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Volume 16, Issue 3
Displaying 1-23 of 23 articles from this issue
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Nobuhisa MATANO, Katsumi ONO, Hideo SENO1967 Volume 16 Issue 3 Pages 175-184
Published: March 05, 1967
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSTo analyse the high alloy steels with fluorescent X-ray method, its exciting conditions have been determined by statistical method. The followings are:
1) It is adequate to apply the voltage of ca. 50 kV to X-ray tube.
2) Investigations on regressions between the intensities of fluorescent X-rays and the concentrations of element indicate that the regression coefficient and the intercept vary with the change of target material.
3) The matrix effect is principally strengthend with increasing absorption of fluorescent X-ray by the matrix.
4) The relations between the compositions of samples and the intensity of the fluorescent X-rays can be expressed approximately by the equation:
Ii=KÎ0Wi/Σ(c+μfij)WjView full abstractDownload PDF (1365K) -
Noboru KUNIMINE, Hiroo KAWADA1967 Volume 16 Issue 3 Pages 185-189
Published: March 05, 1967
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA method for the determination of silver in photographic materials by atomic absorption spectrochemical analysis has been established. The method involves the extraction of silver with potassium cyanide solution and the measurement of the absorbance at 3280 Å. The authors determined silver by this method with high sensitivity, precision and rapidity. Standard deviation of the absorbance of a 10ppm silver solution by 20 measurements was 0.68% with maximum error below 1%. Ten samples can be analysed in 50minutes. Because of the high sensitivity of this method, only 1cm2 of sample is sufficient for an analysis, and photographic materials with very low contents of silver can be treated with the same precision and accuracy as in the analysis of general photographic films.View full abstractDownload PDF (882K) -
Noboru KUNIMINE, Hiroo KAWADA1967 Volume 16 Issue 3 Pages 189-193
Published: March 05, 1967
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA method for the determination of cadmium in photographic materials by atomic absorption spectrochemical analysis which involves the extraction of cadmium with water and potassium cyanide solution has been established. The authors deter. mined cadmium in photographic films by this method with high sensitivity, precision and rapidity. Experimental error in the determination of standard samples was below 1%. The conditions recommended were: wavelength 2288 A, hollow cathode lamp current 6mA, slitwidth 1.0mm, acetylene flow 2.9l/min. and air flow 12.2l/mm.View full abstractDownload PDF (889K) -
Difference quantitative determination. IBunzo Tamura1967 Volume 16 Issue 3 Pages 193-205
Published: March 05, 1967
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSEquivalent point of neutralization reaction can be determined precisely by the use of an absorbance ratio (r) of a pH indicator which is defined as formula (2). A suitable indicator for each neutralization reaction with remarkable r change around equivalent point is selected from Table I and Fig. 1, and the working curve is prepared by least square method as shown in Fig. 2, 4 and Table IV where x is the reciprocal of neutralization grade. The absorbance ratio may be replaced by a pH value of the solution. A definite (V') ml of standard solution is added (with a whole pipette) to the sample, and the theoretical volume V is obtained from formula (1) and the working curve.
The method was applied to the determination of ammonia in semimicro Kjeldahl's, and the standard deviation (0.11%) was much smaller than that (0.27%) of usual method. Similar comparisons were carried out with aminopyrine and disodium succinate, and 0.07% comparing to 0.38% and 0.07% to 0.19% were obtained, respectively. In the latter case, moreover, the period of analysis was much reduced to 1/6.
