,分别测定了²⁰⁰Hg/²⁰²Hg和¹⁹⁹Hg/²⁰²Hg两组比值,并比较测定结果。结果显示：积分时间为0.5 s时,同位素比值的测定精密度较好,对测定样品进行稀释能够消除质谱及基体效应干扰。H₂和He模式均适用于该类样品中铬的测定,²⁰⁰Hg/²⁰²Hg和¹⁹⁹Hg/²⁰²Hg两组比值对汞的测定结果无显著性差异,沉积物中铬和汞含量分别为81.7 mg/kg和0.471 mg/kg,相对标准偏差分别为0.35%和0.99%。采用美国NIST2709a标准物质进行方法验证,验证结果与标准值一致。该方法准确度高、精密度良好,适用于沉积物、土壤等基体样品中铬和汞的高准确度测定。     

液相色谱-电感耦合等离子体质谱联用技术测定水产品中汞化合物形态

The method for determination of mercury speciation analysis in seafood by HPLC-ICP-MS has been established. Using hydrochloric acid extract, C18 Chromatography column (4.6 mm×150 mm), mobile phase is 5% methanol-0.06 mol·L^－1 ammonium acetate-0.1% cysteine , the linear range for three mercury species are all between 0 and 100 μg·L^－1, the linear coefficient(r) are all more than 0.999 0, detection limits are between 0.5—0.8 ·L^－1; the relative standard deviations (RSD) for the determination of three mercury species are all less than 5%; the recoveries of different concentrations of mercury compounds: inorganic mercury is 72.5%—89.8%, methylmercury is 99.2%—117.6%, ethylmercury is 93.1%—111.2%; determination of mercury speciation analysis in fish reference material (GBW10029) and human hair reference material (GBW09101B) are all in the scope of standard values. The International Comparison in FAPAS of methylmercury, the result of Z score is 1.0. The experiments show that: this method had simple pre-treatment method, broad line-arrange, good accuracy and precision, it has been applied for determination of mercury speciation in aquatic product.     

使用汞分析器检测矿渣及水泥中的汞

以矿渣和水泥作为研究对象,采用汞分析器对其中的汞进行检测。水泥是一种建筑过程中广泛使用的高凝结材料。由于汞具有较大的毒性,因此必须严格检测建筑材料中汞的含量以降低其对人体的损害。作为水泥的替代物,矿渣具有许多的优点,例如价格低廉、毒性较小等。     

Accurate Calibration of Mercury Vapour Indicators for Occupational Exposure Measurements using a Dynamic Mercury Vapour Generator

Abstract

An accurate and rapid calibration procedure for mercury vapour indicators used for occupational exposure measurements is described, using a dynamic mercury vapour generator traceable to the standard bell-jar calibration apparatus. The method provides greater flexibility, accuracy, and trace ability than the usual methods for the calibration of mercury vapour indicators used for occupational exposure measurements. The calibration procedure allows a correction to be applied to the mass concentration value displayed by the mercury vapour indicator. Measurement results from the mercury vapour indicator at the occupational exposure limit of 25 µg ·m^?3, following calibration, have been estimated to have an expanded uncertainty of 8%.     

Seawater Mercury Analysis at PPB Levels

Abstract

A new method of mercury detection at ng/mL concentrations in seawater, by total reflection x‐ray fluorescence (TXRF), is presented. Membranes that have complexation affinity to the mercury ions were produced on quartz reflectors. They were immersed in various seawater solutions containing mercury at low concentration (1–50 ng/mL) and they were left to equilibrate for 24 hours; membranes were well fixed on the reflectors. After the equilibration stage, they were taken out of the solution and they were analysed by TXRF; the minimum detection limit was determined to be equal to 0.4 ng/mL. The main ingredient of the membranes was the complexing reagent dithizone. The existence of high salt concentration in seawater did not prevent mercury's complexation from the membrane.     

Method for the Determination of Mercury in Very Small Solid Samples

Abstract

An alternative method for the determination of mercury (Hg) in solid samples is presented in this article. Gaseous Hg is evolved when a solid sample is heated above 500°C in the presence of oxygen. The evolved Hg is collected on silver wool and is analyzed using cold vapor methods. We have found greater than 95% Hg recovery with various sediment and ash standards.     

汞分析仪及其应用

介绍了美国ＴＳＰ公司汞分析仪的工作原理，仪器组成和特点及其应用情况。     

Wide Range Continuous Mercury Vapor Monitor

ABSTRACT

The mercury vapor monitor, MDC-1-01, described in this paper is the first prototype in the MDC series. It was designed and developed in our laboratory to measure airborne mercury vapor on a “continuous” basis in the range of 400 ng to 20 mg mercury per cubic meter of air.

In comparison with other instruments, commercially available, it uses much improved principles as regards electronics, optics, and chemistry [l]. The double beam assembly, in combination with a selective filter, permits the measurement of mercury vapor in the presence of the most commonly encountered organic vapors and dusts. Practical applications are discussed.     

现代测汞技术的发展

简述分光光度、原子吸收、原子荧光、色谱法、电感耦合等离子体质谱法等现代分析仪器在汞分析中的应用,并对各种分析方法进行比较,介绍原子荧光光谱技术在汞分析中的巨大优势。     

原子荧光形态分析仪在汞、锑形态分析中的应用

原子荧光形态分析仪SA-10是基于高效液相色谱和氢化物发生原子荧光联用技术的一台元素形态检测仪,该仪器对汞和锑形态的分析性能是：Hg（Ⅱ）、MetHg、EtHg、Sb（Ⅲ）和Sb（Ⅴ）的检出限分别为0．5．0．3,0．4、1和5μg／L,线性范围分别是0．5～1000、0．3～1000、0．4～1000、1～1000和5～1000μg／L,该区间内的线性相关系数均大于0．9990,标准偏差均小于3．0％。本文主要介绍了该仪器在海产品、环境水样、土壤中的汞形态分析和化妆品中的锑形态的应用。     

同位素稀释-液相/气相-电感耦合等离子体质谱联用等方法为鱼肉中甲基汞成分标准物质准确定值

The fish tissue certified reference material is designed and prepared mainly for evaluating the determining accuracy of methyl mercury in sea fish or other seafood, as well as for a quality control standard. The property value was certified by three different methods, including high performance liquid chromatographic -cold vapor atomic fluorescence spectrometry（HPLC-CVAFS）method and species specific isotope dilution mass spectrometric analysis (IDMS) using an inductively coupled plasma mass spectrometer as detector after liquid chromatography (LC-ICP-MS) or gas chromatography (GC-ICP-MS). The experiment included spiking, extraction, derivatization, separation and detection procedures. The ERM 464 tuna fish reference material was used as the analytical quality control standard. The results obtained from three different methods were in good agreement. And the statistic average values were used as certified values of methylmercury in the fish tissue CRM.