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Mar 1988

Volume 59, Issue 3, pp. 407-515

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Inelastic x‐ray scattering with fluorescence coincidence detection using a pulsed synchrotron source

Vincent Marchetti and Carl Franck

Rev. Sci. Instrum. 59, 407 (1988); http://dx.doi.org/10.1063/1.1140218 (7 pages) | Cited 4 times

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We describe a system used to measure the spectrum of x rays scattered inelastically from K‐shell electrons using a coincidence technique. The source of the x rays was a pulsed synchrotron source. We describe fast–slow coincidence logic adapted for use with a pulsed source of fluctuating intensity, describe in detail the background subtraction and statistical noise in the measurement, and present the results of measurements made with the system. The precautions used to avoid detector‐to‐detector scattering are also described. The combination of high source intensity and coarse time resolution (due to the pulsed nature of the source) put us in the regime for much of the scattered x‐ray spectrum, in which the number of accidental coincidences greatly exceeded the number of true signal counts. We show that in this case significant reductions in statistical uncertainty may not be achieved by further increases in source intensity.
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07.85.-m X- and γ-ray instruments
78.70.Ck X-ray scattering

Calibration of pulsed x‐ray spectra

J. A. Anderson and C. B. Collins

Rev. Sci. Instrum. 59, 414 (1988); http://dx.doi.org/10.1063/1.1140219 (6 pages) | Cited 8 times

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A new technique has recently been described for the absolute calibration of intense sources of pulsed radiation in the 0.2–1‐MeV range of photon energies. An x‐ray activation technique, it depended upon the storage of samples of the irradiating spectrum in the form of populations of nuclei excited to isomeric states with lifetimes of seconds to hours. Accuracy was dependent upon the precision assumed for tabulated values of nuclear parameters. Described here is an extension of this technique to the larger range of photon energies, 0.2–1.5 MeV and to intensities from 1012 keV/keV to 1016 keV/keV using the target nuclei 79Br and 77Se. In this work self‐consistency of the nuclear parameters was directly determined. Important changes were found to be necessary for improved accuracy, particularly over the larger ranges of experimental variables being considered. Values of the now‐consistent set of nuclear parameters are reported.
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07.85.-m X- and γ-ray instruments
29.25.-t Particle sources and targets
29.30.Kv X- and γ-ray spectroscopy

High precision alignment of x‐ray transmission diffraction gratings

Andrew M. Hawryluk and Sherry L. Hill

Rev. Sci. Instrum. 59, 420 (1988); http://dx.doi.org/10.1063/1.1140220 (3 pages)

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Gold transmission diffraction gratings used for x‐ray spectroscopy must often be aligned rotationally to within submilliradian accuracy of an instrument axis. Currently, these gratings have a high line density (grating periods less than 300 nm) so conventional techniques (such as optical imaging or diffraction) which have been used previously to determine the grating orientation cannot work. Other techniques (such as polarization effects) give <1‐mrad accuracy. We describe here a simple technique that allows one to produce an optically observable alignment mark that is oriented parallel to the grating direction within a few microradians. We ‘‘write’’ a line, ∼0.01‐mm wide, directly on the grating by exposing an electron‐beam‐sensitive coating of polymethylmethacrylate (PMMA) on the grating while driving the grating through the beam of a scanning electron microscope (SEM). The direction of motion is made parallel to the grating lines by controlling the stage motion with a joystick while inspecting the grating in the SEM. Using the joystick, one can ‘‘follow’’ a single grating line from end to end. The SEM written line is made a permanent addition to the grating by ion‐beam etching or gold microplating, and can later be used for in situ alignment verification. Our lines have been made parallel to the original grating lines to approximately ±5 μrad; this alignment can be extended to ±1 μrad. Standard optical techniques can be used to align the grating with respect to an arbitrary instrument axis. This technique works equally well with transmission and reflection gratings.
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07.85.-m X- and γ-ray instruments
42.79.Dj Gratings
42.86.+b Optical workshop techniques

Low‐pressure, automated, sample packing unit for diffuse reflectance infrared spectrometry

