奶粉中5种营养元素的微波消解火焰原子吸收测定法

目的建立奶粉中5种营养元素的火焰原子吸收测定方法。方法利用微波消解处理样品，火焰原子吸收法测定奶粉中钙、镁、铁、锌、铜。结果方法检出限在0．050～0．11μgml，平均回收率为92．8％-103％，样品进行6次平行测定，RSD为0．56％～2．31％。结论方法具有快速、简便、灵敏、准确的优点，适于奶粉中5种营养元素的测定。

灰树花中铁的存在形态分析

优化灰树花中铁元素的提取工艺,对灰树花水提液中微量元素铁进行含量测定及形态分析,分别用0.45μm滤膜、D101大孔吸附树脂,将灰树花水提液中铁分为悬浮态和可溶态、有机态和无机态,并对有机态中蛋白结合态、多糖结合态进行分离。结果表明:灰树花中铁元素最佳提取工艺为温度100℃、时间120min、料液比1:60(g/mL),在此条件下,灰树花中铁提取率(水提液)约72.7%,其中可溶态大约占总量的64.4%,悬浮态大约占总量的8.3%;可溶态中无机态约占总量的39.0%,有机态约占总量的26.1%;有机态则多以蛋白结合态和多糖结合态形式存在,分别占到了总量的12.8%和10.5%。

孕妇血清锌浓度与稽留流产关系研究

目的研究孕妇血清锌浓度在孕早期的变化情况，探讨孕妇血清锌浓度与稽留流产的关系。方法2007年6月至2008年6月采用原子光谱吸收法对笔者所在医院64例稽留流产孕妇和66例正常对照孕妇早孕的血清锌浓度进行检测。观察对照组各孕周血锌浓度变化情况，对比对照组和研究组血锌浓度。结果孕妇血清锌浓度在孕早期呈逐渐下降趋势，但其变化不显著（P〉0．05）。研究组孕妇血清锌浓度明显低于对照组（P〈0．05）。结论孕妇血清锌浓度对维持正常妊娠有重要作用，血锌浓度低可能会导致稽留流产。

16批不同来源僵蚕白僵菌素含量测定及微量元素分析

目的:对16批不同来源僵蚕进行白僵菌素含量测定及微量元素分析.方法:采用HPLC法测定白僵菌素的含量,色谱柱为Diamonsil C18(250 mm×4.6 mm,5μm),流动相为乙腈—水—四氢呋喃(5.5∶3.5∶1)梯度洗脱;检测波长为215 nm,流速1 m L·min^(-1),柱温为常温.用原子光谱吸收法对药材中的Mg、Ca、Fe、Zn、Cu、Mn、Cr、Ni、Pb、Cd 10种元素进行测定.结果:白僵菌素含量在线性范围线性关系良好(r=0.9999),加样回收率为99.19%,不同来源僵蚕的蚕白僵菌素含量差异较大.微量元素测定发现,僵蚕中镁、铅的含量较高.结论:16批不同来源僵蚕白僵菌素质量差别较大,无明显地域特征.但条肥壮,断面充实,明亮,质硬的僵蚕及其炮制品,白僵菌素的含量普遍较高,质量较好,与传统经验鉴别一致.

番茄果实不同采收时间矿质元素变化分析

为比较分析番茄果实不同采收时间矿质元素的变化,以粉太郎和181两个番茄品种为材料,通过原子吸收光谱法和钼锑抗比色法测定不同采收时间番茄果实中钾(K)、磷(P)、镁(Mg)、钙(Ca)、铜(Cu)、铁(Fe)、锰(Mn)、锌(Zn)8种矿质元素的含量,研究不同采收时间番茄果实矿质元素的变化趋势。结果表明:8种矿质元素含量在不同采收时间有显著差异,2个参试品种的K、Ca、Mg、Cu元素含量在整个采收期总体呈下降趋势,其中Cu元素下降趋势显著;2种果实的Fe元素含量在整个采收期均呈先上升后下降而后又上升的趋势,粉太郎果实在4月7日含量最高,181果实于4月28日达最高值。相关性分析结果表明,部分矿质元素间存在正相关性,粉太郎果实中Mg元素与K、Cu、Zn元素分别呈显著正相关,181果实中Mg元素与Ca、Cu元素分别呈极显著正相关。研究结果可为高品质番茄栽培和采收时间选择提供理论指导。

Primary Speciation Analysis on 6 Kinds of Microelements in Glycyrrhiza uralensis Fisch.

