微波消解-原子荧光光谱法测定皮革中砷和汞

建立了皮革中砷和汞的微波消解-原子荧光光谱测定方法。在优化的实验条件下,砷、汞含量分别在0.60～150ng/mL和0.10～20ng/mL范围内线性良好。砷、汞检出限分别为0.22ng/mL和0.04ng/mL。方法测定砷的回收率为96.0%～104%,汞的回收率为95.0%～110%。方法准确、灵敏、快速、可应用于皮革样品中砷和汞的同时测定。     

氢化物发生-原子荧光光度法测定鱼体内的砷和汞

采用硝酸-高氯酸湿式消解法消解样品,利用AFS-230E原子荧光光度计测定了赣州市赣江交汇处鱼体内砷和汞的含量,选择了最佳实验条件.结果表明,所得砷和汞的检出限分别为0.020、0.008 μg/L,测定砷、汞标准溶液各6次,所得砷、汞标准溶液的平均值分别为0.099、0.103 μg/mL,相对标准偏差RSD分别为2...     

高压消解-双道氢化物发生-原子荧光光谱法同时测定女贞属苦丁茶中砷与汞

采用HNO3/H2SO4常压预消解,HNO3/H2O2高压消解,硫脲-抗坏血酸溶液预还原等手段,建立了高压消解-双道氢化物发生-原子荧光光谱法同时测定女贞属苦丁茶中砷和汞含量的新方法。考察并优化了分析条件。该方法砷与汞的检出限分别是4.73×10-5 mg.L-1、8.7×10-6 mg.L-1;相对标准偏差(n=10)砷小于2.15%,汞小于3.47%。方法可应用于女贞属六种苦丁茶中砷和汞的测定。     

双通道原子荧光光谱法同时测定土壤中的砷和汞

对现有国标检测方法(GB/T 22105.1-2008和GB/T 22105.2-2008)进行改进,采用王水水浴浸提-双通道原子荧光光谱法同时测定土壤样品中砷、汞的含量。采用土壤国家一级标准物质GSS-3,GSS-8,GSS-9与山西农田土壤样品为试验对象,筛选得到检测砷、汞元素含量最佳实验条件及仪器工作条件。砷、汞的质量浓度分别在0~150μg/L,0~2μg/L范围内与荧光强度成良好的线性关系,线性相关系数均大于0.999,砷、汞的检出限分别为0.021,0.0015 mg/kg。测定结果的相对标准偏差为1.81%~4.64%(n=8),砷、汞的样品加标回收率分别为92.7%~103.0%,82.0%~95.5%。经国家一级标准物质验证,该法检出限、准确度和精密度均满足检测要求。改良后的方法可以同时准确、快速地测定土壤中砷、汞,极大地提高了工作效率,可以更好地适应当前大量的土壤分析工作。     

微波消解-原子荧光光谱法同时测定鱼体中砷和汞

为建立微波消解-原子荧光光谱法同时测定鱼体中砷和汞的测定方法,采用微波消解方法,双道原子荧光光谱法同时测定了鱼体中砷和汞的含量。结果表明,砷与汞的线性范围分别为0.2~2.0μg/L,0.0~50.0μg/L;相关系数分别为r=0.999 8和r=0.999 5;砷回收率为96.5%~101.5%之间,相对标准偏差(n=11)为1.22%,检出限为0.004 2μg/L;汞回收率为98.6%~103.0%,相对标准偏差(n=11)为0.67%,检出限为0.009 6μg/L。用该法测定鱼类中砷和汞,方法灵敏度高、操作简便快速、结果准确可靠。     

微波消解-原子荧光光谱法测定耳草中四种重金属元素含量

目的测定耳草中4种金属元素含量。方法采用微波消解-原子荧光光谱法测定了中药材耳草中砷、汞、硒、镉的含量。结果在最佳实验条件下,砷、汞、硒、镉的检出限分别为0.305、0.016、0.082、0.039 ng/mL,样品中4种元素的加标回收率在97.2%～105.4%之间。结论该法快速、准确、简便且准确度高,为中药材中重金属含量的测定提供了较好的方法。     

