Journal of the Mass Spectrometry Society of Japan
Online ISSN : 1880-4225
Print ISSN : 1340-8097
ISSN-L : 1340-8097
Volume 18, Issue 1
Displaying 1-8 of 8 articles from this issue
  • MASATAKE HONDA
    1970 Volume 18 Issue 1 Pages 866-876
    Published: March 01, 1970
    Released on J-STAGE: June 28, 2010
    JOURNAL FREE ACCESS
    Download PDF (1095K)
  • FUMIYAI KONISH
    1970 Volume 18 Issue 1 Pages 878-886
    Published: March 01, 1970
    Released on J-STAGE: June 28, 2010
    JOURNAL FREE ACCESS
    The relative sensitivity factors of elements contained in the graphite-sample electrodes have been investigated by using samples containing one or several halides, oxides, carbonates, ammonium salts and others, to improve the quantitative accuracy of trace impurity determination in inorganic compounds by source mass spectrography. Correction was made for the linewidth variation and the mass de pendency of emulsion sensitivity. It has been found that, generally speaking, alkalis, alkali earths and III B group elements are among the most sensitive, while halogens are among the least sensitive. We examined the correlation between the relative sensitivity factors experimentally obtained and physicochemical constants of elements. It has been found that the relative sensitivi ty factor may calculated as the ratio of the product of the ionization potential squared and the bond energy of the element in question in a compound to that of the standard element.
    Download PDF (665K)
  • NOBUO TAKAOKA
    1970 Volume 18 Issue 1 Pages 888-893
    Published: March 01, 1970
    Released on J-STAGE: March 01, 2011
    JOURNAL FREE ACCESS
    Preliminary results are reported on the separation of small amount of ruthenium from large amount of molybdenum sulfide and on the neutron-activation analysis of ruthenium in a molybdenite.
    The chemical yield for ruthenium in the distillation was checked by using a radioactive tracer 106Ru (T1/2=1yr.)and by counting 512KeV and 622KeVγ-rays from106Rh(T1/2=30sec)which is in radiation equilibrium with 106Ru.
    The procedures for fusion and distillation are as follows. Molybdenum sulfide of about0.1g was fused with sodium peroxide flux(ca.1.5g)in a nickel crusible, and then the black slurry extracted with 20ml of water was dissolved by 40ml of sulphuric acid(1:2)in a distillation flask. The known amount of tracer 106Ru was added to the solution. Osmium was removed by the distillation with hydrogen peroxide(30%). The ruthenium was distilled using 20ml of sodium bromate(20%)and 5ml of concentrated sulphuric acid added in the flask and with the air current through the distillation apparatus. The distillate was absorbed in two receivers, each containing 5ml of 9N sodium hydoxide or 10ml of 5%ethanol-0.2N hydrogen chrolic acid mixture.
    Comparing the counts of recovered 106Ru with the counts of added one, the distillation yield of 96.5%ruthenium was obtained in a single distillation, and in the doubly repeated 99.5%.
    In order to determine an amount of ruthenium in the molybdenite quantitatively, 85mg of the molybdenite was bombarded by pile-neutrons, together with a standard sample including 7.9μg of ruthenium.
    The ruthenium was separated from each neutron-irradiated sample by the same distillation procedures as described above. As a carrier, 216μg of ruthenium was added at the stage of fusion of the neutron-irradiated molybdenite. The distillate for the molybdenite was compared with the one for the standard sample by counting 498KeV γ-rays from radioactive 103Ru(T1/2=40d.)resulted from the neutroncapture on 102Ru. The countings were undertaken using a NaI(Tl)scintillation counter with an anticoincidence guard, along with a 512-channel pulse-height analyser. The concentration of ruthenium in the molybdenite was estimated to be 37×10-9g/g.
    An isotopic abundance of reagent ruthenium was tentatively measured by a single focusing mass spectrometer with a surface ionization source of a tungsten single filament. About5μg of ruthenium as chrolide was heated to dryness on a tungsten filament in air, and then was pre-heated to dull red in vacuum for two days. The isotopic abundance obtained is reported.
    Download PDF (761K)
  • HIROSHI NISHIMURA, JUN OKANO
    1970 Volume 18 Issue 1 Pages 894-904
    Published: March 01, 1970
    Released on J-STAGE: June 28, 2010
    JOURNAL FREE ACCESS
    A small ion probe mass spectrometer was constracted for the analysis of meteorites. Preliminary analyses of a standard steel, iron meteorites, and stone meteorites have been carried out with this instrument. It was noticed that molecular ions, and multicharged ions, together with instrumental backgro unds such as H+, C+, O+, Al+, were disturbing species for the analysis of trace elements. The dis tributions of nickel concentration along a scanning line on the surface of the iron meteorite, Odessa, were obtained. Enrichment of nickel in taenite phase was clearly shown. Isotopic abundances of lithiu m and boron in stone meteorites. Bruderheim and Leedey, were possible to measure and the preliminary data were shown.
