Determination of Chromium and Zinc in Soil by Microwave Digestion and Flame Atomic Absorption Spectrometry

[Objective] The aim was to develop a rapid, simple method for determination of chromium and zinc in soil samples by flame atomic absorption spectrometry.[Method] The method for determination of Cr and Zn in soil by combined flame atomic absorption spectrometry and microwave digestion was used. [Result] The concentration curve was linear within the range of 0-0.8 mg/L for Cr and 0-0.8 mg/L for Zn, the detection limits of Cr and Zn was 0.0025 mg/L and 0.002 3 mg/L, respectively. Recoveries of 102.4%-103.2% for Cr and 97.7%-98.3% for Zn were obtained for there soil samples. [Conclusion] The proposed method has the advantages of simple operation, high sensitivity, and high efficiency; it was successfully used for determination of Cr and Zn in soil samples.

Determination of Copper and Lead Contents in Soil of the Yellow River Wetland in Shaanxi Province by Flame Atomic Absorption Spectrometry

[Objectives] The contents of copper and lead in the soil of the Yellow River Wetland were determined by flame atomic absorption spectrometry, which provides a theoretical basis for the treatment of soil pollution. [Methods] The soil was digested with a concentrated nitric acid-hydrofluoric acid-perchloric acid system, and the contents of heavy metals such as copper and lead in the Yellow River Wetland of Shaanxi Province were determined by flame atomic absorption spectrometry. [Results] The correlation coefficients reached 0.999 5 in the range of 0.00-1.00 mg/L, indicating good linearity. [Conclusions] The method is simple in operation, good in reproducibility, high in sensitivity to most elements, and can be widely used.

Determination of Trace Elements in Potatoes by Flame Atomic Absorption Spectrometry

[Objective] This study aimed to analyze the contents of trace elements in potatoes from different production areas in Qinghai Province. [Method] By flame atomic absorption spectrometry （FAAS）, the contents of various trace elements in potatoes were determined. [Result] Potatoes contain abundant trace elements such as Cu, Zn, Fe, Mn, Ca, K and Mg. To be specific, the contents of Ca, K and Mg were relatively high. [Conclusion] By using FAAS, the relative standard deviation was 1.17%-2.75% and the recovery rate was 97%-99.5%, indicating accurate and reli-able results with high precision.

Application of multiwalled carbon nanotubes treated by potassium permanganate for determination of trace cadmium prior to flame atomic absorption spectrometry

In this study we investigated the enrichment ability of oxidized multiwalled carbon nanotubes （MWCNTs） and established a new method for the determination of trace cadmium in environment with flame atomic absorption spectrometry. The MWCNTs were oxidized by potassium permanganate under appropriate conditions before use as preconcentration packing. Parameters influencing the recoveries of target analytes were optimized. Under optimal conditions, the target analyte exhibited a good linearity （R^2=0.9992） over the concentration range 0.5-50 ng/ml. The detection limit and precision of the proposed method were 0.15 ng/ml and 2.06%, respectively. The proposed method was applied to the determination of cadmium in real-world environmental samples and the recoveries were in the range of 91.3%-108.0%. All these experimental results indicated that this new procedure could be applied to the determination of trace cadmium in environmental waters.

Preconcentration of copper with multi-walled carbon nanotubes pretreated by potassium permanganate cartridge for solid phase extraction prior to flame atomic absorption spectrometry

A procedure for the preconcentration of copper was described in this paper using multi-walled carbon nanotubes (MWCNTs) oxidized by potassium permanganate as the adsorbent for the enrichment of trace copper in water samples. Important parameters, such as the sample pH, the concentration and volume of eluent, sample flow rate and volume, and interference of coexisting ions, were investigated. The obtained results indicated that proposed method possessed an excellent analytical performance. The linear range, the detection limit, and precison (RSD) were 1–100 ng/mL (R(2) = 0.9993), 0.32 ng/mL and 2.88%, respectively. The results showed that copper could be adsorbed quantitatively on the pretreated MWCNTs with potassium permanganate, and proposed method was very useful in the monitoring of copper in the environment.

