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Primordial radionuclides K, Th and U concentrations in Apollo 12 lunar rocks, breccias and fines, using gamma ray spectrometry
Techniques of mass spectrometry are reviewed and the theory of the quadrupole mass spectrometer (QMS) is discussed. The QMS is shown to have several advantages over older types of mass spectrometers. The QMS has been flown on a large number of rockets and several satellites. More sophisticated versions of the QMS are proposed for future satellites. Special emphasis is placed on problems of contamination which are likely to be encountered on a large and complex satellite like the Advanced Technology Satellite ATS-G. The development of a QMS to detect and forestall such contamination is discussed.
Electron-impact induced fragmentations of o-, m-, and p-hydroxyalkylphenones and their trimethylsilyl (TMS) ethers are studied by means of high-resolution mass spectrometry, metastable defocusing, and deuterium labeling of the TMS ether derivatives. A markedly increased methyl radical loss from the o-TMS ether is attributed to a proximity effect. Minor fragmentation was observed with m- and p-isomers. Significantly intense doubly-charged ions were formed from ketonic cleavage and by the loss of a TMS methyl radical. The sequence of fragmentation was found to depend on the size of the alkyl group attached to the ketone carbonyl.
Review of the present status of mass spectrometry in the light of pertinent recent publications spanning the period from December 1971 to January 1974. Following an initial survey of techniques, instruments, and computer applications, a sharp distinction is made between the chemistry of organic (radical-)ions and analytical applications in biorganic chemistry and medicine. The emphasis is on the chemistry of organic (radical-)ions at the expense of inorganic, organometallic, and surface ion chemistry. Biochemistry and medicine are chosen because of their contemporary importance and because of the stupendous contributions of mass spectroscopy to these fields in the past two years. In the review of gas-phase organic ion chemistry, special attention is given to studies making significant contributions to the understanding of ion chemistry.
A qualitative study of the application of surface ionization and mass spectrometry to the in situ detection and constituent analysis of atmospheric particles was conducted. The technique consists of mass analysis of ions formed as a result of impingement of a stream of particles on a hot filament where, it is presumed, surface ionization takes place. Laboratory air particles containing K, Ca, and possibly hydrocarbons were detected. Other known particles such as Al2O3, Pb(NO3)2, and Cr2O3 were analyzed by detecting the respective metal atoms making up the particles. In some cases, mass numbers indicative of compounds making up the particles were detected showing surface ionization of particles sometimes leads to chemical analysis as well as to elemental analysis. Individual particles were detected, and it was shown that the technique is sensitive to Al2O3 particles with a mass of a few nanograms.
Primordial and cosmogenic radionuclide concentrations are determined nondestructively by gamma-ray spectrometry in soil and rock samples from the returned Apollo 17 sample collection from Taurus-Littrow and Descartes. Geochemical evidence in support of field geology speculation concerning layering of the subfloor basalt flows is demonstrated along with a possible correlation of magmatic fractionation of K/U as a function of depth. The pattern of radionuclide concentrations observed in these samples is distinct due to proton bombardment by the intense solar flares of August 4-9, 1972. Such radionuclide determinations are used in determining lunar sample orientation and characterizing solar flare activity.
A new method of forming a visual image by ultrasound is described. A shadowgraphic transmission image similar to an X-ray radiograph is produced by the application of a technique known as Time Delay Spectrometry. The system uses a repetitive frequency sweep with a linear relationship between frequency and time and the transmitting and receiving crystal are scanned in raster fashion about the subject. By electronic processing, an image may be built up which represents the energy transmitted through the specimen with a given time delay. An intensity modulated picture encompassing the full shades-of-gray capability of the recording system can be produced. A second type of image showing transmission time through the specimen may also be formed. Brightness changes in the displayed image in this case correspond to changes in the ultrasonic transmission time through the specimen.
Mass spectrometry is used for chemical analysis of aerospace materials and contaminants. Years of analytical aerospace experience have resulted in the development of specialized techniques of sampling and analysis which are required in order to optimize results. This work has resulted in the evolution of a hybrid method of indexing mass spectra which include both the largest peaks and the structurally significant peaks in a concise format. With this system, a library of mass spectra of aerospace materials was assembled, including the materials responsible for 80 to 90 percent of the contamination problems at Goddard Space Flight Center during the past several years.
A new class of apodizing functions suitable for Fourier spectrometry (and similar applications) is introduced. From this class, three specific functions are discussed in detail, and the resulting instrumental line shapes are compared to numerous others proposed for the same purpose.
Black body measurements and absorption spectra of methane near 3.3 microns are presented and used as examples in a discussion of upconversion spectrometry for astrophysical application. Factors determining the system conversion efficiency and the minimum detectable flux for a typical system are presented. The spectrometer described uses an Argon-ion laser and a temperature turned LiNbO3 crystal in a CW mode. Satisfactory agreement between measured and calculated performance parameters is obtained. An estimate of the highest performance parameters attainable using current technology is given.