Alfred A. Christy, Jan Erik Tvedt, Terje V. Karstang, and Rance A. Velapoldi

Rev. Sci. Instrum. 59, 423 (1988); http://dx.doi.org/10.1063/1.1140221 (4 pages) | Cited 12 times

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An automatic, low‐pressure packing unit has been designed with control of packing time and pressure to prepare powder samples for diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS). This unit also provides a polished packing surface that ensures constant measurement height of the sample in the spectrometer. Use of this unit coupled with sample rotation during measurement and control of particle size and size distribution, provides excellent precision in obtaining DRIFTS spectra. For example, repackings by a single person or by several untrained people gave coefficients of variation from 0.8% to 2.3% for each digital spectral value for a coal sample and from 1.3% to 3.7% for thymol blue, a sharp spectral featured organic, rather than the 15%–30% normally found for repackings of the same sample. Thus representative DRIFTS spectra can be obtained quickly and efficiently from a powder sample with a single spectrum using this low‐pressure, mechanical packing device, control of particle parameters, and sample rotation as opposed to previous efforts requiring the repacking of several samples and averaging of the spectra.
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07.10.-h Mechanical instruments and equipment
06.60.Ei Sample preparation (including design of sample holders)
07.57.Ty Infrared spectrometers, auxiliary equipment, and techniques

Plasma emission spectroscopy with an optical fiber probe

Z. J. Jin, Chung Chan, and Christopher Whitaker

Rev. Sci. Instrum. 59, 427 (1988); http://dx.doi.org/10.1063/1.1140222 (3 pages) | Cited 3 times

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We have developed an optical fiber probe which is well suited for measuring localized light emission in plasmas. The plasma emission intensity distribution along the axis of a parallel‐plate rf glow discharge has been used as an example for comparing measurements between the optical fiber probe and the standard lens‐slit system.
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42.81.Pa Sensors, gyros
07.07.Df Sensors (chemical, optical, electrical, movement, gas, etc.); remote sensing
07.60.-j Optical instruments and equipment
52.70.Kz Optical (ultraviolet, visible, infrared) measurements

Nanoradian sensitivity Kerr effect apparatus

D. P. Shelton and Ruth E. Cameron

Rev. Sci. Instrum. 59, 430 (1988); http://dx.doi.org/10.1063/1.1140223 (4 pages) | Cited 5 times

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The shot‐noise limit to the sensitivity of ellipsometric phase shift measurements with a laser beam power of a few mW is of the order of 10−9 rad. An apparatus is described that realizes shot‐noise‐limited performance for dc Kerr effect birefringence measurements.
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07.60.Fs Polarimeters and ellipsometers
33.15.Kr Electric and magnetic moments (and derivatives), polarizability, and magnetic susceptibility
07.77.-n Atomic, molecular, and charged-particle sources and detectors
37.20.+j Atomic and molecular beam sources and techniques
51.70.+f Optical and dielectric properties

Electronic device for the analysis of electron diffraction patterns

A. Trzynka and M. Takeo

Rev. Sci. Instrum. 59, 434 (1988); http://dx.doi.org/10.1063/1.1140255 (4 pages) | Cited 1 time

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Using a video camera, a video digitizer, and a microcomputer, an image processing system is assembled to determine the locations of electron diffraction spots on photographic negatives of electron diffraction patterns. This system can help to reduce the measurement time to one third when compared with conventional manual methods and produces results with better accuracy and less operator fatigue.
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61.05.J- Electron diffraction and scattering
07.78.+s Electron, positron, and ion microscopes; electron diffractometers

System for simultaneous count/current measurement with a dual‐mode photon/particle detector

Michael J. Kristo and Christie G. Enke

Rev. Sci. Instrum. 59, 438 (1988); http://dx.doi.org/10.1063/1.1140224 (5 pages) | Cited 4 times