Determination of Iron in Layered Crystal Sodium Disilicate and Sodium Silicate by Flame Atomic Absorption Spectrometry with Boric Acid as a Matrix Modifier

The effects of matrix silicate and experimental conditions on the determination of iron in flame atomic absorption spectrometry （FAAS） were investigated. It was found that boric acid as a matrix modifier obviously eliminated silicate interference. Under the optimum operating conditions, the determination results of iron in layered crystal sodium disilicate and sodium silicate samples by FAAS were satisfactory. The linear range of calibration curve is 0-10.5 μg.mL^-1, the relative standard deviation of method is 1.2%-2.2%, the recovery of added iron is 96.0%- 101%, the sensitivity is 0.19 μg.mL^-l and the detection limit is 77 ng.mL^-1. The effect of the determination of iron of the standard curve method, standard addition calibration and colorimetry method was the same, but the first has the merits of rapid sample preparation, reduced contamination risks and fast analysis.

Speciation of Dissolved Trace Nickel in Environmental Waters by On-Line Sonodigestion-Flow Injection Solid Phase Extraction Coupled to Flame Atomic Absorption Spectrometry

A simple on-line sonodigestion system was successfully used for breakdown organic nickel complexes in environmental waters acidified with diluted nitric acid prior to flow injection total dissolved nickel preconcentration in a microcolumn containing a chelating resin (Chelite Che with iminodiacetic acid groups) and determination by flame atomic absorption spectrometry. For the determination of the dissolved labile nickel fraction, microcolumns packed with the chelating resin were loaded in-situ with the sample without sample pH modification, and once in the laboratory were inserted in the flow injection device where nickel elution-detection was carried out. The performance of the chelating resin was investigated in order to elucidate its behavior in the presence of dissolved nickel species. The results obtained reveal that the resin, at the experimental employed conditions, retained only dissolved free nickel ions and nickel bound to weak complexes (labile fraction). The figures of merit for determinations in both nickel fractions are given and the obtained values are discussed. The speciation scheme is applied to the analysis of nickel in river and seawater samples collected in Galicia (Northwest, Spain). The results of fractionation showed that Ni are mainly in the dissolved labile fraction in river water, while in seawater samples analyzed was mainly present in the organic fraction.

Determination of Manganese in Tri Calcium Phosphate (TCP) by Atomic Absorption Spectrometry

Tricalcium phosphate Anhydrous Powder typically contains less than 10 ppm (mg/Kg) (w/w) manganese. This level can be determined utilizing Flame Atomic Absorption Spectrometer (AAS) and standard based on known standards. A number of analytical methods are presently used for the analysis of metals in the biochemical. The instrumental techniques available are Inductively Coupled Plasma (ICP/MS), X-Ray Fluorescence, UV-VIS Spectrophotometry, and Atomic Absorption Spectrometry. Flame AA has gained widespread acceptance as an analytical technique and is used for many applications. In this study, we have determined the amount of manganese metal present in Tricalcium Phosphate (TCP) using Flame Atomic Absorption Spectrophotometer. The method has high precision and accuracy. The percent recovery was found to be 99.8% for spiked sample. The results meet the requirement.

FLAME ATOMIC ABSORPTION DETERMINATION OF COPPER IN CEREALS FOOD SAMPLES WITH THE PRECONCENTRATION OF POTASSIUM TETRATITANATE WHISKER

A simple and reliable method has been developed for separation and preconcentration of trace amounts of copper ions in cereals food for subsequent measurement by flame atomic absorption spectrometry （FAAS）. The Cu^2＋ ions are adsorbed selectively and quantitatively during the passage. The retained copper ions were desorbed from the potassium tetratitanate whisker with 10.0mL of 2mol/L sulphuric acid solutions as eluent and were determined by FAAS. The linear range was 0.05μg/mL-0.20μg/mL in the original solution with a correlation coefficient of 0.9998. The detection limit of the proposed method is 2. lng/mL in the original solution （3σ, n=9）. Determination of copper in standard ions showed that the proposed method has good accuracy （recovery was more than 95%）. The method was successfully applied for recovery and determination of copper in cereals food samples

