ABSTRACT Coagulant production using red mud and waste base as raw material is described together with phase and chemical composition changes in red mud during coagulant production and usage. Investigation of phase and chemical composition was carried out using X-ray diffraction analysis (XRD) and sequential extraction. Acid treatment of the red mud resulted in the removal of the exchangeable fraction, carbonates and alkalis. Base addition into acid treated and centrifuged red mud caused its flocculation and sorption by surface enlargement. Mineral phase transition in coagulant (activated red mud) with time was not found. An amount of 1g of this coagulant was able to sorb 99.347 mg of Cu, 95.002 mg of Zn and 98.695 mg of Pb from aqueous solution containing 100 mg/l of those metals. Among three metals investigated, Zn sorption was the most affected with changes in pH value of treated solution. The sorption of metal cations (Cu(II), Zn(II) and Pb(II)) from the metal–EDTA solution onto the activated red mud (ARM) for different metal–EDTA concentrations (1–100 mg/l) was also investigated. It was found that, among the three tested metals, the sorption of Cu onto the ARM was most affected by EDTA. The removal of these three metals from the metal–EDTA mixture solution was also studied by using two other types of coagulants: ferric chloride and polyaluminium chloride (PAC). In the case of the FeCl3, the addition of EDTA had a slight influence on the Cu removal and none on the Pb and Zn removal, while in the case of the PAC, the greatest influence was found for all these metals.
{"title":"A STUDY OF COAGULANT PRODUCTION FROM RED MUD AND ITS USE FOR HEAVY METALS REMOVAL","authors":"V. Oreščanin, D. Tibljaš, V. Valković","doi":"10.1081/TMA-120003726","DOIUrl":"https://doi.org/10.1081/TMA-120003726","url":null,"abstract":"ABSTRACT Coagulant production using red mud and waste base as raw material is described together with phase and chemical composition changes in red mud during coagulant production and usage. Investigation of phase and chemical composition was carried out using X-ray diffraction analysis (XRD) and sequential extraction. Acid treatment of the red mud resulted in the removal of the exchangeable fraction, carbonates and alkalis. Base addition into acid treated and centrifuged red mud caused its flocculation and sorption by surface enlargement. Mineral phase transition in coagulant (activated red mud) with time was not found. An amount of 1g of this coagulant was able to sorb 99.347 mg of Cu, 95.002 mg of Zn and 98.695 mg of Pb from aqueous solution containing 100 mg/l of those metals. Among three metals investigated, Zn sorption was the most affected with changes in pH value of treated solution. The sorption of metal cations (Cu(II), Zn(II) and Pb(II)) from the metal–EDTA solution onto the activated red mud (ARM) for different metal–EDTA concentrations (1–100 mg/l) was also investigated. It was found that, among the three tested metals, the sorption of Cu onto the ARM was most affected by EDTA. The removal of these three metals from the metal–EDTA mixture solution was also studied by using two other types of coagulants: ferric chloride and polyaluminium chloride (PAC). In the case of the FeCl3, the addition of EDTA had a slight influence on the Cu removal and none on the Pb and Zn removal, while in the case of the PAC, the greatest influence was found for all these metals.","PeriodicalId":17525,"journal":{"name":"Journal of Trace and Microprobe Techniques","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2002-05-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"87539755","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 aim of this work was to use the determination of trace elements by total reflection X-ray fluorescence (TXRF) for the performance study of three final purification methods of polysaccharide systems. TXRF shows two indispensable advantages to accomplish this study: the small quantities of sample required for the analysis and the avoidance of digesting the organic material. Aqueous scleroglucan systems with only impurity traces were studied, from diluted solutions to gels. The most efficient purification process was selected for each range of concentration.