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A microcomputer‐based control system for a dual‐output Channeltron (TM) detector has been developed and implemented. This system is capable of collecting ion current and ion‐counting information simultaneously. Ion current and ion‐counting data are scaled in software and provide consistent ion intensity values from both outputs. Calculation of the ion current/ion count rate ratio at each peak in the mass spectrum allows the system to compensate for variations in gain from peak to peak. The data collection system maximizes the data collection rate and extends the useful dynamic range of electron multiplier‐based detection to nine orders of magnitude with no change in any of the multiplier conditions. Measurement of such a wide range of ion intensities in a single spectrum is particularly useful for applications in tandem mass spectrometry.
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07.75.+h Mass spectrometers
07.05.Hd Data acquisition: hardware and software
07.05.Kf Data analysis: algorithms and implementation; data management
07.05.Rm Data presentation and visualization: algorithms and implementation

Ion source for production of metastable He+(2S1/2) ions

R. W. Dunford and M. S. Dewey

Rev. Sci. Instrum. 59, 443 (1988); http://dx.doi.org/10.1063/1.1140225 (5 pages)

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The construction and performance of an electron bombardment ion source designed to produce a beam of low‐energy (100–400 eV) singly ionized helium (He+) with a significant fraction of ions in the metastable 2S1/2 state is described. The source operates in the fringe field of a magnet and injects ions along the field lines into the center of the magnet. He+ currents of up to 70 μA with small beam energy spread (3 eV) are obtained. A typical metastable fraction is 0.08% for small He+ currents (2–5 μA).
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29.25.Lg Ion sources: polarized
29.25.Ni Ion sources: positive and negative
79.20.-m Impact phenomena (including electron spectra and sputtering)

Low power, 3.2‐cm, efficient microwave electron cyclotron resonant ion source

L. Mahoney, M. Dahimene, and J. Asmussen

Rev. Sci. Instrum. 59, 448 (1988); http://dx.doi.org/10.1063/1.1139858 (5 pages) | Cited 10 times

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Design improvements in a microwave (2.45‐GHz) plasma disk ion source have resulted in a compact, efficient, and low power ion source capable of delivering ion beam current densities in excess of 10 mA/cm2 . The ion source has been designed for a 3.2‐cm‐diam double graphite extraction grid set. Ion beam extraction was studied using argon and oxygen discharges with input gas flows of 1–5 standard cubic centimeters per minute (sccm) and input powers under 150 W. Ion beam currents of 20 to over 40 mA were obtained at extraction potentials of 1600 V. Double Langmuir probe measurements were made for argon, and by using a free‐fall diffusion model, extracted beam current densities were shown to be consistent with measured discharge electron and ion densities. These experiments demonstrate the ability of microwave plasma technology to produce high beam current densities for both inert and chemically reactive gases. The compact electron cyclotron resonant microwave ion source shows significant improvements in efficiency, lifetime, and ion beam current densities over earlier designs and over similar size conventional broad beam dc and rf ion sources.
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52.75.-d Plasma devices
52.25.Tx Emission, absorption, and scattering of particles
52.50.Gj Plasma heating by particle beams

Small multicusp H− source

K. N. Leung, K. W. Ehlers, C. A. Hauck, W. B. Kunkel, and A. F. Lietzke

Rev. Sci. Instrum. 59, 453 (1988); http://dx.doi.org/10.1063/1.1139859 (4 pages) | Cited 25 times

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High‐quality H− beams have been generated from a multicusp source equipped with a permanent magnet filter. It is shown that a large improvement in H− yield can be achieved by employing a small multicusp source, fabricated with the proper wall material and extraction chamber length. From this small source, H− current densities higher than 250 mA/cm2 have been extracted from a 1‐mm‐diam aperture for a discharge voltage of 150 V and a discharge current of 450 A. When the source is operated with deuterium, the extractable negative ion current density is reduced by approximately 30%.
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29.25.Lg Ion sources: polarized
29.25.Ni Ion sources: positive and negative

Thomson parabola ion energy analyzer with a coincident and jitter‐free applied electric field ramp

H. Yoneda, K. Horioka, Y. Kim, and K. Kasuya

Rev. Sci. Instrum. 59, 457 (1988); http://dx.doi.org/10.1063/1.1139860 (3 pages) | Cited 2 times