微波消解样品-电感耦合等离子体原子发射光谱法测定铅精矿中铅、砷、镉、汞

采用微波消解样品-电感耦合等离子体原子发射光谱法同时测定铅精矿中主体元素铅及有毒有害元素砷、镉、汞的含量。0.20g试样置于消解罐中,先后加入硝酸9mL、盐酸3mL、氟硼酸2mL及过氧化氢2.5mL,密闭罐盖按设定的微波消解程序进行消解。试验选择铅、砷、镉和汞的分析线分别为220.351,189.042,228.802,184.950nm以消除基体干扰。铅、砷、镉、汞的检出限分别为16.0,2.2,0.4,0.8μg.g-1。方法用于铅精矿标准样品(GBW 07617)和铅精矿实际样品分析,此方法的测定值与认定值及原子吸收光谱法或原子荧光光谱法的测定值相一致。方法的相对标准偏差(n=10)在0.15%～3.9%之间。     

300 MW燃煤电站砷、汞排放特征研究

对某300 MW燃煤电站煤、底灰和静电除尘器(ESP)飞灰进行采样并测定了其中的砷、汞含量,同时应用Ontario Hydro Method (OHM) 标准方法和设备对ESP前后烟气中的砷、汞分布进行了直接采样和测试.对砷的检测结果表明,ESP飞灰中砷含量约6.68×10^-6,是原煤中砷含量的2.5倍左右,而底灰中砷含量仅为1.70×10^-6,ESP前烟气中砷含量约153.27 μg/m³,ESP后砷含量急剧降低为41.13 μg/m³;对汞的检测结果表明,原煤中汞含量约2.5×10^-7,飞灰、底灰中的汞含量分别约1.9×10^-7、1.5×10^-7;ESP前后烟气中总汞含量分别为5.49、5.21 μg/m³.砷在飞灰中明显富集,而汞在飞灰和底渣中均不具有富集效果.ESP单元具有明显的协同脱砷效果,平均脱除率约在71%左右,而对汞的协同脱除效果不明显.     

氢化物发生-原子荧光光谱法同时测定食品添加剂碳酸钙中的砷和汞

应用氢化物发生-原子荧光光谱法同时测定食品添加剂碳酸钙中的砷和汞,并对样品中的主要成份及共存元素可能对检验结果的影响和实验条件进行了研究.结果表明,加入硫脲-抗坏血酸溶液后,碳酸钙中主要成份钙及可能存在的共存元素铁、铅、镉、铜、锑、硒、锡、铬、锌等不干扰砷和汞的测定.方法检出限为砷0.0124 μg/L,汞0.0009μg/L,回收率为砷101.8%～102.2%,汞102.5%～106.0%.精密度为砷0.37%,汞0.95%.建立的氢化物发生-原子荧光光谱法同时测定食品添加剂碳酸钙中砷和汞的分析方法能满足日常检验的要求.     

微波消解–原子荧光法同时测定PM2.5中砷、汞含量

采用微波消解–原子荧光法测定PM2.5中砷、汞含量。实验结果表明,当还原剂硼氢化钾的质量分数为2%、溶液介质酸度为4%(体积分数)盐酸时,同时测定砷、汞可获得最佳的荧光值。砷、汞测定的检出限分别为0.027,0.006μg/L,空白滤膜的加标回收率分别为95.3%~101.7%,96.0%~106.0%,样品的加标回收率分别为95.0%~103.5%,93.3%~110.0%。该法检出限低,准确度高,适用于环境空气PM2.5中砷、汞含量的测定。     

Concentrations of hazardous heavy metals in environmental samples collected in Xiamen, China, as determined by vapor generation non-dispersive atomic fluorescence spectrometry.

Non-dispersive atomic fluorescence spectrometry (NDAFS) coupled with vapor generation (VG) sample introduction was applied to the determination of the concentrations of hazardous heavy metals, such as arsenic, cadmium, lead and mercury, in seawater, soils and total airborne particulate matter (PM) collected around the Xiamen area in China. Almost 100% sample introduction efficiency was achieved by using thiourea and ascorbic acid for the pre-reduction of As(V) to As(III), K3Fe(CN)6 and tartaric acid for pre-oxidation of Pb(II) to Pb(IV), and masking the interferences arising from the co-existing transition metals to As, Cd, Hg and Pb during their vapor generation process. Moreover, a novel sample pretreatment device was developed to avoid the loss of mercury, lead, cadmium and arsenic during sample pretreatment. With such methods, the detection limit (DL) of arsenic, cadmium, lead and mercury was down to 0.08, 0.03, 0.05, 0.01 ng mL(-1) (3sigma), respectively. The relative standard deviations (RSD, n = 11) for arsenic, cadmium, lead and mercury at 10 ng mL(-1) were 0.9%, 1.6%, 1.3% and 2.0%, respectively. The concentrations of hazardous heavy metals in the environmental samples collected in Xiamen, China are in the range from 0.02 +/- 0.001 ng mL(-1) in seawater to 15.3 +/- 0.2 microg g(-1) in soils. Besides flame/GF-AAS and ICP-AES/MS, VG-NDAFS should be another choice for the determination of hazardous heavy metals in environmental samples.     

