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A newly developed mass-spectrometry technique employing a tandem Van de Graaff accelerator together with a special beam-transport system and heavy-ion detector has been used to determine the half-life of Si-32. The result obtained, 108 plus or minus 18 yr, disagrees with the accepted value of 330 plus or minus 40 yr. The implications of the new half-life of Si-32, which is used for dating studies, are discussed.
Microwave rotational spectrometry is used to measure tropospheric carbonyl sulfide. The instrument and techniques for using it are described.
A computer system was developed for an emission spectrometry facility consisting of a direct current (DC) argon arc spectrograph optically coupled to an inductively coupled plasma multichannel spectrometer. Custom hardware and software were designed to control analytical functions and perform data acquisition. The software system was designed to make operation of the facility simple for routine operation and flexible for research and development. Special software was written to collect data under controlled conditions to characterize and monitor system response. One sequence collects intensity versus time data on all channels and displays the data graphically. These profiles are useful in studying the effects of operating parameters on measurement precision. Another special sequence performs calibration using a spline curve fit procedure. Routines were also written to measure dark currents and signals from a standard tungsten halogen lamp mounted in place of the DC arc. For quality control purposes, histories of these values are kept and monitored for excess scatter or drift.
Trace gases evolved from a polyimide film during its thermal curing stages have been studied using ion-induced nucleation mass spectrometry. The technique involved exposing the test gas sample to a low energy beta source and recording the masses of the ion-induced molecular clusters formed in the reaction chamber. On the basis of the experimentally observed molecular cluster spectra, it has been concluded that the dominant trace component had a molecular weight of 87 atomic mass units. This component has been identified as a molecule of dimethylacetamide (DMAC) which had been used as a solvent in the preparation of the test polyimide specimen. This identification has been further confirmed by comparing the spectra of the test gas sample and the DMAC calibration sample obtained with a conventional mass spectrometer. The advantages of the ion-induced nucleation mass spectrometer versus the conventional mass spectrometer are discussed.
An instrument that analyzes the chemical composition of biological particles in aerosol or hydrosol form was developed. Efforts were directed toward the acquisition of mass spectra from aerosols of biomolecules and bacteria. The filament ion source was installed on the particle analysis by mass spectrometry system. Modifications of the vacuum system improved the sensitivity of the mass spectrometer. After the modifications were incorporated, detailed mass spectra of simple compounds from the three major classes of biomolecules, proteins, nucleic acids, and carbohydrates were obtained. A method of generating bacterial aerosols was developed. The aerosols generated were collected and examined in the scanning electron microscope to insure that the bacteria delivered to the mass spectrometer were intact and free from debris.
A discussion of the limits of energy resolution in different energy ranges is given. The energy resolution of a spectrometer is analyzed in terms of the parameters characterizing the crystal, the detector, and the amplification electronics. A high-resolution room-temperature HgI2 spectrometry system was used to measure low-energy X-ray fluorescence spectra. For the MgK-alpha X-ray line the measured resolution was 245 eV (fwhm); the electronic noise linewidth of the system was 225 eV. Alpha-particles were used to excite X-ray fluorescence from low-Z elements separately or in combination. The shape of the photopeaks in the spectra is discussed.
Recent developments in the field of mass spectrometry taking place at the Caltech Jet Propulsion Laboratory are highlighted. The pertinent research and development is aimed at producing an ultrahigh sensitivity mass spectrograph for both spaceflight and terrestrial applications. The unique aspect of the JPL developed technology is an integrating focal plane ion detector that obviates the need for spectral scanning since all ions over a wide mass range are monitored simultaneously. The ion detector utilizes electro-optical technology and is therefore referred to as an Electro-Optical Ion Detector (EOID). A technical description of the JPL MS/EOID, some of the current applications, and its potential benefits for internal contamination analysis are discussed.
Initial results of the novel remote earth sensing technique of imaging spectrometry, which is technically feasible from both spacecraft and aircraft platforms, indicate that the direct identification of surface materials on a picture-element basis is possible through proper sampling of absorption features in the reflectance spectrum. Sensors of this type are able to acquire images simultaneously in 100-200 contiguous spectral bands. Computerized data reduction and storage techniques are available for the large data sets thus generated, and novel analytic techniques are under development to maximize information content extraction.
