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Volume 19 (1971)
- Issue 4 Pages 254-
- Issue 3 Pages 179-
- Issue 2 Pages 88-
- Issue 1 Pages 1-
Volume 19, Issue 2
Displaying 1-10 of 10 articles from this issue
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HIFUMI TAMURA, HIROSHI DOI, TOSHIO KONDO1971 Volume 19 Issue 2 Pages 88-100
Published: June 29, 1971
Released on J-STAGE: June 28, 2010
JOURNAL FREE ACCESSIon microprobe mass analysis is said to be non-destructive from a macroscopic viewpoint. Howe ever, it is essentially destructive as it is accompanied by sputtering effect. When thin film or surface layer are to be analyzed, high sensitive analysis with an infinitisimal amount of specimen and with the highest possible accuracy is especially desirable.
In order to increase the sensitivity of the ion microprobe mass analyzer, we developed a new second ary ion extracter with Pierce type electrode. It is constructed of a Pierce electrode, an extracting electrode, an accelerating electrode and an electrostatic lens assembly.
As an application of the method, an aluminum film was analyzed by the ion microprobe mass analyzer. The film was prepared by the evaporation of pure aluminum using a crucible of boron nitride. Assuming that the minimum detectable signal is about twice the noise level, the detection limit of boron in aluminum is a few ppm. In this case, the sputtering rate was about 5Å/s. The detection limit of bulk is on the order of several tenth of ppb.View full abstractDownload PDF (1977K) -
T. Sakai, Y. Ino1971 Volume 19 Issue 2 Pages 102-108
Published: June 29, 1971
Released on J-STAGE: June 28, 2010
JOURNAL FREE ACCESSResolution mode of quadrupole mass filter is well represented by mass scan line on stability diagram. All mass peaks just disappear on the cutoff scan line which passes through the origin and to the apex of the stability diagram. When a scan line is shifted downward by a small amount parallel to the cutoff scan line, it can be expected theoretically that all mass peaks give a constant peak width independent of mass. Adjustment of resolution is carried out based on this theory. As peak height is proportional to the peak width, a mass spectrum obtained experimentally with this mode of operation gives a constant pattern coefficient in adjusting the resolution.View full abstractDownload PDF (553K) -
HIROSHI MIYAKE, MASAMI MICHIJIMA1971 Volume 19 Issue 2 Pages 110-116
Published: June 29, 1971
Released on J-STAGE: June 28, 2010
JOURNAL FREE ACCESSSingle and recurrent multi-channel scaling of ion current was used for the mass spectrometry of very small samples. Isotopic analysis of rare gases was carried out with single multi-channel ion scaling using a low background mass spectrometer. Corrections for background, memory effect and time variations of various factors which cause systematic errors are more easily made with this method than even with direct ion current measurement method although those corrections are impossible or very difficult with simple ion counting method. Recurrent multi-channel scaling made it possible to measure very low pressure for long time operation(more than 100 hours)discriminating the peaks of accidental noise pulses. Mass discrimination caused by ion counting and dead time correction at high counting rate are discussed.View full abstractDownload PDF (833K) -
H. KANNO1971 Volume 19 Issue 2 Pages 118-123
Published: June 29, 1971
Released on J-STAGE: June 28, 2010
JOURNAL FREE ACCESSThe stringent test of Dodson's normalization equation was made for the isotopic fractionation arising from the evaporation of sample from the filament. As an extension of recent papers of Kanno(4)and of Ozard and Russel(6), a new normalization equation has been proposed ΔMit logrjt/R0jt=kii·ΔMit logrit/R0it where rit is the observed isotopic abundance ratio of isotope i to reference isotope t, R0it is the corresponding true isotope ratio, ΔMit is mass difference between isotopes t and i, and kij is the correction factor, which is determined experimentally from a log-log plot of rit and rjt.View full abstractDownload PDF (500K) -
Y. MATSUHISA, O. MATSUBAYA, H. SAKAI1971 Volume 19 Issue 2 Pages 124-133
Published: June 29, 1971
Released on J-STAGE: June 28, 2010
JOURNAL FREE ACCESSThe oxygen of quartz, feldspar, biotite and water was extracted as molecular oxygen using BrF5 and by essentially the same procedures as described by Clayton and Mayeda(1963)and by O'Neil and Epstein(1966). A quantitative conversion of the oxygen gas into carbon dioxide for the mass spectrometric analysis was readily attained by spectrographic graphite wound by platinum wire and heated at 700°C in an externally resistance-heated quartz tube. The platinum catalyst is essential to complete the rapid conversion. The reproducibility of the isotopic analysis of the same tank oxygen by this conversion unit was better than 0.1‰ at the 95% confidence interval over a period of one year(Table2.). The isotopic analyses of standard quartzs, MSQ-1 and -2 and standard waters, MSA-1 and -2 reproduced with in 0.2‰(Tables.4 and 8). On our SMOW scale which is based on the δ18O SMOW of MSA-2 and the isotopic fractionation factor, 1.0407(O'Neil and Epstein, 1966), at 25°C between water and CO2, the δ18O SMOW values of MSQ-1 and -2 are +15.25 and +8. 