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Volume 17 (1969)
- Issue 4 Pages 798-
- Issue 3 Pages 685-
- Issue 2 Pages 589-
- Issue 1 Pages 426-
Volume 17, Issue 3
Displaying 1-9 of 9 articles from this issue
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SATORU MATSUMOTO1969 Volume 17 Issue 3 Pages 685-704
Published: September 01, 1969
Released on J-STAGE: June 28, 2010
JOURNAL FREE ACCESSWhen there are many doublets of the same ion species, of which fractional mass difference is ro, it is possible to construct consistent artficial mass scales in terms of ro by only position measurements of these doublet lines. With one of these mass scale, the author studies on two possibilities of the mass calibration method suitable for a very high dispersion type mass spectrograph without any sacrifices for precisions of calibrations, which are, at least, the same order of magnitude for those of a single doublet separations, …the general mass center and the doublet scaling method. The former is rather useful for estimations dispersion constants α1 and α2 which are main contributions to the correction terms in an artificial mass scale. Preliminary experimental studies on the latter method are carried out to a few spectra photographed with the Bainbridge-Jordan type apparatus, though these spectra are rather unsuitable even for the preliminary analyses. The doublet scaling method would be a proper mass calibration method for spectra on a photographic plate.View full abstractDownload PDF (1692K) -
H. NAKABUSHI, I. KATAKUSE, K. OGATA1969 Volume 17 Issue 3 Pages 705-731
Published: September 01, 1969
Released on J-STAGE: March 01, 2011
JOURNAL FREE ACCESSThe mass differences of(C2H4-CO), (C2H4-N2), (N2-CO)and(C2H4-C2D2)doublets have been measured. The apparatus used is the reconstructed large mass spectroscope of double focusing type with the cylindrical electric field(φe=84°50', ae=1092mm)and the uniform magnetic field(φm=60°, am=1200mm). The dimensions of main parts of this apparatus are quite similar to the old one destroyed by the high-tide typhoon in1961. The half-width resolution of about300, 000is obtained at routine operating condition(the slitwidth of about0.01mm for both main and detector slits). The stabilizing circuits were inserted in the power sources of both the electro-static analyzer and the magnetic one, and the emission stabilizer in the ion source circuit. As the result, the drift of ion beam is reduced to a few parts in 107 per minute, and the good reproducibility of the operation is obtained. Under such operating conditions, the measurements of(C2H4-CO), (C2H4-N2)and(N2-CO)doublet mass differences were performed with the visual orthodox peak matching method. by changing the measuring procedures which may be the causes of systematic errors. On the way of the measurements, a considerable large systematic error was found. This error came from the exciting current of the switching relay coil used for the peak matching. The estimations of the magnitudes of expected systematic errors were done. Moreover, using the closure error of the triplet derived from the mass differences of the above mentioned doublets, the correction factor for the measured values was calculated, and the mass differences corrected by this factor are adopted as the most reliable values. Finally, the doublet mass difference of(C2H4-C2D2) was measured.View full abstractDownload PDF (6037K) -
KIMITAKA SATO, RYO-ICHI SUZUKI, NAOHARU YAMAGUCHI, OHIKO KAMMORI1969 Volume 17 Issue 3 Pages 733-743
Published: September 01, 1969
Released on J-STAGE: June 28, 2010
JOURNAL FREE ACCESSA study was made of the influences of source parameters on ion intensities of various elements in a triggered DC spark source mass spectrometry, in order to apply the mass spectrometric method to the analysis of iron and steel. The experiment was carried out with a CEC#21-11OB type doublefocusing mass spectrograph equipped with a triggered DC spark source system. The source parameters observed are a sustain voltage(0∼800V), a triggered voltage(0∼3000V), a pulse length(0∼10μsec), a sustain capacitance(0.5∼20μF)and a frequency(10∼3000c/s). A sustain voltage is remarkably effective and ion intensities are abruptly varied in the voltage range between 400 and 600V, especially in an iron matrix sample. Generally, it was found that the amount of M2+ produced with this spark source system is greater than that produced with a R. F. spark source. The behavior of each element can be divided into two general classes: V, Cr, Mo and Nb are belong to one class, and As, Ga and Ag the other, whose characteristics depend on the second ionization potential of each element. Ion intensities are not varied by change of source parameters except a sustain voltage. A frequency is suitable as a variable parameter for regulating ion intensities. At the sustain voltage of 300V, the intensity ratio of M+/M2+ increases considerably in comparison with at that of 600V. Darkening curve gets out of parallel shape under a different source condition. Reproducibilities, on the whole, are 3∼30%for coefficients of variation which agree with those in the R. F. spark source system.View full abstractDownload PDF (911K) -
NORIAKI SASAKI, KENJI KUBO, MITSURU ASANO, SABURO MAGARI1969 Volume 17 Issue 3 Pages 745-753
Published: September 01, 1969
Released on J-STAGE: June 28, 2010
