分析化学
Print ISSN : 0525-1931
4 巻, 1 号
選択された号の論文の18件中1~18を表示しています
  • 東野 利昌, 武者 宗一郎
    1955 年 4 巻 1 号 p. 3-8
    発行日: 1955/02/15
    公開日: 2010/02/16
    ジャーナル フリー
    In the case of chrome-plating, the addition of small amounts of the various kinds of fluorides to the baths recently prevails in order to obtain the higher quality of the plate and to improve its procedure. But it has yet been difficult to control the contents of the fluorine owing to the lack of an adequate method for determining it. In the present work this method was investigated and the satisfactory results were obtained with the sample solutions containing from 0.2 to 5mg of fluorine per liter. The analytical procedure is as follows : 5ml of the solution, which is obtained by diluting the original sample solution by 75 times, is taken and the chromium is reduced to chromic by heating with the addition of 2ml of ethanol and 3ml of N-hydrochloric acid. Excess amounts of the chromic ion is exchanged by means of Daiya Ion K. The exchanged solution is added with sodium hydroxide to the faint red color of phenolphthalein and then added with 5ml of alum solution (40γ of aluminium), 8ml of N-hydrochloric acid, 5ml of 3N ammonium acetate, 5ml of 0. 1% solution of aluminon and 0.5ml of 6N ammonium carbonate. The total volume of the solution is brought up to 100ml (pH = 4.6) and is allowed to stand in the thermostat (31°C) for 45 minutes to develop the color. The amounts of fluorine are determined by the electrophotometric method, using the calibration curve. The analytical error is 2% and the time required is 75 minutes. Silicic acid and oxalic acid interferes.
  • 滝山 一善, 水渡 英二
    1955 年 4 巻 1 号 p. 8-11
    発行日: 1955/02/15
    公開日: 2009/06/30
    ジャーナル フリー
    Anion exchange resin (Amberlite IRA-410) was used as RCl, RS, ROH and RCO3 forms. At first the sample solution was passed through the column of RCl form exchanger. The first group metals precipitated as chloride. The precipitates were filtered and the filtrate was passed through the column of RS form exchanger. The second and the third group metals except Al and Cr precipitated as sulfide. The solution containing these precipitates was acidified by HCl (0.3N). The precipitates of the third group metals were dissolved, while those of the second group metals do not. The latter were filtered and the filtrate was passed through the column of ROH form exchanger. The third group metals and Mg precipitated as hydroxide. By the addition of NH4Cl to the suspension, Mg(OH)2 alone was dissolved. The precipitates of the third group metals were filtered and the filtrate was passed through the column of RCO3 form exchanger. The fourth group metals precipitated. The precipitates were filtered and the filtrate containing the fifth group metals was treated by RH form cation exchanger. The precipitates of each group metals were determined by usual method of qualitative analysis. The RCl, RS, ROH and RCO3 form anion exchange resins were regenerated by HCl, yellow ammonium sulfide, NaOH and (NH4)2CO3 respectively.
  • 尾崎 知良
    1955 年 4 巻 1 号 p. 11-14
    発行日: 1955/02/15
    公開日: 2009/06/30
    ジャーナル フリー
    There are many reports in detail on the determination of water in refined tar by Karl Fischer method, but no report has been made on the estimation of water in crude tars, except for using of distillation method. Accordingly, studies are made on this problem and found that the method of direct titration of tar without solvent gave unsatisfactory result on account of disturbance of the electrodes of titration apparatus, but the titration of the sample dissolved in toluene of known content of water gave only a slightly higher value than the theoretical amount and the method could be carried out with far less amount of sample than the distillation method, also, the time required for titration was 515 minutes.
  • 石橋 雅義, 東 慎之介
    1955 年 4 巻 1 号 p. 14-16
    発行日: 1955/02/15
    公開日: 2010/02/16
    ジャーナル フリー
    前報にて,微量トリウムの濃縮,および妨害諸イオンの除去操作に,水酸化物としてAlと共沈させ,更に蓚酸塩としてCdと共沈法を利用し,比色試薬"Thorone"を用いμg量の微量トリウムの比色定量法を報告した.本報にて,分離濃縮操作として硝酸トリウムをシクロヘキサノンにて抽出する方法をとり,新比色試薬として,ο-arsonophenylazo-chromothropic acidを合成し,分析操作の簡便化と,定量感度および精度に満足すべき結果を得たので,報告する.
