Abstract A separation and preconcentration method is described for the determination of copper, nickel, cobalt, lead, iron and cadmium in natural water and some salt samples by flame AAS. The analyte trace metal ions in the samples were sorbed as xylenol orange complexes on Amberlite XAD-16 column at the pH range of 7–9, and then eluted with 1M HNO3 in acetone. The effect of pH, reagent amount, sample volume, and matrix of the sample on the sorption of metal ions has also been investigated. The concentration of analyte ions detected after separation/and preconcentration was in agreement with the added amount of ions. The present method was found to be applicable to the preconcentration of analyte ions in natural water and some salt samples with good results such as relative standard deviations from 3 to 10% (N = 10).
{"title":"Separation/Preconcentration of Xylenol Orange Metal Complexes on Amberlite XAD-16 Column for Their Determination by Flame Atomic Absorption Spectrometry","authors":"M. Soylak, Y. Akkaya","doi":"10.1081/TMA-120023062","DOIUrl":"https://doi.org/10.1081/TMA-120023062","url":null,"abstract":"Abstract A separation and preconcentration method is described for the determination of copper, nickel, cobalt, lead, iron and cadmium in natural water and some salt samples by flame AAS. The analyte trace metal ions in the samples were sorbed as xylenol orange complexes on Amberlite XAD-16 column at the pH range of 7–9, and then eluted with 1M HNO3 in acetone. The effect of pH, reagent amount, sample volume, and matrix of the sample on the sorption of metal ions has also been investigated. The concentration of analyte ions detected after separation/and preconcentration was in agreement with the added amount of ions. The present method was found to be applicable to the preconcentration of analyte ions in natural water and some salt samples with good results such as relative standard deviations from 3 to 10% (N = 10).","PeriodicalId":17525,"journal":{"name":"Journal of Trace and Microprobe Techniques","volume":"23 1","pages":"455 - 466"},"PeriodicalIF":0.0,"publicationDate":"2003-01-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"80392931","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Abstract Sudan Red B, an azo dye, was used as a reagent for the complexation of Ni and Co ions. The studies were carried out spectrophotometrically. The absorption spectra were monitored and the conditions were optimized in terms of dye and metal concentration, pH, and cationic and anionic effects. The log β (stability constants) of the metal–dye complex were calculated using Job's method and these were of the order of 5.5 and 5.6 for Co2+ and Ni2+ complex respectively.
{"title":"Spectrophotometric Studies of the Complexation of Sudan Red B with Co2+ and Ni2+ Ions","authors":"M. A. Rauf, Z. Akhter, S. Kanwal","doi":"10.1081/TMA-120025807","DOIUrl":"https://doi.org/10.1081/TMA-120025807","url":null,"abstract":"Abstract Sudan Red B, an azo dye, was used as a reagent for the complexation of Ni and Co ions. The studies were carried out spectrophotometrically. The absorption spectra were monitored and the conditions were optimized in terms of dye and metal concentration, pH, and cationic and anionic effects. The log β (stability constants) of the metal–dye complex were calculated using Job's method and these were of the order of 5.5 and 5.6 for Co2+ and Ni2+ complex respectively.","PeriodicalId":17525,"journal":{"name":"Journal of Trace and Microprobe Techniques","volume":"19 1","pages":"577 - 581"},"PeriodicalIF":0.0,"publicationDate":"2003-01-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"86156670","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Abstract Polished samples of Cu, Zn and two brasses (CuZn10 and CuZn30) have been treated in synthetic air with 80% relative humidity (RH) and alternatively with 250 ppb SO2 added to the moist air stream in a weathering box. Depth profiles of the corroded surfaces were made with dynamic-SIMS and the courses of the S- and O-signals were traced. The decay of the S- and the O-signal exhibited different behavior. While the O-signal decreased continuously through the corroded layer, the S-signal decreased much faster until it reached the background level at the half of the thickness of the altered layer. Surface features could be found with comparative TM-AFM-measurements that confirmed these SIMS results. The height of these features (measured with TM-AFM) matched with the determined thickness of the S enriched layer.
