Determination of Available Cadmium and Lead in Soil by Flame Atomic Absorption Spectrometry after Cloud Point Extraction

A cloud point extraction (CPE) procedure has been developed for the determination of available cadmium (Cd) and lead (Pb) in soil by flame atomic absorption spectrometry. The proposed method was based on the CPE of a complex from ammonium pyrrolidine dithiocarbamate (APDC) and metal Cd and Pb using emulsifier octyl polyethylene glycol phenol ether (OP) as surfactant. Conditions that would affect the complex formation and separation were researched in detail, including extraction conditions as well as pH, amount of the chelating agent, concentration of the surfactant, equilibration temperature and time, and salt effect. Under the optimized conditions, both of the calibration graphs were linear in range of 0–1.0 μg mL^?1 with detection limits of 0.29 ng mL^?1 for Cd and 2.10 ng mL^?1 for Pb. The relative standard deviation (RSD) for 11 replicate measurements at 0.10 μg mL^?1 of Cd and Pb were 2.18% and 4.04%, respectively. The enhancement factors were 48.8 and 61.6 for Cd and Pb, respectively. The recoveries of Cd and Pb at the spiking level of 0.10 μg g^?1 in soil samples were from 91.7% to 115% and from 91.0% to 115%, respectively. The proposed method has been applied to the determination of available Cd and Pb in soil.     

原子吸收测定土壤镍的测量不确定度评定研究

本文评定了火焰原子吸收测定土壤中镍含量的测量不确定度。以标准土壤样品(GSW 17401)为测试对象,通过应用火焰原子吸收法测定土壤镍含量,对其测量不确定度的来源、计算和结果表示等问题进行探讨。样品消解前处理产生的不确定度最大,标准曲线拟合测定溶液产生的不确定度其次。在测定中前处理和标准曲线拟合测定溶液应给予足够重视,以减小测量不确定度。     

Separation of Ag(I) Ions from Lepidium draba L. Plant and Water and Standard Samples by Carrier Element-Free Coprecipitation Method Prior to their Flame Atomic Absorption Spectrometric Determination

In this work, silver iodide (Ag(I)) ions were separated via the carrier element-free coprecipitation (CEFC) method using an organic coprecipitating agent, 1,6-diamino-4-(4-chlornphenyl)-2-oxo-1,2-dihydropyridine-3,5-dicarbonitrile [DCODD] prior to its determination by ?ame atomic absorption spectrometry (FAAS). Analytical parameters including pH of aqueous solution, amount of DCODD, standing time, centrifugation rate and time, and sample volume were studied and optimized. Under the best experimental conditions, it was found that extraction can be performed from the sample volume of 500.0 for silver ion (preconcentration factor of 100.0). Linearity was maintained between 0.006 and 1.50 µg.mL^?1 for silver. Detection limit for silver based on 3Sb was 1.60 ng.mL^?1. The relative standard deviation of eight replicate measurements of 0.20 µg.mL^?1of silver was 2.10%. Finally, the developed method was successfully applied to extraction and determination of the silver ions in the Lepidium draba L plant, water and standard samples and satisfactory results were obtained.     

石墨炉原子吸收光谱法测定土壤铝的条件优化

酸性土壤中的活性Al是影响作物生长发育的主要因子之一,土壤Al的测定一直是人们关注的问题。石墨炉原子吸收光谱法测土壤Al所需的样品量少、灵敏度高、离子干扰小,目前在国内外应用较为广泛。由于其测试条件多是应用单因素轮换法来确定,存在实验量大且未考虑交互作用的影响等缺点。采用双因素重复实验及正交实验可显著降低确定最佳测试条件的工作量,且实验条件代表性强,对于准确快捷测定土壤Al具有重要意义。通过双因素（波长和灯电流）重复试验对石墨炉原子吸收光谱仪测定土壤Al的波长和灯电流进行了优化选择,确定最佳波长为309.3nm,最佳灯电流为14mA;应用L2（556）正交试验法对控温程序及基体改进剂、基体酸度条件进行了优化,得出最佳的灰化温度为1400℃、灰化时间为10s,原子化温度为2300℃、原子化时间为5s,最佳基体改进剂为0.1%NH4H2PO4、最佳基体酸度为0.2%硝酸。优化后的方法检出限为1.14μg.L-1,加标回收率达到93.6%~104.1%,相对偏差均小于8%。     

Preparation of Modified Magnetic Cobalt Nanoparticles as a New Magnetic Sorbent for the Preconcentration and Determination of Trace Amounts of Lead Ions in Environmental Water and Soil (Air-Dust) Samples

