Journal of the Mass Spectrometry Society of Japan
Online ISSN : 1880-4225
Print ISSN : 1340-8097
ISSN-L : 1340-8097
14 巻, 4 号
選択された号の論文の9件中1~9を表示しています
  • 千田 勝久, 金子 粂太郎, 坂井 光夫
    1966 年 14 巻 4 号 p. 149-156
    発行日: 1966/10/01
    公開日: 2011/03/01
    ジャーナル フリー
    Studies of direct deposition of decelerated ions from an isotope separator on thin foils were reported. Fundamental behavior of decelerated ions was investigated by measurement of ion currents to various electrodes placed in the collector part. A magnetic field of 1000 gauss produced by a permanent maghet was set in the place of decelerating electric field, so that one can measure. the ion current without electron contamination and avoid accelerated electrons from bombardingthe target. The attachment efficiency was studied as a function of final energy of ions, backing materials and their thickness. From these studies, optimum working conditions for obtaining good deposition were obtained. The ion beam used in the present experiments was that of Mg24 and the backing materials were Au, Cu, Ni and Ta foils.
    As examples, Mg24 with a thickness of 500μg/cm2 was obtained on a Au foil of 5 μ thickness with a current density of 30 μA/cm2 and Mg24 with a thickness of 300 μg/cm2 was obtained on a Au foil of 0.5 μ thickness with a current density of 20 μA/cm2.
  • 疋田 強, 土屋 荘次, 末安 重明, 石原 福三郎, 藤井 信行, 田巾 千禾夫, 山口 文衛
    1966 年 14 巻 4 号 p. 157-176
    発行日: 1966/10/01
    公開日: 2010/06/28
    ジャーナル フリー
    Characteristics of the Time-of-Flight Mass Spectrometer Hokushin Model 12(Bendix Model 12-100)have been discussed by the experiment, The important findings and conclusions obtained here are as follows;(i)The space charge in the ionization chamber is very small owing to the fact that neutral atomsor molecules are ionized by the pulsed electron beam. Therefore, the linearity between the ion and the electron trap current is very good except the case of ions whose m/e is smaller than 4.(ii)The characteristic curve of the electron trap current against the electron energy shows an abnormal point at 20 eV of the electron energy; that is, the electron trap current does not increase linearly with the bias voltage of the electron control grid.(iii)It is ascertained by the observation of the time of flight of ions that the flight path of ion is not strictly linear especially in the case of ion of small m/e. This is perhaps due to the existence of the collimating and compensating magnet. However, the time of flight of ion is close to the value calculated theoretically.(iv)The mass resolution has been determined to be about 140 by the measurement of the spectral line width, which increases almost linearly with m/e.(v)The, spectraline of CH3+ion in the spectrum of propane is found to be composed of three peaks, in which two peaks can be assigned to CH 3+ion having an excess kinetic energy.(vi)The absolutesen sitivity gradually decrease after the suppply of the high voltage to the electron multiplier. This phenomenon results in a serious effect on the accuracy of the quantitative analysisby this mass spectrometer.(vii)The cracking pattern coefficients obtained here are almost the same as the ones of A. P. I. The reproducibility is, however, slightly worse than that of the magnetic type mass spectrometer.(viii)The n-and iso-butane mixture of known composition has been analyzed by this mass spectrometer and the mean deviation is 1.5%.(ix)The reproducibility of mass spectrum on the synchroscope depends on the mean number of ions in the ionization chamber. In the present case, the fluctuation of peak intensity is about 20% at 104 ions in the ionization chamber. It has been considered for this problem that there must be some reasons other than the statistical fluctuation of ionization by the electron impact.
  • M. OZIMA, M. GOTO, Y. OGATA, T. SUZUKI
    1966 年 14 巻 4 号 p. 177-182
    発行日: 1966/10/01
    公開日: 2010/06/28
    ジャーナル フリー
    The operation characteristics of a pyrex tube mass spectrometer which was particularly designed for the analysis of very small amount of argon for K-A radiometric dating method is described. The mass spectrometer has very low background: there are no observable background peaks in m/e=36 and 38 and the background in m/e=40 is less than 10-14 ampere during a static operation.
    The minimum amount of argon which can be detected by the present apparatus is about 5×10-9cc STP. By means of isotope dilution method, the mass spectrometer can be used for the determination of radiogenic argon of as small as 10-6 cc STP with the precision of ±5% or less and is suitable for the K-A radiometric dating of very young rocks.
  • 酒井 均, 本間 弘次
    1966 年 14 巻 4 号 p. 183-186
    発行日: 1966/10/01
    公開日: 2011/07/05
    ジャーナル フリー
    A method is described to obtain carbon dioxide from oxygen gas which is extracted by a fluorine decomposition technique from silicate and oxide minerals for the isotope analysis of oxygen. The method is a modification of that described by Taylor and Epstein. A small piece of spectrographic graphite is heated externally in a quartz tube and oxygen is carefully combusted to carbon dioxide, the latter being quickly condensed into a liq.-nitrogen trap near the heated graphite(Fig.1). The yield of carbon dioxide is nearly 100 per cent in the range of temperature examined(440 to 580°C)and the isotope analysis of oxygen can be performed with accuracy of less than 0.2 per mil(Table 2).
    It is also shown that the kinetic isotope effect of oxygen in the combustion process is as large as 2.2 per cent at 500°C (Table 3 and Fig. 2) . A preliminary discussion is made for the reaction mechanism of the process.