A theoretical analysis of constant momentum mass spectrometry was made. A maximum resolving power for the decelerating mode constant momentum mass spectrometer was shown theoretically to exist for a beam of ions of known energy. A vacuum system and an electron beam ionization source was constructed. Supporting electronics for a residual gas analyzer were built. Experimental investigations of various types of accelerating and decelerating impulsive modes of a constant momentum mass spectrometer as applied to a residual gas analyzer were made. The data indicate that the resolving power for the decelerating mode is comparable to that of the accelerating mode.
Advances in mass spectrometry (MS) and its applications over the past decade are reviewed in depth, with annotated literature references. New instrumentation and techniques surveyed include: modulated-beam MS, chromatographic MS on-line computer techniques, digital computer-compatible quadrupole MS, selected ion monitoring (mass fragmentography), and computer-aided management of MS data and interpretation. Areas of application surveyed include: organic MS and electron impact MS, field ionization kinetics, appearance potentials, translational energy release, studies of metastable species, photoionization, calculations of molecular orbitals, chemical kinetics, field desorption MS, high pressure MS, ion cyclotron resonance, biochemistry, medical/clinical chemistry, pharmacology, and environmental chemistry and pollution studies.
IR absorption spectrometry was used to follow the disappearance of NH and CH bonds during the pyrolysis of a polymer film containing 30 weight percent ammonium perchlorate (AP). The remaining 70 weight percent consisted of a mixture of 92.5 weight percent hydroxyl-terminated polybutadiene (HTPB) and 7.5 weight percent isophrone diisocyanate (IPDI). The results indicate that polymer decomposition is induced by products of AP decomposition, and that about 2.5 CH bonds disappear for each NH bond that disappears. The diffusion process occurring in the later stages of the reaction is analyzed in an attempt to account for the unexpectedly low activation energy.
Nitric oxide has been measured in situ between 38.4 and 29.8 km by a new technique, photoionization mass spectrometry. Data indicate a peak mixing ratio of 5.7 plus or minus 0.35 ppbv at 37.5 km and only 0.2 plus or minus 0.2 ppbv at 32.8 km with a sharp gradient in concentration between 33 and 34 km. Simultaneous in-situ measurements of the ozone concentration show no significant feature at that altitude. The rapid decrease in mixing ratio is not predicted by current theory.
The high temperature diffusion of trace elements in metals and alloys was investigated. Measurements were made by high sensitivity mass spectrometry in which individual atoms were detected, and quantitative data was obtained for zircaloy-2, 304 stainless steel, and tantalum. Additionally, a mass spectrometer was also an analytical tool for determining an allotropic phase change for stainless steel at 955 C, and a phase transition region between 772 C and 1072 C existing for zircaloy-2. Diffusion rates were measured in thin (0.001" (0.0025 cm) and 0.0005" (0.0013 cm)) ribbons which were designed as high temperature thermal ion sources, with the alkali metals as naturally occurring impurities. In the temperature and pressure regime where diffusion measurements were made, the solute atoms evaporated from the ribbon filaments when the impurities diffused to the surface, with a fraction of these impurity atoms ionized according to the Langmuir-Saha relation. The techniques developed can be applied to many other alloys important to space vehicles and supersonic transports; and, with appropriate modifications, to the diffusion of impurities in composites.
A description is given of experiments which provide a verification of three features of Penning ionization mass spectrometry. One of these features is related to the ability to simplify a molecular fragmentation pattern and to intensify the molecular ion peak. Another feature is concerned with the ability to identify uniquely geometric isomers which are indistinguishable using high-energy electron impact methods. The third feature involves the ability to identify components in a mixture, which cannot be discerned using electron impact or chemical ionization methods alone. The investigation shows that Penning ionization is an efficient soft ionization technique which can be used to simplify mass spectra of pure compounds as well as mixtures.
This paper describes some recent results of a quiescent-prominence spectrometry program. The observations were made with a 25-cm coronagraph/coude spectrograph system using a silicon vidicon detector. This detector consists of 500 contiguous channels covering approximately 6 or 80 A, depending on the grating used. The instrument is interfaced to a computer system and has the important advantages of wide spectral response, linearity, and signal averaging with real-time display. Its principal drawback is the relatively small target size. For the present work, the aperture was about 3 x 5 arcsec. Absolute intensity calibrations were made by measuring quiet regions near the center of the sun.
A series of kerogens and kerogen precursors isolated from DSDP samples, oil shales and recent algal mats have been examined by Curie point pyrolysis-high resolution gas chromatography and gas chromatography-mass spectrometry. This study has shown that the three main types of kerogens (marine, terrestrial and mixtures of both) can be characterized using these techniques. The marine (algal) kerogens yield principally aliphatic products and the terrestrial kerogens yield more aromatic and phenolic products with some n-alkanes and n-alkenes. The yields of n-alkanes and n-alkenes increase and phenols decrease with increasing geologic age, however, pyrolysis-GC cannot be used to characterize the influence of short term diagenesis on the kerogen structure.