Speciation analysis of inorganic form of arsenic in ground water samples by hydride generation atomic absorption spectrometry with insitu trapping in graphite tube

This paper presents the results of a study on the optimization of the determination of total arsenic and its species using the absorption atomic spectrometry method combined with hydride generation and in-situ concentration on the inner walls of the graphite tube. To ensure a maximum efficiency of the in-situ analyte concentration on the graphite tube walls, a palladium modifier subjected to preliminary thermal reduction was used. The limits of detection (3σ) were 0.019 ng/mL for total As and 0.031 ng/mL for As(III) at the preliminary analyte concentration for 60s. The optimised procedure of the analyte concentration on the inner walls of the atomiser (graphite tube) was applied for determinations of arsenic in samples of ground water. The content of arsenic in the samples studied varied from 0.21 ng/mL to 0.80 ng/mL for As(III), and from 0.19 ng/mL to 1.24 ng/mL for As(V).     

Hydride Generation Atomic Fluorescence Spectrometric Determination of Ultratrace Arsenic in High Purity Indium Oxide

A simple, sensitive, and interference free method was proposed for the determination of total arsenic in high purity indium oxide by hydride generation atomic fluorescence spectrometry (HG-AFS). Preconcentration was carried out by distillation of volatile arsenic trichloride. Hydrazine sulfate was used as a prereductant to reduce As (V) to As (III). The volatile arsenic trichloride generation was based on the reaction between As (III) and hydrochloric acid, and vapors were absorbed with water. The method provides a linear response range of 2 ng/mL–70 ng/mL, a detection limit of 0.1 ng/mL, a recovery of 96%–113%, and an average relative standard deviation of 2.42%. The method was validated by means of interlaboratory comparative analysis with the proposed method HG-AFS, and the comparison of data by using proposed method HG-AFS and reference methods of ICP-OES and spectrophotometry.     

原子荧光光谱法测定蛇粉中汞的方法研究

用微波消解仪消解、氢化物发生-原子荧光光谱法测定蛇粉中的微量Hg,优化了仪器的工作条件。测定汞的检出限为0.7pg/mL。测定0.3及1ng/L Hg标准溶液,相对标准偏差分别为4.1%及0.9%,加标回收率为87%~110%。     

Routine determination of mercury,arsenic and selenium by radiochemical Neutron Activation Analysis

A method for the determination of mercury, arsenic and selenium by neutron activation analysis is described. Radiochemical separations are performed by selective distillation followed by electrolysis of mercury on gold and precipitation of arsenic and/or selenium by reduction to the elemental form. The chemical yields are 80–90% for mercury and 90–100% for arsenic and selenium. Interference tests have been carried out with reference to those elements most likely to interfere with the analysis. Detection limits for mercury, arsenic and selenium using 0.1 g of sample are 0.2 ng g^–1, 2 ng g^–1 and 3 ng g^–1, resp. Detection limits can be improved using greater sample size and neutron flux density. Results from the analysis of several NBS standard reference materials are given.     

Direct Determination of Arsenic in Beet Sugar Molasses Using Nickel as Chemical Modifier by Electrothermal Atomic Absorption Spectrommetry

A simple electrothermal atomic absorption spectrometric (ETAAS) method is described for direct determination of arsenic in sugar beet molasses samples. Pyrolytic graphite tubes were used as atomizers. The compression between modifiers such as nickel nitrate, palladium nitrate and the mixture of palladium and magnesium nitrate were performed and nickel nitrate selected as the best chemical modifier. The effects of pyrolysis and atomization temperature were also studied and the pyrolysis temperature of 900 °C and atomization temperature of 2300 °C have been chosen for temperature program. The detection limit of the method was 1 ng/mL As in sugar beet molasses samples. The relative standard deviation for ten determination of a spiked sample with concentration of 50 ng/mL As was 2.4%. The accuracy of the method was confirmed by the analysis of spiked samples. The linear rang of calibration is in the range of 1‐100 ng/mL of arsenic.     

