Journal of the Mass Spectrometry Society of Japan
Online ISSN : 1880-4225
Print ISSN : 1340-8097
ISSN-L : 1340-8097
29 巻, 3 号
選択された号の論文の10件中1~10を表示しています
報文
  • 田村 一二三, 石谷 亨, 泉 栄一
    1981 年 29 巻 3 号 p. 221-229
    発行日: 1981年
    公開日: 2007/05/01
    ジャーナル フリー
    For the purpose of obtaining meaningful depth profile information in secondary ion mass spectrometry (SIMS), a dynamic depth measuring method employing the total ion monitoring technique has been developed. It was evaluated for Si and GaAs speci mens under oxygen ion bombardment.
    This method utilizes the enhancement of secondary ion yield which results from the presence of implanted oxygen atoms. The implantation effect of oxygen ions was monitored by measuring the total ion intensity, together with the matrix ion signal, as a function of the sputtering time.
    From the experimental results it was found that the degree of enhancement is approximately proportional to the concentration of reactive oxygen implanted into Si and GaAs. That is, the etching depth at the saturated value of the total ion intensity corresponds to the projected range of the primary ions. This means that the etching depth during SIMS analysis can be measured with the scale of the sputtering time equivalent to the projected range.
  • 豊川 文敏, 菊地 正, 古谷 圭一
    1981 年 29 巻 3 号 p. 231-236
    発行日: 1981年
    公開日: 2007/05/01
    ジャーナル フリー
    Multi-built-up layers of barium (II) stearate on a copper substrate were investigated by a static SIMS apparatus equipped with a quadrupole mass spectrometer, and the experimental approach for quantitative SIMS analysis was discussed. Organic layers were built up by Langmuir-Blodgett method and impacted by 430 eV, 20 μA/cm2 Ar+ ions. Ba+, CnHm+ ions from barium (II) stearate and Cu+ ions from the substrate were detected. A variation of peak intensities of CnHm+ showed a complicate change as a function of bombardment time, while Ba+ and Cu+ peak intensities were exponentially decreased. It might be assumed that unexpected strong Cu+ ions sputtered off through multi-built-up layers are attributed to the bulky structure of the layers. A linear relationship was obtained between barium surface concentration and the maximum values of IBa+/(IBa++ICu+).
  • Hirohiko Ezoe, Kiyoshi Watanabe, Atsushi Hirose, Shoji Tanaka
    1981 年 29 巻 3 号 p. 237-247
    発行日: 1981年
    公開日: 2007/05/01
    ジャーナル フリー
    The surface ionization phenomena of Na- and K- compounds are studied by applying the samples directly on a tungsten ionization filament. The transient variations and the steady state characteristics of the ion emission seem to be due to the sample supply taking place by diffusion along the hot filament surface to the ionization spots, and hence it is supposed almost impossible to expect the precise quantitative mass analyses of sample compounds by means of the surface ionization of this sort.
  • 笹本 忠, 小林 迪夫, 佐多 敏之
    1981 年 29 巻 3 号 p. 249-255
    発行日: 1981年
    公開日: 2007/05/01
    ジャーナル フリー
    The vapor species of GeO, GeO2, Ge2O2, and Ge3O3 over germanium dioxide were observed by means of the Knudsen effusion mass spectrometric method. Among them the dioxide vapor, GeO2(g), was first detected and its partial pressure over the temperature range of 1180 to 1370°C was measured and expressed by the equation;
    log {p(GeO2, g)/atm} = 6.05 - (1.88 × 104/T)
    The 3-membered Ge-ring structure of Ge3O3 (g) was proposed to be more possible than the alternate 6-membered structure judging from the fact that the fragment ions of Ge3+ and Ge3O+ were detected and that the approximate molecular orbital calculation revealed the intrinsic stability of Ge3+ ion.
  • Kazuo Arakawa, Tadao Seguchi, Toshio Sugiura
    1981 年 29 巻 3 号 p. 257-265
    発行日: 1981年
    公開日: 2007/05/01
    ジャーナル フリー
    Negative ion-molecule reaction has been investigated for formic acid utilizing a conventional type mass spectrometer. At elevated pressure negative ions react with neutral species in the ion source of mass spectrometer. It was found that a negative ion of mass 91 is produced by the reaction of the HCOO- ion with neutral formic acid as
    HCOO-+HCOOH→HCOOHCOOH-
    This reaction has two processes, i.e. a dissociative resonance electron capture (DREC) process and a high energy electron process. From the studies of HCOOH gas pressure dependence it was observed that the intensities of the HCOO- and HCOOHCOOH- ions in a DREC process increase with first and second order of the HCOOH gas pressure, whereas in a high energy electron process, they increase with fourth and seventh order of the pressure, respectively. The reaction rate constants of two processes were determined as (6.8 ±1.5) ×10-13 cc/molecule.sec for a DREC process and (1.3 ±0.5) ×10-37 cc3/molecule3·sec for a high energy electron process.