In this study, cobalt magnetic nanoparticles (MNPs) were synthesized and then modified by sodium dodecyl sulfate (SDS) and 2-(5-bromo-2-pyridylazo)-5-diethyl aminophenol ligand (5-Br-PADAP), through a chemical precipitation method. Characterization of the prepared MNP adsorbents was performed by Fourier transform infrared and transmission electron microscopy. Cobalt nanoparticles (NPs) surface modified with SDS and 5-Br-PADAP was evaluated as a nanoparticulate solid-phase extraction (SPE) absorbent for lead ions Pb(II) from water and standard samples, prior to its flame atomic absorption spectrometry determination. Effects of pH, amount of sorbent, desorption solvent, adsorption time, desorption time, and interfering ion concentration on extraction efficiency were investigated. Under optimal conditions, the calibration curve was linear in the range of 1.0–500 ng mL^?1of Pb(II) with R² = 0.998. Detection limit was 1.6 ng mL^?1 in the original solution (3S_b/m), and the relative standard deviation for replicate determination of 0.5 μg mL^?1 Pb(II) was ±2.7%.     

原子吸收次灵敏线法直接测定土壤中Fe、Mn

用原子吸收次灵敏线法塞曼效应扣除背景测定土壤中Fe、Mn,实验结果表明:此方法有较好的准确度,精密度,操作简单,适合一般土壤中Fe、Mn的测定。     

乳化剂OP增敏——火焰原子吸收光谱法连续测定土壤中有效铜、锌

研究了用非离子表面活性剂乳化剂OP为增敏剂,火焰原子吸收光谱法测定土壤有效铜、锌的方法。试验结果表明,加入乳化剂OP可使铜吸光度增加70%,锌吸光度增加25%,提高了分析的灵敏度。方法操作简便、快速,相对标准偏差小于8.12%,加标回收率为95.2%~102.5%。     

超声波溶样、APDC-MIBK萃取石墨炉原子吸收法测定土壤中有效钼的研究

研究石墨炉原子吸收法测定土壤中有效钼,采用超声波溶样,APDC-M IBK萃取,抗坏血酸作基体改进剂.实际样品加标回收率为95%~105%,相对标准偏差为:1.35%.与其他方法比较具有快速、准确、灵敏、干扰小、操作简单、重现性好等特点,结果令人满意,值得推广。     

双道原子荧光光谱同时测定土壤中砷、汞的方法研究

研究了土壤中总As、总Hg的同时测定方法,并对消化体系进行了筛选,利用正交试验设计法对测试条件进行了优化.建立了用王水消解样品,在10%盐酸溶液中用双道原子荧光光度计同时测定土壤中As、Hg的新方法.方法线性范围宽(As 0～200μg/L;Hg 0～10μg/L);检出限低(As 0.05μg/L;Hg 0.007μg/L);As的回收率为96.0%～101.0%,Hg的回收率为97.0%～103.7%;相对标准偏差(RSD)As为2.7%,Hg为4.5%.该方法准确、简便、快速,结果令人满意.     

电感耦合等离子体质谱法测定土壤中的总碘

采用碱液热浸提法处理土壤样品,通过电感耦合等离子体质谱法(ICP-MS)测定土壤中碘元素的总量。对前处理的3大参数——碱度、温度和时间进行试验摸索,得出适用于土壤的最佳浸提条件。测定结果显示,该方法的线性范围为0~500μg/L,线性相关系数0.999 8,方法检出限0.12μg/g,加标回收率为91.0%~104%,RSD均小于5%。综上,该法是一种能够快速、灵敏、准确地测定土壤样品中碘元素的先进方法。     

Determination of Trace Amounts of Cadmium Ions in Water and Plant Samples Using Ligand-Less Solid Phase Extraction-Based Modified Co3O4 Nanoparticles

In this study, a new Co₃O₄ nanoparticles (NPs) coated with sodium dodecyl sulphate (SDS) is developed for preconcentration of trace amounts of cadmium ions (Cd ²⁺) as a prior step to its determination by flame atomic absorption spectrometry (FAAS). The effects of various parameters, including pH of sample solution, amount of sorbent, flow rates of solution and eluent, sample volume, type, and least amount of the eluent for elution of the Cd ²⁺ from Co₃O₄ NPs were studied and optimized. Experimental conditions for effective separation of trace levels of the Cd ²⁺were optimized with respect to different experimental parameters in Column method. Under the best experimental conditions, the calibration curve was linear in the range of 1.0–500.0 ng.mL^?1 of cadmium (Cd) with R² = 0.999. The detection limit was 0.4ng.mL^?1 in the original solution (3S_b/m) and the relative standard deviation for eight replicate determination of 0.1µg.mL^?1 Cd was ±2.1%. The method was validated by the analysis of a certified reference material with the results being in agreement with those quoted by manufactures. The developed method was successfully applied to the extraction and determination of Cd in water and food samples with satisfactory results.     

