固相萃取富集高效液相色谱法测定环境水样中的重金属元素

研究了用固相萃取富集高效液相色谱法测定环境水样中痕量重金属镍、铜、银、铅、镉和汞的方法。环境水样中的镍、铜、银、铅、镉和汞用四 -(对二甲氨基苯基 ) -卟啉 (T4 -DMAPP)柱前衍生 ,用C18固相萃取小柱萃取富集镍、铜、银、铅、镉和汞的T4 -DMAPP络合物 ,富集倍数为 1 0 0倍 ,然后用甲醇和四氢呋喃梯度洗脱为流动相 ,WatersXter raTMRP18( 3 9mm× 1 5 0mm)色谱柱为固定相分离 ,用二极管矩阵检测器检测。镍、铜、银、铅、镉和汞的检测限分别为3、2、4、3、1 5ng/L和 3ng/L。方法相对标准偏差为 1 8%— 3 2 % ,标准回收率为 92 %— 1 0 7%。该方法用于测定环境水样中的痕量重金属 ,结果令人满意     

环境污染事故中重金属优先快速监测方法研究

在国内外重金属监测技术的基础上对环境污染事故中重金属（铜、铅、锌、砷、汞、铬、镉）的两种主要快速监测方法进行了研究。研究结果表明：比色法可测试铜、铅、锌、镉、六价铬5种重金属，且精密度与准确度均较好；阳极溶出伏安法（ASV）可测试铜、铅、锌、镉、砷、汞6种重金属，但测定六价铬时偏差较大；除六价铬和铜外，阳极溶出伏安法的测试范围较比色法宽，且检出限较低；阳极溶出伏安法可同时测定镉、铅、铜3种金属，具有较好的适用性。     

强酸型离子交换纤维富集-火焰原子吸收测定水中痕量铜、铅、镉、镍

通过强酸型离子交换纤维柱,在同一水样中同时富集和洗脱了铜、铅、镉、镍,采用火焰原子吸收光谱法测定,并对富集条件及洗脱条件、干扰因素进行了探讨。该方法简便易行,回收率在96.1%~105.5%之间,测定的相对标准偏差小于5.0%。     

电感耦合等离子体质谱法测定水中痕量元素

应用电感耦合等离子体质谱法对水样(地表水、饮用水等)中铜、锌、硒、砷、镉、铬、铅、铁、锰等痕量元素进行分析测定。结果表明,方法检出限为0.01~0.78μg/L,平行测定的相对标准偏差为0.6%~7.9%,实际水样加标回收率为90.5%~103%。该方法快速、简便、线性范围大,具有良好的检出限和准确度。     

浊点萃取-原子吸收光谱法测定水和花粉中痕量铜、铅、镉

以氢氧化钠为沉淀剂,依据Triton X-114的浊点现象分离沉淀,沉淀在浓盐酸作用下溶解,用原子吸收光谱法测定样品中痕量铜、铅、镉。通过试验优化测定条件,使该方法在0 mg/L~6.00 mg/L范围内线性良好,3种元素的方法检出限分别为0.028μg/L、0.006μg/L、0.028μg/L。将该方法用于水样、花粉中痕量铜、铅、镉的测定,RSD为2.8%~7.9%,加标回收率为92.0%~106%。     

共沉富集─单缝石英管火焰原子吸收法测定水中痕量铜、铅、锌、镉

采用共沉富集与单缝石英管技术，以火焰法测定地面水、地下水中的痕量铜、铅、锌、镉，检测限分别为０．５，１．８，０．２，０．１μｇ／Ｌ，四种痕量元素１１次测定的变异系数分别２．８％，２．３％，３．１％和３．９％。     

微分脉冲伏安法测定降水中锌、镉、铅和铜

以量浓度为0．01mol/L的高氯酸为支持电解质，采用微分脉冲阳极溶出伏安法同时测定降水中的痕量Zn^2 、Cd^2 、Pb^2 和Cu^2 ．6次测定的相对标准偏差均小于5％，降水样品镉未检出。锌、铅、铜的加标回收率分别为91．5％－110．0％、91．5％－104．0％和91．0％－106．0％。该方法应用于降水中Zn、Cd、Pb、Cu痕量元素的分析，具有方法简便、快速、准确度高等特点。     