{"title":"SIMS and TM-AFM Studies on Weathered Cu, Zn, and Brass (CuZn10, CuZn30) Surfaces","authors":"M. Rosner, C. Kleber, M. Schreiner, H. Hutter","doi":"10.1081/TMA-120017891","DOIUrl":"https://doi.org/10.1081/TMA-120017891","url":null,"abstract":"Abstract Polished samples of Cu, Zn and two brasses (CuZn10 and CuZn30) have been treated in synthetic air with 80% relative humidity (RH) and alternatively with 250 ppb SO2 added to the moist air stream in a weathering box. Depth profiles of the corroded surfaces were made with dynamic-SIMS and the courses of the S- and O-signals were traced. The decay of the S- and the O-signal exhibited different behavior. While the O-signal decreased continuously through the corroded layer, the S-signal decreased much faster until it reached the background level at the half of the thickness of the altered layer. Surface features could be found with comparative TM-AFM-measurements that confirmed these SIMS results. The height of these features (measured with TM-AFM) matched with the determined thickness of the S enriched layer.","PeriodicalId":17525,"journal":{"name":"Journal of Trace and Microprobe Techniques","volume":"20 2 1","pages":"49 - 62"},"PeriodicalIF":0.0,"publicationDate":"2003-01-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"78119292","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
W. Misiuk, E. Regulska, L. Kuźmicka, H. Puzanowska‐Tarasiewicz
Abstract The complexes of palladium(II) with diethazine hydrochloride were obtained. Their composition and some physicochemical properties were studied by UV–vis and infrared measurements. Stoichiometries and instability constants of the prepared complexes were established. Structure of the complexes was elucidated on the basis of analytical results.
{"title":"Physicochemical and Analytical Properties of the Complexes of Palladium(II) and Diethazine","authors":"W. Misiuk, E. Regulska, L. Kuźmicka, H. Puzanowska‐Tarasiewicz","doi":"10.1081/TMA-120025808","DOIUrl":"https://doi.org/10.1081/TMA-120025808","url":null,"abstract":"Abstract The complexes of palladium(II) with diethazine hydrochloride were obtained. Their composition and some physicochemical properties were studied by UV–vis and infrared measurements. Stoichiometries and instability constants of the prepared complexes were established. Structure of the complexes was elucidated on the basis of analytical results.","PeriodicalId":17525,"journal":{"name":"Journal of Trace and Microprobe Techniques","volume":"1 1","pages":"583 - 592"},"PeriodicalIF":0.0,"publicationDate":"2003-01-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"85602803","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
S. Cerutti, R. F. Orsi, J. Gásquez, R. Olsina, L. Martínez
Abstract In this study, the preconcentration of Pb2+ using a conical minicolumn packed with activated carbon (AC) was studied for preconcentration of Pb2+. The experiments showed that Pb2+ reacts with 8-hydroxyquinoline to form a complex at pH 10.0 and can be retained “on-line” on a conical minicolumn packed with activated carbon, then eluted with 20% (v/v) nitric acid. The conditions for the quantitative and reproducible preconcentration and subsequent ICP-OES determination with ultrasonic nebulization system (USN) were studied. A total enhancement factor (N) of 500 was obtained with respect to ICP-OES using pneumatic nebulization (10 for USN and 50 for enrichment factor) for a sample volume of 25 mL. The detection limit (DL) was 0.04 µg L−1. The relative standard deviation (RSD) were 3.0%. The optimized procedure was successfully applied to the determination of trace levels of Pb+2 in bee honey samples.
摘要本研究采用活性炭填充锥形小柱对Pb2+进行预富集。实验结果表明，Pb2+在pH 10.0时与8-羟基喹啉反应形成络合物，并可在活性炭填充的锥形小柱上“在线”保留，然后用20% (v/v)的硝酸洗脱。研究了超声雾化系统(USN)定量、重复性预富集及后续ICP-OES测定的条件。在样品体积为25 mL时，采用气动雾化(USN为10，富集因子为50)获得ICP-OES的总增强因子(N)为500，检出限(DL)为0.04 μ g L−1。相对标准偏差(RSD)为3.0%。该方法成功地应用于蜜蜂蜂蜜样品中痕量Pb+2的测定。
{"title":"On-Line Preconcentration/Determination of Lead Traces in Bee Honey by Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES) Using a Conical Minicolumn Packed with Activated Carbon","authors":"S. Cerutti, R. F. Orsi, J. Gásquez, R. Olsina, L. Martínez","doi":"10.1081/TMA-120023059","DOIUrl":"https://doi.org/10.1081/TMA-120023059","url":null,"abstract":"Abstract In this study, the preconcentration of Pb2+ using a conical minicolumn packed with activated carbon (AC) was studied for preconcentration of Pb2+. The experiments showed that Pb2+ reacts with 8-hydroxyquinoline to form a complex at pH 10.0 and can be retained “on-line” on a conical minicolumn packed with activated carbon, then eluted with 20% (v/v) nitric acid. The conditions for the quantitative and reproducible preconcentration and subsequent ICP-OES determination with ultrasonic nebulization system (USN) were studied. A total enhancement factor (N) of 500 was obtained with respect to ICP-OES using pneumatic nebulization (10 for USN and 50 for enrichment factor) for a sample volume of 25 mL. The detection limit (DL) was 0.04 µg L−1. The relative standard deviation (RSD) were 3.0%. The optimized procedure was successfully applied to the determination of trace levels of Pb+2 in bee honey samples.","PeriodicalId":17525,"journal":{"name":"Journal of Trace and Microprobe Techniques","volume":"23 1","pages":"421 - 432"},"PeriodicalIF":0.0,"publicationDate":"2003-01-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"83979933","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Abstract Using the freshly precipitated metal diethyl dithiocarbamates Mn(DDTC)2, Zn(DDTC)2, Cd(DDTC)2, Fe(DDTC)3, Co(DDTC)2, Cu(DDTC)2, Ni(DDTC)2, Pb(DDTC)2 and Hg(DDTC)2 as reagents, a new solid phase extraction method (SPE) has been described for the selective extraction of Mn(II), Zn(II), Cd(II), Fe(III), Co(II), Cu(II), Ni(II), Pb(II), and Hg(II) ions in aqueous system. These reagents show excellent selectivity for the extraction of metal ions with higher conditional stability constants (or extraction constants). As an example the application of these reagents has been carried out, where freshly precipitated Ni(DDTC)2 was used for the preconcentration of copper in aqueous system prior to its determination by FAAS.
