两种前处理方法对液相色谱-电感耦合等离子体质谱法测定土壤中有机汞的比对研究

分别采用酸浸提法和碱消解法作为前处理方法,以液相色谱电感耦合等离子体质谱法(HPLC-ICP-MS)作为测定方法测定土壤中的有机汞(甲基汞、乙基汞和苯基汞),对2种前处理方法进行比对分析。结果表明,采用酸浸提法,3种有机汞的方法检出限为0.5~0.9μg/kg,甲基汞和乙基汞的加标回收率为72.4%~86.4%,相对标准偏差(RSD)均<9.3%,苯基汞的回收率均<40%,RSD为7.4%~10.2%;采用碱消解法,3种有机汞的方法检出限为0.3~0.4μg/kg,加标回收率为60.4%~106%,RSD均<8.6%。碱消解法相较于酸浸提法,具有更高的萃取效率,更好的回收率和重复性。     

HPLC-ICP/MS联用测定废水中甲基汞和无机汞

采用高效液相色谱(HPLC)-电感耦合等离子体质谱(ICP/MS)联用测定废水中可滤态的甲基汞和无机汞,优化了仪器工作条件,讨论了方法干扰及校正办法。甲基汞和无机汞在0.500μg/L~25.0μg/L范围内线性良好,检出限分别为0.03μg/L和0.07μg/L,废水样品平行测定的RSD分别为6.5%~7.6%和6.2%~6.8%,加标回收率分别为84.0%~87.0%和88.0%~92.4%。     

高效液相色谱-氢化物发生-原子荧光光谱联用技术测定水中烷基汞

建立了高效液相色谱(HPLC)-氢化物发生(HG)-原子荧光光谱(AFS)联用技术分析地表水及废水中甲基汞和乙基汞的方法。样品经二氯甲烷萃取,再以半胱氨酸+乙酸铵溶液反萃取富集,并进入高效液相色谱分离,经形态分析预处理装置后,借助原子荧光光谱法检测。在优化分离条件下,甲基汞和乙基汞在1～50μg/L范围内呈现良好的线性关系,对于标准水样、地表水和废水实际水样,加标平均回收率均为80%～110%。平行进样7次1μg/L的汞混合标准溶液,甲基汞和乙基汞的色谱峰面积的相对标准偏差分别为5.2%和3.9%,检出限则分别为0.4 ng/L和0.7 ng/L。该检测方法前处理简单、回收率稳定、灵敏度和准确度高、检出限低、杂质干扰少、监测费用低,便于在普通实验室推广和应用。     

液液萃取-HPLC-ICPMS联用技术测定水体中甲基汞

建立了二氯甲烷萃取,半胱氨酸-乙酸铵溶液反萃取,液相色谱-电感耦合等离子体质谱法测定水中甲基汞的方法。取样量为1 L时,方法检出限为0.1 ng/L,相对标准偏差为6.6%~13%,地表水、生活污水和工业废水3种实际水样的加标回收率分别为45.6%~70.5%、37.0%~65.6%、18.4%~61.8%。与5种甲基汞测定方法的前处理过程、分析仪器和检出限进行了比较,并讨论了无机汞的干扰情况及如何降低体系空白和消除无机汞干扰的质量控制手段。     

全自动烷基汞分析系统分析水源水中烷基汞的实验研究

建立了全自动烷基汞分析系统测定水源水中烷基汞(甲基汞、乙基汞)的方法。实验采用直接法测定水源水中的烷基汞含量,在0.5~1 000 pg的范围内,甲基汞及乙基汞标准工作曲线线性均良好;取样体积为30 ml时,甲基汞及乙基汞的检出限分别为0.005 ng/L及0.003 ng/L,低于水源水中限量要求;实际水样甲基汞及乙基汞加标回收率为85.9%~89.4%及87.4%~91.3%;标准样品分析合格;测定甲基汞及乙基汞标准样品的相对误差为1.8%及2.4%;运用优化的仪器条件和适当的质控手段,可较好的满足水源水中痕量烷基汞的测定需求。     

高分辨电感耦合等离子体质谱法测定地下水中稀土元素

采用高分辨电感耦合等离子体质谱法测定地下水中14种稀土元素,并选择Rh作内标,可消除测定中的质谱干扰和非质谱干扰,使方法在0μg/L~100μg/L范围内线性良好。方法检出限为0.002μg/L~0.005μg/L,实际水样的加标回收率为80.0%~117%,RSD为2.1%~3.8%。     

高效液相色谱-原子荧光联用测定天然水中烷基汞

应用在线紫外光照射-高效液相色谱分离-冷原子蒸发/氢化物发生-原子荧光光谱法(HPLC-UV-CV/HG-AFS)测定天然水中烷基汞,实验比较两种前处理方法-巯基棉富集和液液萃取,优化分析条件,建立一种简便、选择性好、高灵敏度分析天然水中烷基汞的方法.取1L水样时,甲基汞和乙基汞的检出限(3S/N)分别为0.3和0.6...     