{"title":"LOW IMPURITIES IN SCLEROGLUCAN AQUEOUS SYSTEMS: REMOVAL PROCESSES CONTROL BY TOTAL REFLECTION X-RAY FLUORESCENCE ANALYSIS","authors":"S. Boeykens, N. Temprano, C. Vázquez","doi":"10.1081/TMA-120003730","DOIUrl":"https://doi.org/10.1081/TMA-120003730","url":null,"abstract":"ABSTRACT The aim of this work was to use the determination of trace elements by total reflection X-ray fluorescence (TXRF) for the performance study of three final purification methods of polysaccharide systems. TXRF shows two indispensable advantages to accomplish this study: the small quantities of sample required for the analysis and the avoidance of digesting the organic material. Aqueous scleroglucan systems with only impurity traces were studied, from diluted solutions to gels. The most efficient purification process was selected for each range of concentration.","PeriodicalId":17525,"journal":{"name":"Journal of Trace and Microprobe Techniques","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2002-05-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"85720089","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 Analytical electron microscopy is used to identify, localize and quantify chemical elements in biological samples with the aim to correlate the element distribution in cells and tissues with the particular functional state. Energy dispersive electron probe X-ray microanalysis of freeze-dried cryosections is considered to be the most efficient technique with respect to spatial analytical resolution and detection limit. The potentialities and limitations of this technique are illustrated by results from 3 current research projects: Element compartmentation in hepatocytes, cytotoxicity of an organotin compound, and calcium movements during osmoregulation of epithelia. At present, the absolute detection limit is 170 atoms in a minimum analytical volume of 30 × 30 × 100 nm3. X-ray microanalysis of cryosections from biological samples is limited by ice crystal growth during cryofixation and by the poor X-ray collection efficiency in most electron microscopes. Therefore, the construction of an analytical electron microscope dedicated to biological X-ray microanalysis is proposed. This microscope features considerably improved X-ray collection efficiency due to an annular X-ray detector. The absolute detection limit is estimated to be less than 10 atoms in a minimal analytical volume of 10 × 10 × 100 nm3 of a cryosection.
{"title":"LIMITATIONS AND PROSPECTS OF BIOLOGICAL ELECTRON PROBE X-RAY MICROANALYSIS","authors":"K. Zierold","doi":"10.1081/TMA-120003723","DOIUrl":"https://doi.org/10.1081/TMA-120003723","url":null,"abstract":"ABSTRACT Analytical electron microscopy is used to identify, localize and quantify chemical elements in biological samples with the aim to correlate the element distribution in cells and tissues with the particular functional state. Energy dispersive electron probe X-ray microanalysis of freeze-dried cryosections is considered to be the most efficient technique with respect to spatial analytical resolution and detection limit. The potentialities and limitations of this technique are illustrated by results from 3 current research projects: Element compartmentation in hepatocytes, cytotoxicity of an organotin compound, and calcium movements during osmoregulation of epithelia. At present, the absolute detection limit is 170 atoms in a minimum analytical volume of 30 × 30 × 100 nm3. X-ray microanalysis of cryosections from biological samples is limited by ice crystal growth during cryofixation and by the poor X-ray collection efficiency in most electron microscopes. Therefore, the construction of an analytical electron microscope dedicated to biological X-ray microanalysis is proposed. This microscope features considerably improved X-ray collection efficiency due to an annular X-ray detector. The absolute detection limit is estimated to be less than 10 atoms in a minimal analytical volume of 10 × 10 × 100 nm3 of a cryosection.","PeriodicalId":17525,"journal":{"name":"Journal of Trace and Microprobe Techniques","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2002-05-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"74940324","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}
L. Tsikritzis, S. Ganatsios, O. Duliu, Costas V. Kavouridis, T. Sawidis
ABSTRACT The concentration of 16 trace elements (V, Cr, Mn, Co, Ni, Cu, Mo, As, Cd, Hg, Sn, Se, Sb, Ba, Ag and Pb) has been determined in 39 points distributed over the 2300 km2 of the Kozani-Ptolemaïda-Amynteon basin (Western Macedonia). In this area there are four lignite power plants, with an installed power of 4048 MW, which discharged into atmosphere around 69500 tons/year of fly ash. Seventy soil samples, 0 to 20 cm depths, from both uncultivated and cultivated soils have been investigated. Except for Cr, Mn, Ni and Co in three uncultivated soil samples, no statistically significant increased concentrations could be evidenced in the considered area.
