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図書 |
図書
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木羽, 敏泰
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論文 |
論文
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松本, 健 ; 木羽, 敏泰
概要:
金沢大学イノベーション創成センター<br />100 ml 分液漏斗に1M塩化アンモニウム-炭酸アンモニウム-アンモニア水溶液(pH10) 50 ml を入れ,窒素を通じ脱酸素してから,金属銅試料を加え振り混ぜると,酸化銅(I)と酸化銅(I
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I)はアンミン錯イオンとなって溶解し,金属は溶けないで残る.水溶液について銅の量を原子吸光法で定量すれば,酸化銅(I)と酸化銅(II)の合量が求められる.一方,水溶液について窒素ふん囲気の下でバクソプロイン-クロロホルム抽出した後,銅を比色定量して酸化銅(I)の量を求める.酸化銅(II)は酸化銅(I)と酸化銅(II)の合量から酸化銅(I)を差し引いて算出した.本法は精度が高く,金属銅表面の酸化銅(I)と酸化銅(II)とを簡単迅速に分別定量できる. Fractional determination of cuprous oxide and cupric oxide attaching on the surface of high purity copper metal. Ken MATSUMOTO and Toshiyasu KIBA (Department of Chemistry, Faculty of Science, Kanazawa University, 1-1, Marunouchi, Kanazawa-shi, Ishikawa) A 50 ml portion of 1 M ammonium chloride-ammonium carbonate buffer solution at pH 10 was placed in a 100 ml separatory funnel and several pieces of high purity copper metal sample were put into the solution. Then a sufficient amount of nitrogen gas to remove oxygen from the solution as well as the vessel was passed through and the whole was agitated vigorously for 5 min. It was found that the cuprous and cupric oxide on the surface of the sample were dissolved as tetraammine copper complex cations and their oxidation states were retained while the metallic copper remained undissolved. The copper content in the resulting solution which should give the sum of the cuprous and cupric oxide was determined by atomic absorption spectrometry. The determination of cuprous oxide was carried out as follows. A 5 ml portion of the sample solution containing both of copper (I) and (II) was placed in a 50 ml separatory funnel which contained a 20 ml portion of 1 M ammonium chloride-hydrochloric acid at pH 1 and a 5ml portion of 0.1 % Bathocuproine-ethanol solution under nitrogen atmosphere. The pH of the solution was about 8. After standing for 5 min, the solution was agitated with 5.00 ml of chloroform for 2 min and the absorbance of the chloroform phase at 477 nm was measured against chloroform. This gave the cuprous oxide content. At the same time, a 5 ml portion of the sample solution was pipetted into a 50 ml separatory funnel and about 20 ml of 1 M ammonium chloride solution adjusted at pH 1, a 5 ml portion of 0.1 % Bathocuproin solution and a 2 ml portion of 10 % hydroxyl amine were added. The copper(I) in the solution was extracted by the same procedures as above and the total copper content was also determined from the absorption of this chloroform phase at 477 nm. The cupric oxide content was calculated from the total copper determined by either the atomic absorption spectrometry or the colorimetry and the copper (I) content obtained by the colorimetry. These procedures enabled the analysis of small amounts of cuprous and cupric oxide on the surface of commercial copper metal samples in various forms and the selectivity and the reproducibility were concluded to be excellent. (Received June 5, 1980)
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| 3.