氢化物原子荧光光谱法测定水溶肥料中的硒

文章介绍了原子荧光光谱法测定水溶肥料中硒含量的方法。该方法具有操作简单、快速、基体干扰少、灵敏度高等优点。该方法检出限为0.24 μg/L,线性范围0 μg/L～300 μg/L,加标回收率96.5%～103.0%。     

Evaluation of a sequential extraction procedure for the fractionation of thallium in soils and determination of the content by flame atomic absorption spectrometry

Abstract

The release of carbonyl sulfide (COS) from 7 unamended paddy soils was estimated under aerobic and waterlogged conditions. The addition of organic materials to the soils increased the amount of COS evolved under waterlogged conditions. To assess the sources of the COS released from the soils, the soils were incubated under aerobic and waterlogged conditions after treatment with 17 inorganic or organic S-containing compounds. It was concluded that the following compounds represented sources of the COS released from the paddy soils: cystine, cysteine, thiocyanate, lanthionine and djenkolic acid.     

Chromium Speciation in Water by Sorption on Calcite and Determination by Electrothermal Atomic Absorption Spectrometry

Abstract

A rapid, sensitive, and accurate method for the separation and speciative determination of chromium (Cr)(VI) and Cr(III) in water samples has been developed using sorption as the separation technique in conjunction with final determination by electrothermal atomic absorption spectroscopy (ETAAS). The present method, where granular calcite is used as selective sorbent, separates Cr(III) with retention values up to 99%, resulting in high accuracy determination of Cr(VI). Total Cr was likewise determined by ETAAS after an efficient reduction of Cr(VI) to Cr(III) using ascorbic acid as reducing agent, deriving Cr(III) concentration from the difference between total Cr and Cr(VI). The parameters of the separation technique, solution pH (4.5–5.5), solution flow rate through the calcite column (0.14–0.42 mL min^?1), and calcite column internal diameter (1.5–3.0 cm), were evaluated. Best results were achieved with pH of 5.5, flow rate of 0.42 mL min^?1, and column internal diameter of 1.5 cm. Optimum determination conditions were found using magnesium nitrate [Mg(NO₃)₂] as chemical modifier, pyrolysis, and atomization temperatures of 1400 and 2200°C, respectively. In such conditions, the detection limits (n=10) were 1.5 and 0.8 µg L^?1 for Cr(III) and Cr(VI), respectively.     

岷江成都段底泥中重金属的原子吸收多元素同时测定及趋势分析

在单元素原子吸收法的基础上，使用瓦里安SpectrAA220FS原子吸收光谱仪，建立了底泥中部分金属元素的原子吸收多元素同时测定方法。应用本法测定了岷江成都段底泥中的部分金属元素铜、镍、锌、铅、镉的含量，分析了污染物质的分布规律与变化趋势，为水环境研究、保护和管理提供更快捷方便的测试方法。     

Selective Determination of Chromium(VI) in Industrial Wastewater Samples by Micro-Electromembrane Extraction Combined with Electrothermal Atomic Absorption Spectrometry

This study describes application of free liquid membrane (FLM) in micro-electromembrane extraction (μ-EME) of Cr(VI) from wastewater samples. Amount of Cr(VI) was quantified by electrothermal atomic absorption spectrometry. The transportation of Cr(VI) across the FLM was explored by electrokinetic migration and ion-exchange process. FLM and acceptor solution types, pH of donor and acceptor solutions, applied electrical potential, as well as FLM thickness were optimized. Presence of an anion exchange carrier (methyl trialkyl-ammonium chloride, Aliquat 336) in FLM facilitated Cr(VI) transportation. The best performance was observed for 1-octanol (containing 5% Aliquat 336) with thickness of 1 mm used as FLM, under applied electrical potential of 75 V, when 0.5 M NaClO₄ and 0.1 M HCl were used as the acceptor and donor phases, respectively; and the extraction time was set to 5 min. Linearity was obtained in the working range of 0.5–14.0 ng mL^?1 Cr(VI) (R²?>?0.98). The calculated limit of detection was below 0.06 ng mL^?1. Application of this method to wastewater samples showed that relative recoveries of the spiked Cr(VI) in the samples were in the range of 73.8–85.1%, based on the standard addition method.     

