牡蛎粉中砷、铅、汞、镉有害金属含量的测定研究

采用微波消解法处理的样品,用原子荧光法来分析测定样品中的痕量Hg,用等离子原子发射光谱法来分析测定样品中As、Pb、Cd的含量。研究了测定不同金属元素的最佳仪器的工作条件,并对方法的准确度和精密度进行考察。结果表明,牡蛎粉中的砷、铅、镉、汞含量分别为9．65μg／g,1．00μg/g,11．1μg/g,0．0511μg/g,加标回收率为89．0％～106．9％,相对标准差为0．50％～4．76％。测定方法简单易行,方便快捷。     

用巯酰胺分离石墨炉原子吸收法测定高温合金中杂质铋EI

本文叙述了用硫酸胺为沉淀剂以分离基体。降低了试剂的空白值,提高了测定的精密度和准确度。回收率在82～106％。对于0.000028％铋含量的测定,相对标准偏差为14.3％。该方法已成功地应用于测定高温合金中痕量铋。     

原子吸收光谱法测定TG6钛合金中痕量镍EI

采用原子吸收光谱测定TG6钛合金中痕量镍。优化了原子吸收测量条件,研究了HCl（1＋1）,HBF4（1＋4）用量,基体钛及其共存元素对测定镍的影响,编制了分析方法。方法的相对标准偏差不大于6．2％,测定范围是0．010％～0．050％,方法检出限为0．059pμg·mL^-1。     

冷蒸气-无色散原子荧光光谱法测定地矿样品中痕量汞

目的一建立测定地矿样品中痕量汞的精细分析方法及仪器测试条件。研究了应用流动注射-氢化物发生-原子荧光光谱法测定地矿样品中痕量汞，讨论了了仪器工作条件，氢化物发生条件，基体干扰和消除，汞的痕量分析对地质找矿和地质环境工作有重要意义。     

牡蛎粉中砷、铅、汞、镉有害金属含量的测定研究

采用微波消解法处理的样品,用原子荧光法来分析测定样品中的痕量Hg,用等离子原子发射光谱法来分析测定样品中As、Pb、Cd的含量。研究了测定不同金属元素的最佳仪器的工作条件,并对方法的准确度和精密度进行考察。结果表明,牡蛎粉中的砷、铅、镉、汞含量分别为9.65μg/g,1.00μg/g,11.1μg/g,0.0511μg/g,加标回收率为89.0%~106.9%,相对标准差为0.50%~4.76%。测定方法简单易行,方便快捷。     

氢化物发生-原子荧光光谱法同时测定食盐中的砷和汞

建立一种氢化物发生-原子荧光光谱法同时测定食盐中砷和汞的方法.研究样品前处理对测定结果的影响,探索同时测定砷、汞的最佳实验条件.优化条件下,砷、汞质量浓度分别在0～10.0 μμg/L和0～2.0μg/L范围内,线性关系良好.方法检出限:As为0.0043 μg/L,Hg为0.003 2 μg/L;相对标准偏差:As为0.37％,Hg为0.61％;样品加标回收率:As为97.80％ ～ 102.40％,Hg为96.78％～ 100.80％.试验表明:该方法具有操作简便、快速、准确度高等优点,可用于食盐中砷汞的同时测定.     

照相级溴化物中痕量铅的测定

本文采用就地镀汞膜指示电极,半微分阳极溶出伏安法测定照相级溴化钠和溴化钾中痕量铅的含量。对某些样品测定结果令人满意,回收率可达到85～107％。     

用原子吸收法测量食品容器防蚀涂料中的痕量铅

采用标准加入法测量以APDC－DDTC－MIBK-环己烷体系草取处理后涂料中的痕量铅，再用空气-乙炔火焰原子吸收法测定其含量。建立了优化革取和测定的条件，并对可能存在的干扰元素进行了实验。本法测定的相对标准偏差为2．1％，回收率为98％，十分令人满意。     

中药材果实、种子类药材中重金属含量的测定分析

本文对果实及种子类中药材连翘、紫苏子的铅、镉、砷和汞含量测定的方法进行了研究。样品经高氯酸、硝酸或双氧水进行消解,用原子荧光、原子吸收进行检测。测得回收率:紫苏子89.8%-97.5%;连翘86.5%-94.1%。测得精密度:紫苏子0.52%-9.2%;连翘2.2%-4.4%。并用该方法对不同产地的;连翘、枸杞子、女贞子和紫苏子、车前子、牛蒡子中的铅、镉、砷和汞含量进行了测定。结果表明:这6种中药材均含铅、镉、砷和汞,但基本上未超过国家规定的粮食和蔬菜的重金属最大允许含量。     

