Determination of Lead in Lime-preserved Egg by Microwave Digestion and Flame Atomic Absorption Spectroscopy

[Objectives] To establish a method for determining the lead content in lime-preserved eggs, to provide a theoretical basis for the quality control of production enterprises and the sampling and testing of supervision departments. [Methods] The lead content in lime-preserved eggs was measured by the microwave digestion and flame atomic absorption spectroscopy. [Results] The method had a correlation coefficient of r2=0.998 in the injection concentration range of 0-4 mg/L. The detection limit of the method was 0.008 2 mg/kg. In the range of 0.2 to 1.0 mg/kg addition concentration, the recovery rate of the method was 92.5%-108.0%, and the relative standard deviation(RSD) was <5%. [Conclusions] This method is accurate and reliable, simple and efficient, and is suitable for the detection of lead in lime-preserved eggs.

Determination of vanadium in food and traditional Chinese medicine by graphite furnace atomic absorption spectroscopy

Various experimental conditions were described for the vanadium determinationby graphite furnace atomic absorption spectroscopy (GFAAS). The experiments showed that whenatomization took place under the conditions where the combination of a pyrolytic coating graphitetube and fast raising temperature were used and the temperature was stable, the signal peak shapescould be improved, the sensitivity was enhanced, and the memory effect was removed. The vanadium infood and traditional Chinese medicinal herbs can be accurately determined using the standard curvemethod.

The Use of Multiwalled Carbon Nanotubes Mini Column for Preconcentration of Trace Metal Ions in Tap Water of Khartoum City and Their Determination by Flame Atomic Absorption Spectrometry （FAAS）

The adsorption behavior of multiwalled carbon nanotubes （MWNTs） toward heavy elements has been investigated systemically, and a new method has been developed for the determination of trace elements in water samples based on preconcentration with mini-column packed with MWNTs prior to its determination by flame atomic absorption spectrometry （FAAS） The recommended parameters of proposed method influencing the preconcentration of the analytes, such as pH of the sample, sample flow rate and volume, elute solution and interfering ions, have been used. Under the optimized conditions, the calibration graphs were linear with the correlation coefficient range 0.9981-0.9995. According to the results, the metals were found 0.019-0.051, 0.011-0.031, 0.00-0.081, 0.00-0.0002, 0.007-0.0925, 0.00-0.0104 μg/L in water samples for Pb, Mn, Zn, Cd, Fe, Cu respectively. The percentage relative standard deviation （%RSD） for five replicate samples were 〈 5% in all cases. The method has been successfully applied to the determination of trace elements in some environmental samples with satisfactory results.

Use of Flame Atomic Absorption Spectroscopy and Multivariate Analysis for the Determination of Trace Elements in Human Scalp

The analysis of trace elements in human hair for use as biomarkers continues to generate considerable interest in environmental and bioanalytical studies, medical diagnostics, and forensic science. This study investigated the concentrations of essential and toxic elements (Fe, Mg, Ca, Cu, Zn, Cr, Cd, and Pb) using flame atomic absorption spectroscopy (FAAS) in human scalp hair obtained from subjects living in Forsyth County, North Carolina, USA. The influence of age, sex, race, and smoking habits on the levels of trace elements in the hair samples were also investigated. Additionally, analyses were subjected to a statistical, regression, and principal component analysis to evaluate inter-elemental association and possible pattern recognition in hair samples. Furthermore, Ca/Mg and Zn/Cu ratios, which are often used to evaluate the degree of Ca and Cu utilization in humans and as markers for various health related issues including, atherosclerosis, hypertension, insulin sensitivity, and pancreatic cancer, were calculated. The overall mean concentrations of Fe (25 μg/g), Ca (710 μg/g), Mg (120 μg/g), Zn (190 μg/g), Cu (12 μg/g), and Cr (0.20 μg/g) were found in hair samples. The trace element concentrations varied widely in hair samples as demonstrated by large range of concentrations obtained for each element. However, levels of Cd and Pb elements of <0.030 μg/g were detected in hair sample. In general, the levels of the trace elements in hair samples were poorly correlated. However, significant correlations were found between Ca and Mg (r = 0.840, p = 0.05). The levels of Fe, Ca, Mg, Zn, Cu, and Cr in hair samples and the calculated Ca/Mg and Zn/Cu ratios were found to be largely correlated with age, race, sex, and smoking habits.