The method is suitable for official quantitative analyses of drugs, reagents, food additives etc.View full abstractDownload PDF (1394K) -
Giichi MUTO, Yoshinori TAKATA, Akira TACHIKI1967 Volume 16 Issue 3 Pages 206-210
Published: March 05, 1967
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA procedure for analyzing thin layers of goldalloys on copper plate was developed by combining an anodic dissolution sampling method and a controlled potential coulometry. The samples were dissolved into 1M KCN solution, and from the same electrolyte were deposited silver at -0.90V vs. S. C. E. and gold at -1.60V to the mercury working electrode. The amount of copper was calculated from the difference between the quantites of electricity for the anodic dissolution and those for the electrodepositions of silver and gold. This procedure allowed analyses to be performed with total electrolysis times of about 1 hour and with precision of less than several percents.View full abstractDownload PDF (751K) -
structure of fragment ionsMasahiko TSUCHIYA, Shinya MATSUHIRA, Satoshi ISHIDO1967 Volume 16 Issue 3 Pages 210-216
Published: March 05, 1967
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSMass spectrometry is a useful method for the structure determination of organic compounds. But, in many cases, several fragment ions with different structures give peaks at the same mass number and the interpretation of mass spectrum is not easy. It was thought possible to determine the structure of a fragment by mass numbers and intensities of several peaks related to it, not by that of only one peak. According to this conception, fragments having a relatively large peak at mass (59) were selected from mass spectra of oxygen-containing compounds among about 3200 organic compounds and the result was shown in tables of structural significance of fragments at mass (59). By these tables, the structure of fragments at mass (59) seems almost to be deduced from 25 other peaks such as those of (43), (31), (29) etc., although many of these peaks do not correspond to ions through simple cleavage. As we had already noticed that mass spectrum at low-energy bombardment (25 eV higher than the ionization potential of a compound) was useful to know which peaks were more important, the effect of electron energy on mass spectrum was also investigated and shown in tables. How to determine the structure of a fragment or a compound by these tables was also described. The tables also give a number of informations concerning dissociation mechanism of a molecule by an electron impact.View full abstractDownload PDF (1235K) -
Tsuyoshi NOMURA, Genkichi NAKAGAWA, Tsurumatsu DONO1967 Volume 16 Issue 3 Pages 216-222
Published: March 05, 1967
Released on J-STAGE: May 07, 2010
JOURNAL FREE ACCESSA copper metal electrode can be used as an indicator electrode for the potentiometric titration of various metal cations with EDTA or tetraethylenepentamine.
A small amount of copper ion is added before the titration to establish a reversible potential with the copper electrode, and it is necessary to remove the dissolved oxygen by bubbles of nitrogen through the solution during titration. The concentration of copper ion in solution and hence the potential of the copper electrode change sharply at the equivalence point of titration.
In the case of titration with EDTA, Bi, In and Th are titrated directly at pH about 2.5 with a monochloroacetic acid medium. Pb, Cd, Co, Mn and Zn are titrated at pH 4 to 6 with an acetate medium, and Ca and Sr are titrated at pH about 8 with a borate medium.
In the case of titration with tetraethylenepentamine, Pb forms with the titrant a complex less stable than Zn and/or Cd, and Cd can be determined selectively in the presence of a 10 fold excess of Pb by the potentiometric titration in an acetate medium (pH=6.5).View full abstractDownload PDF (1133K) -
Studies on spectrochemical analysis of semiconductor materials. IIIShigeru OTSUKA, Shunsuke MATSUOKA1967 Volume 16 Issue 3 Pages 222-229
Published: March 05, 1967
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA simple, rapid and precise method for the spectrographic determination of germanium, gallium and aluminum in indium-germanium-aluminum alloys has been developed. In the recommended procedure, the indium alloy sample solution was dissolved in nitric-phosphoric acid. Sodium hydroxide was added as a spectroscopic buffer and the solution was diluted with water to give a final alloy concentration. The solution was subjected to the spectrographic procedure with a modified quenched-electrode technique and an intermittent a. c. arc excitation.
With indium as an internal standard, a coefficient of variation of the present method was within 5 per cent for each element to be determined in the concentration range of 30600μg per ml.View full abstractDownload PDF (1405K) -
Katsumi YAMAMOTO, Kôhei AMETANI, Kiyohisa AMAGAI1967 Volume 16 Issue 3 Pages 229-233
Published: March 05, 1967
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA Spectrophotometric method for the determination of chromium (VI) and vanadium (V) based on the oxidation of 8-aminoquinoline with chromium (VI) and vanadium (V), respectively, is described.
The oxidation takes place in aqueous solution at pH 2.4 to 2.8 in case of chromium and at pH 1.8 to 2.4 in case of vanadium. The oxidation is accelerated by moderate warming in a water bath.
