共查询到19条相似文献,搜索用时 62 毫秒
1.
2.
3.
电热蒸发钨丝在线捕获原子荧光光谱法直接测定菠菜中痕量镉 总被引:2,自引:0,他引:2
利用钨丝(TC)常温下特异性捕获镉(Cd)消除基体干扰,泡沫碳材料电热蒸发器串联原子荧光光谱仪,实现了固体直接进样测定菠菜鲜样中痕量Cd。研究表明,泡沫碳电热蒸发器性能稳定,样品个体差异对测定无影响;经液氮冷冻粉碎的菠菜鲜样均匀度良好,Pauwels公式估算最小取样量为16.3 mg,满足仪器微量进样要求。采用灰化(50 W保持50 s,70 W保持80 s)、蒸发(70 W保持30 s)过程分离,Ar-H2(9∶1,V/V)载气流速为600 mL/min时,方法检出限可达0.2μg/kg,回收率为90.1%~106.1%,RSD小于10%,分析时间少于5 min,常见金属元素和有机物质对测定无干扰,且与微波消解石墨炉原子吸收光谱法结果无显著性差异(p>0.05)。 相似文献
4.
5.
6.
7.
为了快速低成本测定蒸馏酒中痕量重金属镉,利用钨丝电热蒸发器作为直接进样装置,与原子荧光光谱仪原子化器直接连接,构建了用于蒸馏酒中镉测定的直接进样原子荧光光谱检测系统(W-coil ETV-AFS),并对工作气体的气氛和流速、灰化和蒸发电压、样品承载量等参数进行了优化,建立了蒸馏酒中镉的直接进样快速检测方法.在最优条件下... 相似文献
8.
激光原子荧光光谱分析法的进展 总被引:5,自引:0,他引:5
概述了激光原子荧光光谱分析法的研究现状和发展趋势。对各种原子化学方法与激光原子荧光光谱分析法相结合的分析特性进行了描述,着重介绍了电热原子化作为原子化器的激光原子荧光光谱法近年来的发展和应用。 相似文献
9.
10.
便携式钨丝电热原子吸收光谱仪测定水样中铜、铬、铅和镉 总被引:6,自引:1,他引:6
以钨丝原子化器和小型化CCD检测器为主要部件,组装了便携式钨丝电热原子吸收光谱分析仪,优化了载气(Ar/H2) 流速、空心阴极灯位置、原子化器高度、灰化和原子化电流等主要仪器条件.最佳载气(Ar/H2)流速(mL/min)为600 /300(Cd),800/200(Cu, Pb, Cr);灰化电流为2.9~3.2 A;原子化电流为8.5 A;CCD的积分时间为50 ms.并在优化的仪器条件下准确测定了环境水样中的铜(Cu)、铬(Cr)、铅(Pb)和镉(Cd),进样10 μL时,其检出限分别为2、5、9和0.5 μg/L.此便携式原子吸收光谱仪在环境水样痕量元素分析中可望有良好的应用前景. 相似文献
11.
The analytical utility of a tungsten (W)-coil atomization-laser-induced fluorescence (LIF) approach has been evaluated for trace level measurements of elemental chromium (Cr), arsenic (As), selenium (Se), antimony (Sb), lead (Pb), tin (Sn), copper (Cu), thallium (Tl), indium (In), cadmium (Cd), zinc (Zn) and mercury (Hg). Measurements of As, Cr, In, Se, Sb, Pb, Tl, and Sn were performed by laser-induced fluorescence using a single dye laser operating near 460 nm whose output was converted by frequency doubling and stimulated Raman scattering to wavelengths ranging from 196 to 286 nm for atomic excitation. Absolute limits of detection (LODs) of 1, 0.3, 0.3, 0.2, 1, 6, 1, 0.2 and 0.8 pg and concentration LODs of 100, 30, 30, 20, 100, 600, 100, 20, and 80 pg/mL were achieved for As, Se, Sb, Sn, In, Cu, Cr, Pb and Tl, respectively. Determinations of Hg, Pb, Zn and Cd were performed using two-color excitation approaches and resulted in absolute LODs of 2, 30, 5 and 0.6 pg, respectively, and concentration LODs of 200, 3000, 500 and 60 pg/mL, respectively. The sensitivities achieved by the W-coil LIF approaches compare well with those reported by W-coil atomic absorption spectrometry, graphite furnace atomic absorption spectrometry, and graphite furnace electrothermal atomization-LIF approaches. The accuracy of the approach was verified through the analysis of a multielement reference solution containing Sb, Pb and Tl which each had certified performance acceptance limits of 19.6-20.4 μg/mL. The determined concentrations were 20.05 ± 2.60, 20.70 ± 2.27 and 20.60 ± 2.46 μg/mL, for Sb, Pb and Tl, respectively. The results demonstrate that W-coil LIF provides good analytical performance for trace analyses due to its high sensitivity, linearity, and capability to measure multiple elements using a single tunable laser and suggest that the development of portable W-coil LIF instrumentation using compact, solid-state lasers is feasible. 相似文献
12.
