Determination of Hg in soil by ultrasonic slurry sampling hydride generation atomic fluorescence spectrometry

Ultrasonic aided slurry sampling hydride generation atomic fluorescence spectrometry （USS-HG-AFS） was developed for the determination of Hg in soil samples from a sewage-irrigated farm. 500 mg grounded soil was suspended in agar solution by an ultrasound water bath before the HG-AFS determination. The results for the reference material of soil （serial number GBW-07411） agreed satisfactorily with the certified values. Results obtained by the developed procedure compared well with those after traditional acid digestion of samples. The detection limit are 6.7ngL-1 for Hg respectively, with average relative standard deviation values of 6.4% for analysis of a series of soil samples of different origin. The recoveries of the anatytes varied in the range from 95 to 107%. This observation has stimulated interest in fast, accurate and sensitive analytical methods for determination of metals in soil.

Determination of Trace Elements in Potatoes by Flame Atomic Absorption Spectrometry

[Objective] This study aimed to analyze the contents of trace elements in potatoes from different production areas in Qinghai Province. [Method] By flame atomic absorption spectrometry （FAAS）, the contents of various trace elements in potatoes were determined. [Result] Potatoes contain abundant trace elements such as Cu, Zn, Fe, Mn, Ca, K and Mg. To be specific, the contents of Ca, K and Mg were relatively high. [Conclusion] By using FAAS, the relative standard deviation was 1.17%-2.75% and the recovery rate was 97%-99.5%, indicating accurate and reli-able results with high precision.

Uncertainty Estimation for the Determination of Trace Heavy Metals in Human Hair by Flame and Electrothermal Atomic Absorption Spectrometry

Trace element analysis on hair samples has been widely used to assess wildlife and human exposure to different contaminants present in the environment or at the workplace. Pollutants due to the presence of toxic metals in environment not only enter the body by breading, water, and foodstuff accumulates in hair, but they could be adsorbed directly on the hair from environment. In order to remove adsorbed elements and thus determine the internally bound elements correctly, hair sample must be washed. In the present work, we propose uncertainty estimation for the analytical results that are obtained from determination of cadmium, lead, copper, iron, manganese and nickel in human hair by flame and electrothermal atomic absorption spectrometry （FAAS and ETAAS）. To estimate the uncertainty of analytical result obtained, two types of bias are calculated in the assessment of trueness： a proportional bias and a constant bias. Nested design was applied for calculating proportional bias and Youden method to calculate the constant bias. The results we obtained for proportional bias are calculated from spiked samples. In this case, the concentration found is plotted against the concentration added and the slop of standard addition curve is an estimate of the method recovery. Estimated method of average recovery in human hair is： （1.019 ±0.026）, （0.918 ±0.014）, （1.073±0.016）, （1.0597± 0.017）, （1.073± 0.020） and （0.934± 0.117） for Cd, Pb, Mn, Ni, Fe and Cu respectively.

Determination of Ni, Ca, Mg, Cu and Pb in Wolfram byInductively Coupled Plasma Atomic Emission Spectrometry

The method for the determination of Ni, Ca, Mg, Cu and Pb in wolfram wire by ICP AES was studied. Results showed that perhydrol affects the intensities of elements (Ni, Ca, Mg, Cu, Pb) and this effect can be compensated by internal reference element. It is also showed that the stability of plasma caused by perhydrol matrix was effectively improved. The replicate experiment and recovery experiment revealed perfect precision and accuracy. Results got by two methods were just the same.