The soluble oxidation product obtained is extracted into a 1:1 mixture of benzylalcohol and chloroform at pH 1.8. The absorbance is measured at 550mμ, and it is possible to determine 10100μg chromium in 50ml and 3120μg vanadium in 50ml of aqueous solution. The sensitivities of the determination are 0.0025μg chromium per cm2 and 0.0048μg vanadium per cm2.View full abstractDownload PDF (830K) -
Tsuneo SHIMIZU1967 Volume 16 Issue 3 Pages 233-238
Published: March 05, 1967
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSScandium reacts with NAS [7-(6-sulfo-2-naphthylazo)-8-hydroxyquinoline-5-sulfonic acid] to give a complex at pH 4.1 to 6.3. The colored solution has an absorption maximum at 420 mitt. Beer's law is obeyed over the range 0.4 to 3. 6ppm of scandium. Molar extinction coefficient at 420mμ is 8×103. The absorbance is not highly sensitive to reagent concentration and pH. The complex remains stable for an hour. Many cations interfere, but can effectively be separated from scandium by ion exchange methods enough to permit the spectro photometric determination of scandium with NAS. The ion exchange methods consist of cation and anion exchange in acid sulfate media and anion exchange in hydrochloric acid solution. The presence of 1: 1 complex is confirmed by spectrophotometric, conductmetric and potentiometric studies.View full abstractDownload PDF (1027K) -
Shingo MIYAKE, Isao SAKAMOTO1967 Volume 16 Issue 3 Pages 238-242
Published: March 05, 1967
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe authors had previously presented an automatic potentiometric titrator, in which a complete titration curve is recorded stepwise. Now, they have constructed a simple monochromatic photometer that can be attached to the titrator for the purpose of recording photometric titration. The instrument involves a reflect-type diffraction grating to produce a spectrum, and CdS photoconductive cells as the detector. The useful range of wavelength is 400800mμ with effective band width about 10 mμ. The titration curve is represented as a curve of transmittancy, not of absorbancy, against volume of titrant added. The end point of titration is determined from the curve of transmittancy, and the error in the end point detemination is either negligible or readily compensated, if the titration is carried out so as to its end point has transmittancy higher than 60%. They are examined through some typical titrations.View full abstractDownload PDF (960K) -
Naoharu YAMAGUCHI, Shun ARAKI1967 Volume 16 Issue 3 Pages 243-247
Published: March 05, 1967
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA new method for determination of small amounts of carbon in iron and steel has been investigated. Samples were burned in a combustion tube with open ends. Carbon dioxide formed was introduced into a thermal conductivity cell by pumping system, and its signal was recorded by a pen recorder. Because of an opening combustion system, samples could be inserted and exchanged easily and rapidly. The analysis took approximately 5 minutes and a blank value was lower than 9μg of carbon. The limit of detection in this experiment was 3μg of carbon, which was equivalent to 2ppm in a 2g sample. The proposed method is suitable for the routine determination of small amounts of carbon.View full abstractDownload PDF (902K) -
Studies on the hydroxyl derivatives of chromone as analytical reagents. IIIAkira MURATA, Tetsuo SUZUKI1967 Volume 16 Issue 3 Pages 248-250
Published: March 05, 1967
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSBeryllium reacts with 5-hydroxychromone above the pH ca. 5 to give a yellow water-insoluble complex which can be extracted by a variety of organic solvents. When the complex is extracted with benzene from an aqueous solution at a pH of 7.08.0, the absorbance is measured at λmax 398 mμ. Factors affecting the spectrophotometric determination, e.g., organic solvents, pH, concentration of reagent, volume of aqueous phase, time of shaking, stability and foreign ions, were discussed. Analytical procedure is as follows. To a sample solution containing up to 9μg of beryllium, are added 2ml of 0.3% methanol solution of the reagent and 5 ml of buffer solution (sodium boratehydrochloric acid, 0.075M in sodium borate) to maintain the pH of 7.07.5, and it is made up to 25ml with water. To this is added 10ml of benzene, and after the vigorously shaking for about one minute, the extract is dried over anhydrous sodium sulfate, and the absorbance it mesured at 398mμ. An analytical curve is rectilinear. Al3-, Pd2+, Fe3+, Cu2+ and Ti4+ give a positive error, however In3+, Tl3+, PO3-4 and F- a negative one.View full abstractDownload PDF (461K) -
Ryozô NAKAGAWA1967 Volume 16 Issue 3 Pages 250-253
Published: March 05, 1967
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSTrace element, especially arsenic, in free sulfur has a serious effect upon the characteristics of the products. The amounts of the trace element are conventionally determined by chemical methods including the ashing procedure and the wet oxidation decomposition, which are time consuming and troublesome as routine works in the quality control. A spectrochemical method has been presented by the author for the determination of arsenic, antimony and tellurium in native sulfur without chemical separation by direct current arc with an auxiliary boiler-cap graphite electrode.
Prior to the arcing, sulfur powder is mixed with an equal amount of graphite powder containing 14.4% germanium dioxide as an internal standard.
The excitation conditions are as follows: arc current 5 A at D. C. 315 V and 25 seconds exposure.The line pairs of As I 2349. 84/Ge I 2327. 90, Sb I 2311. 47/Ge I 2314. 20 and Te I 2385. 76, Ge I 2379. 14 are used.