JOURNAL FREE ACCESSThe ionic species emitted from uranium dioxide on the tungsten and rhenium filaments by the surface ionization have been identified as UO2+, UO+ and U+. The ion of UO3+ could not be observed in any conditions. By measuring the ionic currents of 238U16O2+ and 238U16O+ the values of the heats of vaporization of UO2+ and UO+ have been estimated. The value of UO2+ changes at about 2230 °K for the tungsten filament and 2080 °K for the rhenium, respectively, and the values for the higher temperature range are larger than those for the lower range, irrespective of the filament materials. The thermoelectronic properties of uranium dioxide have been studied. The work function of the filament covered with the uranium dioxide changes at the specific temperature similarly to the ionic emission of UO2+. From the experimental data of the ionic emissions of UO2 and UO, and those of the thermoelectronic emissions, the heats of vaporization of uranium dioxide and monoxide molecules from uranium dioxide on the tungsten and rhenium filaments have also been calculated.View full abstractDownload PDF (795K) -
TETSUO NAGATA, SADAYUKI OKUDAIRA, YOZABURO KANEKO, ICHIRO KANOMATA1969 Volume 17 Issue 3 Pages 755-760
Published: September 01, 1969
Released on J-STAGE: June 28, 2010
JOURNAL FREE ACCESSIonization efficiency curves for Ca++, Sr++ and Ba++ near threshold have been studied with the crossed beam method. The difficulties arising from the thermal energy spread of the ionizing electrons are eliminated with the E. D. D. method which was proposed by Winters et al. The I. E. curve obtained for Ca++ has some structures above 24eV, and it increases steeply from 30eV. The shape of the curve agree well with the previous one by Kaneko and Kanomata except for gradually increasing portion above the threshold. In this portion, the present curve shows a linear rather than a second power dependence on the excess energy. The I. E. curve obtained for Sr++ has structures above 20eV, and increases steeply from 28eV. The present curve agrees with the previous one by Fayard et al. in the shape of curve but the absolute energy scale is a little shifted. The shape of the I. E. curve for Sr++ is similar to that of Ca++, and it is suggested that there are three different kinds of processes in the formation of Ca++ and Sr++ that is, direct ionization, autoionization and Auger ejection caused by ionization of 3p- or 4p- electron. The I. E. curve for Ba++ has no structures which can be related to the autoionization processes, although there exists a steep increasing from 20eV, which is attributed to Auger ejection caused by ionization of 5p- electron.View full abstractDownload PDF (571K) -
T. TAKAHASHI, Y. HAMADA, I. TAKEUCHI, A. TATEMATSU, H. NAKATA1969 Volume 17 Issue 3 Pages 761-765
Published: September 01, 1969
Released on J-STAGE: June 28, 2010
JOURNAL FREE ACCESSThe mass spectra of pyridyl phenyl ether(I)and three isomeric pyridyl tolyl ethers(II, III, and IV)are recorded and their fragmentations are discussed. In the spectrum of pyridyl phenyl ether(I)(Fig. 1), the formation of the M-1 peak at m/e 170 is accounted for by the fragmentation shown in Scheme 1. On the other hand, the accurate mass measurement indicated that the ion at m/e 143 corresponds to M-CO, and therefore, the ion would be formed by a mechanism depicted in Scheme 2. While the spectral features of p-and m-tolyl ethers(II and III)(Fig. 2 and 3)are essentially the same as those of I, the spectrum of o-tolyl ether(IV)(Fig. 4)exhibited a different fragmentation pattern. Thus, a very intense M-17 peak appeared but the M-CO peak was absent. A meta-stable ion peak at m/e 152.6 suggests a one step formation of the M-17(M-OH)ion from the molecular ion, and a probable pathway is shown in Scheme 3. The formation of both M-1 and M-15 ions from IV justifies the mechanism in Scheme 1.View full abstractDownload PDF (363K) -
TAKASHI SHIMA, MASAO NISHIKAWA, AKIRA OUCHIDA, YUTAKA ASAHI1969 Volume 17 Issue 3 Pages 767-772
Published: September 01, 1969
Released on J-STAGE: June 28, 2010
JOURNAL FREE ACCESSFragmentations of16derivatives related to thiamine were examined with the aid of high-resolution mass spectrometry, deuterium exchange and model compounds. The amine salts decomposed thermally to the free bases(M)whereas thiamine homologues gave M-H ions(a)lost the4'NH hydrogen. Further fragmentation from the ions(a)gave(a-SH)ions and 2-methylpyrimido[4, 5-d]pyrimidine. The CN bond of methylene bridge in thiamine homologues cleaves easily to form pyrimidylmethyl moieties, chloromethylpyrimidines and the other rings such as thiazole, thiothiazolone, imidazole, pyrazole, quinoline and pyridine. The base peak of thiazolium derivatives were due to the thiazole portion whereas those of tertiary amines examined were owing to the pyrimidines. Fragments of the pyrimidines undergo successive elimination of CH3CN, HCN or NH2CN. Fragmentations of the thiazole moieties and the model compounds(I, II)were interpreted that the substituents(CH3, CH2 OH), HCN, and CH, CN were eliminated successively to form fragments such as C4H5S, C3H3S, CH3CS, HCS, etc.View full abstractDownload PDF (436K) -
Food Additives(1). Analysis of Antiseptic Agents.AKIRA TATEMATSU, TANEKAZU NADAI, HIDEO YOSHIZUMI, TOSHIO GOTO1969 Volume 17 Issue 3 Pages 773-786
Published: September 01, 1969
Released on J-STAGE: March 01, 2011
JOURNAL FREE ACCESSMicrodetermination of antiseptic agents in drinks and foods by mean of mass spectrometry has been studied; some typical antiseptic agents(I-IX in Fig. 1)could be detected and characterized easily without such complicated separetions as described in Standard Methods of Analysis for Hygienic Chemists — with Commentary(authorized by the Pharmaceutical Society of Japan, 1965.). Even when a few antiseptic agents were contained in a drink or food, all of them could be characterized by measuring a mass spectrum of the mixture which was obtained simply by extraction of the acidified drink or food with ether. Lowering the ionizing potential made the characterization much easier.View full abstractDownload PDF (5894K) -
1969 Volume 17 Issue 3 Pages 796
Published: 1969
Released on J-STAGE: March 01, 2011
JOURNAL FREE ACCESSDownload PDF (41K)
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