Over the past years, Tandem Accelerator Mass Spectrometry (TAMS) has become established as an important method for radionuclide analysis. In the Arizona system the accelerator is operated at a thermal voltage of 1.8MV for C-14 analysis, and 1.6 to 2MV for Be-10. Samples are inserted into a cesium sputter ion source in solid form. Negative ions sputtered from the target are accelerated to about 25kV, and the injection magnet selects ions of a particular mass. Ions of the 3+ charge state, having an energy of about 9MeV are selected by an electrostatic deflector, surviving ions pass through two magnets, where only ions of the desired mass-energy product are selected. The final detector is a combination ionization chamber to measure energy loss (and hence, Z), and a silicon surface-barrier detector which measures residual energy. After counting the trace iosotope for a fixed time, the injected ions are switched to the major isotope used for normalization. These ions are deflected into a Faraday cup after the first high-energy magnet. Repeated measurements of the isotope ratio of both sample and standards results in a measurement of the concentration of the radionuclide. Recent improvements in sample preparation for C-14 make preparation of high-beam current graphite targets directly from CO2 feasible. Except for some measurements of standards and backgrounds for Be-10 measurements to date have been on C-14. Although most results have been in archaeology and quaternary geology, studies have been expanded to include cosmogenic C-14 in meteorites. The data obtained so far tend to confirm the antiquity of Antarctic meteorites from the Allan Hills site. Data on three samples of Yamato meteorites gave terrestrial ages of between about 3 and 22 thousand years.
The method of particle analysis by mass spectrometry has been applied to the quantitative measurement of sodium chloride in individual particles on a real-time basis. Particles of known masses are individually introduced, in the form of a beam, into a miniature Knudsen cell oven (1600 K). The oven is fabricated from rhenium metal sheet (0.018 mm thick) and is situated in the ion source of a quadrupole mass spectrometer. A particle once inside the oven is trapped and completely volatilized; this overcomes the problem of partial volatilization due to particles bouncing from the filament surface. Individual particles are thermally volatilized and ionized inside the rhenium oven, and produce discrete sodium ion pulses whose intensities are measured with the quadrupole mass spectrometer. An ion pulse width of several milliseconds (4-12 ms) is found for particles in the mass range 1.3 x 10 to the -13th to 5.4 x 10 to the -11th g. The sodium ion intensity is found to be proportional to the particle mass to the 0.86-power. The intensity distribution for monodisperse aerosol particles possesses a geometric standard deviation of 1.09, showing that the method can be used for the determination of the mass distribution function with good resolution in a polydisperse aerosol.
The first use of tandem accelerator mass spectrometry (TAMS) to measure the content of Ca-41 in a natural sample, the iron Bogou meteorite, is reported. Ca in the samples was extracted by hydroxide precipitation and purified by means of a caution exchange resin (AG 50W-X8). After adding 4 percent ammonium oxide, the precipitate was ignited to CaO in a quartz vial at about 1100 C. The Ca-41/Ca ratios were determined following acceleration by alternate measurements of the Ca-40 beam current in an image Faraday cup. Ca-41 particles were also measured using a gas counter. The measured Ca-41/Ca ratio was 3.8 + or -0.6 x 10 to the 12th, which corresponds to a Ca-41 activity of 6.9 + or -1.1 d.p.m. per kg. Calculation of the half-life of Ca-41 in the Bogou meteorite yielded an age of 103,000 years.
Imaging spectrometry for the remote sensing of the Earth from aircraft and satellites is discussed. Results with an aircraft instrument show that remote, direct identification of surface materials is possible. The airborne and spaceborne sensors can acquire images in 100 to 200 spectral bands. The next generation aircraft scanner (AVIRIS) is expected to be operational in 1987. Plans are underway for a Shuttle instrument (SISEX) to fly in 1991.