Flow-Injection Flame Atomic Absorption Determination of Hexavalent Chromium with On-Line Preconcentration on an Anion Imprinted Polymer

A flow injection preconcentration system for the flame atomic absorption spectrometric determination of hexavalent chromium has been developed. The method employs on-line preconcentration of Cr(VI) on a minicolumn packed with Cr(VI)-imprinted poly(4-vinyl pyridineco-2-hydroxyethyl methacrylate) placed into a flow injection system. Hexava-lent chromium was eluted with a small volume of diluted hydrochloric acid into the nebulizer-burner system of a flame atomic absorption spectrometer. An enrichment factor of 550 and a 3σ detection limit of 0.04 μg·L-1 along a sampling frequency of 4 h-1 at a sample flow rate of 3.5 mL·min-1. The relative standard deviation is 2.9% for 1 μg·L-1 Cr(VI) (n = 11). The flow injection system proposed has the advantage of being simpler because the use of expensive and sophisticated instruments is avoided. Ease of use, continuous process and selectivity make this method suitable for Cr(VI) determination in different environmental samples such as sea and river waters, soils and sediments.

GF-AAS与ICP-MS测定水中总铬含量的方法比对及其不确定度评定

石墨炉原子吸收光谱(GF-AAS)法和电感耦合等离子体质谱(ICP-MS)法是灵敏度较高的2种测定水中铬含量的方法。文中采用357.9 nm与429.0 nm波长条件下GF-AAS法、52与53质核比条件下ICP-MS法测定水质铬标准物质中总铬元素含量,从标准曲线、准确性、重复性、加标回收率、检出限、定量限、测量不确定度评定多个方面进行对比分析。结果表明,4组测定条件下,标准物质测定结果均在标准值不确定度范围内。其中,429.0 nm波长GF-AAS法测定结果相对其他3组显著偏低(P<0.05);ICP-MS法在检出限、定量限方面优于GF-AAS法;GF-AAS法测定结果357.9 nm波长优于429.0 nm波长。

微波消解-AAS法测芦荟中微量金属元素锌、锰、镉、铅

应用具有压力控制附件的MSP 10 0D型微波样品制备系统 ,进行新鲜芦荟叶外皮及凝胶中锌、锰、镉、铅元素的微波消解研究 ,并采用原子吸收法测定其元素的含量。讨论了混合酸体系、混酸配比、固液比和微波消解时间对于微波消解结果的影响。在混合酸体系HNO3 HCl中 ,当混酸HNO3 HCl配比为 8∶3、固液比为 1∶12、最高功率时微波消解时间为 6min的条件下 ,消解结果最佳。在微波消解最佳条件下 ,进行了精密度实验和回收率实验 ,所得结果的相对标准偏差均在 0 3%～ 6 2 %之间 ,回收率在 95 0 %～ 110 0 %之间。结果表明 ,微波消解法处理新鲜芦荟叶片 ,具有快速、简便、节省试剂、消解完全等特点 ,测定结果的精密度和准确度令人满意。

薯类中营养元素锌、钾的FAAS测定研究

研究了用火焰原子吸收分光光度法测定甘薯中的微量元素锌、钾的方法 ,采用高温灰化法对样品进行处理 ,并对 4 0多种不同品种和不同种植地区的甘薯进行了实样测定和含量差异比较。测定回收率在91.9%— 10 8.0 %之间。取得了令人满意的结果。

微波消解-FAAS法测定大鼠肝脏中的微量元素

研究了采用微波消解样品,利用火焰原子吸收分光光度法(FAAS)测定了大鼠肝脏中的钙、锌、铜、镁、铁.考察了微波消解条件对分析结果的影响,同时选择了火焰原子吸收分光光度法测定的最佳条件.实验结果表明,与传统的湿法消解样品相比,该方法操作简便、快速、样品消解完全,空白值低,选择性好,准确度和精确度都能满足分析要求.利用该法对大鼠肝脏中的微量元素进行了分析,测定结果令人满意.方法回收率在96%～103%,相对标准偏差为1.0%～2.6%.

