巻号一覧
18 巻 (1970)
- 4 号 p. 1214-
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18 巻, 4 号
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鈴木 真言, 立松 晃1970 年 18 巻 4 号 p. 1214-1229
発行日: 1970/12/01
公開日: 2010/06/28
ジャーナル フリーPDF形式でダウンロード (1083K) -
TAKANOBU SHIOKAWA, KENJI YOSHIHARA, MASUO YAGI, TAKASHI OMORI, HARUMI ...1970 年 18 巻 4 号 p. 1230-1238
発行日: 1970/12/01
公開日: 2011/07/05
ジャーナル フリーThis report describes the specific features of the Tohoku Charge Spectrometer(TOHOKU CS)which has been constructed for the study of chemical effects of the nuclear transformations in gases, especially of the charge distribution of the residual atoms and of ion-molecule reactions in order to elucidate the primary and elemental stages in hot-atom chemistry. The facility is available for a chargespectrometer with a large source volume and a double mass spectrometer connected in perpendicular. Ions can be produced by the electron impact, X-ray irradiation or nuclear decay processes in the source volume. Charge spectrum of the residual atom after the Auger process of the nuclear decay can be measured through the first stage mass spectrometer, and products of ion-molecule reactions in the reaction chamber can be separated through the second mass spectrometer and detected by an aid of a16stages Cu-Be electron multiplier. Pulse countings are applicable in the both cases as well as direct current recordings to estimate the charged atoms or the fragment distribution. The specific availabilities of this facility are shown in some typical results by the preliminary experiments.抄録全体を表示PDF形式でダウンロード (690K) -
渡辺 稔, 楠 勲, 恩地 勝, 小寺 熊三郎1970 年 18 巻 4 号 p. 1240-1252
発行日: 1970/12/01
公開日: 2011/03/01
ジャーナル フリーOperation characteristics of the7-5-3-1cycle5-stage Bennett-type radio-frequency mass spectrometer(Bennett-type MS)with the secondary electron multiplier, designed for the square wave operation, was investigated in the pressure range from10-5to10-9Torr, simultaneously using the omegatron mass spectrometer as a reference. As the Bennett-type MS has many electrodes, the determination of relative electrode potentials for nice operation has been said difficult. In this investigation, however, getting the reference data with the omegatron mass spectrometer made it easy to determine the relative electrode potentials for obtaining good operation characteristics. The important factors of the Bennett-type MS operation are the voltage and the wave form of the applied radio-frequency, the drift voltages and the stability of the barrier voltage. As a result of the ion accelerating-voltage scanning method at a fixed radio-frequency, the ion background current wasincreased gradually in the high mass range. The reproducibility of the mass spectra obtained with the Bennett-type MS was satisfactory under the same conditions throughout the experiment. Even in the ultra-high vacuum conditions(-10-9Torr), Bennett-type MS can be used in the low mass range(1-10)without any significant ghost peaks though the operation in this mass range was difficult in the past, and can also be used up to the high mass range(-200). The minimum detectable partial pres sure was about10-13Torr and obtaining the resolution of50was relatively easy. The mass spectrum was also observed on the synchroscope screen in the range from10-5to10-9Torr. A so-called broad surface peak appeared around M=15was gradually predominant in the ultra-high vacuum region, and this peak could probably be due to the O ions produced from adsorbed CO on the tungsten grid surface under electron bombardment because of the inadequate structure of the ion source.抄録全体を表示PDF形式でダウンロード (2127K) -
GC-MSのデータ処理大島 昌三, 西下 孝夫, 小西 忠雄, 杉山 靖1970 年 18 巻 4 号 p. 1254-1258
発行日: 1970/12/01
公開日: 2011/03/01
ジャーナル フリーA data processing system of GS-MS having an excellent cost-performance was constructed by the introduction of the off-line system using an analog data recorder. HITACHI RMU-5B mass spectrometer was partially modified to process mass spectra, and the PDP-8/I digital computer with 8K core memory and the A/D converter was adopted. M/e values were calculated from the relations between mass number and time which is based on the He peak; then, there were no error to M/e300 during the operation of two monthes. Coefficient of variation of the pattern coefficient is about3to5%.抄録全体を表示PDF形式でダウンロード (415K) -
山口 直治, 鈴木 良一1970 年 18 巻 4 号 p. 1260-1269
発行日: 1970/12/01
公開日: 2011/07/05
ジャーナル フリーReproducibility of ion intensities, relative senisitivities of various elements by a spark source mass spectrograph were invesigated, and iron and steel were analyzed. Reproducibilities in repeated measurements with constant source parameters were5-35% in coefficients of variation, and in separate measurements6-70%. It seemed that inhomogeneity of emulsion and samples did not attribute to the fluctuation. Relative sensitivities(platinum was unity)of various elements in low alloy steel, nickel base temperature alloy, copper alloy, aluminum alloy, zinc base die casting alloy and stainless steel were 0.17-24.6. They were not related with sample materials, but with heat of sublimation of each element, however, some problems in reproducibility and measuring condition remain to be resolved. More accurate determination was performed by calibrating with relative sensitivities in analysis