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A simple Thomson parabola ion energy analyzer for intense pulsed ion beam is demonstrated. Beam ions collimated by two apertures, are deflected by a time ramping electric field and a static magnetic field. The ramping electric field is produced with a stacked cable pulser powered by a voltage divider of the pulse power generator. As there is no additional switching tube and no high‐voltage generator other than the main machine, the analyzer has an electric field ramp that is coincident and has no jitter with the ion beam. A temporal history of ion beam energy is measured as an example and a reasonable agreement with the measured diode voltage is obtained.
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07.78.+s Electron, positron, and ion microscopes; electron diffractometers
07.77.-n Atomic, molecular, and charged-particle sources and detectors
41.20.Cv Electrostatics; Poisson and Laplace equations, boundary-value problems
41.20.Gz Magnetostatics; magnetic shielding, magnetic induction, boundary-value problems

Magnetic surface mapping with highly transparent screens on the Auburn torsatron

G. J. Hartwell, R. F. Gandy, M. A. Henderson, J. D. Hanson, D. G. Swanson, C. J. Bush, R. J. Colchin, A. C. England, and D. K. Lee

Rev. Sci. Instrum. 59, 460 (1988); http://dx.doi.org/10.1063/1.1139861 (7 pages) | Cited 28 times

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In stellarator‐type magnetic confinement devices (of which the torsatron is one), the magnetic field is produced entirely by external, current‐carrying coils. Two methods for mapping magnetic surfaces in the Auburn torsatron were tested and compared, both of which involve the use of highly transparent screens. The first method consists of coating the screen with a phosphor that emits light when struck by electrons emitted by an electron gun. A pattern representative of a magnetic surface is formed on the screen, and this pattern is recorded photographically. The second method uses an uncoated screen to collect electrons emitted from an emissive probe, which is scanned over a poloidal cross section of the torus. Under certain conditions, the collected current is a constant over a particular magnetic surface so that a contour plot of the current versus position is equivalent to a plot of the magnetic surfaces. Parametric studies of the two methods are presented, and the effectiveness of each technique is discussed.
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52.55.Jd Magnetic mirrors, gas dynamic traps
52.70.Ds Electric and magnetic measurements
07.50.-e Electrical and electronic instruments and components
07.55.-w Magnetic instruments and components

Automatic system for the control of batch‐produced 11CO2 for continuous labeling experiments

C. J. McKinney, Y. Fares, C. E. Magnuson, C. H. Jaeger, J. D. Goeschl, and J. L. Need

Rev. Sci. Instrum. 59, 467 (1988); http://dx.doi.org/10.1063/1.1139862 (3 pages) | Cited 2 times

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A system for storage and continuous dispensing of constant activity 11CO2 from batch production is described. The system has been used successfully to maintain constant activity levels for 2‐h plant tracer kinetic experiments. This development now allows any existing cyclotron facility to supply a radioisotope stream continuously from a short batch irradiation. It requires no modification for use with other isotopes such as N‐13 or O‐15 in gaseous form and can be used in other biological and clinical investigations as well as the plant physiology investigations for which it was developed.
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87.56.bd Accelerators
87.85.E- Neural prosthetics
87.85.F- Smart prosthetics
87.80.-y Biophysical techniques (research methods)
87.16.D- Membranes, bilayers, and vesicles
87.85.-d Biomedical engineering

Apparatus for the measurement of compressibility isotherms of gases up to 10 kbar: Experimental data for argon at 298.15 K

S. N. Biswas, N. J. Trappeniers, P. J. Kortbeek, and C. A. ten Seldam

Rev. Sci. Instrum. 59, 470 (1988); http://dx.doi.org/10.1063/1.1139863 (7 pages) | Cited 10 times

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An apparatus for the measurement of compressibility isotherms of gases up to pressures of 10 kbar and at temperatures between 273 and 350 K is described. It is based on a gas expansion method in which the pressure distortion of the experimental volume is evaluated by calibration with the measuring gas at lower pressures. The apparatus can easily be adapted for isochoric measurements over a wide temperature range. Measurements on argon at 298.15 K show that the method is capable of giving a precision of 0.02%–0.06% for the density, 0.1% for the pressure, and 2 mK for the temperature.
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07.35.+k High-pressure apparatus; shock tubes; diamond anvil cells
51.30.+i Thermodynamic properties, equations of state