FAAS测定铅矿石中铜含量的不确定度评定

本研究采用FASS检测技术,根据GB/T14353.1-2010的实验标准方法对铅矿石中铜元素的含量进行测定。然而实验测量过程中会产生不可避免的不确定度,因此对实验过程中产生的不确定度进行评定,结果表明测量铅矿石样品中铜的含量为284±27.49μg/g,确定了实验过程中产生不确定度的主要来源,包括样品重复性测量、样品称量、样品体积定容、标准曲线拟合及标准溶液的配制,对比发现标准曲线拟合的不确定度对测量结果的影响最大。

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。

Determination of Five Metallic Elements in Guoshangye from Guizhou by Microwave Digestion-flame Atomic Absorption Spectrometry

In the study, the contents of 5 trace elements including Fe, Cu, Mg, Mn and Ca were directly analyzed by flame atomic absorption spectroscopy in Gu- oshangye. The sample was subjected to microwave digestion with HNO3 and H2O2, and detected by the standard curve method. The results showed that Guoshangye contained abundant trace elements which rates of these trace elements were in the curacy and satisfactory. were necessary for human. The recovery range of 96%-103%. The method is ac-

Solid Phase Extraction and Determination of Nickel in Water Samples by Using Novel Thiol-Containing Sulfonamide Polymeric Resin and Atomic Absorption Spectrophotometer

Interest in preconcentration techniques for the determination of metals at ultratrace levels still continues increasingly because of some disadvantages of flameless atomic absorption spectrometry as well as the high costs of other sensitive methods in compared to flame atomic absorption spectrometry.In this study,thiol-containing sulfonamide resin was synthesized,characterized and applied as a new sorption material for solid phase extraction of nickel in drinking water samples.After preconcentration procedure,flame atomic absorption spectrometry was used for determinations.Optimum parameters were found to be pH=3.2,contact time=20 min and eluate volume=3 mL.The limit of detection was found to be 0.75 ng·mL-1.The synthesized resin exhibits the superiority in compared to the other adsorption reagents because of the fact that there is no necessity of any complexing reagent,high sorption capacity as well as the relatively fast extraction rate.The Ni concentrations in the studied 21 kind of water samples were found to be in the range of BDL-4.0 ng·mL-1.

Branched Polyamines Functionalized with Proposed Reaction Pathways Based on ¹H-NMR, Atomic Absorption and IR Spectroscopies

Three novel branched polyamines N,N,N’,N’-tetrakis-[3((pyridine-2-methyl)-amine) propyl]-1,4- butanediamine (1), N,N,N’,N’-tetrakis-[N-((2-methylpyridine)ethyl)propanamide]ethylenediamine (2) and N,N,N’,N’-tetrakis-[3((2-hidroxibenziliden)-amine)propyl]-1,4-butanediamine (3), were synthesized starting from 2-pyridinecarboxaldeyde with DAB-Am-4 for 1, PAMAM G0 for 2 and from salicylaldehyde with DAB-Am-4 for 3. The pathway reactions have been proposed by 1H-NMR, IR and Atomic Absorption Spectroscopy. The optimal reaction time was set by IR spectroscopy following aldehyde? peak modification. 1 and 2 were obtained as both hydrochlorides and as free amines and 3 only as free imine. These polyamines were characterized by UV-Vis, IR, 1H-NMR and 13C-NMR and Mass Spectrometry.

Preconcentration of Lead in Sugar Samples by Solid Phase Extraction and Its Determination by Flame Atomic Absorption Spectrometry

A simple and sensitive solid phase extraction utilizing C18 filled cartridges incorporated with dithizone for preconcentration of lead and its subsequent determination by flame atomic absorption spectrometry (FAAS) was developed. Several parameters such as type, concentration and volume of eluent, pH of the sample solution, flow rate of extraction and volume of the sample were evaluated. The effect of a variety of ions on preconcentration and recovery was also investigated. At pH = 7.4 and 1.0 mol?L–1 HCl eluting them, lead ions were recovered quantitatively. The limit of detection (LOD) defined as 3Sbl was determined to be 8.1 μg L–1 for 500 mL of sample solution and eluted with 5 mL of 1.0 mol?L–1 HCl under optimum conditions. The accuracy and precision (RSD %) of the method were >90% and <10%, respectively. In the end, the proposed method was applied to a number of real sugar samples and the amount of lead was determined by spiking a known concentration of lead into the solution.