自来水中铅和镉的分离富集和原子吸收测定

采用PAN[1-(2-吡啶偶氮)-2-萘酚]—Ni(Ⅱ)共沉淀体系,在pH=10条件下分离富集自来水中的铅和镉,再采用微量注射进样火焰原子吸收法(FAAS)进行测定,水样中的共存离子不干扰测定,加入铅和镉的回收率均在90—106％之间。对铅含量为0.1μg/ml和镉含量为0.05μg/ml的水样进行8次平行测定,其相对标准偏差分别为2.9％和6.4％。溶液中铅的浓度在0—0.4μg/ml,镉的浓度在0—0.2μg/ml范围内,工作曲线呈线性。     

巯基棉富集分离水中痕量铅,镉,铜——火焰原子吸收测定法的研究

水中痕量铅、镉、铜的测定一般需采用石墨炉原子吸收法,此法对仪器要求高,耗费大,精密度、准确度相对较差.本文对巯基棉富集后用火焰原子吸收测定上述元素的方法进行了研究,并与蒸发浓缩和石墨炉原子吸收法作了对比.结果证明巯基棉富集——火焰原子吸收法测定水中微量铅、镉、铜能获得满意的结果.     

共沉富集——单缝石英管火焰原子吸收法测定水中痕量铜,铅,锌,镉

采用共沉富集与单缝石英管技术，以火焰法测定地面水，地下水中的痕量铜，铅，锌，镉，检测限分别为０．５，１．８，０．２，０．１μｇ／Ｌ，四种痕量元素１１次测定的变异系数分别为２．８％，２．３％，３．１％和３．９％。     

Surfactant-mediated complex formation for determination of traces amounts of zinc, cadmium, and lead with 4-(2-thiazolylazo) resorcinol and chemometric methods

The partial least squares modeling is a powerful multivariate statistical tool applied to the spectrophotometric simultaneous determination of the divalent ions of zinc, cadmium, and lead based on the formation of their complexes with 4-(2-thiazolylazo) resorcinol in surfactant media. The linear concentration range for zinc, cadmium, and lead were 0.10-1.31, 0.148-1.92, and 0.148-3.70 mg L(?-1), respectively. The experimental calibration set was composed of 36 sample solutions using a mixture design for three component mixtures. The absorption spectra were recorded from 380 through 650 nm. The effect of pH on the sensitivity in determination of zinc, cadmium, and lead was studied in order to choose the optimum pH (pH = 8) for determination. The root-mean-square errors of predictions for zinc, cadmium, and lead were 0.0466, 0.0282, and 0.050, respectively. The proposed method was successfully applied for the determination of zinc, cadmium, and lead in water samples.     

Solid phase extraction of Cd,Pb, Ni,Cu, and Zn in environmental samples on multiwalled carbon nanotubes

A simple and sensitive solid phase extraction (SPE) method on multiwalled carbon nanotubes (MWCNTs) is presented for the determination of cadmium, lead, nickel, copper, and zinc at trace levels combined with flame atomic absorption spectrometry. The effects of parameters like pH, sample volume, sample and eluent flow rates, eluent concentration, and volume and type of eluent on the recovery of trace elements was examined. The metals retained on the nanotube at pH 6.5 as α-benzoin oxime complexes were eluted by 10 mL 2 M HNO₃ in acetone. The influence of matrix ions on the developed method was also evaluated. The preconcentration factor of the method was found to be 50. The detection limits for Cd(II), Pb(II), Ni(II), Cu(II), and Zn(II) were found as 1.7, 5.5, 6.0, 2.3, and 2.4 μg L^?1, respectively. To test the accuracy of the method, the method was applied to TMDA-70 fortified lake water and Spinach 1570A standard reference materials. Addition recovery studies were applied to tap water and cracked wheat samples, and determination of the analyte elements was carried out in some food samples with good results.     

