火焰原子吸收光谱法测定工业废水中铊

研究了火焰原子吸收光谱法测定工业废水中铊。检出限 (3 σ)为 0 5mg L,相对标准偏差小于 2 0 % ,回收率在92 %～ 1 0 6 %范围 ,方法简便快速。     

Determination of total chromium by flame atomic absorption spectrometry after coprecipitation by cerium (IV) hydroxide

A method for the preconcentration of the total chromium based on coprecipitation with cerium (IV) hydroxide is proposed for determination of chromium by flame atomic absorption spectrometry. Different factors including carrier element amount, pH, sample volume and matrix ion effects for the precipitation were examined. The detection limit of the total chromium (k = 3, N = 15) was 0.18 μg l⁻¹. The presented method was applied for the determination of chromium in the wastewater samples from Kayseri and Nigde Organized Industrial Region-Turkey and in drinking water from our laboratory, Kayseri with satisfactory results (relative standard deviations below 8%, recoveries 95%). The analytical results obtained by the proposed method for certified copper sample was in good agreement with the certified value.     

Evaluation of metal contents of household detergent samples from Turkey by flame atomic absorption spectrometry

The concentrations of cadmium, copper, chromium, cobalt, iron, lead, manganese, nickel, and zinc in detergent samples from Kayseri, Turkey were determined by flame atomic absorption spectrometry. HClO₄ (10 mL)/HNO₃ (10 mL) mixture was used for the digestion of household detergent samples. The correctness of the analytical procedures was checked with standard addition–recovery tests in different detergent samples for the investigated metal ions. The concentration ranges of the elements in the detergent samples were found as 17.2–60.1, 11.1–40.1, 2.5–32.3, 8.1–10.5, 7.2–21.6, 9.8–17.9, 1.7–3.8, 12.5–22.5, and 2.0–5.8 μg/g for iron, manganese, zinc, copper, lead, cobalt, cadmium, nickel, and chromium, respectively. The values found in this work were compared with some other studies around the world conducted on detergent samples.     

Determination of traces of copper and zinc in honeys by the solid phase extraction pre-concentration followed by the flame atomic absorption spectrometry detection

A simple and fast solid phase extraction procedure was developed to pre-concentrate traces of Cu and Zn prior to their determination in honey samples by flame atomic absorption spectrometry. The sample preparation included dissolution of honey samples and the passage (at 20 ml/min) of resulting 10 % m/v solutions (100 ml) through Dowex 50W?×?8-400 resin beds in order to quantitatively retain Cu and Zn and separate them from the glucose and fructose matrix. Enriched Cu and Zn traces were recovered with 5.0 ml of a 3.0 mol/l HCl solution and quantified by flame atomic absorption spectrometry. The procedure proposed was used to analyze sixty nine commercially available and freshly ripened honey samples coming from the Lower Silesia region (Poland). It enabled to measure Cu and Zn within the range of 0.01–1.42 and 0.03–15.38 μg/g, respectively, with precision better than 4 %. Accuracy, assessed on the basis of the recovery test and the comparison of results with those obtained using wet digestion and inductively coupled plasma optical emission spectrometry, was ranged from ?4 % to +6 %. Detection limits of Cu and Zn achieved with this method were 5 and 7 ng/g, respectively.     

火焰原子吸收法测定土壤中的铅

建立了一种以 HNO3-HCl-HCl O4 -HF对土壤样品进行消化 ,火焰原子吸收测定铅的方法。该法用于实际样品的测定时 ,相对标准偏差小于 2 .3 % ,加标回收率为 98%～ 1 0 2 %。     

Determination of bismuth in environmental samples by slurry sampling graphite furnace atomic absorption spectrometry using combined chemical modifiers

