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流动注射预富集─石墨炉原子吸收联用测定海水中痕量钼 总被引:2,自引:1,他引:2
用二乙基二硫代氨基甲酸钠作络合剂、乙醇作洗脱液的流动注射固相吸附萃取预富集─石墨炉原子吸收联用测定海水中痕量钼。设计了以固定体积取样法为基础的预富集装置。考察了实验参数对分析性能的影响。本法能在线分离干扰、富集被测物,当样品上柱体积为1.35mL时,富集倍数为13.3倍,检测下限为0.027μg/L,用于测定海水等标样中钼含量,精密度较好。 相似文献
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报道了用热解石墨涂层管快速无干扰直接测定金属钴中镉的方法,并提出以草酸为基体改进剂降低背景吸收直接测定海水中微量镉. 相似文献
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石墨炉原子吸收法测定食品中铅和镉 总被引:15,自引:0,他引:15
本文选用铵盐作为基体改进剂,有效地解决了石墨炉原子吸收分光光度法基体干扰问题,成功地测定了食品中的铅和镉。在仪器最佳工作条件下,对美国国家标准局标准参考物质NBS-SRM-1570(菠菜)及NBS-SRM-1566(牡蛎)中Pb、Cd进行了测定,相对标准偏差分别为2.5%和4.5%及1.8%和1.7%。 1 试验部分 1.1 仪器与试剂 Perkin-Elmer 2100型原子吸收分光光度计 氘灯校正背景 铅标准液:用1mg·ml~(-1)的Pb,逐级稀释成10、20、50、80、100ng·ml~(-1)的标准使用液。 镉标准液;用1mg·ml~(-1)的Cd,逐级稀释成1、2、5、8、10ng·ml~(-1)的标准使用液。 1.2 最佳工作条件(见表1) 相似文献
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脱脂棉富集-火焰原子吸收测定水中铜、铅、镉 总被引:1,自引:0,他引:1
1 引言 本文在pH6.5~7.0范围内,用脱脂棉富集水中痕量Cu、Ph、Cd原子吸收光谱法测定,方法简便快速、灵敏度高,用于水中痕量Cu、Pb、Cd的测定,结果满意。 2 实验部分 相似文献
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介绍了用石墨炉原子吸收分光光度法测定大气颗粒物中的锡,并进行了全程序空白值的测定、精密度测定,准确度测定,以及加标回收率实验,各项指标均符合实际要求。 相似文献
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液膜富集——火焰原子吸收法测定茶中微量铜,铁,钴,锌,镉 总被引:1,自引:0,他引:1
茶中微量元素的含量是评价茶叶质量的重要指标,由于这些微量元素的含量很低。通常在测定前进行预富集,本文提出了一个用液膜法富集的方法,其富集倍数可达100倍,回收率在95%~103%之间,5种元素的火焰原子吸收法测定结果,均令人满意,实验条件的选择用正交试验法,较一般常用的因素轮换法更为准确,也更为省时省力。 相似文献
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石墨炉原子吸收法连续测定气溶胶中重金属 总被引:7,自引:0,他引:7
提出了用石墨炉原子吸收法连续测定气溶胶中六种重金属的方法.气溶胶样品经处理后,直接用石墨炉原子吸收法测定其中的铜、钴、镍、镐、铅和铬.其检出限在 1.9×10~(-12)~1.6×10~(-10)g,仪器的精密度(RSD)<6.1%,标准加入回收率为90.4%~106.5%,已用于大批气溶胶样品的测定,结果令人满意. 相似文献
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微波消解石墨炉原子吸收法测定人发中的铅、镉 总被引:2,自引:0,他引:2
采用石墨炉原子吸收分光光度法(GFAAS)测定人发中的铅、镉含量.采用微波消解法消解样品,加入(NH4)2SO4+KH2PO4基体改进剂消除干扰,对消化剂种类、消解压力、仪器条件等进行了探索.方法简便、准确度高,Pb和Cd的平均回收率分别为101.8%和107.1%,相对标准偏差(RSD)为5.14%和6.80%,方法检出限Pb为9.53 ng/mL,Cd为0.78 ng/mL. 相似文献
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建立石墨炉原子吸收法测定土壤中铅、镉、钴、锑、铍含量的方法。优化了石墨炉原子吸收光谱法测定条件,在最佳实验条件下,采用硝酸-盐酸-氢氟酸-双氧水混合酸体系微波消解土壤样品,选用抗坏血酸-硝酸镁混合溶液为基体改进剂。铅、镉、钴、锑、铍的质量浓度在各自的范围内与吸光度成良好的线性关系,相关系数均大于0.999,各元素的检出限为0.008~0.06 μg/g。样品加标回收率为90.5%~104.0%,测定结果的相对标准偏差均小于2.5%(n=6)。该方法样品前处理简便,灵敏度高,检出限低,测定结果准确、可靠,可用于土壤中铅、镉、钴、锑、铍的测定。 相似文献
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A new method has been developed for the determination of trace molybdenum based on separation and preconcentration with TiO2 nanoparticles immobilized on silica gel (immobilized TiO2 nanoparticles) prior to its determination by graphite furnace atomic absorption spectrometry (GFAAS). The optimum experimental parameters for preconcentration of molybdenum, such as pH of the sample, sample flow rate and volume, eluent and interfering ions, have been investigated. Molybdenum can be quantitatively retained by immobilized TiO2 nanoparticles at pH 1.0 and separated from the metal cations in the solution, then eluted completely with 0.5 mol L?1 NaOH. The detection limit of this method for Mo was 0.6 ng L?1 with an enrichment factor of 100, and the relative standard deviation (RSD) was 3.4% at the 10 ng mL?1 Mo level. The method has been applied to the determination of trace amounts of Mo in biological and water samples with satisfactory results. 相似文献