[Objective]The aim was to analyze the primary speciation of 6 microelements in Glycyrrhiza uralensis Fisch. and provide theoretical basis for explaining pharmacodynamic principle of liquorice and discussing quality control of liquorice planting. [Method]The 6 elements Cu,Zn,Ca,Fe,Mg and Mn in roots of G.uralensis were extracted based on traditional decoction method and were separated into water-soluble state and suspension state by micro porous filtering film. The elements in water-soluble state were detected by flame atomic adsorption spectrophotometry （FAAS）. [Result]The results showed that extractive rates of the elements were in the range of 1.71%-60.06%,and immerse-residue ratio in 0.018 3-1.682 0; the results also indicated that the immerse-residue ratio of Zn was biggest （1.68）,Zn played an important medical role and might be considered as the best characteristic element in G.uralensis; the recoveries of the elements were ranged from 95.72% to 103.15% and relative standard deviations （RSD） were less than 2.38%. [Conclusion]Because of its high accuracy,FAAS method is feasible for analyzing primary speciation of microelements in G.uralensis.

Determination of Ca,K,Mg and Fe in Four Fish Species by FAAS

A method for determining calcium （Ca）, potassium （K）, magnesium （Mg） and iron （Fe） in four fish species was opti- mized and validated. It included microwave mineralization of the samples and subsequent quantification by flame atomic absorption spectroscopy （FAAS） with Zeeman-effect background correction. Using HNO3 （65%） and H202 （33%） as extraction solutions, the optimal conditions of extraction were established as follows： 0.5 g of sample mass; microwave time program of 300 W/5 min and 600 W/5 min. The method was free of matrix interferences. The linear correlation coefficients were ≥0.9991, the recovery percentage of analytes was from 99.31% to 103.70% and the RSD （relative standard deviation） was lower than 2.06%. The detection limits obtained were 32.3, 43.2, 14.0 and 68.6ng mL^-1 for Ca, K, Mg and Fe in FAAS respectively. It is shown that the method is rapid, simple, sensitive and accurate. The method was applied to the studies of digestibility and measurement of these nutrients in samples of fish collected from Norway, Japan and China.

Germanium separation and purification by leaching and precipitation

In this research work, extraction and purification of germanium from zinc leach residues(ZLR) were investigated. The results of ICP, XRF, and atomic adsorption spectroscopy(AAS) tests show that contents of germanium, iron, lead, and zinc within the leaching residue were 105×10^(-6), 3.53%, 10.35%, and 8.8%, respectively. XRD results indicate that the main minerals were in different forms of sulfates(CaSO_4·2H_2O, PbSO_4 and ZnSO_4·6H__2O), silicate(SiO_2), and oxide(Fe_2O_3). Dissolution of leaching filter cake was carried out using 5 parameters and each in 4 levels(acid concentration, temperature, time, liquid-to-solid ratio, and stirring speed) by Taguchi method(L_(16)), and then optimization of the effective parameters by response surface method. Under optimum conditions, zinc and germanium dissolution efficiencies were 88.71% and 8%, respectively. Leaching tests with sulfuric acid(added di-ammonium oxalate monohydrate) and hydrochloric acid(HCl) on the residues obtained from previous-stage sulfuric acid dissolution, yielded germanium and iron recoveries of 83%, 88%, 40%, and 90%, respectively. Thus, leaching experiment with sulfuric acid(added di-ammonium oxalate monohydrate) was superior to that with hydrochloric acid due to high and low extraction amounts of germanium and iron, respectively. Precipitation experiments revealed that germanium purification with tannic acid presented a better result compared to sodium hydroxide and ammonia. Under optimum conditions, contents of germanium and iron in the solution after precipitation were 0.1505% and 14.7% with precipitation yields of 91% and 52%, respectively.

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.