FAAS直接法测定环境和生物试样中Zn、Pb和Cd

本文系统研究了海水、土壤、沉积物和生物中Cd、Pb和Zn用火焰原子吸收直接法测定时的干扰与背景校正。由于这些物质基体中含有大量Al、Na、K、Ca、Mg、Fe等元素 ,在火焰中形成MX、MO和MOH分子光谱与分析元素线重叠 ,经背景校正后可获得更准确的结果和更好的回收率 。

FAAS法测定原生态硒米中的微量元素铁和镍

[目的]测定黔东南苗族侗族自治州原生态丹寨精硒米中微量元素铁和镍的含量。[方法]采用正交试验优化仪器最佳工作条件,湿法消解硒米样品,火焰原子吸收光谱法(FAAS)测定微量元素铁和镍。[结果]原生态丹寨精硒米中微量元素铁和镍的含量分别为8.00和0.50 mg/kg。[结论]该研究方法操作简便,灵敏度高,检出限低。

FAAS测定嫩、老荷叶中7种营养元素含量

采用火焰原子吸收光谱法对嫩、老(成熟)荷叶中K、Ca、Mg、Mn、Fe、Zn、Cu7种营养元素的含量进行测定。结果表明,嫩、老荷叶中7种营养元素含量高低顺序一致,依次为K>Ca>Mg>Mn>Fe>Zn>Cu,但成熟荷叶中钙、锰含量明显高于嫩荷叶,约为嫩荷叶的两倍,铁含量稍高于嫩荷叶,钾、镁、锌、铜含量略低于嫩荷叶。其中成熟荷叶中锰的含量为738.04μg.g-1,比一般中药高出近20倍,荷叶的多种药用价值可能与富含微量元素锰有密切关系。

石墨炉AAS法分析冬青科苦丁茶树系统中镉及其分布

采集海南大学苦丁茶种质资源库中6种冬青科(Ilex)苦丁茶树的根、茎、叶及对应土壤样品,通过试验研究,建立了高压密封消解-石墨炉原子吸收光谱法测定样品中镉的方法。对植物样和土壤样分别采用硝酸-双氧水和硝酸-高氯酸-氢氟酸混酸体系进行消解。以磷酸二氢铵作为基体改进剂,并开启氘灯校正背景,在优化的工作条件下测定样品中镉。该方法的检出限为0.300ng/mL,用于实验样品中镉的测定,其相对标准偏差RSD<5%,加标回收率介于94%～108%之间。用该方法对茶叶(GBW10016)和土壤(GBW-07407)标准参考物中镉进行了测定,测定结果与标准值相符合,相对误差小于7%。冬青科苦丁茶树及其土壤中镉的分布具有特征性,主要表现为:土壤>>茶树,根际土壤>非根际土壤,吸收根>主根或茎,嫩叶>老叶>枯叶。

烟叶中Cu、Fe、Mn的FAAS连续测定分析方法

采用火焰原子吸收光谱法在同一体系中连续测定烟叶中金属元素 Cu、Fe、Mn的含量 ,方法简单 ,精密度和灵敏度高 ,相对标准偏差为 0 .5 6 %— 3.12 % ,回收率为 10 3.4 2 %— 97.6 2 %。

澳洲坚果果仁中4种关键微量元素的FAAS法测定

为探明澳洲坚果果仁中Fe、Mn、Cu、Zn 4种关键微量元素的含量及其测定方法,运用火焰原子吸收分光光度法(FAAS),采用干灰化、混酸消解、微波消解3种不同样品消解方式,对4个澳洲坚果品种果仁中Fe、Mn、Cu、Zn的含量进行了测定。结果表明:Fe、Cu经3种不同消化方式处理后的含量测定结果无显著差异;而Mn、Zn经微波消解处理后的测定值虽然略高于干灰化和混酸消解2种方式,但未达到显著水平;澳洲坚果果仁中4种微量元素的含量为Mn>Fe>Zn>Cu,其中Mn元素含量在品种间的变异较大;在4个供试品种中,‘云澳51号’的Fe含量为最高,而‘云澳58号’的Mn、Cu、Zn 3种微量元素含量均为最高。3种样品消解方式均可用于澳洲坚果果仁微量元素含量的FAAS法测定。