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《Spectrochimica Acta Part B: Atomic Spectroscopy》2001,56(10):1859-1873
Solid sampling graphite furnace atomic absorption spectrometry (SS-GF AAS) was investigated as a potential technique for the routine determination of trace elements in mineral coal and cadmium, copper and lead were chosen as the model elements. Cadmium and lead could be determined at their main resonance lines at 228.8 nm and 283.3 nm, respectively, but an alternate, less sensitive line had to be used for the determination of copper because of the high copper content in coal. No modifier was necessary for the determination of copper and calibration against aqueous standards provided sufficient accuracy of the results. For the determination of cadmium and lead two different modifiers were investigated, palladium and magnesium nitrates in solution, added on top of each sample aliquot before introduction into the atomizer tube, and ruthenium as a ‘permanent’ modifier. Both approaches gave comparable results, and it is believed that this is the first report about the successful use of a permanent chemical modifier in SS-GF AAS. Calibration against solid standards had to be used for the determination of cadmium and lead in order to obtain accurate values. The agreement between the values found by the proposed procedure and the certificate values for a number of coal reference materials was more than acceptable for routine purposes. The detection limits calculated for 1 mg of coal sample using the ‘zero mass response’ were 0.003 and 0.007 μg g−1 for cadmium with the permanent modifier and the modifier solution, respectively, approximately 0.04 μg g−1 for lead, and 0.014 μg g−1 for copper. 相似文献
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《Spectrochimica Acta Part B: Atomic Spectroscopy》2005,60(5):667-672
The phase-separation phenomenon of non-ionic surfactants occurring in aqueous solution was used for the extraction of Cd and Pb from digested biological samples. After complexation with O,O-diethyldithiophosphate (DDTP) in hydrochloric acid medium, the analytes are quantitatively extracted to the phase rich in the non-ionic surfactant octylphenoxypolyethoxyethanol (Triton X-114) after centrifugation. Methanol acidified with 0.1 mol L−1 HNO3 was added to the surfactant-rich phase prior to its analysis by electrothermal atomic absorption spectrometry (ET AAS). The adopted concentrations for DDTP, Triton X-114 and hydrochloric acid were all optimized. Pyrolysis and atomization temperatures were optimized using the extracts and pyrolysis temperatures of 700 °C for both elements and atomization temperatures of 1400 and 1600 °C for cadmium and lead, respectively, were used without adding any modifier, which shows that considerable analyte stabilization is provided by the medium itself. A more detailed investigation was carried out to determine which components of the extract were responsible for