Journal of Trace and Microprobe Techniques最新文献

{"title":"Changes of Silica Species in Sodium Chloride Solution by Fast Atom Bombardment Mass Spectrometry: Silicate Complex Substituted by Sodium Ion","authors":"Miho Tanaka, Kazuya Takahashi","doi":"10.1081/TMA-120025806","DOIUrl":"https://doi.org/10.1081/TMA-120025806","url":null,"abstract":"Abstract The types of chemical species of silicate complex ion exchanged with sodium ions (silicate–Na+ complex) with increasing concentration of sodium chloride (NaCl) and their numbers of chemical species of silicate–Na+ complexes formed were examined. Silicate–Na+ complexes in several concentrations of NaCl were identified by fast atom bombardment mass spectrometry (FAB-MS). The basic structures of silicate species are not complexes with Na+, such as the dimer, trimer, cyclic tetramer, linear tetramer, cyclic pentamer, linear pentamer, cyclic hexamer and linear hexamer, were identified. When the peak intensity ratios of silicate–Na+ complexes were plotted against the concentration of NaCl, the changes with increasing concentration of NaCl were mainly classified into two patterns. One is the linear silicate–Na+ complex pattern (dimer–Na+ complex, trimer–Na+ complex and linear tetramer–Na+ complex), and the other is the cyclic silicate–Na+ complex pattern (cyclic tetramer–Na+ complex and cyclic pentamer–Na+ complex). In the linear silicate–Na+ complex pattern, the peak intensity ratios of the linear silicate–Na+ for the basic structures vary largely between 0.001 and 0.1 mol dm−3 (M) NaCl, and they become constant at above 1 M NaCl. In the cyclic silicate–Na+ complex pattern, the peak intensity ratios of the basic structures of cyclic silicate–Na+ change slightly between 0.001 and 0.1 M NaCl and change considerably above 1 M NaCl. The basic structure of cyclic silicate has a stable structure and hydrophobic part. By substituting Na+, the hydrophobicity of the cyclic silicate complex increases. The linear silicate complex is not as stable as the cyclic silicate complex and it possesses a higher degree of hydration than the cyclic silicate. The hydrophobicity of the linear silicate also increases by the substitution of silanol groups by Na+. These changes of the hydrophobicity of the linear silicate due to the substitution of Na+ are larger than those for the cyclic silicate. The dissolution system of the silicate species in NaCl solution should be elucidated by considering the relationship between the stabilities of the basic structure and Na+-containing silicate complexes, and their hydration effect.","PeriodicalId":17525,"journal":{"name":"Journal of Trace and Microprobe Techniques","volume":"35 1","pages":"561 - 576"},"PeriodicalIF":0.0,"publicationDate":"2003-01-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"77099223","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}

{"title":"Studies on Quantification Analysis of Thin Film Layers (Si3N4, SiO2, and TiW) in Wafer Fabrication Using Energy-Dispersive X-Ray Microanalysis Technique and SEC Factors","authors":"Younan Hua","doi":"10.1081/TMA-120017889","DOIUrl":"https://doi.org/10.1081/TMA-120017889","url":null,"abstract":"Abstract Currently standardless EDAX ZAF quantification method has been widely used in many new generation FESEM machines. This method is able to provide good and reliable elemental results for bulk samples and some films for some particles and contamination analysis, but for some cases, EDX results may not be accurate, especially for thin film layer identification in wafer fabrication. In this paper, standardless EDAX ZAF quantification method will be further studied and an EDX quantification analysis method with the SEC factor correction will be introduced. The SEC factors can be calculated using current EDAX software. Application results from passivation thin film Si3N4, SiO2 layers and barrier metal thin film TiW layer show that the EDX results have been greatly improved after performing the SEC factor correction and the relative error is greatly reduced from 64.3–101% to 0.23–3.93% for passivation Si3N4 layer, from 51.5–62.3% to 0.73–3.10% for passivation SiO2 layer and from 18.2–77.0% to 0.04–11.5% for barrier metal TiW layer. If we assume that the passivation and barrier metal layers always have a stoichiometric composition, this method could be used for the monitoring purpose in wafer fabrication.","PeriodicalId":17525,"journal":{"name":"Journal of Trace and Microprobe Techniques","volume":"70 1","pages":"25 - 34"},"PeriodicalIF":0.0,"publicationDate":"2003-01-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"76538158","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}