偏振能量色散X射线荧光光谱法快速测定汽油中微量元素

建立偏振能量色散X射线荧光光谱法测定汽油中微量元素含量。样品无需预处理,利用质量分数在0~50μg/g范围的标准工作曲线,消除元素共存干扰影响,使用偏振能量色散X射线荧光光谱仪测定汽油中微量元素。汽油中硫、氯、硅、铅、锰、铁等元素的质量分数与荧光强度的线性相关系数不小于0.9997,样品加标回收率为91.2%~109.4%,测定值的相对标准偏差为2.0%~7.2%(n=6),检出限不大于1.0μg/g。该方法各微量元素测定结果与SH/T 0689—2000《轻质烃及发动机燃料和其他油品的总硫含量测定法(紫外荧光法)》、SH/T 1757—2006《工业芳烃中有机氯的测定微库仑法》、GB/T 33647—2017《车用汽油中硅含量的测定电感耦合等离子体发射光谱法》、GB/T 8020—2015《汽油中铅含量的测定原子吸收光谱法》、NB/SH/T 0711—2019《汽油中锰含量的测定原子吸收光谱法》和SH/T 0712—2002《汽油中铁含量测定法(原子吸收光谱法)》相比较,具有较好的一致性,能够满足汽油中硫、氯、硅、铅、锰、铁等微量元素的快速测定要求。

复古金饰品中金及微量元素的检测研究

复古金饰品是一种新型足金饰品,作为一种新产品,因其款式多样,硬度较高,可以满足人们的特色需求。为研究这种产品,实验中采用X射线荧光光谱法、ICP光谱法、火试金法、硬度仪对黄金样品进行了测试和研究。研究结果表明:复古金饰品因加工特性和杂质元素种类较多,又缺少合适的标准物质,X射线荧光光谱法分析结果不理想,可选用ICP光谱法和火试金法进行检测。硬度测试结果显示,复古金饰品硬度远高于普通足金。

Comparison of 66 chemical element contents in normal and benign hyperplastic prostate

Objective:The aim of this study was to clarify the differences between the prostatic levels of chemical elements in patients with benign prostatic hyperplasia(BPH)and healthy male.Methods:We evaluated the prostatic level of 66 chemical elements in 43 patients with BPH and 37 healthy males.Measurements were performed using five instrumental analytical methods.Results:In the hyperplastic prostates,we have observed a significant increase in the mean level of Bi,Cr,Hg,K,Sb,and Se accompanied a significant decrease in the mean level of Al,Ce,Cs,Dy,Er,Gd,Ho,La,Mo,Nd,Pb,Pr,Sm,Sn,Tb,Tm,U,and Y.No differences were found in the mean prostatic level of other chemical elements including Ag,Al,Au,B,Ba,Be,Br,Ca,Cd,Co,Cu,Fe,Li,Mg,Mn,Na,Nb,Ni,P,Rb,S,Sc,Si,Th,Ti,Tl,Yb,Zn,and Zr between BPH patients and healthy males.Conclusions:The finding of chemical element contents and correlation between pairs of chemical element mass fractions indicates that there is a great disturbance of prostatic chemical element metabolism in BPH gland.Trace elements Bi,Cr,Hg,K,Sb,and Se may be regarded as the possible tissue biomarkers of hyperplastic transformation of prostate gland.Obtained data did not confirm a critical role of Cd and Pb accumulation in the pathogenesis of BPH.A potential age-related Zn,Fe,and Se deficiency in the prostate tissue has not been found as being involved in the etiology of BPH.

原子荧光光谱法测定氧化铟中的微量砷

样品采用硝酸-盐酸溶解,用原子荧光光谱法测定了氧化铟中微量砷。方法研究了原子荧光光谱仪工作参数的选择,溶液残留硝酸的影响,还原剂浓度的影响以及铟基体对砷测定的影响等条件试验,最后采用基体匹配法进行测定。在选定的试验条件下,样品加标回收率在95.6%~105.5%之间,相对标准偏差(RSD)为3.29%~5.14%(n=11)。结果表明:方法具有灵敏度高、精密度高、线性关系好、分析结果准确可靠等优点,可测定氧化铟中0.000 50%~0.004 0%范围内的砷,能用于氧化铟中微量砷的测定。

基于氧化/吹扫捕集-冷原子荧光光谱法测定海水中痕量总汞

基于氧化/吹扫捕集-冷原子荧光光谱法,建立了准确测定海水中痕量总汞的方法.采用硫酸和过硫酸钾体系氧化海水样品,盐酸羟胺预还原,再经氯化亚锡将全部的汞离子还原为单质汞,原位吹扫和金汞齐捕集,在波长253.7 nm处原子荧光光谱法分析测定.结果表明:该方法回收率为94%—104%,精密度相对标准偏差为2.1%—3.6%,方法检出限为0.1 ng·L^(−1),测定下限为0.4 ng·L^(−1),与现行国标方法相比,该方法增加了原位吹扫捕集的前处理步骤,因而灵敏度更高,检出限更低,也具有很好的稳定性.用不同海区实际海水样品进行验证,结果显示,该方法满足实际样品的分析需求,建议在海水水质的汞监测领域能够拓展应用.