  • Kenzo Hiraoka
    1981 年 29 巻 3 号 p. 267-275
    発行日: 1981年
    公開日: 2007/05/01
    ジャーナル フリー
    The reaction of C2H6+ with C2H6 was studied in a pulsed electron beam high ion source pressure mass spectrometer. Ethane at variable pressures in the 16—150 mTorr range in ~4 Torr hydrogen was used in experiments covering the temperature range from −145 to 400°C. Reaction: C2H6++C2H6 was found to have a rate constant k=10-6.6 T-1.5 whose magnitude decreased with temperature. The reaction proceeds via a (C4H12+)* intermediate, which at low temperature can be stabilized and becomes the major product. A very slow decrease of C4H12+ with time was observed at low temperature which was completely accounted for by an appearance and an increase of the trimer ion C6H18+. The two isomeric structures for C4H12+ are proposed in order to interpret the slow clustering reactions of C4H12+ with C2H6.
  • 代島 茂樹, 飯田 芳男
    1981 年 29 巻 3 号 p. 277-286
    発行日: 1981年
    公開日: 2007/05/01
    ジャーナル フリー
    To obtain useful CI mass spectra, several kinds of solvents with methane have been introduced into a Finnigan 3300E-GC/QMS CI ion source via its direct introduction portion by means of a micro LC pump for utilization as reagent gas. With solvent alone, the pressure of the ion source and the analyzer could not be kept under control at any condition, but addition of methane from the GC carrier gas line enabled the pressure to stabilize as well as increasing the reactant ion abundance by a several to ten fold magnitude or even more. The optimum ion source condition for this method was as follows, solvent flow rate: 0.8μl/min (corresponding to 0.05~0.1 Torr), total pressure of ion source with methane: 1.0 Torr, ion source temperature: 70°C. It was found that methane mainly functioned as a proton donor in the methane mixture system. In complex system containing more than two solvents, ions derived from those possesing the highest proton affinity became dominant reactant ions except the non polar solvents such as n-hexane. Because of its high proton affinity, ammonia often acted as a terminal proton acceptor resulting in NH4+ as the dominant reactant ion within the ammonia containing system, thus enabling constant ionization. The proposed method facilitated acquisition of plural CI mass spectra in GC/MS mode using several solvents. An on-off cock situated on line with the direct introduction portion enabled measurement of plural CI mass spectra within a GC peak. The usage of deuterium oxide as reagent gas enabled determination of active hydrogen of unknown samples without deuteration pretreatment and identification of isomers such as N-methylaniline and o-toluidine difficult to be distincted by EI, CI (CH4) or CI (i-C4H10) mode.
  • 岡田 静子, 飯田 芳男
    1981 年 29 巻 3 号 p. 287-294
    発行日: 1981年
    公開日: 2007/05/01
    ジャーナル フリー
    Organic labile compounds such as nucleic acids, amino acids, catechol amines and mono-, di-saccharides dissolved in an appropriate solvent, were introduced together with solvent into the Cl ion source held at 130°C of a Finnigan 3300 E GC/QMS through a simple interface. The interface consists of an internal capillary stainless steel tube in which the 1μg/μl sample solution and solvent are passed through by a micro LC pump at a flow rate of 2 μl/min, and also an external one which passes methane. Methane was introduced to aid sample introduction in aerosol form to assure stable ionization. In some cases an ammonia water reservoir was located on another line. Solvent-methane mixture was applied as reagent gas and (S+H)+ from solvent(S) possessing the highest proton affinity was the dominant ion which acted as reactant ion as reported in our previous paper. Consequently significant CI mass spectra were readily obtained without derivatization, and especially noteworthy was that ammonia-containing reagent gas produced peaks showing molecular weight information.
  • 小田 雅庸
    1981 年 29 巻 3 号 p. 295-304
    発行日: 1981年
    公開日: 2007/05/01
    ジャーナル フリー
    The mechanism of specific fragments which give [M—OH]+ in o-methyl and o-ethyl-formanilide was discussed and the paths to the formation of the fragment ion at m/z 106 in methylformanilides and methylacetanilides were investigated using deuterium labeled compounds.
    It was ascertained that the [M—OH]+ ion was produced by the hydrogen-transfer from the ortho-methyl or ethyl group to the acyl oxygen, followed by the OH elimination and that the intensity of [M—OH]+ in o-methylformanilides was enhanced strongly by the nitro group at para position to the methyl group.
    It was suggested that the simple cleavage of the —NH—CO— bond which is a route to produce an ion at m/z 106 was more prominent in o-methylformanilide than those in p-methylformanilide and o- or p-methylacetanilide.
  • 中井 晶
    1981 年 29 巻 3 号 p. 325-344
    発行日: 1981年
    公開日: 2007/05/01
    ジャーナル フリー
    In the preceding paper, we described the geometrical aberrations in a 3rd-order approximation for the sector type magnetic analyzer with pole pieces of linear boundaries and of parallel flat faces taking account of both effects of the fringing field and of the tilt of central ray to the virtual field boundaries. As further development of the study, trajectories of large current ion beam are derived analytically in a 3rd-order approximation under consideration of the effective space charge which is affected by neutralization due to secondary electrons. To express simply the effect of space charge, a new factor "index of space chage: κ" is introduced which is common in sector type magnetic analyzers. The attenuation of beam intensity and the influence of abundance ratio are also taken into account. The formulae of ion trajectory are programmed in MALT (Magnetic Analyzer with Linear Terminations), which can give ion trajectories and their coefficients individually in the field-free spaces of ion source side and of image side, and in the deflection space.
    As examples of calculation of these formulae some maps are presented which show clearly the effect of space charge on ion trajectories.
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