Engineering topics
Publications and source records attributed to Lincoln, K. A..
New equipment has speed and capacity to process time-of-flight data. System relies on fast, compact waveform digitizer with 32-k memory coupled to personal computer. With digitizer, system captures all mass peaks on each 25- to 35-microseconds cycle of spectrometer.
Briefly described are the essential features of a computer program designed to interface a personal computer with the fast, digital data acquisition system of a time-of-flight mass spectrometer. The instrumentation was developed to provide a time-resolved analysis of individual vapor pulses produced by the incidence of a pulsed laser beam on an ablative material. The high repetition rate spectrometer coupled to a fast transient recorder captures complete mass spectra every 20 to 35 microsecs, thereby providing the time resolution needed for the study of this sort of transient event. The program enables the computer to record the large amount of data generated by the system in short time intervals, and it provides the operator the immediate option of presenting the spectral data in several different formats. Furthermore, the system does this with a high degree of automation, including the tasks of mass labeling the spectra and logging pertinent instrumental parameters.
Recent advances in commercially available data acquisition electronics embodying high speed A/D conversion coupled to increased memory storage have now made practical (at least within time intervals of a third of a millisecond or more) the capturing of all of the data generated by a high repetition rate time-of-flight mass spectrometer producing complete spectra every 25 to 35 microseconds. Such a system was assembled and interfaced with a personal computer for control and management of data. The applications are described for recording time-resolved spectra of individual vapor plumes induced from the pulsed-laser heating of material. Each laser pulse triggers the system to generate automatically a 3-dimensional (3-D) presentation of the time-resolved spectra with m/z labeling of the major mass peaks, plus an intensity versus time display of both the laser pulse and the resulting vapor pulse. The software also permits storing of data and its presentation in various additional forms.
In the mass spectrometric sampling of dynamic systems, measurements of the relative concentrations of condensable and noncondensable vapors can be significantly distorted if some subtle, but important, instrumental factors are overlooked. Even with in situ measurements, the condensables are readily lost to the container walls, and the noncondensables can persist within the vacuum chamber and yield a disproportionately high output signal. Where single pulses of vapor are sampled this source of error is avoided by gating either the mass spectrometer ""on'' or the data acquisition instrumentation ""on'' only during the very brief time-window when the initial vapor cloud emanating directly from the vapor source passes through the ionizer. Instrumentation for these techniques is detailed and its effectiveness is demonstrated by comparing gated and nongated spectra obtained from the pulsed-laser vaporization of several materials.
Previosuly cited in issue 17, p. 2910, Accession no. A81-39069
The relative concentrations of vapors produced from carbon phenolic composites under thermal loadings approximating those expected at peak heating during vehicle entry into the atmospheres of the outer planets have been determined. The technique of vaporizing the surface of bulk samples by laser irradiation while measuring in situ the vapor species by mass spectrometry is described. Results show that vapor composition varies with irradiance level and with depth of heating (or extent of pyrolysis). Attempts are made to compare these experimental results with the theoretical predictions from computer codes.
Mass spectra are produced in most mass spectrometers by sweeping some parameter within the instrument as the sampled gases flow into the ion source. It is evident that any fluctuation in the gas during the sweep (mass scan) of the instrument causes the output spectrum to be skewed in its mass peak intensities. The time of flight mass spectrometer (TOFMS) with its fast, repetitive mode of operation produces spectra without skewing or varying instrument parameters and because all ion species are ejected from the ion source simultaneously, the spectra are inherently not skewed despite rapidly changing gas pressure or composition in the source. Methods of exploiting this feature by utilizing fast digital data acquisition systems, such as transient recorders and signal averagers which are commercially available are described. Applications of this technique are presented including TOFMS sampling of vapors produced by both pulsed and continuous laser heating of materials.
External signal-conditioning electronics assembled from commercially available components improves dynamic capability of time-of-flight mass spectrometer.
Characteristics of free-jet vapor expansions created by the pulsed-laser vaporization of some refractory materials are examined. Such expansions were generated from planar surfaces at laser power densities up to 2.5 MW/sq cm. Time-integrated and time-resolved photography were used to show that the structure and pressures of such flows are correlated by the same relationship that is valid for free jets from orifice flows. Data show that the vapor velocity becomes sonic at or very near the vaporizing surface. A method is presented for deriving vaporization pressure from flow-field photos; such pressures from carbon-vaporization data for temperatures to 4500 K are in good agreement with extrapolated equilibrium vapor pressures. It is shown that this technique may be a means to determine vapor pressures of refractory materials at high temperatures.
Mass spectrometric techniques and instrumentation for the dynamic sampling of laser-induced vapor clouds during their submillisecond expansion periods are discussed. Illustrations are drawn primarily from the results of pulsed-laser heating of some oxides and graphites; these include comparisons of incident laser beam pulses with the resultant pulses of positive ions and selected neutral species. Observed characteristics of vapor pulses from graphite are shown to correlate with calculated surface temperature response. Dynamic velocity measurements of individual vapor species are described and, from these velocities, vaporization temperatures are derived and compared using four gas dynamic models for vapor expansion into vacuum. Additional measurements indicate that the laser beam may interact directly with the neutral vapors to produce ions.
A laser has been combined with a mass spectrometer in a new configuration developed for studies of high-temperature materials. A vacuum-lock, solid-sample inlet is mounted at one end of a cylindrical, high-vacuum chamber one meter in length with a nude ion-source, time-of-flight mass spectrometer at the opposite end. The samples are positioned along the axis of the chamber at distances up to one meter from the ion source, and their surfaces are vaporized by a pulsed laser beam entering via windows on one side of the chamber. The instrumentation along with its capabilities is described, and results from laser-induced vaporization of several graphites are presented.
Several types of artificial graphite have been irradiated by laser pulses in vacuum, and the composition of the resulting vapor cloud has been determined in situ by mass spectrometric techniques in order to gain information pertaining to nonequilibrium ablation of graphitic probes entering planetary atmospheres. Results are discussed in terms of variations in concentrations of carbon species from their equilibrium values, and plotted curves illustrate the effect of nonequilibrium ablation on radiative shielding for simulated Jupiter entry conditions.
Development of time of flight mass spectrometer using laser powered vaporization source is discussed. Operation of equipment to measure thermal velocities of individual mass species is described. Illustration of test equipment installation and detailed line drawing of ion producing equipment are provided.