the high thermal stability achieved and it revealed that the amount of DDTP added and the phosphorus content of the digested samples contributed significantly to this phenomenon. Detection limits (3σB) of 6 and 40 ng g−1, along with enrichment factors of 129 and 18 for Cd and Pb, respectively, were achieved. The proposed procedure was applied to the analysis of five certified biological reference materials after microwave-assisted acid digestion in a mixture of H2O2 and HNO3. Comparison with certified values was performed for accuracy evaluation, resulting in good agreement according to the t-test for a 95% confidence level. The high efficiency of cloud point extraction to carry out the determination of the studied analytes in complex matrices was, therefore, demonstrated. 相似文献
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Determination of lead in water samples by graphite furnace atomic absorption spectrometry after cloud point extraction 总被引:6,自引:0,他引:6
Cloud point extraction (CPE) has been used for the pre-concentration of lead, after the formation of a complex with 2-(5-bromo-2-pyridylazo)-5-(diethylamino)-phenol (5-Br-PADAP), and later analysis by graphite furnace atomic absorption spectrometry (GFAAS) using octylphenoxypolyethoxyethanol (TritonX-114) as surfactant. The chemical variables affecting the separation phase were optimized. Separation of the two phases was accomplished by centrifugation for 15 min at 4000 rpm. Under the optimum conditions i.e., pH 8.0, cloud point temperature 40 °C, [5-Br-PADAP] = 2.5 × 10−5 mol l−1, [Triton X-114] = 0.05%, added methanol volume = 0.15 ml, pre-concentration of only 10 ml sample permitted an enhancement factor of 50-fold. The lower limit of detection (LOD) obtained under the optimal conditions was 0.08 μg l−1. The precision for 10 replicate determinations at 5 μg l−1 Pb was 2.8% relative standard deviation (R.S.D.). The calibration graph using the pre-concentration system for lead was linear with a correlation coefficient of 0.9984 at levels near the detection limits up to at least 30 μg l−1. The method was successfully applied to the determination of lead in water samples. 相似文献
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H. Heinrichs 《Fresenius' Journal of Analytical Chemistry》1979,295(5):355-361
Summary Serious systematic errors inherent in the determination of lead in geological and biological samples by flameless atomic-absorption spectrometry are demonstrated. The reduced absorption of lead is due to partial interaction with alkaline, alkaline-earth and iron chlorides during the atomization stage. Incomplete dissociation of the volatile monochloride of lead in the gaseous phase reduces the absorption signal. An addition of 20% hydrogen to nitrogen (purge gas) diminishes signal suppression by removing the chlorine in form of volatile HCl. The detection limit is about 0.6 ppm in rocks and about 0.3 ppm in plant materials. Depending on the content in the samples the relative standard deviation is between 1 and 12%. The accuracy of the method was tested on 39 international standard reference samples.