The lower determination limit is 1 ppm for arsenic, antimony and tellurium. The standard deviation in this method was below 12 percent.View full abstractDownload PDF (660K) -
Nobuyoshi YAMAGUCHI, Akihisa HATA, Minoru HASEGAWA1967 Volume 16 Issue 3 Pages 253-255
Published: March 05, 1967
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA simple and rapid determination method for calcium in ferro silicon by chelatometric titration has been established.
A half g of sample is decomposed with nitric acid and hydrogen floride, and white fume is emitted by the addition of hydrogen perchloride. The acid concentration is adjusted with hydrochloric acid methylisobutylketon is added to it for the seperation of iron and other metals. With ammonia water and bromine water, aluminum, titanium and manganese are seperated. To the filtrate, triethanolamine, sodium cyanate and sodium hydroxide are added to adjust the pH at 12.513.0, and then calcium is tritrated with EDTA standard solution.
No influence is given upon the existence of 3% and less of Al, and also 0.4% and less of Ti, Cr, Cu and Ni.View full abstractDownload PDF (601K) -
Analyses of drugs and chemicals by infrared spectroscopy. XVINaobumi OI, Eiji INABA1967 Volume 16 Issue 3 Pages 255-257
Published: March 05, 1967
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSAlthough sodium lauryl sulfate is little soluble in organic solvents for IR determination, high molecular weight amine is attempted to utilize for the solvent extraction method and employment has been found to be applicable as a new determination method by solution method. A quantitative extraction with 5% CS2 solution of Amberlite LA-2 is found to be capable, followed by the determination at 1194cm-1 as a key band. By this method, even if sodium chloride, sodium sulfate and Tween 40 are present in an equivalent amount to sodium lauryl sulfate, they will not interfere with the determination, and in the case of coexistence of sodium lauryl benzene sulfonate, both components are determined quantitatively at 1250cm-1 and 1164cm-1, key bands, respectively as a binary system.View full abstractDownload PDF (571K) -
Analysis of drugs and chemicals by infrared spectroecopy. XVIINaobumi Oi, Hiroshi TAKEDA1967 Volume 16 Issue 3 Pages 257-259
Published: March 05, 1967
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSAn attempt was made to apply the solvent extraction methods by using high molecular weight amine to the IR analysis of water soluble mono-and di-thiophosphoric acid ester. Both O, O-dimethylthiophosphoric acid and O, O-dimethyldithiophosphoric acid are found to be effective for the qualitative analysis, being extractable with 5% of CS2 solution of Amberlite LA-2, and the latter O, O-dimethyldithio compound is found to be applicable also as a quantitative method. As to "Sumithion" and "Malathion", one of the effective organophosphoric insecticides, solvent extraction was carried out with the hydrolyzed water solution and the presence of O, O-dimethylthiophosphoric acid and O, O-dimethyldithiophosphoric acid have been identified.
This method has been proved to be applicable to the investigations of hydrolytic mechanism and partial structures of thiophsphoric acid ester series of insecticides.View full abstractDownload PDF (468K) -
Akira NONAKA1967 Volume 16 Issue 3 Pages 260-261
Published: March 05, 1967
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSSteam can be used as the carrier gas for gas-solid adsorption chromatography so that mixtures of alcohols and organic acids are separated without any marked tailing. A crushed diatomaceous fire brick containing a little phosphoric acid and activated alumina serve as good adsorbents for alcohols, ketones and esters and for hydrocarbon mixtures, respectively. Use of the steam as the carrier gas may considerably extend the applicability of adsorption gas chromatography. Water-containing samples can also be subject to the analysis without any difficulty. Even the separation of 0.5ppm C1C4 alcohols in aqueous solution can be achieved in this way.View full abstractDownload PDF (246K) -
[in Japanese]1967 Volume 16 Issue 3 Pages 262-265
Published: March 05, 1967
Released on J-STAGE: June 30, 2009
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[in Japanese], [in Japanese]1967 Volume 16 Issue 3 Pages 266-273
Published: March 05, 1967
Released on J-STAGE: February 16, 2010
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[in Japanese]1967 Volume 16 Issue 3 Pages 274-282
Published: March 05, 1967
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESS -
[in Japanese]1967 Volume 16 Issue 3 Pages 283-288
Published: March 05, 1967
Released on J-STAGE: June 30, 2009
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[in Japanese], [in Japanese]1967 Volume 16 Issue 3 Pages 294-295
Published: March 05, 1967
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSDownload PDF (320K)
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