{"title":"TRACE ELEMENTS DISTRIBUTION IN SOIL IN AREAS OF LIGNITE POWER PLANTS OF WESTERN MACEDONIA","authors":"L. Tsikritzis, S. Ganatsios, O. Duliu, Costas V. Kavouridis, T. Sawidis","doi":"10.1081/TMA-120003729","DOIUrl":"https://doi.org/10.1081/TMA-120003729","url":null,"abstract":"ABSTRACT The concentration of 16 trace elements (V, Cr, Mn, Co, Ni, Cu, Mo, As, Cd, Hg, Sn, Se, Sb, Ba, Ag and Pb) has been determined in 39 points distributed over the 2300 km2 of the Kozani-Ptolemaïda-Amynteon basin (Western Macedonia). In this area there are four lignite power plants, with an installed power of 4048 MW, which discharged into atmosphere around 69500 tons/year of fly ash. Seventy soil samples, 0 to 20 cm depths, from both uncultivated and cultivated soils have been investigated. Except for Cr, Mn, Ni and Co in three uncultivated soil samples, no statistically significant increased concentrations could be evidenced in the considered area.","PeriodicalId":17525,"journal":{"name":"Journal of Trace and Microprobe Techniques","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2002-05-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"81158344","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}
V. Oreščanin, N. Mikulić, J. Obhodas, K. Nad, V. Valković
ABSTRACT Distributions of trace elements in the coastal sea sediments of Punat Bay in the Northern Adriatic have been investigated. The concentrations of 16 elements (Ca, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, As, Br, Rb, Sr, Y, Zr and Pb) were measured by energy dispersive XRF. Two predominant types of sediments were observed: the first (sediment “A”), which consists of 87% pelitic fraction and the second (sediment “B”), where coarse-grained fraction (0.315–0.1 mm) prevails. Enrichment factors had elevated values in two upper-most segments for the elements Cu, Zn and Pb in sediment “A.” The highest percentage of exchangeable fraction with respect to the total composition was characteristic for Cr, Cu and Zn in both types of sediments. By means of the linear regression analysis it was established that metals present in the antifouling paints were dispersed all over the bay because of an inefficient cleaning mechanism, poor communication with the open sea, and the good mixing of water and suspended mater in the bay by tide and wind currents.
{"title":"DISTRIBUTION OF TRACE ELEMENTS IN THE COASTAL SEA SEDIMENTS: PUNAT BAY IN THE NORTHERN ADRIATIC","authors":"V. Oreščanin, N. Mikulić, J. Obhodas, K. Nad, V. Valković","doi":"10.1081/TMA-120003727","DOIUrl":"https://doi.org/10.1081/TMA-120003727","url":null,"abstract":"ABSTRACT Distributions of trace elements in the coastal sea sediments of Punat Bay in the Northern Adriatic have been investigated. The concentrations of 16 elements (Ca, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, As, Br, Rb, Sr, Y, Zr and Pb) were measured by energy dispersive XRF. Two predominant types of sediments were observed: the first (sediment “A”), which consists of 87% pelitic fraction and the second (sediment “B”), where coarse-grained fraction (0.315–0.1 mm) prevails. Enrichment factors had elevated values in two upper-most segments for the elements Cu, Zn and Pb in sediment “A.” The highest percentage of exchangeable fraction with respect to the total composition was characteristic for Cr, Cu and Zn in both types of sediments. By means of the linear regression analysis it was established that metals present in the antifouling paints were dispersed all over the bay because of an inefficient cleaning mechanism, poor communication with the open sea, and the good mixing of water and suspended mater in the bay by tide and wind currents.","PeriodicalId":17525,"journal":{"name":"Journal of Trace and Microprobe Techniques","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2002-05-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"72560426","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 reaction of Vanadyl(II), Manganese(II) and Iron(III) as metal ion with 1,10-phenanthroline as primary ligand and eosin as secondary ligand was examined spectrophotometrically. The solution spectra of mixed ligand complexes formed are characterized by an absorption band with λmax at 550 nm for VO(II), 560 for Mn(II) and 555 nm for Fe(III) at pH 6.0, 5.2 and 5.6, respectively. These association complexes obey Beer's Law over the concentration range 3.0–12.0, 0.4–2.0 and 0.5–2.0 ppm with molar absorption coefficient of 1.73 × 104, 1.95 × 104 and 2.80 × 104 L mole−1 cm−1, respectively. Stability constants and diverse ion effects on these complexes have also been investigated.