Effect of PSA tin plating process on trace lead in tin coating

In this paper,effects of conditions in phenol sulfonic acid(PSA) plating for tin coating of MR low carbon aluminum killed steel on trace Pb were examined.Trace Pb was measured by atomic absorption spectrometry(AAS)and glow discharge spectrometry,and coating morphology was observed by scanning electronic microscopy(SEM).Corrosion resistance of the tin coating was analyzed by electrochemical methods.The results indicated that Pb content in the tin coating reduced as bath temperature increased.When the temperature exceeded40 ℃,the grains in the coating were coarse and loose,reducing the corrosion resistance.As current density increased,Pb content increased rapidly,while low current density plating could lead to drain regions.The plating speed had no obvious effect on trace Pb in tin coating.In the tin plating layer,Pb was enriched at the surface and gradually reduced to zero along the depth.At bath temperature of 40 ℃ and current density of 20 A·dm^(-2),the amount of Pb could be less than 100 mg·kg^(-1) with excellent corrosion resistance.

Comparison between sequential and single extraction procedures for metal speciation in fresh and dried Sedum Plumbizincicola

Sequential and single extraction procedures were applied to both fresh and dried Sedum Plumbizincicola leaves and stems.The extractants, different from those of soil, sediment or sewage sludge metal fractions, were water, 80%(v/v) ethanol, 1 mol/L Na Cl,2% HAc and 0.6 mol/L HCl. Zn, Cd and Cu in the extracts and samples were measured by flame atomic adsorption spectrometry. In sequential extraction procedures, water soluble form and ethanol soluble form are the main fractions for Zn, while water soluble form and Na Cl soluble form for Cd, and comparatively uniform distribution for Cu with the residue form most and HCl soluble form second. Single extraction procedures are used to compare the extraction efficiencies of the five reagents to screen appropriate extractants and operating conditions for liquid extraction to deal with large amount of harvested metal-contained biomass, which will pose a threat to the environment if treated improperly. The sequences of extraction efficiencies are HCl>Na Cl≈HAc>Water≈Ethanol for Zn and HCl≈Na Cl≈HAc>Water>Ethanol for Cd. As for Cu, all the five extractants cannot effectively extract Cu, but HCl achieves a higher efficiency(>70% in fresh samples, and 45%-60% in dried samples). Besides, extraction efficiencies for most extractants in fresh samples are higher than those in dried samples, and extraction efficiencies of stems and leaves for the five extractants are close. The two extraction procedures can obtain high degree of accuracy with the relative standard deviation(RSD)lower than 10%, and metal recoveries are controlled between 80%-120% with most of 90%-110%.

Determination of Exchangeable Ca and Mg Contents in Tobacco Growing Area by Atomic Absorption Spectrometry

[Objective] A method for the determination of exchangeable Ca and Mg contents in tobacco growing area by atomic absorption spectrometry was established. [Method] Factors in the extraction process, sample weight, ammonium acetate volume, extraction time and strontium chloride volume were tested, and the stability, precision and accuracy of the method were also investigated. Meanwhile, samples at different pH values were determined by this method. [Result] The results showed that this method operation has simple operation with good stability and high precision. [Conclusion] This method could be applied to determine exchangeable Ca and Mg contents in tobacco growing area.

Influence of Cu（II） on Ag（I） Recovery by Photocatalytic Reduction Method with TiO2 Suspension

Photocatalytic reduction method using TiO2 suspension for removal as well as possibly recovery of silver （Ag（I）） in the presence of Cu（II） is examined. The photocatalytic reduction was performed by batch technique in a closed reactor equipped with UV lamp. The concentration of unreduced Ag（I） was analyzed by atomic absorption spectrophotometry method. The research results indicate that Ag（I） in the solution can be removed and recovered effectively as silver metal Ag（0） deposited on the surface of TiO2 for photocatalytic reduction. In addition, the presence of Cu（II） ion with increasing concentration leads to a proportional decline in Ag（I） photoreduction due to the prominent competition in the adsorption on the surface of TiO2. The effectiveness of Ag（I） ion photoreduction in the presence of Cu（II） ion is strongly influenced by solution pH and the highest photoreduction is obtained at pH 5 - 8, which is related with the speciation ofAg（I）, TiO2 surface as well as Cu（II） in the solution.