用原子吸收法测量食品容器防蚀涂料中的痕量名

采用标准加入法测量以ＡＰＤＣ－ＤＤＴＣ－ＭＩＢＫ－环己烷体系萃取处理后涂料中的痕量铅，再用空气乙炔火焰原子吸收法测定其含量。建立了优化萃取和测定的条件，并对可能存在的干扰元素进行了实验。本法测定的相对标准偏差为２．１％，回收率为９８％，十分令人满意。     

天然气以及大气中微量汞的监测方法的研究

本研究了天然气以及大气中微量汞的监测方法：以高精密度的冷原子吸收光谱法和便携式塞曼效应原子吸收光谱法为基础,建立了完整的大面积网络快速实时监测系统。     

Removal and recovery of mercury(II) from hazardous wastes using 1-(2-thiazolylazo)-2-naphthol functionalized activated carbon as solid phase extractant

As a part of removal of toxic heavy metals from hazardous wastes, solid phase extraction (SPE) of mercury(II) at trace and ultra trace levels was studied using 1-(2-thiazolylazo)-2-naphthol (TAN) functionalized activated carbon (AC). The SPE material removes traces of mercury(II) quantitatively in the pH range 6.0 +/- 0.2. Other parameters that influence quantitative recovery of mercury(II), viz. percent concentration of TAN in AC, amount of TAN-AC, preconcentration time and volume of aqueous phase were varied and optimized. The possible means of removal of Hg(II) from other metal ions that are likely to be present in the wastes of the chloroalkali industry is discussed. The potential of TAN-functionalized AC SPE material for decontaminating mercury from the brine sludge and cell house effluent of a chloralkali plant has been evaluated.     

Solid phase extraction and determination of sub-ppb levels of hazardous Hg2+ ions

A simple, rapid and reliable method has been developed to selectively separate and concentrate ultra trace amounts of mercury(II) ions from aqueous samples for its highly sensitive measurement by cold vapor atomic absorption spectrometry (CV-AAS). The Hg(2+) ions were adsorbed selectively and quantitatively during the passage of aqueous samples through octadecyl silica membrane disks modified by isopropyl 2-[(isopropoxycarbothiolyl)disulfanyl]ethane thioate (IIDE). The retained Hg(2+) ions were then stripped from the disk with minimal amounts of 0.5 M hydrobromic acid (two 8 ml portions) as eluent, and determined by CV-AAS. The break-through volume of the method is greater than 3000 ml, which results in enrichment factors >150. Maximum capacity of the membrane disks modified with 10mg of the ligand was found to be 350+/-30 microg of mercury(II), and the limit of detection is 0.005 ng ml(-1). The effect of various cationic interferences on the recovery of mercury in binary mixtures was studied. The method was applied to the recovery of Hg(2+) ions from different synthetic and tap water samples, as well as the determination of mercury in human hair samples.     

水中汞的电感耦合等离子体-质谱法测定

为解决水中汞不稳定以及易吸附而引起记忆效应的问题,建立分析水中汞的电感耦合等离子体质谱新方法,汞标准溶液中加金形成金汞齐,采用200μg/LAu2＋-5%HNO3溶液作为清洗液,选取Rh103作为内标元素。结果标明：在79d内,汞溶液的标准曲线稳定,其相关系数在0.9993~0.9998之间,仪器检出限在1.15×10-3~3.11×10-2μg/L范围内。该方法分析水中痕量汞具有检出限低、数据准确性高、再现性好的特点,所用试剂种类少且毒性小。     

微波消解-氢化物原子荧光法测定海水与表层底泥中的痕量汞

采用微波消解一氢化物原子荧光光谱法,测定了福清市沿海周边地区的海水与表层底泥样品中的汞含量.对实验条件进行了优化,改进了传统消解方法中试剂用量大、手续繁琐、易交叉感染等不足.实验同时对海水与表层底泥的测量检出限及方法回收率进行试验,结果表明在优化的实验条件下海水与表层底泥汞的检出限分别0.0005μg/L和0.0317...     