85‰, respectively. The same quartz samples were analyzed to be +15.08 and +8.70‰ by Clayton's laboratory in Chicago(Table 5). MSA-1 and -2 were also analyzed by CO2-H2O isotopic equihbration method, giving the difference between the two waters to be 7.52‰. This is in close agreement with 7.38‰ given by the BrF5method. The isotopic fractionation factor between CO2 and water at the equilibration temperature(25°C)was calculated from our data to be 1.0412. The observed isotopic ratios of biotite showed a variation with grain size of the sample powder and the preheating scheme(Table 7). Satisfactory results were obtained by using sample from 100 to 150 meshes and by 3 hr-preheating at 200°C. The reproducibility and accuracy of the isotopic results of silicates greatly depend on the history of the nickel reaction tubes in which samples are attacked by BrF5. A brand new tube often does not give a correct answer until after quite a few number of samples are processed in it(Table 3). Our experience suggests that repeated attacks by BrF5 of the walls at a higher temperature than usual reaction temperatures, each followed by nitric acid wash, can eliminate quickly the causes of the instable results.View full abstractDownload PDF (870K) -
REISUKE GENSHO, MASATAKE HONDA1971 Volume 19 Issue 2 Pages 134-143
Published: June 29, 1971
Released on J-STAGE: June 28, 2010
JOURNAL FREE ACCESSA method of boron isotope analysis using the M2BO2+ ion(M is the alkaline metal)has been investigated. In the case of the M2BO2+ where the alkaline metal has two or more isotopes, this method has the following characteristics.(1)Three or more peaks are obtained from the combination of isotopes of boron and the alkaline metal.(2)Using the enriched isotopes of the alkaline metal, the relative peak heights can be adjusted so as to read with minimum errors.(3)The discrimination effect may be corrected from the known isotopic composition of the alkaline metal.(4)The error of measurements can be examined by a pair of the appropriate combination of peak heights. As results of the investigation on a series of alkaline borates, it was concluded that the Rb2BO2+ ion has the most appropriate combination of peak heights. In the case of Rb2BO2+, four peaks of m/e 212-215 are effectively obtained. The error of measurements can be examined from the relation 213/212=215/214. The discrimination effect for the measured boron isotopic ratio it 11B/10B=213/212 may be corrected using the measured value of 215/213=87Rb/85Rb+18O/16O and the standard isotopic ratio of rubidium and oxygen. In this method, the examination of the error of measurements is always feasible, but the correction of the discrimination effect may be significant only when the deviation of the observed value due to the discrimination effect is greater than the statistical fluctuation or the variation of the standard isotopic composition due to the fractionation effect.View full abstractDownload PDF (858K) -
YOSHIHIRO MASUDA1971 Volume 19 Issue 2 Pages 144-149
Published: June 29, 1971
Released on J-STAGE: June 28, 2010
JOURNAL FREE ACCESSSpectrum of hydrogen is unstable in mass spectrometry, fluctuation of the H2+ of hydrocarbon is very pronounced, and the peak hight increases gently with time. It was found that with hydrocarbons this was caused chiefly by not only the rearrangement of H but also by the adsorption to and desorption from the ion source or analyser tube.
If the hydrogen is flashed to ion source beforehand, analytical values of hydrogen in ethylene can be relatively good.View full abstractDownload PDF (507K) -
YOSHIHIRO MASUDA1971 Volume 19 Issue 2 Pages 150-157
Published: June 29, 1971
Released on J-STAGE: June 28, 2010
JOURNAL FREE ACCESSSamples containing water vapour are sometimes analysed by mass spectrometry. It was found that in such a case, not only is the background made higher but the impure components formed by the reaction of H2O with the ion source filament and/or impure components in the inner surface of ion source act as the major cause.View full abstractDownload PDF (506K) -
YOSHIHIRO MASUDA1971 Volume 19 Issue 2 Pages 158-164
Published: June 29, 1971
Released on J-STAGE: June 28, 2010
JOURNAL FREE ACCESSWhen mass spectra of ethylene are measured at about the same sample pressure generally used in analysis, C3H3+, C3H5+, etc., can be determined by rearrangement.
Hence, if measurement is made at low enerey electron bombardment, both C3H5+(m/e 41)and C4H7+(m/e 55)can be observed, and it became clear that they can be formed according to the following process:
C2H3++C2H4→C4H7+→C3H5++CH2,
C2H3+C2H4+→C4H7+→C3H5++CH2.View full abstractDownload PDF (541K) -
TATSUO ARIKAWA1971 Volume 19 Issue 2 Pages 166-167
Published: June 29, 1971
Released on J-STAGE: June 28, 2010
JOURNAL FREE ACCESSDownload PDF (187K)
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