Bestimmung von Blei in geologischen und biologischen Materialien durch AAS mit der Graphitrohrküvette
Zusammenfassung Schwerwiegende systematische Fehler bei der Bestimmung von Blei in geologischen und biologischen Materialien mit der Graphitrohrküvette werden aufgezeigt. Die Reaktion von Blei mit Alkali-, Erdalkali- und Eisenchloriden während der Atomisierungsphase führt zur Bildung von Bleimonochlorid, das nur unvollständig dissoziiert und eine Signalunterdrückung zur Folge hat. Ein Zusatz von 20% Wasserstoff zu Stickstoff als Spülgas vermindert die Signalunterdrückung, indem überschüssiges Chlor als Chlorwasserstoff entfernt wird. Die Nachweisgrenze liegt bei ca. 0,6 ppm für Gesteine und bei ca. 0,3 ppm für Pflanzenmaterialien. Je nach der Konzentration beträgt die relative Standardabweichung 1–12%. Die Genauigkeit der Methode wurde an 39 internationalen Standardreferenzproben überprüft.相似文献
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Luiz Frederico Rodrigues Julio Cezar Paz de Mattos Valderi Luiz Dressler Dirce Pozebon Érico Marlon de Moraes Flores 《Spectrochimica Acta Part B: Atomic Spectroscopy》2007
Trace impurities of Cd, Cu and Pb were determined in alumina based catalysts using direct solid sampling graphite furnace atomic absorption spectrometry (DSS-GF AAS). The analyzed catalysts are widely used in petrochemical processes. The following analytical parameters were evaluated: pyrolysis and atomization temperatures, feasibility of calibration with aqueous solutions, the necessity for palladium as chemical modifier and the sample mass introduced into the atomizer. Test samples between 0.05 and 8.5 mg were used. Palladium was investigated as chemical modifier but no improvement in analytical performance was obtained and its use was considered unnecessary for all elements. The results obtained by DSS-GF AAS were compared with those of inductively coupled plasma optical emission spectrometry (ICP OES) and also with conventional solution analysis by GF AAS (Sol-GF AAS). Characteristic masses were 1.4, 9 and 20 pg, for Cd, Cu and Pb, respectively. Using DSS-GF AAS the relative standard deviation was always less than 10% and the results agreed with those obtained by Sol-GF AAS and ICP OES. Calibration using aqueous solutions showed good linearity within the working range (R2 better than 0.99). Limits of detection (3σ, n = 10) for Cd, Cu and Pb using the proposed procedure were 0.2, 22, and 1.2 ng g− 1, respectively. 相似文献
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A graphite furnace atomic absorption spectrometry (GFAAS) method with optical temperature control for the determination of trace cadmium in paint samples is described. Optical temperature control was superior in many respects to current temperature control. The sensibility increased by 60%, the linear range widened by 60%, and the life of graphite tube showed a 200–300% increase because atomization temperature was lowered distinctly and atomization time was shortened. Use of lanthanum chloride as a matrix modifier was investigated. The linear range of calibration curve was 0–24 ng mL−1. The detection limit was 9.6 ng L−1. The characteristic mass was 3.0 pg. The method also resulted in excellent reproducibility (≤2.5% R.S.D.) at such low levels, and the recovery of added cadmium in paint samples was from 94.6% to 102%. This method is readily applicable to the determination of cadmium in paint samples. 相似文献
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A system for molybdenum separation and enrichment aiming its determination in water and biological samples by graphite furnace atomic absorption spectrometry (GFAAS) is proposed. The procedure is based on the sorption of the molybdenum (VI) thiocyanate complex onto a mini-column packed with polyurethane foam (PUF). The elution is accomplished by a 3.0 mol l−1 nitric acid solution. Flow variables were optimized and an enrichment factor of 10 as well as a limit of detection (LOD) (3 s) of 0.08 μg l−1 in the sample solution were achieved. The coefficient of variation showed values of 3 and 2% for molybdenum solutions of 2.0 and 10.0 μg l−1, respectively. The accuracy of the method was confirmed by the good concordance between found and certified values in the analysis of certified reference materials (CRMs) (CASS-3 Nearshore Seawater, NIST 1547 Peach Leaves, NIST 1515 Apple Leaves and NIST 1572 Citrus Leaves). The procedure was also applied for the molybdenum determination in mineral waters as well as in produced water samples. The results obtained for the mineral water samples compared well with those obtained by ICP-MS. Concerning the produced water samples, in spite of their large salinity, recoveries of 90 to 120% at the 1 μg l−1 were observed. 相似文献