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.

羰基镍粉中铜、锰、钴含量的连续测试技术

建立了一种用AIR-C2H2火焰原子吸收光谱法连续测试镉镍电池羰基镍粉中铜、锰、钴含量,介绍了铜、锰、钴最佳测试条件,同时对样品硝化处理条件及在测试样品中的干扰因素进行了综合考虑。该方法具有很好的精密度和准确度,具有操作简便、时间快速、灵敏度高、重现性好、容易掌握等特点。铜、锰、钴含量的相对标准偏差均小于1.0%（n=6）。标准加入回收率均在97.0%-99.0%范围内。适用于镉镍电池羰基镍粉中含有较多共同被测离子铜、锰、钴的生产现场控制分析和样品系统分析。

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.

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%.

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 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.

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.

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.

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.

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.

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）.

Acid volatile sulfide and simultaneously extracted metals in superficial sediments from Baihua Lake, China

The bioavailability of five divalent cationic heavy metals （Pb, Cd, Cu, Zn and Ni） in 10 superficial sediment samples from Baihua Lake was assessed based on the molar ratio of simultaneously extracted metals （SEMs） to acid volatile sulfide （AVS）. Atomic absorption spectrometry （AAS） and X-ray powder diffraction （XRD） were used to determine the heavy metal concentrations and examine the mineralogy of the crystalline phases, respectively. The AVS loadings in sediments from Baihua Lake ranged from 64.30 to 350.08 ~rnol/g （dry weight）. The corresponding SEM levels for the sampling sites varied from 1.770 to 14.660 vrnol/g. The molar ratio of SEMs to AVS ranged from 0.014 to 0.084 with a mean value of 0.034. The XRD analysis also confirmed the presence of some metal sulfides in sediments from Baihua Lake. The SEMs/AVS ratios for all sampling sites were significantly lower than 1.0, indicating that AVS in the sediments was sufficient to bind the five heavy metals; thus, these heavy metals are currently not significantly bioavailable to benthic organisms. Comparing the SEMs results to published guideline values for metal toxicity to benthic organisms in sediments, however, suggests that Zn and Ni pose a risk at some sampling locations in Baihua Lake.

Blood Lead Levels During Pregnancy and Its Influencing Factors in Nanjing,China

Objective To investigate the blood lead levels （BLLs） in the duration of pregnancy and 6-12 weeks after delivery, and analyze the influencing factors of BLLs in healthy pregnant women. Methods Pregnant women were recruited from September 2009 to February 2010 at the prenatal clinic in Nanjing Maternity and Child Health Care Hospital. Altogether 174 healthy pregnant women without pregnant or obstetric complications or abnormal pregnancy outcomes were enrolled as the gravida group, and 120 healthy non-pregnant women as the control group. BLLs during pregnancy were determined by flame atomic absorption spectroscopy. Results BLLs in all the three pregnancy trimesters and postpartum were 59.8±24.3, 55.4±20.1, 55.9±19.7, and 67.6±17.4 μ/L, respectively, and the mean BLL in control group was 67.5±21.3 μg/L. BLLs during all the three trimesters were lower in the gravida group than in the control group （P=0.043, 0.021, and 0.028）. Furthermore, occupations, nutrients supplementation, and time of house/apartment painted were associated with BLLs in pregnant women. Lead-related occupations, cosmetics use, and living in a house painted less than 1 year before are risk factors of high BLLs among pregnant women, while calcium, iron, zinc, and milk supplements are protective factors. Conclusion Supplementing calcium, iron, zinc, and milk, or avoiding contact with risk factors may help people, especially pregnant women, to reduce lead exposure.

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.

Characterization of Humic System in Fertilizer Raw Materials

The aim of the study was to characterize humus system of natural and artificial products. Humus systems from leonardite, lignite biotransformed with Trichoderma sp. （Plantagra）, plant materials after pyrolisis （charcoal） and composts are compared. Humus systems are characterized by Kononova-Belchikova＇s method, and heavy metals content was measured by atomic absorption spectroscopy （AAS）. Humic acids from the International Humic Substances Society （IHSS） collection are the standards for humus substances quality of compared products. Data obtained for leonardite indicate that the studied substances from factory, Izmir, Turkey contain humic acids over 94%. Compared to the standard, heavy metals content in these materials demonstrate high amounts. Organic carbon content in the composts is very low compared to the leonardite materials and IHSS collection, where the heavy metals content is lower. Biotransformed lignite is characterized with lower content of organic carbon, but humic acids are with high degree of humification. Results obtained show that the fourth studied humus systems may be used in agriculture on base of the high humic acids content. It is recommended to measure heavy metals content before applying the materials in agriculture.

Assessment of Heavy Metals Control from Soil and Vegetable Plants in Different Growing Systems

Heavy metals contents of soils and vegetable edible parts were studied at three crop systems （conventional, in conversion and organic） from seven traditional sites for vegetable growing in North-eastern Romania, during 2010. The main goal of the research was to find a correlation between the heavy metals contents and the crop systems. Determination of heavy metals was performed by atomic absorption spectrometry （AAS）, using a Shimadzu spectrophotometer, 6300 version, equipped with graphite furnace and autosampler. Heavy metals contents in the soils varied with the metals and locations, according to the crop system. The following experimental average contents were determined： Mn-262.03 mg kg1, Zn-45.60 mg kgq, Cu-28.53 mg kgl, Pb-5.20 mg kg1 and Cd-1.84 mg kg1. In vegetable edible parts, heavy metal varied with metals, sites and plant species, without a significant correlation with crop system. The trend of heavy metals in conventional and organic crops was Zn 〉 Cu 〉 Mn = Pb 〉 Cd, but in conversion crops it was Zn 〉 Mn = Pb 〉 Cu 〉 Cd. The highest content was of Zn （4.85 mg kg＇t）, at a cabbage crop in conversion. Cd was not detected in vegetable products and Pb was detected only in some vegetable samples. Research emphasized that heavy metals contents from soil and vegetable edible parts did not exceed the admitted maximum limits, according to Romanian and European Regulations. Final conclusion of research is that no correlations exist between crop systems and heavy metals contents from soil and plant.

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.

New Easy Method for the Monitoring of Hg Concentration in Fish, Using a Nanostructured Gold Electrode

The applicability of a gold nanoparticle-modified glassy carbon sensor （AuNPs-GCS） for the determination of inorganic mercury in fresh and canned tuna fish by square wave anodic stripping voltammetry （SW-ASV） is demonstrated. Mercury content in sample Tuna Fish ISPRA T22 was determined to value the accuracy of the determination. The concentration in this sample is not certified, so, the Hg amount was determined also with atomic absorption spectroscopy （AAS）： the results obtained with ASV were in good agreement and confirmed literature value reported for this sample. Then, real samples of tuna fish were analyzed. The voltammetric analyses were performed using previously optimized conditions （deposition potential 0 V, step potential 0.004 V, frequency 150 Hz and amplitude 0.003 V）. Medium exchange technique permitted to eliminate possible matrix effects. The concentrations in the real samples were found to be in agreement with the common Hg levels reported in literature for commercialized tuna fish in different countries.