    Download PDF (2012K)
  • MICHI ARATANI, NOBUFUSA SAITO
    1970 Volume 18 Issue 1 Pages 906-919
    Published: March 01, 1970
    Released on J-STAGE: June 28, 2010
    JOURNAL FREE ACCESS
    A specially designed mass spectrometer of a pulse counting mode has been constructed for studies on the chemical effect of nuclear transformations.The ion source has been examined by a beam experiment method using non-radioactive rare gas ions from an electron bombardment chamber. Measurements have been made of ion detection with 10 and 16 stage Cu-Be electron multipliers, the gains of which are 106and108, respectively. The results have shown that. a gain of at least 5×104is needed for the so-called“one to one” pulse counting. Charge spectra of recoil ions from a-emitting nuclides have been also measured and discussed in connexion with the decay scheme.
    Download PDF (1058K)
  • YOZABURO KANEKO, NOBUO KOBAYASHI, I CHIRO KANOMATA
    1970 Volume 18 Issue 1 Pages 920-938
    Published: March 01, 1970
    Released on J-STAGE: June 28, 2010
    JOURNAL FREE ACCESS
    Detailed descriptions of the drift tube technique of Kaneko-Megill-Hasted and a newly constructed apparatus are given. The apparatus consists of two sector type mass analyzers and a drift tube. Mass-identified primary ions are injected into the drift tube and thermalized by collisions with gasmolecules in the tube. After drifting through the tube, population of ions at the end of the tube is sampled with the second mass analyzer. The drift velocity of ions is measured by gate pulse technique the ionic mobility is determined. The average kinetic energy of drifting ions is calculated by Wannier's formula using the drift velocity measured experimentally. The cross section of reaction is calculated from the peak height ratio in the second mass spectra. By the use of buffer gas to dilute reactant gas, study of reactions having ordinary size of cross section, which would have dissipatall the primary ions if the reactant gas was not diluted, has become possible. Usually He gas is as buffer gas. Two mass analyzers are nearly the same. Each one has the radius of10cm. Whole apparatus differentially pumped so that the gas pressure in the drift tube can be increased as high as 1.8 The effective length of the drift tube is 8.4cm. The apparatus can cover the energy range from 0.044 eV(-330°K)to several eV. Reliability test of the apparatus has been made for both mobility measurement and cross section measurement.
    Download PDF (1580K)
  • AKIRA TATEMATSU, HIROSHI SAKURAI, HISAO NAKATA
    1970 Volume 18 Issue 1 Pages 940-947
    Published: March 01, 1970
    Released on J-STAGE: March 01, 2011
    JOURNAL FREE ACCESS
    In recent years accurate mass measurements in mass spectra of organic compounds have been used as a reliable technique to determine their elemental compositions.Usually perfluorokerosine or heptacosa fluorotributylamine is employed as an internal standard.
    In this paper a new method of measuring accurate masses without a standard sample is proposed. Thisis especially powerful for fragment ions, but in certain cases molecular ions and/or fragment ions of higher mass number may not be applicable to. The plinciple of the method is as follows. If an abundant peak is present at m/e R, peaks including heavy isotopes are also observed at m/e(R+1)and so on. Additionally these peaks are often constituted from not a nuclide combination but a few. So that mass differences among peaks in the same mass number are a criterion in selection of possible nuclide combinations. The relative abundance ratio among the main peak at m/e R and isotopic peaksat m/e(R+1)should also be examined. As an example this method is applied to determine nuclide combinations of three main fragment ions in the mass spectrum of ethyl p-arninobenzoate and the following results were obtained.
    Two peaks at m/e39 have compositions C3H3 and C3 13CH2, respectively. Abundunt C5H5 and weak C4H3N fragment ions correspond to two peaks at m/e65. Compositions of two peaks at m/e92 are shown to be C6H4O and C6H6N. However, for two fragment ions at m/e120 it was found that two combinations C6H2NO2-C7H6NO and C7H6N0-C8H10N are both possible, and could not be differentiated because of theexperimental difficulties.
    Download PDF (2643K)
  • Food Additives(3). Quantitative Determination of Ethyl p-hydroxybenzoate.
    AKIRA TATEMTSU, TANEKAZU NADAI, HIDEO YOSHIZUMI, KUNIHIRO NAITO, TOSHI ...
    1970 Volume 18 Issue 1 Pages 948-955
    Published: March 01, 1970
    Released on J-STAGE: June 28, 2010
    JOURNAL FREE ACCESS
    Quantitative analysis of ethyl p-hydroxybenzoate by means of mass spectrometry was established by using benzoic acid as an internal standard. Thus, the amount of ethyl p-hydroxybenzoate can be calculated from the ratio of the peak hights of m/e 121(base peak, ethyl p-hydroxybenzoate)to m/e 105(base peak, benzoic acid), as the ratio was found to be proportional to the amount of ethyl phydroxybenzoate. This method made possible to determine ethyl p-hydroxybenzoate between 40 μg and 200μg within the error of±3%.
    Download PDF (525K)
feedback
Top