Persistence behavior of insecticides chlorpyriphos, profenofos, triazophos, cypermethrin, and deltamethrin following the use of three combination formulations Action 505 (chlorpyriphos?+?cypermethrin), Roket 44EC (profenofos?+?cypermethrin), and Anaconda Plus (triazophos?+?deltamethrin) was studied in cabbage following the spray application at the recommended and double doses. Bio-efficacy of these formulations was also evaluated against mustard aphids (Lipaphis erysimi Kaltenbach) and diamondback moth (Plutella xylostella L.). The residues of different insecticides persisted for 5–8 days at low dose and 8–12 days at high dose. The residues dissipated with time and 87–100 % dissipation was recorded on the 8th day. The half-life values varied from 0.4 to 1.6 days. Based on the acceptable daily intake (ADI) values, a safe waiting period of 1 day has been suggested for the formulations Action 505 and Roket 44EC and 3 days for Anaconda Plus at the recommended dose of application. Action (1.6 L/ha) treatment was found to be the best as it significantly reduced the diamondback moth (DBM) (~60 %) and aphid population (~70 %) besides giving the highest yield (170 % increase over control).     

流动注射--氢化物发生原子吸收法测定天然水中的丁基锡化合物

建立用流动注射--氢化物发生原子吸收法同时测定天然水中一丁基锡、二丁基锡、三丁基锡和四丁基锡化合物的方法.首先用NaBH4还原丁基锡化合物后冷凝富集、加热,氢化物根据沸点的不同依次解吸从而得到分离,由原子吸收法测定.本方法可测每升几十纳克(以锡计)的各种丁基锡化合物.     

Monitoring of trace amounts of heavy metals in different food and water samples by flame atomic absorption spectrophotometer after preconcentration by amine-functionalized graphene nanosheet

We are introducing graphene oxide modified with amine groups as a new solid phase for extraction of heavy metal ions including cadmium(II), copper(II), nickel(II), zinc(II), and lead(II). Effects of pH value, flow rates, type, concentration, and volume of the eluent, breakthrough volume, and the effect of potentially interfering ions were studied. Under optimized conditions, the extraction efficiency is >97 %, the limit of detections are 0.03, 0.05, 0.2, 0.1, and 1 μg L^?1 for the ions of cadmium, copper, nickel, zinc, and lead, respectively, and the adsorption capacities for these ions are 178, 142, 110, 125, and 210 mg g^?1. The amino-functionalized graphene oxide was characterized by thermogravimetric analysis, transmission electron microscopy, scanning electron microscopy, and Fourier transform infrared spectrometry. The proposed method was successfully applied in the analysis of environmental water and food samples. Good spiked recoveries over the range of 95.8–100.0 % were obtained. This work not only proposes a useful method for sample preconcentration but also reveals the great potential of modified graphene as an excellent sorbent material in analytical processes.     

强酸型离子交换纤维富集-火焰原子吸收测定水中痕量铜、铅、镉、镍

通过强酸型离子交换纤维柱,在同一水样中同时富集和洗脱了铜、铅、镉、镍,采用火焰原子吸收光谱法测定,并对富集条件及洗脱条件、干扰因素进行了探讨。该方法简便易行,回收率在96.1%~105.5%之间,测定的相对标准偏差小于5.0%。     

Determination of Pb(II), Zn(II), Cd(II), and Co(II) ions by flame atomic absorption spectrometry in food and water samples after preconcentration by coprecipitation with Mo(VI)-diethyldithiocarbamate

A new, simple, and rapid separation and preconcentration procedure, for determination of Pb(II), Cd(II), Zn(II), and Co(II) ions in environmental real samples, has been developed. The method is based on the combination of coprecipitation of analyte ions by the aid of the Mo(VI)–diethyldithiocarbamate–(Mo(VI)-DDTC) precipitate and flame atomic absorption spectrometric determinations. The effects of experimental conditions like pH of the aqueous solution, amounts of DDTC and Mo(VI), standing time, centrifugation rate and time, sample volume, etc. and also the influences of some foreign ions were investigated in detail on the quantitative recoveries of the analyte ions. The preconcentration factors were found to be 150 for Pb(II), Zn(II) and Co(II), and 200 for Cd(II) ions. The detection limits were in the range of 0.1–2.2 μg L^?1 while the relative standard deviations were found to be lower than 5 % for the studied analyte ions. The accuracy of the method was checked by spiked/recovery tests and the analysis of certified reference material (CRM TMDW-500 Drinking Water). The procedure was successfully applied to seawater and stream water as liquid samples and baby food and dried eggplant as solid samples in order to determine the levels of Pb(II), Cd(II), Zn(II), and Co(II) ions.     