論文 |
論文
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木羽, 敏泰 ; 寺田, 喜久雄 ; 本浄, 高治 ; 松本, 健 ; 飴野, 清
概要:
金沢大学イノベーション創成センター<br />神通川上流の高原川本川及び支川、梓川上流の上高地周辺及び旧平金鉱山廃坑を中心とする小八賀川上流より採取した河底でい53試料の、イオン交換水で懸濁する部分につき、銅、鉛、亜鉛、カドミウム、ニッケル
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、コバルト、ビスマス、銀、ヒ素及びアンチモン含量を定量した。これら10元素の濃度(ppm)について濃度比マトリクスを作成し、次いでそれぞれ2個の試料間の濃度比マトリクスの比マトリクスを求め、これらマトリクスの各項の数値のうち、符合判定基準1/M[<!_]yij(k,l)[<!_]について、M=1.5及びM=1.3にあてはまるものの数を求めた。これより各試料相互閥の相関マトリクスを作成し、各河川の合流点近傍地点についての相関性を典型的なlOの場合について示した。 Chemical analyses of geochemical or environmental samples get useful when generic relationships among the samples are discovered, as the latters tell the mechanism participating in the flow of a stream as well as the transfor of materials in the environment. The present study concerns the river bottom sedimentsfor which a technique of the conentration correlation matrix to discover the origin of various trace element. The investigators collected the river-sediment samples from the rivers running through the mountains of the middle Japan area. The water-suspended materials of the samples were submitted to the chemical analyses for ten elements, Cu, Pb, Zn, Cd, Ni, Co, Bi, Ag, As, and Sb. Experimental data based on 53 samples of river-sedoments are presented. Among ten examples eight show the relatively high generic correlations between the samples at the confluence of the main course of the river and the feeders. Relatively low correlations found in the other two examples could be internpreted in terms of the geographical and geological reasons.
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| 4.
論文 |
論文
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木羽, 敏泰 ; 松本, 健 ; 清水, 源治
概要:
金沢大学イノベーション創成センター<br />l00ml分液漏斗に1M塩化アンモニウム-アンモニア水溶液(pPH10) 50ml、水銀2・5mlを入れ、窒素ガスを通じ脱酸素してから、試料の高純度金属カドミウム片を加え振り混ぜると、金属はアマ
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ルガムとなって水銀中に溶解し、酸化物はアンミン錯イオンとなって水溶液中に溶ける。水銀を分離した後、水溶液についてカドミウムの量を原子吸光法で定量すれば酸化物を求められる。本法は精度は高く、金属表面及び内部の酸化物を分別的に定量できることにも特長がある。 In a 100ml separating funnel were added 50ml of 1M ammonium chloride-aqueous ammonia buffer solution(pH1O) and 2.5ml mercury; after passing nitrogen gag sufficiently to remove oxygen from the vessel and also from the aqueous solution, several pieces of cadmium metal of high purity were put into the vessel. The content was shaken vigorously; the metal went into mercury forming cadmium-amalgam, while the cadmium oxide dissolved itself in the aqueous solution to form cadmium tetrammine complex cations. After removal of mercury from the funnel, the solution was submitted to the determination of cadmium dissolved in it by means of the atomic absorption spectrophotometry or the EDTA titration. By the above procedure a minute amount of cadmium oxide could be determined precisely with high reproducibility. The critical experiments were also done to clarify the behaviors of cadmium metal and cadmium oxide in this separation process for the purpose of establishing a suitable procedure.
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| 5.
論文 |
論文
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松本, 健 ; 小泉, 貞之 ; 木羽, 敏泰
概要:
金沢大学イノベーション創成センター<br />100m1二ロフラスコにフェノール40mlを入れ,予備加熱して脱水してからフラスコ内を窒素ふんい気とした後,試料の高純度マグネシウム片を加え,加熱還流すると,金属はマグネシウムフェノオキシドとな
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って溶解し,酸化物は溶けないで残さとなる.無水メタノールを加えて希釈後,酸化物残さを濾別し希塩酸で溶解した水溶液について,マグネシウムの量を原子吸光法で定量し酸化物量を求める.本法の精度は高く,金属表面及び内部の酸化物の総量を簡単迅速に定量できる. A 40 ml of phenol was put in 100 ml two neck round-bottom flask equipped with a conventional distillation device and a ground glass stopper, and heated to the boiling point of phenol, 180℃. During this treatment, a slight amount of water contained in phenol was eliminated from phenol as the azeotropic vapor mixture of phenol and water at 99.5℃, and phenol was thoroughly dehydrated. After the distillation device was replaced by a reflux condenser, a piece of magnesium metal sample was put quickly into the flask through the side neck. Then the content was heated under stirring at 180℃, until magnesium metal diminished completely in phenol, forming magnesium phenoxide, while magnesium oxide remained as residue. The reaction mixture was cooled to (50〜60) ℃, and anhydrous methanol was added to keep phenol and magnesium phenoxide in dissolving form. The residual magnesium oxide was caught on a sintered glass filter (1G5) and dissolved in 50 ml of 2 M hydrochloric acid. The solution was diluted to a definite volume and magnesium in the solution was determined by the atomic absorption spectrometry. All the experiments were carried out in a glove box in dry nitrogen atmosphere to avoid the influence of oxygen and water from air. By the above procedure a minute amount of magnesium oxide could be determined precisely with high reproducibility. To clarify the behaviors of magnesium metal and magnesium oxide in this separation process additional experiments were also done.