{"title":"FIA-Spectrophotometric Determination of Ascorbic Acid in Rat's Lung by Reduction of Iron(III)","authors":"E. Kleszczewska","doi":"10.1081/TMA-120017894","DOIUrl":"https://doi.org/10.1081/TMA-120017894","url":null,"abstract":"Abstract A FIA indirect spectrophotometric determination of ascorbic acid (vitamin C) was developed using its reducing action on Fe(III) and following the spectrophotometric determination of the reduced ion by 2,2′-dipyridyl and monitoring the absorbance signal at 520 nm. The procedure is based on the reduction of iron(III) to iron(II) with ascorbic acid. The iron(II) obtained is then able to react with 2,2′-dipyridyl in order to form a colored complex. The linear range of the method was 1.0–10.0 ppm ascorbic acid. The proposed method was sensitive, rapid (40 samples/h) and reproducible (relative standard deviation 1.2%, n = 40). Satisfactory results were obtained in the determination of ascorbic acid in rat's lung.","PeriodicalId":17525,"journal":{"name":"Journal of Trace and Microprobe Techniques","volume":"94 1","pages":"85 - 94"},"PeriodicalIF":0.0,"publicationDate":"2003-01-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"83555523","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}

{"title":"Determination of Some Trace Heavy Metals in Some Water Samples by FAAS After Their Preconcentration Using DETA","authors":"Yasemin Bakircioglu, S. Akman, N. Bıçak, F. Şenkal","doi":"10.1081/TMA-120020259","DOIUrl":"https://doi.org/10.1081/TMA-120020259","url":null,"abstract":"Abstract Diethylenetriamine, DETA polymer was used as a preconcentration of cobalt, iron and nickel prior to their determination by flame atomic absorption spectrometry (FAAS). Both batch and column methods were used for the separation and concentration of above metals. These metals were quantitatively retained on the proposed adsorbent at pH 2, then were quantitatively eluted with 2 M hydrochloric acid or nitric acid. The recoveries of metal ions were greater than 98%. Detection limits (3 δ) were 1.5 µg/L for Co, 2.1 µg/L for Fe and 1.9 µg/L for Ni. The relative standard deviations for the determinations were found to be 1.0–8.8%. The effect of Na on the preconcentration of trace metals has also been investigated. The method was applied to tap, ground and lake water samples.","PeriodicalId":17525,"journal":{"name":"Journal of Trace and Microprobe Techniques","volume":"6 1","pages":"239 - 248"},"PeriodicalIF":0.0,"publicationDate":"2003-01-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"88790206","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}

{"title":"Dead Time Based Correction for the Combined Electronic Losses in INAA Based on Short-Lived Radionuclides","authors":"H. A. Das, E. Akaho","doi":"10.1081/TMA-120025811","DOIUrl":"https://doi.org/10.1081/TMA-120025811","url":null,"abstract":"Abstract The combined negative bias in gamma-spectrometry due to pile-up and (residual) dead time losses in case of short-lived radionuclides can be corrected for by way of dead time readings. The combined loss-factor depends on the ratio of the time-constants in amplifier and ADC, and on the average decay-constant over the total spectrum during measurement. Both parameters can be determined once and for all for a given routine application. The procedure is applicable up to total dead time fractions of at least 0.3 and thus covers routine instrumental neutron activation analysis (INAA) practice with short-lived radionuclides.","PeriodicalId":17525,"journal":{"name":"Journal of Trace and Microprobe Techniques","volume":"46 1","pages":"601 - 607"},"PeriodicalIF":0.0,"publicationDate":"2003-01-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"77357769","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}