A new voltammetric method for the simultaneous monitoring of heavy metals in sea water,sediments, algae and clams: application to the Goro Bay ecosystem

Arsenic(III), selenium(IV), copper(II), lead(II), cadmium(II),zinc(II) have been determined in sea water, sediments, algae andclams by differential pulse cathodic (DPCSV) and anodic (DPASV)stripping voltammetry. The voltammetric measurements are carriedout using a conventional three-electrode cell and the ammonia-ammonium chloride buffer pH 9.2 as supporting electrolyte.The analytical procedure has been verified by the analysisof the standard reference materials (Estuarine SedimentBCR-CRM 277, Ulva Lactuca BCR-CRM 279 and Mussel Tissue BCR-CRM278). The precision and the accuracy are less than 5%. Thisprocedure is utilized for the monitoring of heavy metals inthe Po river mouth area (Italy).     

Ultra-sensitive quantification of copper in food and water samples by electrochemical adsorptive stripping voltammetry

A new electrochemical adsorptive stripping voltammetry method was developed for the determination of trace amounts of copper in food and water samples. The study of electrochemical behavior of Cu ion indicated that Cu(II) and Schiff base formed a complex in H₃BO₄–NaOH buffer solution (pH?=?7.25). An accumulation potential of ?100 mV (vs Ag/AgCl) was applied while the solution was stirred for 60 s. The response curve was recorded by scanning the potential, and the peak current of ?0.31 V (vs Ag/AgCl) was recorded. The peak current and concentration of copper accorded with linear relationship in the range of 0.04–120 ng mL^?1. The relative standard deviation (for 12 ng mL^?1 of copper) was 1.73 %, and the detection limit was 0.007 ng mL^?1. The possible interference of some common ions was studied. The proposed method was applied to the determination of copper in water, rice, wheat, tea, milk, and tomato with satisfactory results.     

Study on determination of iron,cobalt, nickel,copper, zinc and manganese in drinking water by solid-phase extraction and RP-HPLC with 2-(2-quinolinylazo)-5-diethylaminophenol as precolumn derivatizing reagent

A new method for the determination of iron, cobalt, nickel, copper, zinc and manganese in drinking water by the reversed-phase high-performance liquid chromatography (RP-HPLC) with 2-(2-quinolinylazo)-5-diethylaminophenol (QADEAP) as precolumn derivatizing reagent was studied in this paper. The iron, cobalt, nickel, copper, zinc, and manganese ions react with QADEAP to form color chelates in the presence of cetyl trimethylammonium bromide (CTMAB) and acetic acid-sodium acetic buffer solution medium of pH 4.0. These chelates were enriched by solid-phase extraction with a Waters Nova-Pak C18 cartridge and eluted the retained chelates from the cartridge with tetrahydrofuran (THF). The enrichment factor of 100 was achieved. Then the chelates were separated on a Waters Nova-Pak C18 column (3.9 x 150 mm, 5 microm) by gradient elution with methanol (containing 0.2% of acetic acid and 0.1% of CTMAB) and 0.05 mol L(-1) acetic acid-sodium acetic buffer solution (containing 0.1% of CTMAB) (pH 4.0) as mobile phase at a flow rate of 0.5 ml min(-1), and monitored with a photodiode array detector from 450 approximately 700 nm. The detection limits (S/N = 3) of iron, cobalt, nickel, copper, zinc and manganese are 0.8, 1.1, 0.9, 1.1, 1.5 and 2.0 ng L(-1), respectively, in the original sample. This method can be applied to determination at the microg L(-1) level of iron, cobalt, nickel, copper, zinc and manganese in drinking water with good results.     