  • 清田 寿, 山本 俊夫
    1955 年 4 巻 1 号 p. 16-21
    発行日: 1955/02/15
    公開日: 2009/06/30
    ジャーナル フリー
    It is well known that the estimation of liberated hydrochloric acid by the thermal decomposition of P. V. C. (Polyvinyl chloride) is important in various studies of P. V. C., but there are many unsatisfactory points for experimental studies by use of usual A. S. T. M. or similar method. Anew procedure of using calcium carbonate as an arresting agent for liberated hydrochloric acid was proposed by the authors. While the usual method is an estimation of liberated hydrochloric acid from untreated P. V. C., this method is an estimation of liberated hydrochloric acid from a mixture of P. V. C. and a substance stable for heating. Porcelain crucible was used and the experimental procedure could be carried out simply and accurately. The method could be applied for thermostability test below 200°C as well as thermal decomposition test above 200°C; also, the method could be applied for estimation of both of liberated hydrochloric acid and total chlorine. The limit of application is large since the test is a simple procedure.
  • イオン形成による無機陽イオンの分離
    牧 正文
    1955 年 4 巻 1 号 p. 21-25
    発行日: 1955/02/15
    公開日: 2009/06/30
    ジャーナル フリー
    1.Ethylendiamine-NH4 tartrate溶液による錯イオン形成による分離
    2.Triethanolamine-NH4 tartrate溶液による錯イオン形成による分離
    さきに電気クロマトグラフ法第4報1)として,NH4OH-NH4 tartrate溶液によって混合陽イオンの錯塩を形成せしめると,錯基が正に帯電する錯塩(アムミン錯塩と推定)と錯基が負に帯電する錯塩(酒石酸錯塩と推定)とが生じ,混合陽イオンを濾紙の原点を中心として,陽陰両極に分離し得,極めて分離能が増大して,いわゆる電気クロマトグラフ法の特色を発揮することができることをのべた.本報においては,これと同じ目的でNH4OHの代りにEthylendiamineおよびTriethanolamineを用いて陽イオンの分離をおこない,それぞれ異った分離状況を得たので報告する.錯
  • 深間内 久雄, 小幡 幸子
    1955 年 4 巻 1 号 p. 25-26
    発行日: 1955/02/15
    公開日: 2009/06/30
    ジャーナル フリー
    It is generally described that the reaction of manganese salts with bromic acid is a confirming test for bromate ion in the presence of chlorate. This is based on the repotts of Vitali1) and Monnier2), according to which manganous salts are oxidized to manganic salts or manganese dioxide by bromic acid, but not by chloric acid. In order to examine the above statement, experiments have been carried out and found that manganese salts are also oxidized by chloric acid; as a result, for identification of bromate ion by the reaction of manganese salts, it is necessary to detect the bromine produced by this reaction. The limit of detection of bromate ion by this method is 13γ/0.25cc, and the limit of concentration is 1/20000; the sensitivity is better than that given by Feigl3).
  • 鉛の定量について
    杉原 喜四郎, 斎藤 俊英
    1955 年 4 巻 1 号 p. 27-30
    発行日: 1955/02/15
    公開日: 2009/06/30
    ジャーナル フリー
    Heavy metal impurities, especially of lead, in reagent grade sodium chloride were extracted with dithizone and quantitatively estimated by polarography. In order to examine the percentage of extraction of lead by dithizone, 20-60γ lead was extracted from 150-450ml. aqueous sodium chloride solution at pH 9 with dithizone-carbon tetrachloride, rextracted with hydrochloric acid, the hydrochloric acid evaporated off, the residue dissolved in tartaric acid-ammonium acetate supporting electrolyte and polarogram was recorded. The result showed that the percentage of extraction of lead was 95 %, and, in case of insufficient evaporating operation, it caused an appearance of waves due to the presence of decomposition product of dithizone and it disturbed the estimation of wave height of lead and the detection of other metals. Quantitative estimation of lead was made on 4 samples of sodium chloride; also, lead, zinc, copper and a trace of nickel were detected by a combined use of potassium thiocyanate-ammonium acetate supporting electrolyte.