石墨炉原子吸收光谱法检测曲阜市河流中微量元素含量

石墨炉原子吸收光谱法在元素定量分析中具有原子化效率高、绝对灵敏度高、检出限低等优点,故选取石墨炉原子吸收光谱法检测曲阜市河水中Fe、Cu、Cd、Mn微量元素含量。结果表明:通过与国家标准进行比较,除了城墙北中Mn的含量略高于国标要求,其他均低于国标要求,在正常范围内。测得加标回收率RSD在95%~105%,含量结果准确、可靠。但是对于测定多种元素,此方法比较费时。

火焰原子吸收光谱法测定混合型饲料添加剂、微量元素预混料和矿物质饲料原料中铬含量的研究

试验旨在建立火焰原子吸收光谱法测定混合型饲料添加剂、微量元素预混料、矿物质饲料原料中铬含量的分析方法。试验通过改变样品溶解体系,优选狭缝宽度、燃助比等,将混合型饲料添加剂、微量元素预混合饲料、矿物质饲料原料样品经盐酸、硝酸、氢氟酸和高氯酸溶解,于原子吸收分光光度计上进行检测。结果显示,试验方法检出限为0.0009 mg/kg,线性相关系数为0.9999,样品加标回收率为95.50%~103.10%;矿物质饲料原料相对标准偏差(RSD)小于5.91%,微量元素预混料RSD小于3.06%,混合型饲料添加剂RSD小于3.00%。研究表明,试验所用方法具有良好的灵敏度、精密度和准确度,可操作性强,可实现快速准确测定混合型饲料添加剂、微量元素预混合饲料、矿物质饲料原料中铬的含量。

原子荧光光谱法测定微量元素预混料中砷含量的方法改进

[目的]改进样品前处理方法后,采用改进后的原子荧光光谱法检测微量元素预混料中的砷含量,以提高检测结果的准确性。[方法]用湿法消解微量元素预混料样品后,在样品溶液中加入适量的氢氧化钠溶液,使样品溶液中的Cu^(2+)、Fe^(3+)等干扰因子和氢氧化钠反应生成氢氧化铜、氢氧化铁等沉淀物质,通过离心去除其干扰因子,再检测样品中的砷含量。[结果]原方法测定的结果稳定性差,改进后,检测结果稳定性好,加标回收率较高。[结论]采用改进后的方法测定砷含量的结果更准确。

微波消解-原子荧光光谱法测定铁皮石斛中的重金属元素

本文建立了微波消解-原子荧光光谱法测定铁皮石斛中重金属的分析方法。优化了微波消解条件,同时对方法学进行了验证。结果表明,消解剂为硝酸-盐酸混合酸,以5∶2(体积比)为最佳配比,砷、汞、铅线性范围分别为1.0~100.0μg·L^(-1)、0.4~10.0μg·L^(-1)、1.0~50.0μg·L^(-1),检出限分别为0.0162μg·mL^(-1)、0.0048μg·mL^(-1)、0.5311μg·mL^(-1),加标回收率为94.6%~109.7%。微波消解-原子荧光光谱法能够满足铁皮石斛中重金属含量的测定。

陈皮、淡竹叶等5种药材重金属含量分析

采用微波消解法处理竹叶青酒配方的5种中药材(陈皮、淡竹叶、檀香、栀子、当归),然后利用原子吸收光谱法和原子荧光光谱法测定这5种中药材铜、镉、铅、砷、汞元素的含量。结果表明,样品中5种重金属元素的含量均未超过《中国药典》2020版限量规定,各个元素线性相关性好,检出限低,准确度高。该方法可为药材中重金属元素的检测及公司产品生产原料的质量控制提供参考。