{"title":"Solid-Phase Extractions with Freshly Precipitated Metal-Diethyldithiocarbamates and Atomic Absorption Spectrophotometric Determination of Copper","authors":"H. Cesur","doi":"10.1081/TMA-120025814","DOIUrl":"https://doi.org/10.1081/TMA-120025814","url":null,"abstract":"Abstract Using the freshly precipitated metal diethyl dithiocarbamates Mn(DDTC)2, Zn(DDTC)2, Cd(DDTC)2, Fe(DDTC)3, Co(DDTC)2, Cu(DDTC)2, Ni(DDTC)2, Pb(DDTC)2 and Hg(DDTC)2 as reagents, a new solid phase extraction method (SPE) has been described for the selective extraction of Mn(II), Zn(II), Cd(II), Fe(III), Co(II), Cu(II), Ni(II), Pb(II), and Hg(II) ions in aqueous system. These reagents show excellent selectivity for the extraction of metal ions with higher conditional stability constants (or extraction constants). As an example the application of these reagents has been carried out, where freshly precipitated Ni(DDTC)2 was used for the preconcentration of copper in aqueous system prior to its determination by FAAS.","PeriodicalId":17525,"journal":{"name":"Journal of Trace and Microprobe Techniques","volume":"63 1","pages":"627 - 636"},"PeriodicalIF":0.0,"publicationDate":"2003-01-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"78388674","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Abstract The suitability of derivative spectrophotometry for examination of complexation equilibria was elaborated by the determination of stability constants of Zn-PAR and Pd-PAR complexes. Derivatization minimized the influence of an excess of a colored reagent on the absorbance of the complex and allowed the direct measurement of its true value. The stability constants determined using two different methods were compared with available published data. In the case of the Zn(PAR)2 complex the error of determination did not exceed ± 5%.
{"title":"Derivative Spectrophotometry as a Tool for Determination of Stability Constants of Some 4-2(-Pyridylazo)-resorcinol Complexes with Divalent Metal Ions","authors":"J. Karpińska, Edyta Hryniewicka","doi":"10.1081/TMA-120023061","DOIUrl":"https://doi.org/10.1081/TMA-120023061","url":null,"abstract":"Abstract The suitability of derivative spectrophotometry for examination of complexation equilibria was elaborated by the determination of stability constants of Zn-PAR and Pd-PAR complexes. Derivatization minimized the influence of an excess of a colored reagent on the absorbance of the complex and allowed the direct measurement of its true value. The stability constants determined using two different methods were compared with available published data. In the case of the Zn(PAR)2 complex the error of determination did not exceed ± 5%.","PeriodicalId":17525,"journal":{"name":"Journal of Trace and Microprobe Techniques","volume":"21 1","pages":"443 - 453"},"PeriodicalIF":0.0,"publicationDate":"2003-01-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"88843025","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Abstract The concentrations of heavy metals in the street dust samples collected from Tokat, Turkey have been determined using flame atomic absorption spectrometry after wet and microwave digestion. Good accuracy was assured by the analysis of standard reference material. Recoveries were nearly quantitative for all elements studied (≥ 95%). The mean concentration levels of Pb, Ni, Cd, Zn, Mn, Cu, Co, and Cr were found to be 149, 65, 3.0, 63, 285, 29, 20, and 30 µg/g, respectively. The concentrations of heavy metals in the samples vary depending on the traffic density.