Márcia M. Silva Francisco J. Krug Pedro V. Oliveira Joaquim A. Nóbrega Boaventura F. Reis Daniel A.G. Penteado 《Spectrochimica Acta Part B: Atomic Spectroscopy》1996,51(14):1925-1934
A flow injection system coupled to a tungsten coil electrothermal atomizer has been developed for on-line separation and preconcentration, using lead as a model element. The system utilizes three-way solenoid valves for sampling, buffering, washing and reconditioning solution management, and the resin column is inserted in the tip of the autosampler arm of a Varian GTA-96. The solenoid valves and tungsten coil power supply were controlled by a computer program written in Visual Basic, interfaced with the built-in Varian software. The system performance was tested by loading the resin column with the sample flowing at 3 ml min−1 for 60 s. Elution was performed automatically by sampling 20 μl of the eluent from a sample cup of the autosampler, and this aliquot was delivered into a 150 W tungsten coil. With Chelex-100 resin, the separation of concomitants was tested with lead in the presence of as much as 1000 mg l−1 of Ca, Mg, Na or K. The model system presented an enrichment factor of 64 at a sampling rate of 30 samples per hour. 相似文献
13.
Chemical modifiers in arsenic determination in biological materials by tungsten coil electrothermal atomic absorption spectrometry 总被引:2,自引:0,他引:2
Palladium, iridium, and rhodium are evaluated as possible chemical modifiers in the determination of As in digest solutions of biological materials (human hair and clam) by tungsten coil electrothermal atomic absorption spectrophotometry (TCA-AAS). The modifier in solution was applied onto the coil and thermally pre-reduced; the pre-reduction conditions, the amount of modifier, and the thermal program were optimized. Palladium was not satisfactory, whereas Ir and Rh were effective modifiers and rendered better relative sensitivity for As by a factor of 1.4 and 1.9, respectively compared to the case without modifier. Upon optimization of thermal conditions for As in pre-reduced Ir (2.0 µg) and Rh (2.0 µg) modifiers and in the digest solutions of the study matrices, Rh (2.0 µg) was more effective modifier and was selected as such. The mean within-day repeatability was 2.8% in consecutive measurements (25–100 µg L–1) (3 cycles, each of n=6) and confirmed good short-term stability of the absorbance measurements. The mean reproducibility was 4.4% (n=20 in a 3-day period) and the detection limit (3
blank/slope) was 29 pg (n=15). The useful coil lifetime in Rh modifier was extended to 300–400 firings. Validation was by determination of As in the certified reference material (CRM) of Oyster tissue solution with a percentage relative error (E
rel%) of 2% and percentage relative standard deviation (RSD%) of 3% (n=4), and by analytical recovery of As spiked in CRM of human hair [94±8% (n=4)]. The methodology is simple, fast (sample readout frequency 21 h–1), reliable, of low cost, and was applied to the determination of As in hair samples of exposed and unexposed workers. 相似文献
14.
15.
用原子荧光分光光度计测定食品中的蛋白 总被引:5,自引:0,他引:5
在碱性条件下,用原子荧光分光光度计直接测定氨的吸收,建立了定氮新方法。相对标准偏差为5%,检出限为73μg mL。食品中蛋白的测定结果与传统方法相比具有很好的一致性。 相似文献
16.