Characteristics of a thermal gas flowmeter

K. Komiya, F. Higuchi, and K. Ohtani

Rev. Sci. Instrum. 59, 477 (1988); http://dx.doi.org/10.1063/1.1139864 (3 pages) | Cited 6 times

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The characteristics of a thermo tube type thermal gas flowmeter were analyzed and experimental results were described. The output of this flowmeter is temperature difference between two points along an electrically heated capillary. An analytical expression of its outputs was derived assuming a simple flow condition. An experimental prototype was constructed. The temperature distribution was measured and the outputs were obtained for three kinds of gases: nitrogen, carbon dioxide, and argon. Those outputs were compared with theoretical ones, and those agree well in the case of small flow rate. The relationship among temperature difference, mass flow rate, and specific heat of gas was discussed.
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47.80.-v Instrumentation and measurement methods in fluid dynamics
51.30.+i Thermodynamic properties, equations of state

In situ magnetization loop tracer for thin‐film growth

J. B. Haugdahl and D. R. Miller

Rev. Sci. Instrum. 59, 480 (1988); http://dx.doi.org/10.1063/1.1139865 (4 pages) | Cited 7 times

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A thin‐film loop tracer is described which is straightforward to construct, rugged, has a sensitivity of at least 10−6 emu at fields to 3000 Oe, and a bandwidth of 1 megacycle. The device is readily adaptable for in situ ultrahigh‐vacuum measurements.
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07.55.-w Magnetic instruments and components
75.70.Ak Magnetic properties of monolayers and thin films

Rapid separation of fine particles with narrow size distribution

Ichiro Aoki, Kotaro Shirane, Takayuki Tokimoto, and Masatugu Kimura

Rev. Sci. Instrum. 59, 484 (1988); http://dx.doi.org/10.1063/1.1139866 (2 pages)

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In a rotating tube with steady (laminar) flow (RSF) or with alternate flow (RAF) method for separation of fine particles, a simple and practical formula giving the relationship between the particle velocity (RSF velocity) along the tube length and parameter Aω0/V0 is derived, where A is the tube radius, ω0 is its angular velocity, and V0 is the sedimentation velocity of a particle. The chromatographic classification by these helical orbit sedimentation methods with laminar flow have been investigated with the formula in detail. In the flow methods the lowest size for biological and chemical samples with density ρ(≳1.05 g/cm3) is estimated as ∼10 μm when the tube with 2–4 mm i.d. and length L∼1 m is used.
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07.10.-h Mechanical instruments and equipment
47.80.-v Instrumentation and measurement methods in fluid dynamics

High‐accuracy oxygen polarograph for photosynthetic systems

P. C. Meunier and R. Popovic

Rev. Sci. Instrum. 59, 486 (1988); http://dx.doi.org/10.1063/1.1139867 (6 pages) | Cited 5 times

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A new system is presented here, whose design is based on the electrochemical phenomena occurring on the platinum electrode that we examined before [P. Meunier and R. Popovic (unpublished)]. The architecture of the system is articulated around an IBM‐PC computer which controls the polarization of the electrodes, the triggering of the flash lamp, and the acquisition of data. The potentiostat circuit and new electrode design improve the response of the electrode to a rise time of 4 ms and a decay time constant of 21 ms, without the signal being distorted by filters and without using the first derivative of the signal. This polarograph shows a 50‐dB signal‐to‐noise ratio (0.3% error) during experiments with the motile algae Dunaliella tertiolecta. The determination of amplitudes of oxygen production is performed with third‐order cubic spline interpolations, after subtraction of the current base line. The resulting accuracy and reproducibility will enable researchers to attain a higher degree of refinement in the quantification of properties of the oxygen evolving complex.
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82.80.Yc Rutherford backscattering (RBS), and other methods of chemical analysis
07.60.-j Optical instruments and equipment
07.05.Hd Data acquisition: hardware and software
07.05.Kf Data analysis: algorithms and implementation; data management
07.05.Rm Data presentation and visualization: algorithms and implementation
82.50.-m Photochemistry

Automated system for relative sound velocity and ultrasonic attenuation measurements