{"title":"Ion Exchange Separation of Lead from Strontium in Certified Reference Samples and Spectrophotometric Determination of Lead as Extractable Ion-Pair of Eosin2− and the Lead–Cryptand (2.2.2)2+ Complex","authors":"R. Al-Merey, O. Al-Shayah","doi":"10.1081/TMA-120017888","DOIUrl":"https://doi.org/10.1081/TMA-120017888","url":null,"abstract":"Abstract A two-step procedure including anion exchange separation of lead from strontium in geological reference samples and a spectrophotometric determination of the separated lead as lead–cryptate (2.2.2) complex is presented. The exchangeable anion Cl− of the ion exchange resin (Dowex 1 × 4) is changed to Br− in 6 M HBr solution. Lead is quantitatively retained in the column from 0.5 M HBr medium, while Sr2+, Ba2+, Ca2+, Mg2+, Na+, K+, Fe3+, Cr3+, and Al3+ are passed through. Subsequently the retained Pb is eluted from the column with 6 M HBr. The separation efficiency of the resin is controlled using mixed standard solution of (Pb, Sr, Ca, Mg, Ba, Na, K, Fe, Cr and Al), and radioactive tracers of 85Sr and 131Ba. The resin selectivity coefficient (K) of separating Pb from Sr is found to be . The Spectrophotometric method of lead determination is based on the formation of lead–cryptate (2.2.2) complex at pH 8.3 using borate/HCl as a buffer solution. Then the ion-pair of eosin2+ and lead–cryptand (2.2.2) complex is extracted with chloroform, finally the absorbance of the extractable legend is measured at 550 nm. The extraction recovery, accuracy, precision, linearity and detection limit of the spectrophotometric method are 99.58%, 1.7%, 0.080 µg mL−1, 0–9 µg mL−1, and 0.060 µg mL−1, respectively.","PeriodicalId":17525,"journal":{"name":"Journal of Trace and Microprobe Techniques","volume":"67 1","pages":"13 - 24"},"PeriodicalIF":0.0,"publicationDate":"2003-01-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"86014555","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}

{"title":"Flow Injection Spectrophotometric Determination of Perazine","authors":"W. Misiuk, P. Hałaburda","doi":"10.1081/TMA-120017896","DOIUrl":"https://doi.org/10.1081/TMA-120017896","url":null,"abstract":"Abstract The flow injection method, involving spectrophotometric detection, is proposed for the determination of perazine. The procedure is based on the oxidation of perazine by cerium(IV) sulphate(VI). Concentrations with perazine in the range 120–300 ppm have been determined with the relative standard deviation of 1.0%. The presented method was applied to the determination of perazine in pharmaceutical formulations.","PeriodicalId":17525,"journal":{"name":"Journal of Trace and Microprobe Techniques","volume":"95 1","pages":"102 - 95"},"PeriodicalIF":0.0,"publicationDate":"2003-01-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"91124552","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}