Chitosan Removes Toxic Heavy Metal Ions from Cigarette Mainstream Smoke

This study investigated the removal of heavy metal ions from cigarette mainstream smoke using chitosan. Chitosan of various deacetylation degrees and molecular weights were manually added to cigarette filters in different dosages. The mainstream smoke particulate matter was collected by a Cambridge filter pad, digested by a microwave digestor, and then analyzed for contents of heavy metal ions, including As（Ill/V）, Pb（II）, Cd（II）, Cr（III/VI） and Ni（II）, by graphite furnace atomic absorption spectrometry （GFAAS）. The results showed that chitosan had a removal effect on Pb（II）, Cd（II）, Cr（III/VI） and Ni（II）. Of these, the percent re- moval of Ni（II） was elevated with an increasing dosage of chitosan. Chitosan of a high deace tylation degree exhibited good binding performance toward Cd（II）, Cr（III/VI） and Ni（II）, though with poor efficiency for Pb（II）. Except As（III/V）, all the tested metal ions showed similar tendencies in the growing contents with an increasing chitosan molecular weight. Nonetheless, the percent removal of Cr（III/VI） peaked with a chitosan molecular weight of 200 kDa, followed by a dramatic decrease with an increasing chitosan mo- lecular weight. Generally, chitosan had different removal effects on four out of five tested metal ions, and the percent removal of Cd（II）, Pb（II）, Cr（III/VI） and Ni（II） was approximately 55%, 45%, 50%, and 16%, respectively. In a word, chitosan used in cigarette filter can remove toxic heavy metal ions in the mainstream smoke, improve cigarette safety, and reduce the harm to smokers.

Effect of sample treatment on determination of arsenic （Ⅲ） and arsenic （Ⅴ） in aqueous and tissue samples by hydride generation atomic absorption spectrometry

The purpose of this procedure was to optimize and improve a method that used for the determination of arsenic （Ⅲ） and arsenic （Ⅴ） in biological and environmental samples. The method is based on hydride generation and atomic absorption spectrometry. For both As （Ⅲ） and As （Ⅴ） the parameters such as NaBH4, HCI concentration, and pH were optimized. Absorption signal of As （Ⅴ） was approximately 17% of As （Ⅲ） signal. Therefore, for estimation of As （Ⅲ） and As （Ⅴ） concentrations in various samples the difference between the absorbance obtained for arsenic, without and with previous treatment of samples with potassium iodide （KI）, can be applied. The calibration graphs were linear （r〉0.99）, and the detection limits of the method based on three times the standard deviation of the blank were 0.14 and 0.64 μL^-1 for As （Ⅲ） and As （Ⅴ）, respectively. The relative standard deviation （R.S.D.） of measurements was less than 10%. As a means of checking performance method, water samples were spiked with known concentrations of both As （Ⅲ） and As （Ⅴ）, and recovery above 94% was obtained. The proposed method was applied successfully to determine inorganic As （Ⅲ） and As （Ⅴ） in various environmental and total As in biological samples.

Prediction of XRF analyzers error for elements on-line assaying using Kalman Filter

Determination of chemical elements assay plays an important role in mineral processing operations.This factor is used to control process accuracy,recovery calculation and plant profitability.The new assaying methods including chemical methods,X-ray fluorescence and atomic absorption spectrometry are advanced and accurate.However,in some applications,such as on-line assaying process,high accuracy is required.In this paper,an algorithm based on Kalman Filter is presented to predict on-line XRF errors.This research has been carried out on the basis of based the industrial real data collection for evaluating the performance of the presented algorithm.The measurements and analysis for this study were conducted at the Sarcheshmeh Copper Concentrator Plant located in Iran.The quality of the obtained results was very satisfied;so that the RMS errors of prediction obtained for Cu and Mo grade assaying errors in rougher feed were less than 0.039 and 0.002 and in final flotation concentration less than 0.58 and 0.074,respectively.The results indicate that the mentioned method is quite accurate to reduce the on-line XRF errors measurement.