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| 6.
論文 |
論文
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木羽, 敏泰 ; 寺田, 喜久雄 ; 中川, 千枝
概要:
金沢大学理学部<br />An oxidizing reagent consisting of the mixture of 2.5g of potassium dichromate, 10g of silver sulfate, 600m
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l of sulfuric acid and 400ml of phosphoric acid was recommended to use for the simple and rapid determination of COD of various waste waters. A 10-ml portion of sample water was put into a 50-ml Kjeldahl flask with 0.3g of mercury(II) sulfate and several pieces of boiling stone, and 25ml of the reagent-mixture was added. The solution was boiled at 160℃ for 30 min, setting a cooling finger inside the neck of the flask. The contents of the flask was transferred into a 50-ml measuring flask and was diluted with water to the mark. The absorbance of the solution was measured at the wavelength of 630nm with a 50-mm glass cell. Beer's law was obeyed over the range of 0〜1000ppm COD. The calibration curves using glycine, glucose, ethanol and starch, as the reference, gave their slope of 7.05×10^<-4> as the mean. Therefore, the COD value can be calculated from the following equation : GOD=absorbance/7.05×10^<-4>. An appropriate volume ratio of sulfuric add to phosphoric acid for the decomposition of glycine was found to be 3:2. The reaction time could be reduced to about one fourth of JIS(COD_<Cr>) method. The analytical results obtained for several kinds of industrial waste water are in good agreement with those obtained by JIS(COD_<Cr>) method.
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| 7.
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論文
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木羽, 敏泰 ; 赤岩, 英夫 ; 一国, 雅巳 ; 小沢, 竹二郎 ; 鎌田, 政明 ; 北野, 康 ; 重松, 恒信 ; 鈴木, 信男 ; 外林, 武 ; 長島, 弘三 ; 西川, 泰治 ; 西村, 雅吉 ; 浜口, 博 ; 松尾, 力 ; 村上, 悠紀雄 ; 室住, 正世 ; 森田, 良美 ; 山県, 登 ; 山本, 勇麓 ; 綿抜, 邦彦
概要:
金沢大学理工研究域<br />文部省科学研究費特定研究(1)「環境汚染の検知と制御」のサブグループである「環境分析における標準物質と分析値の精度に関する研究」班は20名の班員によって構成されていて,試料処理法,微量分析法の実施検討並びに標準
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対照試料の作成などの基礎研究と併行して,共通試料を選び,班員に配布し,指定された成分についての分析を実施し,そのデータを持ち寄り,いわゆるクロスチェックを行うとともに,誤差範囲の検討や分析法の優劣を討議している.本稿では(1)渡良瀬川河川水(1975.11.14採取)中の銅,亜鉛,鉛,(2)調製水溶液試料についての銅,亜鉛,鉛,カドミウム,クロム,鉄に関しての結果について報告する. During the last two years 1975〜1976 a research group was organized to evaluate jointly the precision of trace analysis values for environmental samples. The twenty-membered group (chairman Prof. T. Kiba), supported by a Grant-in-aid for Scientific Research from the Ministry of Education(No. 011910), cooperated in the interlaboratory comparison tests of two reference standard materials, i.e. a natural water sample and a composite heavy metal salts solution. The natural water sample was collected at Watarase River on November 11, 1975. The river water and the salts solution were distributed among the members and analyzed, respectively, for Cu, Zn, and Pb and for Cu, Zn, Cd, Pb, Cr, and Fe. Results are listed in Tables 1 and 3. In these trials all members were free of a specified pre-treatment and of a defined measurement technique, and therefore the results obtained seem to give the average precision of the analyses carried out arbitrarily in the university laboratories
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