Tunable-diode laser absorption spectrometry (TDLAS) affords a number of advantages for atmospheric measurements. It is a universal method, applicable, in principle, to all gases of atmospheric interest. Because of its extremely high spectral resolution it provides unequivocal identification of the target species, with no interferences from other gases. It provides real-time, in situ measurements with time resolutions better than 1 minute. The sensitivity of the current TDLAS system is marginally capable of measuring HO2. This species exists in the troposphere at concentrations which are up to 2 orders of magnitude higher than those of HO and, in addition, is much less susceptible to removal by the surfaces of the instrument and its sampling system. HO2 is an important HO sub x species in its own right but can also give direct information on the HO concentration by virtue of the rapid partitioning between these two species. The addition of the high-frequency modulation technique to the TDLAS system would ensure its ability to measure HO2 under most atmospheric conditions. The ability of the TDLAS to measure hydrogen peroxide (H2O2) in the ambient atmosphere was also demonstrated. H2O2 measurements give a clear indication of HO sub x mixing ratios and are also important as a photolytic source of HO and as an important oxidant for other atmospheric consitituents such as SO2.
Imaging spectrometry for the remote sensing of the Earth is introduced. Reflected solar energy from the surface is dispersed in a spectrometer and used to form up to 200 registered spectral images. Each pixel has associated with it sufficient information for the reconstruction of a complete reflectance spectrum. The technique allows the diagnostic narrow band spectral features that are characteristic of many surface materials to be used to identify those materials. These spectral features are typically 20 to 40 nm wide; spectral imaging systems which acquire data in contiguous 10 nm bands therefore have sufficient resolution for direct identification of those materials with diagnostic spectral bands.
Samples of epitaxial GaAs grown on (100) Si substrates using molecular beam epitaxy were annealed at four different temperatures, from 800 to 950 C. Following annealing, the samples were analyzed using secondary ion mass spectrometry. Depth profiles of Ga, As, and Si reveal optimum conditions for annealing, and place a lower limit on a damage threshold for GaAs/Si substrates.
Unattended diode array spectrometers have been designed for ground based stratospheric trace species monitoring by zenith sky visible spectrometry. Measurements are performed with a 1.0 nm resolution between 290 nm and 590 nm in order to allow simultaneous evaluations of column densities of ozone, nitrogen dioxide. Field tests have shown that the species can be monitored with a precision of + or - 2 Dobson for the first and + or - 2.10 to the 15th mol/sq cm for the second, although the absolute accuracy of the method is limited by the error of the estimation of the atmospheric optical path of the scattered light. Two identical instruments were set up in January 1988, one in Antarctica at Dumont d'Urville (66 S, 140 E) to be operated all year and another one in the Arctic at ESRANGE at Kiruna (68 N; 22 E) which will operate to the final warming of spring 1988. The data are processed in real time at both stations. O3 and NO2 columns are transmitted together with surface and stratospheric temperature and winds. They are also recorded for further treatment and search for OClO and BrO. Only one month of data from Antarctica is available at the moment. Obtained during polar summer, they cannot show more than stable columns of O3 and NO2 and for the last species, the buildup of its diurnal variation.
High spectral resolution Airborne Imaging Spectrometer (AIS) data were acquired over 20 well-studied Wisconsin forest sites to evaluate the potential of remote sensing for estimating forest canopy chemistry. Intensive nutrient cycling research in these forests demonstrates that canopy lignin content is strongly related to measured annual nitrogen mineralization at the undisturbed sites and may serve as an accurate index for nitrogen cycling rates. Ground measurements were made of foliar biomass and canopy nitrogen and lignin content, the latter within two weeks of the AIS overflight. The spectral data were transformed using derivative techniques modified from laboratroy spectroscopy. Stepwise regression assisted in determining combinations of wavelengths most highly correlated with canopy chemistry and biomass. Strong correlations between AIS data and total canopy lignin content in deciduous forests and canopy lignin concentration (total lignin/biomass) in both deciduous and coniferous stands indicate that imaging spectrometry can be used to estimate canopy lignin content and, from that, the spatial distribution of annual nitrogen mineralization rates.
The use of monoenergetic positrons for the ionization of organic molecules in the gas phase is described. The ionic products are analyzed with a time-of-flight mass spectrometer and detected to produce a mass spectrum. The ionization mechanisms which can be studied in this way include positron impact at energies above the ionization limit of the target molecules, positronium formation in the Ore gap energy range, and positron attachment at energies less than 1eV. The technique of positron ionization mass spectrometry (PIMS) may have analytical utility in that chemical selectivity is observed for one or more of these processes.