  • TOSHIO SUGIURA, KAZUO ARAKAWA, AKIRA MATSUMOTO
    1966 年 14 巻 4 号 p. 187-200
    発行日: 1966/10/01
    公開日: 2011/03/01
    ジャーナル フリー
    Utilizing a conventional electron gun and mass spectrometer, the formation of negative ions at wide electron energies(0 to 100 ev)have been investigated for an acrylonitrile. The ionization efficiency curves have been obtained for the negative ions including C-, CH-, C2-, C2H-, CN-, HCN-, C3-, CCN-, CHCN-, C2CN-, C2HCN-and C2H2CN-. The appearance potentials of these negative ions have been determined for both processes of the dissociative resonance capture and ion-pair production, and some of the ions have two or more appearance potentials in each processes. The O-ions produced from O2 and CO were used for an energy calibration establishing the appearance potentials, and SF6-ions from SF6 were also used on energy calibra tion for the electron energy near zero ev. The pressure effects of the formation of these negative ions have been studied in various electron energies over the whole pressure ranges(presumably from10-4to 10-7 mmHg in the ionization chamber). From the studies of the pressure effects the negative ion formation, it has been observed that the intensities of the negative ions produced by the processes of all dissociative resonance capture were increased lineary for pressure increased, but on the other hand the processes of the ion-pair production indicated more complicated depen dency, that the dependencies of the ion intensity on the pressure have various mode among the ions from 1st to 4th order against the pressure. Possible explanations of the formation mechanisms of the negative ions are discussed.
  • 立松 晃, 中田 尚男, 中島 康雄, 津山 斉, 土井 紘
    1966 年 14 巻 4 号 p. 201-208
    発行日: 1966/10/01
    公開日: 2010/06/28
    ジャーナル フリー
    The mass spectral fragmentation patterns of methyl p-aminosalicylate were examined with the aid of high-resolution mass spectrometry. The conventional spectrum of this compund is shown in Fig. 1, and several meta-stable ion peaks(Table 1)indicate the presence of two fragmentation pathways(Fig. 2). The accurate masses of each peak were measured by the peakmatching technique with suitably chosen standard substances. i)m/e 167 Ion(Molecular Ion): In order to test the reliability of the present method, the m/e167 peak(Fig. 3)of methyl p-aminosalicylate was compared with the corresponding peak of anthracene(Figs. 4A and 5A)and of stilbene(Figs. 4B and 5B). The observed and the calculated masses of the peak agree satisfactorily. ii)m/e 136 and 135 Ions: The high-resolution spectrum(Fig. 6)reveals that each peak consists of a single fragment ion. By using phenylacetic acid(Fig. 7)as an internal standard, the elemental composition of the peaks was established as follows(Fig. 8): m/e 136, C7H6NO2(M-CH3O), m/e 135, C7H5NO2(M-CH3OH). The fragmentation pathways are depicted in Eqs.1 and 2, respectively. iii)m/e 108 and 107 Ions: From comparisons of the peaks(Fig. 10)to those of phenacetin (Figs. 9 and 11)and of o-xylene(Figs. 12 and 13), the major fragment ions at m/e 108 and 107 were proved to be C6H6NO and C6H5NO, respectively. The fragmentations are not very simple and the formulations(Eqs. 3 and 4)are still tentative. iv)m/e 80 and 79 Ions: The composition of principal ions in Fig. 14 was determined with l-menthol(Fig. 15)as an internal standard. Both peaks were shown to be-13-14m. m. u. lower than the standard peaks(Fig. 16), and this results lead to the composition of C5H6N for m/e 80 and C5H5N for m/e 79 ions(Table II). Formations of these ions are rationalized in Eqs. 5 and 6. v)m/e 53 and 52 Ions: By the similar manner it was found that these ions are hydrocarbon fragments. Naphthalene was selected as a standard. Finally, elemental compositions of major fragment ions of methyl p-aminosalicylate are listed in Table III and the fragmentation pathways are summarized in Fig. 17.
  • 大島 昌三, 藤井 勤也, 中井 元康
    1966 年 14 巻 4 号 p. 209-214
    発行日: 1966/10/01
    公開日: 2010/06/28
    ジャーナル フリー
    The mass spectrometric analysis was devised to analyse quantitatively aromatic hydrocarbons and thiophenic sulfur compounds separated from the aromatic fraction in high boiling range of petroleum. Thiphenic sulfur compounds in sample were oxidized to sulfons by hydrogen peroxide treatment and the oxidation mixture was separated sulfon fraction and hydrocarbon fraction by liquid chromatography. Aromatics in hydrocarbon fraction were analyzed by the mass spectrometry low voltage ionization method. Sulfon fraction was reduced to thiophenic sulfur compounds by ithium aluminum hydride treatment, and the thiophenic sulfur compounds were analyzed by the mass spectrometry of low voltage ionization method
  • 平松 勤司
    1966 年 14 巻 4 号 p. 215-224
    発行日: 1966/10/01
    公開日: 2010/06/28
    ジャーナル フリー
    Mass spectrometric study was carried out in the analysis of gaseous mixtures produced by the pyrolysis of wood components under various conditions. Following compounds were detected as pyrolytic products: hydrogen, carbon monoxide, carbon dioxide, methanol, ethanol, acetone, methyl ethyl ketone, dimethyl furan, methyl furan, acetic acid, acetaldehyde, methane, acetylene, ethylene, ethane, propane, propylene, butene, butane, water, benzene and toluene. As a result of the pyrolytic studies under varying conditions, it was found that the composition the pyrolytic product mixture was greatly influenced by the pyrolysis temperature and duration. The results of the present work suggest that most of the aromatic compounds are produced by the pyrolysis of lignins. From the result of this work, mass spectrometry seems to be an effective method for the analysis of the pyrolysis product of wood components.
  • 立松 晃
    1966 年 14 巻 4 号 p. 225-237
    発行日: 1966/10/01
    公開日: 2010/06/28
    ジャーナル フリー
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