Use of the BCR three-step sequential extraction procedure for the study of the partitioning of Cd, Pb and Zn in various soil samples

A slightly modified three-step sequential extraction procedure proposed by the Community Bureau of Reference (BCR) for analysis of sediments was successfully applied to soil samples. Contaminated soil samples from the lead and zinc mining area in the Mezica valley (Slovenia) and natural soils from a non-industrial area were analysed. The total concentrations of Cd, Pb and Zn and their concentrations in fractions after extraction were determined by flame or electrothermal atomic absorption spectrometry (FAAS, ETAAS). Total metal concentrations in natural soils ranged from 0.3 to 2.6 mg kg^-1 for Cd, from 20 to 45 mg kg^-1 for Pb and from 70 to 140 mg kg^-1 for Zn, while these concentrations ranged from 0.5 to 35 mg kg^-1 for Cd, from 200 to 10000 mg kg^-1 for Pb and from 140 to 1500 mg kg^-1 for Zn in soils from contaminated areas. The results of the partitioning study applying the slightly modified BCR three-step extraction procedure indicate that Cd, Pb and Zn in natural soils prevails mostly in sparingly soluble fractions. Cd in natural soils is bound mainly to Fe and Mn oxides and hydroxides, Pb to organic matter, sulphides and silicates, while Zn is predominantly bound to silicates. In contaminated soils, Cd, Pb and Zn are distributed between the easily and sparingly soluble fractions. Due to the high total Cd, Pb and Zn concentrations in contaminated soil close to the smelter, ! and their high proportions in the easily soluble fraction (80% of Cd, 50% of Pb and 70% of Zn), the soil around smelters represents an environmental hazard.     

硝酸一次消解同时测定土壤中Cd、As、Hg的方法研究

硝酸在水浴中一次性消解土壤样品,用石墨炉原子吸收测定镉、原子荧光光谱法同时测定砷和汞。其检出限镉为0.053 ng m l-1、砷为0.011 ng m l-1、汞为0.008 ng m l-1,线性范围镉为0~4 ng m l-1、砷为0~40ng m l-1、汞为0~2 ngm l-1。回收率在93.0~104.0%。本方法简便了消煮过程,一次消解能同时测定土壤中的多种重金属。     

Determination of molybdenum in plant tissue by graphite furnace atomic absorption spectrophotometry (GFAAS)

Abstract

The analysis of molybdenum in plant tissue using graphite furnace atomic absorption spectrophotometry (GFAAS) is described. The method involved wet digestion using a mixture of sulphuric, nitric and perchloric acids followed by a solvent extraction procedure. Molybdenum was extracted into di‐iso butyl ketone (DIBK) as the iron‐thiocyanate complex. The extract was then analysed for molybdenum by GFAAS.

The results of analyses of the reference plant materials (orchard leaves and citrus leaves) of the National Bureau of Standards (NBS) compared very well with the certified values. Other types of plant tissue were also analysed and the results correlated well with those obtained by an alternative method.     

Development of Analytical Procedure for the Determination of Exchangeable Cr(VI) in Soils by Anion-exchange Fast Protein Liquid Chromatography with Electrothermal Atomic Absorption Spectrometry Detection

Analytical procedure for the determination of exchangeable Cr(VI) was developed. In order to optimise the extraction procedure, the efficiency of extraction of exchangeable Cr(VI) in soil samples was investigated in KH₂PO₄–K₂HPO₄ buffer solutions (0.015 up to 0.2 mol l^?1), adjusted to the pH of the soil. Phosphate buffer was used to efficiently desorb Cr(VI) from soil particles. The extraction time (mechanical shaking) ranged from 1 up to 72 h. Cr(VI) in soil extracts was determined by anion-exchange fast protein liquid chromatography with electrothermal atomic absorption detection (FPLC-ETAAS). The study was performed on soil samples from the field treated with the tannery waste for seventeen years. Samples were analysed in the 16 year after the last waste application. It was experimentally proven that the optimal phosphate buffer concentration was 0.1 mol l^?1 and extraction time 16 h. An additional experiment was done to confirm that during the extraction, soluble Cr(III) was not oxidised to Cr(VI) by Mn(IV) oxides present in soil samples. For this purpose soil with the same characteristics, but not treated with tannery waste, was spiked with Cr(III) and the analytical procedure performed. No measurable Cr(VI) concentrations were detected. The repeatability of measurement was 2.5%, while the reproducibility of measurement was 6.9%. The accuracy of the analytical procedure was tested by spiking of soil samples with Cr(VI). The recoveries were better than 95%. The analytical procedure with limit of detection (LOD) 15 ng g^?1 of Cr(VI) was sensitive enough for the determination of exchangeable Cr(VI) in soils. In field soil samples analysed the concentrations of exchangeable Cr(VI) were found to be about 200 ng g^?1.