Coherent Resonance of Saturated Absorption in Spectroscopy of Counterpropagating Waves

Results of theoretical researches of the saturated absorption resonance shape in a method of the probing field on V-type of transitions are represented. It is shown that in case of opposite circulary polarized optical fields the resonance is shown in the form of cross, and its form strongly depends on relaxation constants of levels and it can be represented as in the form of a dip, and absorption peak. Thus the peak form has exclusively coherent character. Atomic transitions are offered, on which observation of the given effect is possible.

Dental Erosion by Beverages and Determination of Trace Elements in Teeth by Atomic Absorption Spectrometry

The analysis of trace elements in human tooth for use as biomarkers continues to generate considerable interest in environmental and bioanalytical studies, medical diagnostic and forensic science. This study investigated concentrations of essential and toxic elements (Zn, Cu, Pb, Ni, Co and Cd) using flame atomic absorption spectroscopy (FAAS) and (Na and K) flame atomic emission spectroscopy (FAES) in human tooth obtained from Misan province, Iraq. The influence of smoking habits and born children on the levels of trace elements in additional to dental erosion by some beverages in the tooth samples were investigated. The overall of mean concentrations of (Zn 185.2 ppm, Cu 36.11 ppm, Pb 18.63 ppm, Ni 13.44 ppm, Co 3.45 ppm, and Cd 0.58 ppm, Na 11.683 ppm and K 115.27 ppm), (Zn 178.243 ppm, Cu 35.877 ppm, Pb 15.64 ppm, Ni 12.89 ppm, Co 3.421 ppm, Cd 0.455 ppm, Na 11,558.04 ppm and K 114.04 ppm) in smokers and non-smokers tooth groups respectively, (Zn 81.12 ppm, Cu 24.37 ppm, Pb 11.18 ppm, Ni 13.68 ppm, Co 3.32 ppm, Cd 0.44 ppm, Na 8227 ppm and K 76.42 ppm), (Zn 80.58 ppm, Cu 24.30 ppm, Pb 10.86 ppm, Ni 12.74 ppm, Co 2.71 ppm, Cd 0.23 ppm, Na 8165 ppm and K 72.80 ppm) in mothers and wives tooth groups respectively. However the w/w% loss of tooth immersed in following order of beverages (green tea, black tea, cinnamon, hibiscus, vinegar and citrus aurantifolia (9.09, 9.68, 12.36, 15.01, 16.77 and 17.38), (8.19, 8.25, 9.76, 13.37, 14.02 and 15.33) in smokers and non-smokers groups respectively, (11.25, 11.47, 13.30, 15.75, 19.58, and 20.91), (8.31, 7.96, 11.39, 13.49, 17.40, and 17.67) in mothers and wives groups respectively. However, there is a statistically significant variance found Zn (tcal 5.029, ttab 2.131), Pb (tcal 4.8538, ttab 2.131), Ni (tcal 5.243, ttab 2.131), Cd (tcal 3.9062, ttab 2.131) and Na (tcal 3.0832, ttab 2.131) between smokers and non-smokers tooth groups. However, the Co (tcal 2.7403, ttab 2.131) also shows statistically significant variance between mothers and wives groups. There is no statistically significant variance in w/w% loss after immersed the tooth in some beverages but in general it was higher in smokers than non-smokers and in mothers higher than wives.