  • 能登 武治, 松岡 学
    1955 年 4 巻 1 号 p. 30-34
    発行日: 1955/02/15
    公開日: 2009/06/30
    ジャーナル フリー
    Quantitative determination of terramycin is made by colorimetric method with ferric chloride, spectrophotometric method or by microbiological method, but these methods require time and give larger allowable errors. In order to eliminate these effects, terramycin is converted into nitrosoterramycin by 100 % of its nitrosoation to make a product comparatively stable in N NH4OH-NH4Cl, under the condition of measurement, and gives a relation, id = K. C, and constant half-wave potential when the concentration range is 1 × 10-52 × 10-3 M/l. The nitrosoation of terramycin is carried out at room temperature with HCl and NaNO2, neutralized with NH4OH and its half-wave potential is determined in N NH4OH-NH4Cl.
  • 高木 誠司, 前川 義裕
    1955 年 4 巻 1 号 p. 34-36
    発行日: 1955/02/15
    公開日: 2009/06/30
    ジャーナル フリー
    Estimation of pH of commercial glucose injections by use of glass electrode showed to be pH 3.54.3. These lower pH values are attributed to the decomposition of glucose by heating to 5-(hydroxymethyl)-2-furaldehyde, its further decomposition gives an equimolar mixture of formic acid and levulinic acid and glucose injection's buffer action are very slight and cause much error when estimated by pH indicating papers. The concentration of formic acid and levulinic acid, respectively, is 5 × 10-5 to 5 × 10-4 N. The acidiy can be estimated by high frequency titration or it can be estimated by making a graph from relations of concentration of acid and pH values. Although these lower pH values are considered to be harmless for injection due to its weak buffer action, it is rather striking to note such lower pH values and a sugestion for revision of Pharmacopoeia Japonica VI is made, since it specifies to be pH 5. 07. 0
  • 新海 重行
    1955 年 4 巻 1 号 p. 37-38
    発行日: 1955/02/15
    公開日: 2009/06/30
    ジャーナル フリー
  • 北野 康
    1955 年 4 巻 1 号 p. 38-39
    発行日: 1955/02/15
    公開日: 2009/06/30
    ジャーナル フリー
  • 西田 宏
    1955 年 4 巻 1 号 p. 39-41
    発行日: 1955/02/15
    公開日: 2009/06/30
    ジャーナル フリー
  • 日比野 三成, 林 陽, 品川 睦明
    1955 年 4 巻 1 号 p. 41-43
    発行日: 1955/02/15
    公開日: 2010/05/25
    ジャーナル フリー
    アルミニウムのポーラログフフ的定量はPrajzler以来幾つかの研究があるが,動物生肉灰分については特に見受けない.著者等はマガキ生肉灰分の分析のため,まずアルミニウム塩につき吟味し一般試料にも通ずる改良法をえたので報告する.
    明瞭な波をうるための最適pHについては第1表に示すよう研究者により種々であり,用いる支持塩,pH調整法も夫々異っている.
  • 北野 康
    1955 年 4 巻 1 号 p. 43
    発行日: 1955/02/15
    公開日: 2009/06/30
    ジャーナル フリー
    Mohr法により塩素イオンを定量しようとする場合予め炭酸根を除く必要がある.炭酸根を多量含む溶液を硝酸で酸性にして煮沸し,炭酸根を炭酸ガスとして除き微量のCl-を定量しようとする場合2つの問題がある. 即ちその1つは炭酸根を炭酸ガスとして完全に除去する場合炭酸ガスとともにCl-がHClとして失われないかどうかということと他の1つはHNO3で酸性にする場合硝酸アルカリが多量析出してくるので飽和硝酸アルカリ溶液中の微量Cl-の定量が精確に出来るかどうかということである.後者についての検討は別に詳述し, 精確に定量しうる方法を考案した.そこでこの結果を利用して次の如き方法により,前者の検討を考慮しつつ炭酸カリ飽和溶液中の微量塩素イオンの定量法を検討したので得られた結果について報告する.
  • 岡崎 浩
    1955 年 4 巻 1 号 p. 44-47
    発行日: 1955/02/15
    公開日: 2009/06/30
    ジャーナル フリー
  • 島尾 和男
    1955 年 4 巻 1 号 p. 47-53
    発行日: 1955/02/15
    公開日: 2009/06/30
    ジャーナル フリー
  • 荒木 峻
    1955 年 4 巻 1 号 p. 54-58
    発行日: 1955/02/15
    公開日: 2009/06/30
    ジャーナル フリー
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