of standard samples stainless steel. Commercial pure iron was analyzed, and comparison with results in wet chemical methods was tried. The limit of detection was0.005 Reproducibility of ion intensities, relative senisitivities of various elements by a spark source mass spectrograph were invesigated, and iron and steel were analyzed.Reproducibilities in repeated meas urements with constant source parameters were5-35%in coefficients of variation, and in separate measurements6-70%. It seemed that inhomogeneity of emulsion and samples did not attribute to the fluctuation.Relative sensitivities(platinum was unity)of various elements in low alloy steel, nickel base temperature alloy, copper alloy, aluminum alloy, zinc base die casting alloy and stainless steel were0.17-24.6.They were not related with sample materials, but with heat of sublimation of each element, however, some problems in reproducibility and measuring condition remain to be resolved. More accurate determination was performed by calibrating with relative sensitivities in analysis of standard samples stainless steel. Commercial pure iron was analyzed, and comparison with results in wet chemical methods was tried. The limit of detection was0.005-1ppm.抄録全体を表示PDF形式でダウンロード (1677K) -
小森 卓二, 田村 修三, 郡司 勝文, 田村 公子1970 年 18 巻 4 号 p. 1270-1274
発行日: 1970/12/01
公開日: 2010/06/28
ジャーナル フリーA study has been made on the precise measurement of the isotopic ratio of uranium using a surface ionization mass spectrometer(CEC21-702B)equipped with an expanded scale recorder.By stabilizing the ion current and controlling the measuring conditions, such as sample mounting and filament heating, the relative standard eviation was improved to0.1%for observed 235U/238U ratio in a reference sample of uranium. Time variations of 235U/238U ratio during one run were investigated.抄録全体を表示PDF形式でダウンロード (1770K) -
ITSUO KATAKUSE, HIROMITSU NAKABUSHI, KOREICHI OGATA1970 年 18 巻 4 号 p. 1276-1292
発行日: 1970/12/01
公開日: 2010/06/28
ジャーナル フリーIn order to increase the measurement accuracy of the doublet mass differences, the digital readout method using a400-channel pulse height analyzer as a memory scope was adopted and the six methods finding out the mismatching degree of the doublet mass peaks displayed step-wise function f(X)channel number X were investigated. The true matching points obtained from six one seem to be good agreement compared to their associated errors. Under the condition of tbe half-height resolution of250, 000-500, 000, the mass differences of H35Cl-C3, H35Cl-C2D6and C3-C2D6doublets were measured. The results areΔM(H35Cl-C3)=23, 321.83±0.63ΔM(H35Cl-C2D6)=107, 934.90±0.54ΔM(C3-C2D6)=84, 611.60±0.34Combining those results and previously measured CO-N2, CO-C2H4andC2H4-C2D2mass differences the atomic masses of following ones are preliminary determined. D=2, 014, 101.933±0.057H=1, 007, 825.005±0.049 35Cl=34, 968, 851.70±0.64fromC2D6-H35ClandC2D6-C3or=34, 968, 853.17±0.64from H35Cl-C3 O=15, 994, 913.99±0.30N=14, 003, 073.78±0.14抄録全体を表示PDF形式でダウンロード (1848K) -
H.G.J.de Wilt, T. Tsuchiya1970 年 18 巻 4 号 p. 1294-1299
発行日: 1970/12/01
公開日: 2011/03/01
ジャーナル フリーPDF形式でダウンロード (628K) -
立松 晃, 福島 清吾, 野呂 忠敬, 斉木 保久, 上野 明, 赤堀 幸男, 中田 尚男1970 年 18 巻 4 号 p. 1300-1305
発行日: 1970/12/01
公開日: 2010/06/28
ジャーナル フリーThe mass spectra and fragmentations of several benzochromone derivatives, Ia-IIId, are discussed. For unsubstituted benzochromones, Ia, IIa, and IIIa, the expulsion of carbon monoxide and the retro-Diels-Alder(RDA)cleavage of their hetero rings were shown to be the two majior fragmentation pathways(Scheme1). The three mono-methoxylated derivatives, Ib, IIb, and IIIb, exhibited a strong M-15 peak that is attributed to the loss of a methoxyl methyl group from the molecular ion. For the compounds IIb and IIIb, this M-15 ion then undergoes an RDA clevage of the hetero ring to afford an intense peak at m/e 185, followed by the loss of carbon monoxide to give the m/e 157 ion(Scheme2). In the case of Ib, however, the M-15 ion gave an ion at m/e 169 with simultaneous loss of two carbon monoxide units(Scheme3). The stability of a respective ion appears to be responsible for these differences. On the M-15 peak was observed in the spectra of Ic, IIc and IIIc. This result is accounted for by assuming the localization of an ion radical at an ether oxygen atom in ther molecular ions. The fragmentations of Ic are shown in Scheme4. When the methoxyl group and the carbonyl group are in a peri-position, an intense M-CHO peak appears. The participation of the methoxyl group on this fragmentation is confirmed by the deuteriated derivative, IIIc-d3. dimethoxylated compounds, Id and IIId, showed M-CH3and M-CH3-CO peaks, while isomeric IId afforded M-CH3-CHO peaks. Their fragmentations are depicted in Scheme 5.抄録全体を表示PDF形式でダウンロード (374K) -
正田 芳郎, 橋本 圭二, 井上 武久, 正木 清孝1970 年 18 巻 4 号 p. 1306-1312
発行日: 1970/12/01
公開日: 2010/06/28
ジャーナル フリーThe use of volatile derivatives of3α-hydroxy-17-ketosteroids for gaschromatographic separation have been recomended. Mass spectra of3α-hydroxy-17-ketosteroids, trifluoroacetate and trimethylsilylether derivatives were investigated, and trimethylsilyl ether derivatives were found particularly suitable for combained gaschromatography and mass spectrometory.抄録全体を表示PDF形式でダウンロード (419K)
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