Journal of the Mass Spectrometry Society of Japan

Mass Spectrometry of the Neutral Constituents of the Upper Atmosphere

ALFRED O. NIER

1967 Volume 15 Issue 2 Pages 67-81
Published: June 25, 1967
Released on J-STAGE: June 28, 2010

DOIhttps://doi.org/10.5702/massspec1953.15.67

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A discussion is given of problems which arise in using rocket-borne mass spectrometers to determine the composition of the atmosphere at altitudes above100km. A description is given of a magnetic deflection instrument which has been used. Some of the results obtained are discussed.

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A Mass Spectrometer for Ultra Trace Gas Analysis

HITOSHI TSUYAMA, JUNICHI OKAMOTO, TAKESHI KOIKE, NOZOMU MORITO

1967 Volume 15 Issue 2 Pages 82-94
Published: June 25, 1967
Released on J-STAGE: March 01, 2011

DOIhttps://doi.org/10.5702/massspec1953.15.82

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A mass spectrometer for the analysis of ultra trace samples of gases, particularly noble gsaes, is described. The mass spectrometer is 90°-sector type and its ion trajectory radius is 200mm. Its main parts are made of stainless steel. The vacum system is extremely clean and easily maintainable. The evacuating system includes a molecular pump or a 3″oil diffusion pump (Apiezon oil C). By 48 hours evacuation and thorough bakeout, the ultimate pressure of the analyser in the order of 10^-9mmHg is attainable. The instrument may be operated in the static mode and the detailed procedure is described. The incremental characteristics of back ground peaks and the diffused peak of argon at M_A=80 were investigated. Fission product isotopic rare gases and isotopic ratios of uranium were determined.

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Isotope Analysis of Oxygen in Rocks and Minerals II. KHF2-CoF3Method for the Liberation of Oxygen from Silicate-and Oxide-Minerals

H. SAKAI, H. HONMA

1967 Volume 15 Issue 2 Pages 95-103
Published: June 25, 1967
Released on J-STAGE: June 28, 2010

DOIhttps://doi.org/10.5702/massspec1953.15.95

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A new technique was described for the liberation of oxygen from various rock-forming minerals by which the samples are decomposed in the fused flux of KHF₂ with CoF₃ as an oxydizing agent. The liberated oxygen was converted to carbon dioxide by a graphite furnace for the mass spectrometric analysis of the oxygen isotope ratio. The technique has been satisfactorily applied to magnetite and olivine as well as to quartz. In the case of olivine, which is the most resistant to the decomposition among the three minerals, the yield of oxygen close to 100% was obtained within 10 hrs. reaction at 380°C.
δ¹⁸O_ow values, the isotope ratios of oxygen in the absolute mean oceanic water scale, found for a magnetite from a granodiorite, for an olivine from a peridotite and for a quartz from a pegmatite were -1.3±0.3, +3.6±0.3 and +12.0±0.9⁰/00, respectively. These values are in fair agreement with those reported by other investigators for the minerals of the similar occurrences.
It was also shown that the liberated oxygen tends to be enriched in the heavy isotope when the sample is only partially decomposed. This and other factors which bring serious errors into the final isotope measurements were discussed.

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Mass Spectra of Proaporphine Type Alkaloids and Their Derivatives

MASAO TOMITA, AKIRA KATO, TOSHIRO IBUKA, HIROSHI FURUKAWA, SHOZO ASADA ...

1967 Volume 15 Issue 2 Pages 104-111
Published: June 25, 1967
Released on J-STAGE: June 28, 2010

DOIhttps://doi.org/10.5702/massspec1953.15.104

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Mass spectra have been measured for typical members of the proaporphine type alkaloids and of the hydroproaporphine series, containing a spirocyclohexane moiety. Assignments have been made to the principal fragments, and the fragmentation mechanisms are proposed on the basis of the existence of metastable peaks and the mass spectrometric shift technique.

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The High-Resolution Mass Spectrum of Barbital

HISAO NAKATA, AKIRA TATEMATSU, HITOSHI TSUYAMA, HIROSHI DOI

1967 Volume 15 Issue 2 Pages 112-121
Published: June 25, 1967
Released on J-STAGE: June 28, 2010

DOIhttps://doi.org/10.5702/massspec1953.15.112

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The mass spectral fragmentation patterns of barbital (diethylbarbituric acid) were studied by using the high-resolution mass spectrometry. As is shown in Fig. 1, barbital exhibits several characteristic peaks correlated each other by the existence of meta-stable ion peaks (Fig. 2) .
The accurate masses of apeak at m/e156 were determined by the peak-matching technique with an M+2 peak of diphenyl as a standard (TableI) . Peaks at m/e 155, 141, 112, and 83 were examined in the similar manner with suitably chosen standard substances, and the results were summarized in Table II.
Elemental compositions of the main fragment ions of peaks at m/e 98, 70, 69, 55, 44, and 41 were assigned from comparison of allowed atomic combinations with the number of observed peaks (Fig. 3-8, Table III-VIII). Fragment ions and fragmentation sequences of barbital were represented in Fig. 9.
Plausible mechanistic formulations of each fragmentation step were depicted in Eq. 1, 2, 3, 4, and 5, respectively. It was noted that the interconversion of keto-and enol-forms of M-28 ion(m/e156)(Eq. 6)was not possible in a mass spectrometer.

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Organic Mass Spectrometry

AKIRA TATEMATSU

1967 Volume 15 Issue 2 Pages 122-134
Published: June 25, 1967
Released on J-STAGE: June 28, 2010

DOIhttps://doi.org/10.5702/massspec1953.15.122

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