吹扫捕集/GC-冷原子荧光法测定包装饮用水中烷基汞

采用吹扫捕集/气相色谱-冷原子荧光法测定包装饮用水中烷基汞(甲基汞和乙基汞)。通过优化试剂和仪器条件,使方法在0.100 ng/L～10.0 ng/L范围内线性良好。当取样体积为25 mL时,甲基汞和乙基汞的方法检出限分别为0.005 5 ng/L和0.004 2 ng/L,市售某品牌包装饮用天然泉水3个质量浓度水平的加标回收率为90.5%～106%,6次测定结果的RSD为0.4%～1.9%。将该方法用于各品牌包装饮用水样品的测定,甲基汞和乙基汞均为未检出。     

固相萃取-液相色谱-串联质谱法测定水中5种雌激素

建立了固相萃取-液相色谱-串联质谱组合联用技术同时测定地表水、饮用水和污水处理厂出厂水中的5种雌激素(17β-雌二醇、雌三醇、雌酮、17α-炔雌醇、己烯雌酚)的方法。水样经过全自动固相萃取仪富集,以OASIS HLB柱为萃取柱,甲醇为洗脱剂,用液相色谱-串联四极杆质谱联用仪分析定量。分别在0.5~8、5~80μg/L范围内线性良好,相关系数为0.995~0.998。17β-雌二醇、雌三醇、17α-炔雌醇的检出限均为5μg/L,雌酮与己烯雌酚的检出限为0.5μg/L。5种雌激素的纯水加标回收率为63.6%~120.2%,地表水加标回收率为59.8%~91.5%,自来水加标回收率为55.3%~92.1%,精密度为3.7%~10.7%,该方法简单、可靠,可用于水中雌激素类污染物的同时测定。     

超高效液相色谱-串联质谱法测定水中痕量双酚A

采用超高效液相色谱-串联质谱法测定水中痕量双酚A,水样经预处理后,以BEH C18超高效液相色谱柱分离,在质谱电喷雾离子源负离子多反应监测模式下测定.方法在0.200μg/L～10.0μg/L范围内线性良好,相关系数r为0.9992,方法检出限为0.06μg/L,空白及实际样品加标回收率为87.4% ～114%,RSD为3.6% ～7.4%.     

Exposure Assessment to Mercury Vapor in Chloralkali Industry

The aim of the study was to develop a sampling method aimed at individual sampling of mercury vapor and subsequent individualexposure assessment of the worker. Hopcalite available fromInowrocawskie Zakady Chemiczne (in Poland) was founduseful for mercury vapor sampling in active and passive individual samplers. However the sampling rate determined forpassive sampler in steady-state laboratory chamber cannot be usedunder fluctuating conditions of mercury vapor concentration andair movement typical for field measurement. In order to check comparativeness of passive and active sampling methods, sampleswere taken in the same time and individual samplers fixed toworker's clothes were used. Mercury vapor concentration wasmeasured at two chloralkali industries in Poland and the resultswere presented. Excessive exposure in both industries wasconfirmed by finding elevated mercury concentration in urinesamples from the workers.     

提高环境水中纳克级超痕量汞测定灵敏度的研究

对ｎｇ／Ｌ级超痕量汞测定中的消解、测定各步骤对灵敏度的影响进行了研究。得出结论：采用高纯氩气作载、屏气，选择高负压值和高扩展倍率能明显提高灵敏度；选择合适的消解时间和缩短测定时间能使灵敏度略有提高；试剂和玻璃器皿所带给空白的痕量汞对提高灵敏度不利，应作除汞处理。     

热分解齐化原子吸收光度法测定土壤中汞

固体测汞仪采用热分解齐化原子吸收光度法,此方法可以直接测定土壤中汞的含量。通过实验分析表明:此方法相关系数r≥0.999,检出限为0.01 ng,精密度为6.0%~9.1%,准确度为0%~6.7%,加标回收率为95%~107%。本方法具有简便、快速、准确、干扰少、成本低等优点,适合大批量土壤样品的测定。     