J. Toulouse and C. Launay

Rev. Sci. Instrum. 59, 492 (1988); http://dx.doi.org/10.1063/1.1139868 (4 pages) | Cited 9 times

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In order to facilitate measurements of ultrasonic velocity and attenuation, we have developed an automated version of the phase sensitive technique with quadrature detection. The technique is outlined and the precision of relative transit time or velocity measurements that can be obtained from it is analyzed. We describe the computer‐controlled experimental setup and report relative velocity and attenuation results obtained on a single crystal of pure KZnF3 . The temperature dependence of the elastic constants C11 and C44 calculated from these results agree very well with that obtained from echo overlap measurements performed on the same crystal. The relative error on the present velocity measurements is Δv/v∼10−5 .
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43.35.Cg Ultrasonic velocity, dispersion, scattering, diffraction, and attenuation in solids; elastic constants
07.05.Hd Data acquisition: hardware and software
07.05.Kf Data analysis: algorithms and implementation; data management
07.05.Rm Data presentation and visualization: algorithms and implementation

Four‐probe single‐crystal holder for conductivity measurements

John Papaioannou and James L. Dye

Rev. Sci. Instrum. 59, 496 (1988); http://dx.doi.org/10.1063/1.1139869 (2 pages) | Cited 3 times

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The development and testing of a four‐probe small single‐crystal holder for conductivity studies down to liquid‐helium temperature is described. A single crystal of the reactive sodide, Na+C222⋅Na–, was successfully mounted, but its resistance was too high to permit determination of the conductivity. The method should be useful for single‐crystal conductivity measurements of reactive and/or thermally unstable crystals.
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07.10.-h Mechanical instruments and equipment
07.50.-e Electrical and electronic instruments and components

Small oven for obtaining temperatures to 1350 °C

J. E. Gordon

Rev. Sci. Instrum. 59, 497 (1988); http://dx.doi.org/10.1063/1.1139870 (2 pages)

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A small, inexpensive oven capable of achieving a temperature of 1350 °C with a power consumption of less than 1 kW is described. The oven has a working volume which is roughly 10×6×12 cm. It has been used for bonding gold to sapphire substrates, but would be suitable for use in any application which requires elevated temperatures in a working volume of 500–1000 cm3.
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07.20.Hy Furnaces; heaters

Time response of small side‐on photomultiplier tubes in time‐correlated single‐photon counting measurements

Erich C. Meister, Urs P. Wild, Peter Klein‐Bölting, and Alfred R. Holzwarth

Rev. Sci. Instrum. 59, 499 (1988); http://dx.doi.org/10.1063/1.1139871 (3 pages) | Cited 8 times

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The position‐dependent time response of eight small side‐on type photomultiplier tubes (Hamamatsu R928 and R955) has been investigated. Using the method of time‐correlated single‐photon counting relative transit times, single‐photon response widths and relative quantum yields have been determined. This characterization provides the basis for the proper selection and use of fast photomultiplier tubes in single‐photon counting experiments.
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85.60.Ha Photomultipliers; phototubes and photocathodes
85.60.Gz Photodetectors (including infrared and CCD detectors)
07.57.Kp Bolometers; infrared, submillimeter wave, microwave, and radiowave receivers and detectors

Optical alignment device for x‐ray diffraction systems

S. Prawer and S. W. Wilkins

Rev. Sci. Instrum. 59, 501 (1988); http://dx.doi.org/10.1063/1.1139872 (2 pages)

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A device is described which enables x‐ray diffraction systems to be aligned optically using a collimated laser beam to mimic the x‐ray beam path through the system. Alignment using the device is faster and safer than the conventional procedures.
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07.85.-m X- and γ-ray instruments
61.05.C- X-ray diffraction and scattering

Dark‐field microscopy of transparent objects with a bright‐field objective

A. W. Hartman

Rev. Sci. Instrum. 59, 502 (1988); http://dx.doi.org/10.1063/1.1139873 (2 pages)

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Described is a simple modification of a standard bright‐field objective to produce dark‐field imagery of transparent objects.
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07.60.Pb Conventional optical microscopes
06.60.Ei Sample preparation (including design of sample holders)
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