气态元素汞校准的一致性光学评定检测实验研究

利用低压汞灯作为光源,结合单色仪,对汞渗透管法和汞饱和蒸气法气态元素汞校准进行一致性光学评定检测研究。在汞渗透管实验中,吸收度面积值与理论浓度的皮尔逊相关系数为0.9968,拟合优度为0.9936,说明两组数据相关性较好且符合郎伯比尔定律。取实验的吸收截面作为标准参考吸收截面,对相同浓度汞蒸气横向对比及不同浓度汞蒸气纵向对比,浓度误差最大为7.45%,表明渗透管法的稳定性较好且精度较高,验证了渗透管法作为汞标气法的可行性。在渗透管实验中加入SO2,气态汞浓度测量误差最大为12.82%,说明SO2对汞吸收度测量产生一定程度的干扰。汞饱和蒸气法实验中,以渗透管为基准测得的最大误差在标准允许误差之内,表明2种校准方法具有一致性。但汞饱和蒸气法与渗透管法相比,其重复性及精度仍有不足,待提升空间较大。     

HPLC-ICP-MS法测定水样中的甲基汞、乙基汞和无机汞

建立了高效液相色谱(HPLC)和电感耦合等离子体质谱(ICP-MS)联用测定环境水样中的甲基汞、乙基汞和无机汞的方法。实验使用的高效液相色谱流动相为含有0.06mol/L乙酸氨,20μg/LBi,0.1%(V/V)2-巯基乙醇的5%(V/V)甲醇-水溶液,色谱柱为C18反相柱(5μm,2.1mm×50mm),经前处理的水样在液相色谱中分离后,进入电感耦合等离子体质谱检测其甲基汞、乙基汞和无机汞的浓度。甲基汞、乙基汞和无机汞检出限分别为0.05μg/L、0.10μg/L和0.10μg/L。     

A method for screening total mercury in water using a flow injection system with piezoelectric detection

An automatic microgravimetric screening system based on piezoelectric detection and the use of acidic stannous chloride as reductant was developed for the fast detection and determination of total mercury in water. Reduced mercury is detected as an amalgam by using a gold-coated piezoelectric crystal, the sensor subsequently being regenerated by passing it through a peroxydisulfate solution. The gold-coated piezoelectric crystal is a highly efficient retention unit for the main soluble mercury species (inorganic, complexed, and organometallic) previously reduced to elemental mercury and is free of interferences from other metal ions. This detector exhibits good sensitivity: it allows the determination of mercury at sub-parts-per-billion concentration levels (0.30-1.00 microg/L). The precision, expressed as relative standard deviation, was +/- 2.7% (n = 11; P = 0.05) at 0.5 microg/L total mercury. The proposed method was successfully used as a rapid screening method for mercury monitoring in natural waters.     

Removal of trace level aqueous mercury by adsorption and photocatalysis on silica–titania composites

Silica–titania composites (STCs) were applied to trace level mercury solutions (100 μg/L Hg) to determine the degree of mercury removal that could be accomplished via adsorption and photocatalysis. STCs are a porous, high surface area silica substrate (>200 m²/g), manufactured using sol–gel methodology, impregnated with TiO₂ nanoparticles. The performance of this material along with its precursors, silica and Degussa P25 TiO₂ were compared. Under adsorption alone (no UV illumination), STCs were able to achieve approximately 90% removal of mercury, which is comparable to that of Degussa P25. Silica without TiO₂ performed poorly in comparison and was minimally affected by UV illumination. Contrary to expectations, the performance of Degussa P25 was not largely changed by UV irradiation and the STC was detrimentally affected under the same conditions. It was concluded that elemental mercury was formed under UV irradiation with or without the presence of TiO₂ due to photochemical reactions, decreasing the mercury removal by STC. Additionally, the primary particle size of the STC was reduced to increase mass transfer. The result was improved Hg removal under adsorption and photocatalysis conditions. Improved adsorption kinetics were also achieved by altering the STC pore size and TiO₂ loading.     

基于高温还原及差分吸收光谱监测烟气汞的实验研究

高温还原法在不需要催化剂的条件下可将烟气排放中的二价汞转化为零价汞,便于进行烟气总汞的监测。运用差分吸收光谱法（DOAS）反演出烟气汞浓度,与没有加高温装置的测量结果作对比,验证高温设备的适用性,并配比不同浓度的零价汞和二价汞进行混合实验。在传统的DOAS算法基础上,研究遗传算法、傅里叶变换滤波及积分面积法对烟气汞浓度的影响。实验结果表明:传统算法具有偶然性,整体误差大;傅里叶变换反演出的浓度误差较大;积分面积法较遗传算法误差偏低,整体波动也小,反演出的偏差最小为0.55%,适合用于反演低浓度排放的烟气汞测量。