{"title":"Investigation of Heavy Metal Levels in Street Dust Samples in Tokat, Turkey","authors":"M. Tüzen","doi":"10.1081/TMA-120023067","DOIUrl":"https://doi.org/10.1081/TMA-120023067","url":null,"abstract":"Abstract The concentrations of heavy metals in the street dust samples collected from Tokat, Turkey have been determined using flame atomic absorption spectrometry after wet and microwave digestion. Good accuracy was assured by the analysis of standard reference material. Recoveries were nearly quantitative for all elements studied (≥ 95%). The mean concentration levels of Pb, Ni, Cd, Zn, Mn, Cu, Co, and Cr were found to be 149, 65, 3.0, 63, 285, 29, 20, and 30 µg/g, respectively. The concentrations of heavy metals in the samples vary depending on the traffic density.","PeriodicalId":17525,"journal":{"name":"Journal of Trace and Microprobe Techniques","volume":"76 1","pages":"513 - 521"},"PeriodicalIF":0.0,"publicationDate":"2003-01-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"86484682","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Abstract Marine sediment, seawater and several species of seaplants along the Kenya-Mombasa coastal region were analyzed to determine the levels of heavy metals by AAS and EDXRF and organochlorine pesticides (OCPs) by GLC-ECD. In marine sediments, there were high levels of manganese (1100 µg/L) at Vanga, compared to other study sites. In seawater, the heavy metals were detected in levels higher than those considered as natural in the ocean and the range was 0.01–0.30 mg/L. OCPs were detected in marine sediments and in seaplants. The trend of concentration of these pollutants in ascending order in seawater, marine sediment and seaplants was observed.
{"title":"Heavy Metals and Pesticides in Marine Sediment, Seawater, and Seaplants Along the Kenya-Mombasa Coastline","authors":"M. Oyugi, S. Chhabra, W. Njue, A. M. Kinyua","doi":"10.1081/TMA-120017907","DOIUrl":"https://doi.org/10.1081/TMA-120017907","url":null,"abstract":"Abstract Marine sediment, seawater and several species of seaplants along the Kenya-Mombasa coastal region were analyzed to determine the levels of heavy metals by AAS and EDXRF and organochlorine pesticides (OCPs) by GLC-ECD. In marine sediments, there were high levels of manganese (1100 µg/L) at Vanga, compared to other study sites. In seawater, the heavy metals were detected in levels higher than those considered as natural in the ocean and the range was 0.01–0.30 mg/L. OCPs were detected in marine sediments and in seaplants. The trend of concentration of these pollutants in ascending order in seawater, marine sediment and seaplants was observed.","PeriodicalId":17525,"journal":{"name":"Journal of Trace and Microprobe Techniques","volume":"12 1","pages":"147 - 159"},"PeriodicalIF":0.0,"publicationDate":"2003-01-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"81045645","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Abstract Computer Axial Tomography (CAT) maps the distribution of the linear attenuation coefficient (LAC) over a section or over an entire object. LAC represents the product between density and mass attenuation coefficient (MAC). These parameters are influenced in complete different manners by porosity provided that pore sizes are much smaller than voxels: density lineally decreases with porosity while MAC is almost independent of it. Consequently, in the case of single energy tomography, CAT images will be strongly influenced by the porosity. In the case of dual-energy tomography, when it results for the same section two CAT images, one depicting density and the other one the effective atomic number distributions, only the first one will reflect the sample porosity while the second one remains independent of the specimen porosity. This fact could be very useful in investigating complex samples such as rocks or soils.
{"title":"How Sensitive Is CAT to Porosity?","authors":"O. Duliu","doi":"10.1081/TMA-120025812","DOIUrl":"https://doi.org/10.1081/TMA-120025812","url":null,"abstract":"Abstract Computer Axial Tomography (CAT) maps the distribution of the linear attenuation coefficient (LAC) over a section or over an entire object. LAC represents the product between density and mass attenuation coefficient (MAC). These parameters are influenced in complete different manners by porosity provided that pore sizes are much smaller than voxels: density lineally decreases with porosity while MAC is almost independent of it. Consequently, in the case of single energy tomography, CAT images will be strongly influenced by the porosity. In the case of dual-energy tomography, when it results for the same section two CAT images, one depicting density and the other one the effective atomic number distributions, only the first one will reflect the sample porosity while the second one remains independent of the specimen porosity. This fact could be very useful in investigating complex samples such as rocks or soils.","PeriodicalId":17525,"journal":{"name":"Journal of Trace and Microprobe Techniques","volume":"31 1","pages":"609 - 614"},"PeriodicalIF":0.0,"publicationDate":"2003-01-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"79087624","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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