全自动甲基汞分析仪测定水和废水中甲基汞

建立了全自动甲基汞分析仪测定水和废水中甲基汞的方法,对较清洁的地表水和一般废水样品可直接衍生化测定,对基体复杂水样则需蒸馏后再衍生化测定。该法在水样中甲基汞含量为0~1 000 pg范围内线性良好,相关系数r为0.999 7,检出限为0.002 ng/L,标准参考物质测定结果均在参考值范围内,相对标准偏差为1.1%,加标回收率为83.2%~96.6%。该法适用于水及废水中甲基汞的检测。     

氯磺酚偶氮硫代若丹宁光度法测定环境水样中的汞

研究了氯磺酚偶氮硫代若丹宁(HSCT)与汞的显色反应。在pH3 8的HAc-NaAc缓冲介质中,TritonX-100存在下,HSCT与汞反应生成2∶1稳定络合物,λmax=550nm,体系ε=8 46×104L·mol-1·cm-1。汞含量在0—1 5mg/L内符合比耳定律。方法可用于水样中痕量汞含量的测定。     

离子色谱-串联质谱法测定4类水质中7种极性有机磷

应用离子色谱-串联质谱法(IC-MS/MS)同时测定了地下水、地表水、生活污水和工业废水等4类水质中的草甘膦、草铵膦、氨甲基膦酸、杀木膦、乙烯利、双甘膦和增甘膦.这7种有机磷极性和水溶性强,用常规气相或液相的方法需要经衍生化后才能测定,且要严格控制前处理条件.该法水样用微孔滤膜和离子净化柱过滤后直接进样,经Ion Pa...     

Atmospheric Monitoring at Abandoned Mercury Mine Sites in Asturias (NW Spain)

Mercury concentrations are usually significant in historic Hg mining districts all over the world, so the atmospheric environment is potentially affected. In Asturias, northern Spain, past mining operations have left a legacy of ruins and Hg-rich wastes, soils and sediments in abandoned sites. Total Hg concentrations in the ambient air of these abandoned mine sites have been investigated to evaluate the impact of the Hg emissions. This paper presents the synthesis of current knowledge about atmospheric Hg contents in the area of the abandoned Hg mining and smelting works at ‘La Peña–El Terronal’ and La Soterraña, located in Mieres and Pola de Lena districts, respectively, both within the Caudal River basin. It was found that average atmospheric Hg concentrations are higher than the background level in the area (0.1 μg Nm^?3), reaching up to 203.7 μg Nm^?3 at 0.2 m above the ground level, close to the old smelting chimney at El Terronal mine site. Data suggest that past Hg mining activities have big influences on the increased Hg concentrations around abandoned sites and that atmospheric transfer is a major pathway for Hg cycling in these environments.     

冷原子吸收法对水中汞溶液浓度测量结果的不确定度评定

对冷原子吸收法测量水中汞溶液浓度的影响因素作了全面分析,对各因素的不确定度进行评估,评定了冷原子吸收法对水中汞溶液浓度测量结果的不确定度。     

总汞环境样品的前处理技术及分析方法研究进展

对2005—2012年间的环境样品中总汞检测的前处理技术及分析方法文献进行了综述。总结了水体、土壤及废气中总汞样品前处理采用的主要方法及存在的问题,并且对环境样品总汞的现行国标分析方法及新方法(光度法、冷原子吸收法、原子荧光法、电感耦合等离子体-质谱法及生化检测等)的原理和应用进行了归纳。展望了环境样品中总汞检测的发展趋势,为研究者进行总汞新分析方法的开发和标准化提供了借鉴。     

Background Mercury Concentrations in River Water in Maine, U.S.A.

Mercury concentrations in 58 rivers in Maine was measured to range from below detection up to 7.01 ng L^-1 and averaged 1.80±1.29 ng L^-1. The concentration gradient for mercury in rivers across the state was not uniform. Mercury strongly correlated with dissolved organic carbon (DOC) and aluminum, and less strongly with copper, lead, and zinc. Mercuryexhibited significant differences in correlations with chemical variables and local geology when partitioned by flow state (high or low). Mercury concentrations were greatest in rivers flowingacross either wacke-type bedrock at low metamorphic grade, or glacial-till deposits. Elevated concentrations of mercury formed a locus in northern Maine under both high and low-flow states while in southwestern Maine a locus formed only during high-flowstates. These regional differences were statistically significantwhen compared by geographical location. We suggest that there is a bedrock source of mercury in northeastern Maine that is dilutedduring periods of high runoff. The elevated concentrations detected under high-flow states, as noted in southwestern Maine, may reflect mercury released from storage in association withDOC during periods of high runoff. The association of mercury with flow state indicates that watershed processes and local geology can modulate the concentration of mercury in rivers.