{"title":"Maternal Serum Hormone Concentrations in Long-Evans Rats","authors":"M. D. Mordechai Hallak, John W. Hotra","doi":"10.1081/TMA-120017898","DOIUrl":"https://doi.org/10.1081/TMA-120017898","url":null,"abstract":"Abstract The purpose of this study was to determine the effect of pregnancy on serum concentrations of estradiol, progesterone and prolactin in Long-Evans rats. Female Long-Evans rats, both pregnant and non-pregnant, were used. Four groups (n = 10 rats in each group) were studied: Non-pregnant rats; pregnant rats at 7, 14, and 20 gestational days. Maternal blood was collected transcardially, and serum estradiol, progesterone, and prolactin were measured by radioimmunoassay. Commercial kits from Diagnostic Products Corporation for estradiol and progesterone, and an established in-house double antibody assay for prolactin, were utilized. Statistical analysis was performed using ANOVA, followed by Newman-Keuls post hoc test when applicable. Estradiol concentrations were increased throughout gestation from 16.2 ± 6.2 pg/mL (mean ± SD) in the non-pregnant rat to 23.2 ± 8.8, 25.0 ± 7.7, and 30.3 ± 29.6 pg/mL on gestational days 7, 14, and 20, respectively. Progesterone showed the same trend, increasing from 7.2 ± 3.6 ng/mL in the non-pregnant rats to 25.9 ± 4.8, 43.0 ± 8.6, and 47.3 ± 8.8 ng/mL on gestational days 7, 14, and 20, respectively (p<0.05). Prolactin levels were decreased from the non-pregnant state (39.2 ± 22.8 ng/mL) through the early and mid-pregnancy (25.2 ± 20.4, 16.5 ± 16.9 ng/mL, respectively; p<0.05) and rose to pre-pregnancy levels on pregnancy day 20 (39.2 ± 20.4 ng/mL). The effect of pregnancy on serum hormone concentrations in Long-Evans rats were determined and compared to non-pregnant controls. This data may assist in simulating various stages of pregnancy for use in hormonal and receptor binding studies, and in isolating pregnancy hormone effects on the central nervous system in the Long-Evans rat.","PeriodicalId":17525,"journal":{"name":"Journal of Trace and Microprobe Techniques","volume":"4 1","pages":"103 - 110"},"PeriodicalIF":0.0,"publicationDate":"2003-01-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"90924975","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}

{"title":"Preconcentration and Determination of Manganese in Water Samples Using N , N ′- bis (2-Hydroxy-5- bromo-benzyl)1,2 Diaminopropane","authors":"M. Alkan, D. Kara","doi":"10.1081/TMA-120023064","DOIUrl":"https://doi.org/10.1081/TMA-120023064","url":null,"abstract":"Abstract The synthesis and analytical applications of N,N ′-bis(2-hydroxy-5-bromo-benzyl)1,2 diaminopropane (HBDAP) are described. The investigation includes a study of the characteristics that are essential for solvent extraction and for spectrophotometric determination and preconcentration of manganese. The organic phase loaded with Mn(II) from aqueous phase was stripped in one stage by using different mineral acid solutions. It was found that stripping efficiency was quantitative in case of HNO3. A highly sensitive, selective and rapid spectrophotometric method is described for the determination of trace amounts of manganese(II) by HBDAP. This compound reacts with manganese(II) in the range of pH 7–10 to produce a brownish complex (2:3 mol ratio of Mn(II)/HBDAP) soluble in chloroform. The complex obeys Beer's law from 0.12 to 13.2 mg L−1 with an optimum range. The relative standard deviations were % 0.02 (10 samples, each containing 3.2 mg L−1 Mn(II)). The precision was determined from 30 results obtained for 2.75 mg L−1 Mn(II); the mean value of a Mn(II) was 2.77 mg L−1 with a standard deviation of 0.018 mg L−1 Mn(II).","PeriodicalId":17525,"journal":{"name":"Journal of Trace and Microprobe Techniques","volume":"22 1","pages":"479 - 491"},"PeriodicalIF":0.0,"publicationDate":"2003-01-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"87487699","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}

{"title":"Computation and Experiments on the Beam Spread in the VP-SEM: Application to X-Ray Microanalysis","authors":"A. Kadoun, R. Belkorissat, C. Mathieu, B. Khelifa","doi":"10.1081/TMA-120020258","DOIUrl":"https://doi.org/10.1081/TMA-120020258","url":null,"abstract":"Abstract X-ray microanalysis (XRMA) coupled to a variable pressure scanning electron microscope (VP-SEM) using air atmosphere in the specimen chamber performed on test structures were used to make comparison with a Monte Carlo simulation program based on the modeling of the electron beam-gas interaction. The results show that the extent of the beam spreading can be significantly reduced at relatively high pressures by using helium gas instead of air and considerably reduced even at low pressure by lowering the analytical distance.","PeriodicalId":17525,"journal":{"name":"Journal of Trace and Microprobe Techniques","volume":"71 1","pages":"229 - 238"},"PeriodicalIF":0.0,"publicationDate":"2003-01-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"89242329","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}