“原子吸收光谱”实验教学的探讨与改进

原子吸收光谱法是《仪器分析》课程中重要的仪器分析内容,它广泛用于各个领域中微量及痕量元素的分析。在中药学领域更是中药重金属及有害元素测定的主要方法,是检测药材重金属及有害物质残留的主要手段。文章结合多媒体教学和实验教学两方面探讨原子吸收光谱在中药学学科实验课程中的现状,就目前存在的问题提出可改进的方法。在改进的方法之上尝试对原子吸收实验教学内容优化,提高学生学习自主性。

原子吸收光谱法测定土壤中铜、锌、镉含量

文章研究了原子吸收光谱法测定土壤中铜、锌、镉含量的方法,优化了仪器测定条件、微波消解试剂等。铜的浓度在0.05~0.4μg·mL^(-1)范围内线性相关系数r=0.99930,锌的浓度在0.02~0.8μg·mL^(-1)范围内线性相关系数r=0.99940,镉的浓度在0.2~2.4μg·L^(-1)范围内线性相关系数r=0.99840。加标回收率在95.3%~104.6%之间,方法的相对标准偏差(n=6)在0.87%~5.91%之间。通过对某农田8个土壤样品铜、锌、镉含量检测,建立了良好的方法,实验结果表明,该方法准确度高,精密度好,为监管部门提供了一定的参考。

铅的MIP-AAS测定

通过测铅来研究用常压氩微波诱导等离子体(MIP)作为原子吸收光谱法(AAS)的原子化器的可行性。样品用钽丝电热蒸发并经浓硫酸去溶后引入MIP。文中考查了各实验参数对测铅的影响。用本法测铅的特征浓度为O.1μg/mL。对实际样品的测定,取得了令人满意的结果。

微波消解-FAAS法测定新疆6种红枣中的8种金属元素

目的采用微波消解-火焰原子吸收光谱法(FAAS)测定新疆6种红枣中金属元素的含量。方法采用硝酸作为消解液,利用微波消解的方法处理红枣样品,火焰原子吸收光谱法测定新疆6种红枣中钠、钾、钙、镁、铁、锌、锰、铜8种微量、常量元素的含量。结果红枣中金属元素含量丰富,且钠、钾、钙和镁的含量普遍较高,铁、锌、铜、和锰的含量也较高。该方法的标准曲线线性关系良好(r=0.998 9～0.999 9),实验方法加入标准样回收率为95.52%～105.60%,相对标准偏差为1.35%～4.49%。结论该法具有灵敏度高、快速、准确的特点,可用于红枣中多种金属元素的测定。

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。

AAS、ICP-MS与NAA的特点及其应用比较

比较元素分析领域中原子吸收光谱、电感耦合等离子体质谱和堆中子活化分析等3种主要方法的利弊,评述其在元素种态分析中的应用,旨在推进科学利用微型核反应堆这一实验平台.

火焰原子吸收光谱法检测烟梗草木灰中的钾含量

使用火焰原子吸收光谱法测量废弃烟梗中钾离子的含量,并与其他常见农作物钾素含量做对比,为废弃烟梗的再利用提供一定的解决思路。通过自主设计并进行实验,能够培养学生独立思考和解决实际问题的能力,强化对理论与实践二者间联系的理解,进一步了解并正视能源和环境问题,充分发挥知识育人和实践育人的作用。

电感耦合等离子体质谱(ICP-MS)法与氢化物发生-原子吸收光谱(HG-AAS)法测定土壤中硒含量的对比研究

基于氢化物发生器与原子吸收光谱联用(HG-AAS),测定土壤样品中硒的含量,并与电感耦合等离子体质谱(ICP-MS)法测定值进行了对比。在两种仪器的最佳工作条件下,测定土壤硒的含量,实验结果表明:ICP-MS法和HG-AAS法对土壤硒含量测定的线性范围分别为0.85~100.00μg/L和0.08~16.00μg/L,检出限分别为0.25μg/L和0.02μg/L,精密度分别为1.3%和2.1%;用加标回收实验和测定国家标准土壤样品(GSS-7)对这两种方法的准确性进行了验证,ICP-MS法和HG-AAS法的加标回收率分别为96.7%~99.4%和94.9%~99.5%,GSS-7标准土样的结果均在标准值范围内,说明这两种测定土壤中硒含量的方法是准确可靠的。HG-AAS法测定线性范围窄,部分样品需要稀释,而且氢化物发生系统是手动进样,导致操作复杂,分析周期长;ICP-MS法仪器测定快速,但是仪器昂贵。