Carmen Ibáñez-Palomino J. Fermín López-Sánchez 《International journal of environmental analytical chemistry》2013,93(7):909-921
A systematic study of Hg2+ and CH3Hg+ (MeHg+) speciation using hyphenated techniques, was performed for high-performance liquid chromatography coupled to on-line UV irradiation and cold-vapour atomic fluorescence spectroscopy (HPLC-UV-CV-AFS). First, a comparative study of the behaviour of three mobile phase compositions (using tetrabutylammonium bromide (TBAB), L-cysteine and ammonium pyrrolidinedithiocarbamate (APDC)) is presented. The separation and detection system was optimised by considering factors that modify fluorescence signal and the separation such as, the addition of different percentages of an organic modifier (methanol (MeOH) and acetonitrile (ACN)) to the mobile phase, the type of reducing agent used (SnCl2 and NaBH4) and the potential memory effects of the material of which the injection system is made (stainless steel, PEEK). The mobile phase selected for its sensitivity was a mixture 80?:?20 MeOH?:?0.0015?mol?l–1 APDC and 0.01?mol?l–1 NH4CH3COO (pH 5.5). The detection and quantification limits were close to 1.5 and 5?µg?l?1 for both species (as Hg), respectively. Recoveries obtained using fortified water samples of distinct origin (soft mineral, tap, river, seawater, and wastewater), ranged from 90 to 115% for concentrations about 2 and 20 times over quantification limits. Good repeatability was obtained (about 5%) independently of the concentrations, with reproducibility values about 20% at low concentrations and 5–10% at higher concentrations. Our proposed method proved to be straightforward for use by environmental laboratories for routine Hg2+ and MeHg+ determinations in polluted water samples. 相似文献
17.
原子吸收和原子荧光光谱分析 总被引:1,自引:0,他引:1
本文是《分析试验室》期刊定期评述中关于原子吸收光谱(AAS)及原子荧光光谱(AFS)分析的第11篇综述文章. 文中对2004年12月~2007年4月期间我国在AAS/AFS领域所取得的主要进展进行评述. 内容包括概述、仪器装置与数据处理、火焰原子吸收光谱法、电热原子吸收光谱法、化学蒸气发生技术以及原子荧光光谱法等. 收集文献670篇. 相似文献
18.
Arsine trapping on resistively heated tungsten coil was investigated and an analytical method for ultratrace arsenic determination in environmental samples was established. Several chemical modifiers, including Re, Pt, Mo, Ta and Rh, were explored as permanent chemical modifiers for tungsten coil on-line trapping and Rh gave the best performance. Arsine was on-line trapped on Rh-coated tungsten coil at 640 °C, then released at 1930 °C and subsequently delivered to an atomic fluorescence spectrometer (AFS) by a mixture of Ar and H2 for measurement. In the medium of 2% (v/v) HCl and 3% (m/v) KBH4, arsine can be selectively generated from As(III). Total inorganic arsenic was determined after pre-reduction of As(V) to As(III) in 0.5% (m/v) thiourea-0.5% (m/v) ascorbic acid solution. The concentration of As(V) was calculated by difference between the total inorganic arsenic and As(III), and inorganic arsenic speciation was thus achieved. With 8 min on-line trapping, the limit of detection was 10 ng L−1 for As(III) and 9 ng L−1 for total As; and the precision was found to be <5% R.S.D. (n = 7) for 0.2 ng mL−1 As. The proposed method was successfully applied in total arsenic determination of several standard reference materials and inorganic arsenic speciation analysis of nature water samples. 相似文献
19.
用标准的150 W幻灯灯泡的钨丝作原子化加热材料,设计制作了一种新颖的、结构简单的钨丝电热原子化器,同时还设计了该原子化器的电源电路和信号的数据采集电路.该原子化器能的最高原子化温度可达3100 K左右;编写了硬件的控制软件和信号处理的应用软件.用该原子化器将实验室一台火焰原子吸收光谱仪改装成钨丝原子吸收光谱仪,并以铜元素标准溶液和PerkinElmer公司多元素标准溶液对仪器性能作了研究.仪器对铜的检出限为0.0133 μg/mL,线性范围为0.10~4.0 μg/mL;对1.0 μg/mL的铜标准溶液测试的相对标准偏差为RSD=4.1%(测试次数n=10),每次分析所需样品量20 μL. 相似文献