{"title":"SPECTROPHOTOMETRIC STUDIES OF TERNARY COMPLEXES OF VANADYL, MANGANESE, AND IRON WITH o-PHENANTHROLINE AND EOSIN","authors":"M. A. Rauf, M. Ikram, M. Ahmad","doi":"10.1081/TMA-120003722","DOIUrl":"https://doi.org/10.1081/TMA-120003722","url":null,"abstract":"ABSTRACT The reaction of Vanadyl(II), Manganese(II) and Iron(III) as metal ion with 1,10-phenanthroline as primary ligand and eosin as secondary ligand was examined spectrophotometrically. The solution spectra of mixed ligand complexes formed are characterized by an absorption band with λmax at 550 nm for VO(II), 560 for Mn(II) and 555 nm for Fe(III) at pH 6.0, 5.2 and 5.6, respectively. These association complexes obey Beer's Law over the concentration range 3.0–12.0, 0.4–2.0 and 0.5–2.0 ppm with molar absorption coefficient of 1.73 × 104, 1.95 × 104 and 2.80 × 104 L mole−1 cm−1, respectively. Stability constants and diverse ion effects on these complexes have also been investigated.","PeriodicalId":17525,"journal":{"name":"Journal of Trace and Microprobe Techniques","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2002-05-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"84815693","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 A totally 33 soil samples influenced mainly by traffic density collected from around of highways in various locations of Turkey were analyzed by FAAS using three different extractant solutions, namely; 0.1 M HCl, 1 M CH3COONH4, and aqua regia solutions for determining the concentrations of various physicochemical forms of metals (Cu, Pb, Cd, Fe, Ni, Mn, Cr, Co, Bi and Zn) which are acid-soluble, exchangeable, and total, respectively. Accuracy of the method was tested by spiking the known amount of the elements interested to soil extracts for each extraction procedure. The accuracy of results for each extraction procedure was found to be satisfactory. Also, the standard addition method was applied for the soil leachings obtained by using each extractant. The detection limits of metals for different extraction procedures were between 0.02 and 1.08 µg ml−1. Correlation analysis and principal component analysis were applied to the data matrix to evaluate the analytical results and to identify the possible pollution sources of metals.