Seasonal and spatial distribution of trace elements in the water and sediments of the Tsurumi River in Japan

The Tsurumi, a class-one Japanese river, has a significant metal loading originating from urban environment. Water and sediment samples were collected from 20 sites in winter and summer, 2009 and were analyzed to determine and compare the extent of different trace element enrichment. A widely used five-step sequential extraction procedure was also employed for the fractionation of the trace elements. Concentrations of zinc, copper, lead, chromium, and cadmium were three to four times higher than that of reference values and downstream sediments are much more polluted than the upstream sites. Geochemical partitioning results suggest that the potential trace metal mobility in aquatic environment was in the order of: cadmium > zinc > lead > copper > cobalt > chromium > molybdenum > nickel. About 80.2% zinc, 77.9% molybdenum, 75.3% cobalt, 63.7% lead, 60.9% copper, 55.1% chromium, and 39.8% nickel in the sediment were contributed anthropogenically. According to intensity of pollution, Tsurumi river sediments are moderately to heavily contaminated by zinc, lead, and cobalt. Enrichment factor values demonstrated that zinc, lead, and molybdenum have minor enrichment in both the season. The pollution load index (PLI) has been used to access the pollution load of different sampling sites. The area load index and average PLI values of the river were 7.77 and 4.93 in winter and 7.72 and 4.89 in summer, respectively. If the magnitude of pollution with trace metal in the river system increases continuously, it may have a severe impact on the river’s aquatic ecology.     

Concentrations of cadmium and lead heavy metals in Dardanelles seawater

Cadmium and lead were determined simultaneously in seawater by differential pulse stripping voltammetry (DPSV) preceded by adsoptive collection of complexes with 8-hydroxyquinoline (oxine) on to a hanging mercury drop electrode (HMDE). In preliminary experiments the optimal analytical condition for oxine concentration was found to be 2.10⁻⁵ M, at pH 7.7, the accumulation potential was −1.1 V, and the initial scannig potential was −0.8 V. The peak potentials were found −0.652 V for Cd and −0.463 V for Pb At the 60 s accumalation time. The limit of detection (LOD) and limit of quantitatification (LOQ) were found to be by voltammetry as 0.588 and 1.959 μg l⁻¹ (RSD, 5.50%) for Cd and 0.931 and 3.104 μg l⁻¹ (RSD, 4.10%) for Pb at 60 s stirred accumulation time respectively. In these conditions the most of the seawater samples are amenable for direct voltammetric determination of cadmium and lead using a HMDE. An adsorptive stripping mechanism of the electrode reaction was proposed. For the comparison, seawater samples were also analysed by ICP-atomic emission spectrometry method (ICP-AES). The applied voltammetric technique was validated and good recoveries were obtained.     

Trace element content in marine algae species from the Black Sea, Turkey

Trace element content of marine algae species collected from the Black Sea coasts were determined by atomic absorption spectroscopy after microwave digestion. Trace element content in marine algae species were 1.70-17.1 microg/g for copper, 3.64-64.8 microg/g for zinc, 9.98-285 microg/g for manganese, 99-3,949 microg/g for iron, 0.50-11.6 microg/g for chromium, 0.27-36.2 microg/g for nickel, 11-694 microg/kg for selenium, 0.50-44.6 microg/kg for cadmium, 1.54-3,969 microg/kg for lead, 1.56-81.9 microg/kg for cobalt. While iron was the highest trace element concentration, cadmium was the lowest in samples. Most of the analyzed samples were edible. The samples are consumed for human diet in several countries.     

Concentration of Cd, Cu, Pb, Zn, Al, and Fe in soils of Manresa, NE Spain

The aims of this study were to determine the contents of cadmium (Cd), copper (Cu), lead (Pb), zinc (Zn), aluminium (Al), and iron (Fe) (aqua regia-extractable) in 27 soil plots (54 samples) from Manresa, NE Spain, and to establish relationships between heavy metals and some soil properties. The main soil types were surveyed and the median concentrations (mg kg(-1)) obtained were Cd 0.28, Cu 20.3, Pb 18.6, Zn 67.4, Al 22,572, and Fe 21,551. Element concentrations for these soils were lower than the published values for the Valencia region (Spain) and Torrelles and Sant Climent municipal districts (Catalonia, Spain). In terms of soil properties, the results of this study suggest that, in Manresa soils, both trace element adsorption and retention are influenced by several properties such as clay minerals, carbonates, organic matter, and pH. All element contents were positively correlated with clay content. Pb and Zn were negatively correlated with pH and CaCO(3).