Preparation and adsorption behaviors of Cu(Ⅱ) ion-imprinted polymers

Imprinted polymers were prepared for selective removal of Cu（Ⅱ） ions from metal solutions. Three ion-imprinted polymers were synthesized with methacrylic acid （MAA）, acrylamide （AA） and N,N＇-methylenebisacrylamide （MBAA） respectively as the functional monomers, ethleneglycoldimethacrylate （EGDMA） as the cross-linking agent, 2,2＇- azobisisobutyronitrile （AIBN） as the initiator and Cu （Ⅱ） ion as the imprint ion. The template Cu （Ⅱ） ion was removed from the polymer by leaching with a liquid of a 1：1 volumetric ratio of HCl to ethylenediaminetetraacetic acid （EDTA）. The capacity and selectivity of Cu（Ⅱ） ion adsorption were investigated with the three imprinted polymers and their non-imprinted counterparts. The polymers have a maximum adsorption capacity at pH 7.0. The isotherm of their batch adsorption of Cu（Ⅱ） ions shows a Langmuir adsorption pattern. Imprinted polymers all have a much higher capacity and higher selectivity of Cu（Ⅱ） adsorption than nonimprinted ones. MAA polymer benefits the most from imprinting. Imprinted MAA polymer has the highest selectivity when used to rebind Cu （Ⅱ） ion from an aqueous solution in the presence of other metal ions. Ion imprinting can be a promising technique of preparing selective adsorbents to separate and preconcentrate metal in a medium of multiple competitive metal ions through solid phase extraction （SPE）.

Uncertainty Estimation for the Determination of Trace Heavy Metals in Human Hair by Flame and Electrothermal Atomic Absorption Spectrometry

Trace element analysis on hair samples has been widely used to assess wildlife and human exposure to different contaminants present in the environment or at the workplace. Pollutants due to the presence of toxic metals in environment not only enter the body by breading, water, and foodstuff accumulates in hair, but they could be adsorbed directly on the hair from environment. In order to remove adsorbed elements and thus determine the internally bound elements correctly, hair sample must be washed. In the present work, we propose uncertainty estimation for the analytical results that are obtained from determination of cadmium, lead, copper, iron, manganese and nickel in human hair by flame and electrothermal atomic absorption spectrometry （FAAS and ETAAS）. To estimate the uncertainty of analytical result obtained, two types of bias are calculated in the assessment of trueness： a proportional bias and a constant bias. Nested design was applied for calculating proportional bias and Youden method to calculate the constant bias. The results we obtained for proportional bias are calculated from spiked samples. In this case, the concentration found is plotted against the concentration added and the slop of standard addition curve is an estimate of the method recovery. Estimated method of average recovery in human hair is： （1.019 ±0.026）, （0.918 ±0.014）, （1.073±0.016）, （1.0597± 0.017）, （1.073± 0.020） and （0.934± 0.117） for Cd, Pb, Mn, Ni, Fe and Cu respectively.

Detection of Total Phenols, Essential and Toxic Elements in Latvian Whole Grain Bread

A survey was carried out with the aim of assessing the level of the total phenolic compounds （TPC）, essential （Na, K, Ca, Mg, Cu, Zn） and toxic （Cd and Pb） elements in 10 Latvian whole grain rye and/or wheat flour bread samples, obtained from the local market. The quantities of the TPC were determined by spectrophotometry. Mineral content was determined by flame photometry, flame atom absorption spectrometry （FAAS） and electrothermal atomic absorption spectrometry （ETAA） after wet digestion in concentrated HNO3. The values were comparable to the literature data. The average content in all the samples was （on a basis of weight of the product） 547 ± 28 mg/100 g for Na; 280 ±20 mg/100 g for K; 32 ± 2 mg/100 g for Ca; 88 ±5 mg/100 g for Mg; 0.49 ± 0.09 mg/100 g for Cu; 1.6 ±0.2 mg/100 g for Zn. Both Pb and Cd were determined below the limit of detection （LOD 5 0.10 mg/100 g）. The LOD values were determined for each element. The TPC content in defatted samples was slightly lower than the non-defatted ones, showing the dependence on the sample preparation. The calculated average levels of the elements were compared with the maximum levels recommended or regulated by the national legislation.

Content of Cadmium in Poppy Seeds and Poppy Seeds Containing Products Marketed in Czech Republic

Concentration of cadmium in poppy seeds, semi-finished products and baked goods with poppy seeds was determined by graphite furnace atomic absorption spectrometry （GF-AAS）. Homogenous samples of poppy seeds and products containing poppy seeds were digested by means of microwave digestion system by using of nitric acid and hydrogen peroxide as reagents. The measurements were carried out using an atomic absorption spectrometer with Zeeman background correction. Detection limit was 0.003 mg/kg. A total of 208 samples of poppy seeds （from years 2004-2009） and 17 samples of semi-finished and baked goods were analysed. The average content was 0.64 mg/kg （median 0.64 mg/kg） for poppy seeds and 0.079 mg/kg （median 0.069 mg/kg） for semi-finished and baked goods. The relative standard deviation was lower than 5% for all measurements.