摘要/ ABSTRACT摘要:采用火焰原子吸收光谱法分析了土耳其不同地区公路周围受交通密度影响较大的33个土壤样品，分别使用3种不同的萃取剂溶液;0.1 M HCl, 1 M CH3COONH4和王水溶液，分别用于测定各种物理化学形式的金属(Cu, Pb, Cd, Fe, Ni, Mn, Cr, Co, Bi和Zn)的浓度，这些金属分别为酸溶性，交换性和总金属。该方法的准确性是通过在每个提取过程中添加已知的对土壤提取物感兴趣的元素来测试的。各提取方法结果的准确性均令人满意。对各萃取剂所得土壤浸出物采用标准添加法。不同提取方法对金属的检出限在0.02 ~ 1.08µg ml−1之间。对数据矩阵进行相关分析和主成分分析，对分析结果进行评价，确定可能的金属污染源。
{"title":"ATOMIC ABSORPTION SPECTROMETRIC DETERMINATION OF HEAVY METAL CONTENTS OF SOILS AROUND DIFFERENT HIGHWAYS IN TURKEY AND STATISTICAL INTERPRETATION OF THE DATA","authors":"Ş. Tokalıoğlu, Ş. Kartal","doi":"10.1081/TMA-120002466","DOIUrl":"https://doi.org/10.1081/TMA-120002466","url":null,"abstract":"ABSTRACT A totally 33 soil samples influenced mainly by traffic density collected from around of highways in various locations of Turkey were analyzed by FAAS using three different extractant solutions, namely; 0.1 M HCl, 1 M CH3COONH4, and aqua regia solutions for determining the concentrations of various physicochemical forms of metals (Cu, Pb, Cd, Fe, Ni, Mn, Cr, Co, Bi and Zn) which are acid-soluble, exchangeable, and total, respectively. Accuracy of the method was tested by spiking the known amount of the elements interested to soil extracts for each extraction procedure. The accuracy of results for each extraction procedure was found to be satisfactory. Also, the standard addition method was applied for the soil leachings obtained by using each extractant. The detection limits of metals for different extraction procedures were between 0.02 and 1.08 µg ml−1. Correlation analysis and principal component analysis were applied to the data matrix to evaluate the analytical results and to identify the possible pollution sources of metals.","PeriodicalId":17525,"journal":{"name":"Journal of Trace and Microprobe Techniques","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2002-02-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"75990663","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}
V. Orešcanin, J. Franekić-Čolić, K. Durgo, V. Valković
ABSTRACT Disposal of the dredged material from the harbour to the sea bottom represents a route through which many contaminants could be transported towards the open sea and enter to the food chain. In this study, five sediment samples were taken from different depths and locations within Plomin bay (Istria Peninsula, Northern Adriatic Sea, Croatia). Water sediment extract were prepared and analysed for chemical and physical properties, and subjected to cytotoxic and mutagenic investigation. We used two strains of Salmonella typhimurium, TA98 (determination of frameshift mutation) and TA100 (detection of base pair substitution) as a test system. Result showed that concentrations of heavy metals measured in extracts represent exchangeable fraction and are 500–1000 times smaller than the content of the same elements in solid mud. Nine elements were determined in extract: V, Cr, Mn, Fe, Ni, Cu, Zn, As and Pb. None of sediment sample extracts were cytotoxic or mutagenic for S. typhimurium TA98 nor TA100 in presence/absence of metabolic activation.
{"title":"INVESTIGATION OF MUTAGENIC EFFECT OF METALS IN THE PLOMIN BAY SEDIMENTS BY MODIFIED PREINCUBATION AMES ASSAY","authors":"V. Orešcanin, J. Franekić-Čolić, K. Durgo, V. Valković","doi":"10.1081/TMA-120002461","DOIUrl":"https://doi.org/10.1081/TMA-120002461","url":null,"abstract":"ABSTRACT Disposal of the dredged material from the harbour to the sea bottom represents a route through which many contaminants could be transported towards the open sea and enter to the food chain. In this study, five sediment samples were taken from different depths and locations within Plomin bay (Istria Peninsula, Northern Adriatic Sea, Croatia). Water sediment extract were prepared and analysed for chemical and physical properties, and subjected to cytotoxic and mutagenic investigation. We used two strains of Salmonella typhimurium, TA98 (determination of frameshift mutation) and TA100 (detection of base pair substitution) as a test system. Result showed that concentrations of heavy metals measured in extracts represent exchangeable fraction and are 500–1000 times smaller than the content of the same elements in solid mud. Nine elements were determined in extract: V, Cr, Mn, Fe, Ni, Cu, Zn, As and Pb. None of sediment sample extracts were cytotoxic or mutagenic for S. typhimurium TA98 nor TA100 in presence/absence of metabolic activation.","PeriodicalId":17525,"journal":{"name":"Journal of Trace and Microprobe Techniques","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2002-02-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"80545866","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 With the aid of the analytical energy dispersive X-ray fluorescence technique with radioisotope excitation, the concentrations of metals in commercial tablets containing 0.25 mg of digoxin were estimated. Concentrations ranging from 2.99 to 10.70 µg of Fe; 1.59 to 2.30 µg of Ni; 0.94 to 5.48 µg of Cu and 0.11 to 5.72 µg of Zn were found per tablet analyzed. The experimental detection limits for these elements varied from 13.03 to 22.57 µg l−1, while the relative errors made in the quantification of these metals were lower than 15%.