Solid-phase extraction and separation procedure for trace aluminum in water samples and its determination by high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS)

In the present study, a separation/preconcentration procedure for determination of aluminum in water samples has been developed by using a new atomic absorption spectrometer concept with a high-intensity xenon short-arc lamp as continuum radiation source, a high-resolution double-echelle monochromator, and a charge-coupled device array detector. Sample solution pH, sample volume, flow rate of sample solution, volume, and concentration of eluent for solid-phase extraction of Al chelates with 4-[(dicyanomethyl)diazenyl] benzoic acid on polymeric resin (Duolite XAD-761) have been investigated. The adsorbed aluminum on resin was eluted with 5 mL of 2 mol L^-1 HNO₃ and its concentration was determined by high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS). Under the optimal conditions, limit of detection obtained with HR-CS FAAS and Line Source FAAS (LS-FAAS) were 0.49 μg L^?1 and 3.91 μg L^?1, respectively. The accuracy of the procedure was confirmed by analyzing certified materials (NIST SRM 1643e, Trace elements in water) and spiked real samples. The developed procedure was successfully applied to water samples.     

Solid phase extraction of gold(III) on silica gel modified with benzoylthiourea prior to its determination by flame atomic absorption spectrometry

A new method has been developed for the determination of gold based on separation and preconcentration using silica gel modified with benzoylthiourea. The optimum experimental parameters for preconcentration of gold, such as acid concentration, sample flow rate, eluent and matrix ions, have been investigated. Gold could be quantitatively retained in the 0.25-2.0 mol L(-1) HCl and HNO(3) concentrations, and then eluted completely with 0.5 mol L(-1) thiourea in 1.0 mol L(-1) HCl. The sorption capacity of gold(III) is 0.92 +/- 0.04 mmol g(-1) with a high enrichment factor of 267. The relative standard deviation of the method, RSD%, was found as 1.2% for 0.1 microg mL(-1). The detection limit for gold was 1.4 microg L(-1). The validation of the proposed method was checked by the analysis of certified reference soil materials. The presented procedure was applied to the determination of gold in some environmental samples.     

Cu、Pb、Zn火焰原子吸收多谱线分析在环境监测中的应用

对铜的 3条谱线 (2 49.2 nm、2 61 .4nm,3 2 4.8nm ) ,铅的 2条谱线 (2 83 .3 nm、2 1 7.0 1 nm )以及锌的 2条谱线(3 0 7.6nm、2 1 3 .9nm ) ,共 7条谱线的灵敏度、检测限、线性范围进行了归纳性总结 ,并对多种共存元素可能存在的干扰情况进行了研究 ,认为利用元素不同分析谱线的分析灵敏度差异 ,根据被测元素在样品消解液中含量 ,选择合适的谱线进行分析 ,既降低工作强度 ,又能获得满意结果     

石墨炉原子吸收法测定水中硒

利用石墨炉原子吸收法,加入基体改进剂测定水中硒,并优化了测定条件。结果表明,本方法检出限低(0 85μg L),准确度高,精密度好。     

氢化物发生-原子荧光法测定环境水样中痕量锡

以醋酸 醋酸钠缓冲溶液为反应酸介质 ,应用氢化物发生 原子荧光法 (HG AFS)测定环境水样中痕量 Sn。该方法同 HCl为反应酸测 Sn方法相比 ,不仅扩大了酸浓度测定范围 ,某些阳离子干扰也降至最小或消除。其相对标准偏差(RSD)小于 3% ;回收率在 94 4 %～ 1 0 0 %之间 ;检测限为 0 76 μg L。     