川贝母中重金属元素的测定方法研究

建立了微波消解-原子荧光光谱法测定川贝母中重金属的分析方法。考察了消解剂类型、用量以及载流酸度和还原剂浓度对测定结果的影响,最终确定硝酸-盐酸混合酸为消解剂,将其体积比(5∶2)作为最佳用量配比,载流浓度为5%,还原剂浓度为2%。实验结果表明,砷、汞、铅线性范围为1.0~100.0μg·L^(-1)、0.4~10.0μg·L^(-1)、1.0~50.0μg·L^(-1),检出限为0.0162μg·L^(-1)、0.0048μg·L^(-1)、0.5311μg·L^(-1),加标回收率在95.3%~107.7%,能够满足川贝母中重金属含量的测定。

微波消解-石墨炉原子吸收光谱法测定秦皮中金属元素的含量

通过微波消解-石墨炉原子吸收光谱法分别测定了陕西中药材秦皮中微量金属元素Fe、Ca、Cu、Se、Mn、Pb的含量,测定结果表明:秦皮中Fe元素的含量最高,为4.7727 mg/kg,而Cu、Pb、Se元素的含量相对稀少,分别为0.0033,0.0057,0.0723 mg/kg,Mn、Pb的测定结果符合国家标准要求的最低限度;样品加标回收率为97.1%~101.8%,测定元素的相对标准偏差(RSD)为0.15%~4.41%,均小于5%,检出限低(0.102μg/L).该检测方法高效便捷、精密度良好、准确性高.

粉末法和熔片法在XRF测定土壤样品中的适用性

建立了波长色散X荧光射线光谱法测定土壤样品中痕量元素的分析方法。分别采用粉末压片法和熔片法对土壤样品进行前处理,通过控制压片时间、压片压力、助熔剂和脱模剂的选择、熔融温度与时间等实验条件来达到最佳前处理效果。实验结果表明,两种前处理方法均有较高的精密性;熔片法对痕量元素的测定有较高的准确性,适用于准确度要求较高的分析测试任务;粉末压片法有较高的前处理效率,适用于样品量较大的分析测试任务。

原子吸收光谱法测定大豆及其制品中的微量元素

利用原子吸收光谱法测定了大豆及其制品中的14种微量元素。研究了样品灰化温度、灰化时间和浸取液HNO3浓度对测定结果的影响及SrCl2对测定Ca,Mg含量的影响。结果表明大豆及其制品中K,Na,Ca,Mg,Fe,Cu,Zn,Mn等元素含量比较丰富。

原子吸收光谱法测定芦荟中微量元素

用 HNO3 - HCl O4(4 :1)混酸作消化液处理样品 ,用原子吸收光谱法测定了样品中的 Cu、Zn、Fe、Mn、Co、Ni、Ca、Mg、Cd、Pb等 10种微量元素 ,方法简便、快速 ,标准加入回收率在 96 .0 %～ 10 5 .0 %之间 .

微波消解-原子吸收光谱法测定不同产地淡竹叶中微量元素的含量

利用微波消解技术处理样品,采用原子吸收光谱法测定了我国广东、湖北、湖南、重庆、广西、江苏、福建、浙江、安徽九个不同产区淡竹叶中Zn,Fe,Cu,Mn,K,Ca,Mg,Ni,Cd,Pb,Cr,Co,Al,Se,As 15种微量元素的含量。该方法的相对标准偏差（RSD）在1.23%~3.32%之间,平均回收率在95.8%~104.2%之间。研究表明,该方法简便、快速、灵敏,适合于淡竹叶中微量元素的测定。试验分析结果表明,不同产地淡竹叶中微量元素的含量呈现地域性差异。各地区的淡竹叶中对人体有益的元素K,Mg,Ca,Fe,Mn含量普遍较丰富 对人体有害的重金属元素,除湖南产的淡竹叶中Pb的含量稍高,广东、安徽产的淡竹叶中Cu的含量偏高外,其他产区的淡竹叶中有害重金属元素Cd,Cu,Cr,Pb,As的含量均低于《中国药典》、《药用植物及其制剂进出口绿色行业标准》及《国家标准食品卫生标准》的限量标准。该测定结果为进一步探讨淡竹叶中微量元素的含量与其功效的相关性提供了科学依据。