{"title":"APPLICATION OF X-RAY FLUORESCENCE TO DETERMINATION OF METALS IN COMMERCIAL TABLETS CONTAINING DIGOXIN","authors":"O. Zucchi, V. N. Filho, H. S. Neto","doi":"10.1081/TMA-120002467","DOIUrl":"https://doi.org/10.1081/TMA-120002467","url":null,"abstract":"ABSTRACT With the aid of the analytical energy dispersive X-ray fluorescence technique with radioisotope excitation, the concentrations of metals in commercial tablets containing 0.25 mg of digoxin were estimated. Concentrations ranging from 2.99 to 10.70 µg of Fe; 1.59 to 2.30 µg of Ni; 0.94 to 5.48 µg of Cu and 0.11 to 5.72 µg of Zn were found per tablet analyzed. The experimental detection limits for these elements varied from 13.03 to 22.57 µg l−1, while the relative errors made in the quantification of these metals were lower than 15%.","PeriodicalId":17525,"journal":{"name":"Journal of Trace and Microprobe Techniques","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2002-02-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"79932990","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 A sensitive and simple method for flame atomic absorption spectrometric determination of Cu, Fe, Pb, Ni and Mn after separation/preconcentration by sorbing 8-hydroxiquinoline (OXINE) complex of analytes on the Diaion HP-20 column has been established. The metal/oxine complexes were quantitatively retained on the Diaion HP-20 at pH 9. Metals retained on the column were quantitatively (<95%) eluted with 1 M HNO3 in acetone. The accuracy of the method was demonstrated by the analysis of a stream sediment standard reference material (GBW7309) sample and by recovery on spiked samples. The method was applied to the determination of copper, iron, lead, nickel and manganese in drinking water samples and good results were obtained (Recoveries >95%, relative standard deviations <9%, relative error <3%).
{"title":"SOLID PHASE EXTRACTION OF SOME METAL IONS ON DIAION-20 RESIN PRIOR TO FLAME ATOMIC ABSORPTION SPECTROMETRIC ANALYSIS","authors":"F. Armagan, M. Soylak, L. Elçi, M. Doğan","doi":"10.1081/TMA-120002457","DOIUrl":"https://doi.org/10.1081/TMA-120002457","url":null,"abstract":"ABSTRACT A sensitive and simple method for flame atomic absorption spectrometric determination of Cu, Fe, Pb, Ni and Mn after separation/preconcentration by sorbing 8-hydroxiquinoline (OXINE) complex of analytes on the Diaion HP-20 column has been established. The metal/oxine complexes were quantitatively retained on the Diaion HP-20 at pH 9. Metals retained on the column were quantitatively (<95%) eluted with 1 M HNO3 in acetone. The accuracy of the method was demonstrated by the analysis of a stream sediment standard reference material (GBW7309) sample and by recovery on spiked samples. The method was applied to the determination of copper, iron, lead, nickel and manganese in drinking water samples and good results were obtained (Recoveries >95%, relative standard deviations <9%, relative error <3%).","PeriodicalId":17525,"journal":{"name":"Journal of Trace and Microprobe Techniques","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2002-02-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"82029606","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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