Development of an efficient and sensitive analytical method for the determination of copper at trace levels by slotted quartz tube atomic absorption spectrometry after vortex-assisted dispersive liquid-liquid microextraction in biota and water samples using a novel ligand

This study describes the determination of trace levels of copper by slotted quartz tube atomic absorption spectrometry after dispersive liquid-liquid microextraction. A ligand synthesized from the reaction of salicylaldehyde and 1-naphthylamine was used to form coordinate copper complex prior to extraction. All parameters that influence the output of complex formation, extraction, and instrumental measurement were optimized to enhance the absorbance signal of copper. Under the optimum conditions, about 104-fold enhancement in sensitivity was recorded over the conventional flame atomic absorption spectrometer, corresponding to a 0.51 ng/mL detection limit. The percent relative standard deviation calculated for the lowest concentration (4.8%) indicated high precision for the experimental procedure. Accuracy and applicability of the optimum method were determined by performing spiked recovery tests on urine, lake water, and mineral water samples. Satisfactory recovery results were obtained between 82.2 and 106.3% at four different concentrations. Matrix matching method was also performed to increase the accuracy of quantification, and the percent recovery calculated for 175 ng/mL was 105.14%.     

石墨炉原子吸收法测锌的研究

研究了石墨炉原子吸收法在锌的次灵敏特征谱线测定锌的方法 ,并与火焰原子吸收法做比较。     

火焰原子吸收分光光度法测定总铬的研究

用火焰原子吸收分光光度法直接测定水和废水中的总铬.通过不同条件的实验,确定了最佳的分析条件;并通过标准样品和实际样品的分析,验证了方法的准确度和精密度.在大量实验基础上,建立空白实验、准确度质量控制图,以便定期对各种监测数据提供可行的质量保证措施.实验结果表明,该法快速方便,提高了分析效率,准确度高,精密度好,值得普及和推广.     

2-Nitroso-1-naphthol as a selective reagent for preconcentration of cobalt by vortex assisted combined with solidification of organic droplet and its determination by flame atomic absorption spectrometry

Highly rapid and selective vortex-assisted liquid–liquid microextraction based on solidification of organic drop has been used for determination of cobalt ion. 2-Nitroso-1-naphthol (2N1N) was used as a selective complexing agent to form stable cobalt–2N1N complex which can be extracted with 1-undecanol at a short time by the assistance of vortex agitator system followed by its determination using flame atomic absorption spectrometry. In vortex assisted, vigorous vortex stream as well as the vibrant effect of vortex system cause very fine droplets of extraction solvent to be produced and extraction occurred at a short time. Some parameters influencing the extraction process such as pH of samples, concentration of 2-nitroso-1-naphthol, extraction solvent volume, extraction time, ionic strength and surfactant addition, as well as interferences were evaluated in detail and optimum conditions were selected. At the optimum conditions, the calibration curve was linear in the range of 15 to 400 μg L^?1 of cobalt ions. The relative standard deviation based on ten replicate analysis of sample solution containing 50 μg L^?1 of cobalt was 3.4 %. The detection limit (calculated as the concentration equivalent to three times of the standard deviation of the blank divided by the slope of the calibration curve after preconcentration) was 5.4 μg L^?1. The accuracy of the proposed method was successfully evaluated by the analysis of certified reference materials. This selective and highly rapid method was used for determination of cobalt ions in different water samples.     

热分解齐化原子吸收光度法测定土壤中汞

固体测汞仪采用热分解齐化原子吸收光度法,此方法可以直接测定土壤中汞的含量。通过实验分析表明:此方法相关系数r≥0.999,检出限为0.01 ng,精密度为6.0%~9.1%,准确度为0%~6.7%,加标回收率为95%~107%。本方法具有简便、快速、准确、干扰少、成本低等优点,适合大批量土壤样品的测定。