Sequential determination of tin, arsenic, bismuth and antimony in marine sediment material by inductively coupled plasma atomic emission spectrometry using a small concentric hydride generator and L-cysteine as prereductant

A hydride generation system using a small concentric hydride generator combined with inductively coupled plasma atomic emission spectrometry (ICP-AES) was established to determine tin, arsenic, bismuth and antimony in a marine sediment material with L-cysteine as a pre-reductant. Influences of concentrations of three kinds of acids (HCl, HNO₃ and HClO₄), L-cysteine, and sodium tetrahydroborate(III) as well as sodium hydroxide were investigated. The interferences from transition ions were found to be insignificant for determination of the four elements in presence of L-cysteine. Under optimized conditions the detection limits were 0.6 ng/mL for arsenic(III), 0.8 ng/mL for antimony(III), 1.7 ng/mL for tin(IV), and 1.2 ng/mL for bismuth(III). The method was applied to determine the four elements in standard marine sediment materials and the results were in agreement with certified values.     

液相色谱–原子荧光光谱法检测水产品中汞形态

建立了液相色谱–原子荧光光谱联用测定水产品中无机汞和甲基汞含量的方法。对影响测定结果的分析条件,如流动相组成、载流、还原剂、氧化剂、载气和屏蔽气进行了研究和优化,同时考察了该方法的有效性。结果表明:无机汞和甲基汞在质量浓度1~20 ng/m L范围内线性关系良好,相关系数分别为0.999 4,0.999 1;检出限分别为0.19,0.17 ng/m L;色谱峰面积的相对标准偏差分别为3.16%,2.16%(n=7);加标回收率分别为74%~100%,71%~91%。该方法可用于水产品中汞元素的形态分析。     

微波消解-液相色谱-原子荧光光谱联用(LC-AFS)法测定稻米样品中砷形态

建立了稻米中4种砷元素形态的液相色谱-原子荧光光谱联用法(LC-AFS),样品用0.15mol/L的硝酸溶液微波提取50min,提取液经离心分离后,采用Hamilton PRP-X100色谱柱,45mmol/L KH2PO4-5mmol/L Na2HPO4缓冲液为流动相,砷形态4个组分能够在7min内达到基线分离,且无需调pH。优化了氢化物发生条件,使用了更低浓度的载流和还原剂。方法学实验结果表明,各组分在2~10ng/mL范围内线性关系良好,相关系数为0.9988~0.9998,各组分的检出限分别为0.29 ng/mL、0.47 ng/mL、0.62 ng/mL和1.16 ng/mL；各组分峰面积的相对标准偏差均低于3.11%；加标回收率为85.3%～112.8%；对稻米标准物质的分析测定结果表明该方法定值准确。最后,与GB 5009.11-2014中使用的提取及测量条件进行对比,表明该方具备法快速、环保、高效的特点。     

Sequential determination of tin, arsenic, bismuth and antimony in marine sediment material by inductively coupled plasma atomic emission spectrometry using a small concentric hydride generator and L-cysteine as prereductant

A hydride generation system using a small concentric hydride generator combined with inductively coupled plasma atomic emission spectrometry (ICP-AES) was established to determine tin, arsenic, bismuth and antimony in a marine sediment material with L-cysteine as a pre-reductant. Influences of concentrations of three kinds of acids (HCl, HNO₃ and HClO₄), L-cysteine, and sodium tetrahydroborate(III) as well as sodium hydroxide were investigated. The interferences from transition ions were found to be insignificant for determination of the four elements in presence of L-cysteine. Under optimized conditions the detection limits were 0.6 ng/mL for arsenic(III), 0.8 ng/mL for antimony(III), 1.7 ng/mL for tin(IV), and 1.2 ng/mL for bismuth(III). The method was applied to determine the four elements in standard marine sediment materials and the results were in agreement with certified values. Received: 4 September 1997 / Revised: 14 October 1997 / Accepted: 7 November 1997