fluorescence x-ray spectrometer system zsx · pdf filewavelengths are characteristic of the...
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1 IntroductionThe ZSX is a revolutionary WDXRF system that
combines innovative and powerful software with thebest available hardware technology. ZSX softwareincorporates Rigaku's long accumulated experienceand expertise in X-ray spectrometry analysis withcutting edge technology. While the ZSX is built onsolid, state-ofthe-art technology, it features a simpleuser interface. The novice is guided along with tem-plates that cover everything from sample preparationto control samples. And, the experienced XRF analyst can utilize the same interface to operate independently with a full suite of analytical capabilities. ZSX soft-ware contains the most advanced FP program avail-able and its EZ scan program allows rapid measure-ment of unknown samples with no prior setup.
The ZSX hardware incorporates the best available technology for high-sensitivity and high-resolutionmeasurements. Its design incorporates modular com-ponents that allow a wide variety of configu-rations.This design means that the ZSX is capable ofhardware upgrades on site. The ZSX can be configu-red with normal (tube above) or inverted (tube below)optics and high-powered side or end window X-raytubes. Its flexible layout means that valuable lab-
oratory space can be saved by remote location of theX-ray generator and heat exchanger.
ZSX Options include an R-Theta sample stage, aCCD camera and mapping capability for easy andrapid surface mapping for contamination testing.Micro-area analysis is possible down to 0.5 mm; and,with the exclusive high focus end window tube andhigh sensitivity optical system, there is a 10X increase in intensity when compared to existing micro areaanalysis systems offered.
The optional X-Y automatic sample changerprovides quick and reliable sample transport with orwithout sample cups. Applications Packages thatprovide turnkey solutions to applications problems,such as steels, brass, oils, refractories and cement, arealso available.
2. Features
(1) A new 3-axis (2-22-22) goniometer makes itpossible to select a detector arrangement according tothe analysis objective, specifically, high-sensitivityanalysis or high-resolution analysis.
(2) Accurate mapping and point analysis can berealized with the use of a CCD camera. This enablesthe operator to identify faulty portions of the sample
58 The Rigaku Journal
The Rigaku Journal
Vol. 16/ number 2/ 1999
Product Information
Fluorescence X-ray Spectrometer SystemZSX Series
The ZSX: Innovative XRF Technology-Accelerated.
with CCD viewing and to specify the location ofanalysis simply by a click of the mouse.
(3) A new r-2 stage is employed to allowmicroarea analysis with optimized conditions. Inmapping and point analysis, there is no effect from theunevenness of radiation from the X-ray tube or fromreflection with the analyzing crystal.
(4) The ZSX produces wavelength dispersive X-ray fluorescence analysis with a measurable samplediameter down to 50 :m.
(5) A variety of X-ray tubes are availableincluding a 30 :m thin window X-ray tube featuringhigh sensitivity for light elements and an X-ray tubeoptimal for small diameter samples.
(6) A tray system incorporated in the ASC(automatic sample changer) facilitates the control andconveyance of samples.
(7) The revolutionary software package contains a full suite of analysis capabilities with a simple,straightforward user interface.
(8) Windows NT Operating System.
3. Application Field
Application fields and specific examples are listed below.
Applications Examples
Electronics andmagnetic
LSI, memory disk, CRT parts, magnetic materials
Chemical industryCatalyst, polymer, pharma ceuticals,fertilizer, pigment, paint, oil & fat,detergent, cosmetics
Ceramics Silicon nitride, alumina, glass,refractories, enamel, cement
Steel Special steel, surface treat ment steelplate, ferroalloy, cast iron, cast steel,iron ores, plating liquid
Nonferrous metalsAluminum, shape memory alloy, copper alloy, precious metal, Ni alloy, solder,plating liquid
Mining Ore, rock, volcanic ash
Petroleum, coal Grease, lubricant, cutting oil, kerosene,heavy oil
Environmental analysis Waste water, seawater, river water, air-borne dust, in- dustrial wastes
Other Soil , rock, plant, organisms, foodstuff
4. Optical SystemFig. 1 shows the optical system of the ZSX. When
a sample is irradiated with the primary X-ray beamfrom an X-ray tube, fluorescent X-rays whose
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Fig. 1. New Optics of ZSX
wavelengths are characteristic of the elements in thesample will transpire. These secondary X-rays thenundergo spectral processing with the analyzing crystal and are detected by the detector (SC, F-PC). The ZSX
is equipped with a 3-axis (2-22-22) independentdriving goniometer. This allows for the selection ofthe offset arrangement for high-resolution analysis orfor the tandem arrangement for high-sensitivityanalysis (SC+F-PC arranged in series).
The SC detector can be equipped with an optionalhigh-sensitivity slit. This can be installed in additionto the standard high-resolution slit. This allows anoptimal combination to meet the desired analyticalrequirement. Fig. 2 shows a sensitivity comparisonchart for the tandem arrangement. The samplechamber employs a double vacuum system. Apreliminary vacuum chamber is also provided toenable evacuation for a subsequent sample whilemeasurement of the current sample is occurring.
5. r-2 Sample Stage and CCD Point AnalysisFigure 3 depicts the X-ray intensity distribution
that takes place with the primary X-rays. Theconventional design enables the maximum X-rayintensity to be obtained with a standard diametersample. However, for small diameter samples, themeasurement will occur at a position deviating fromthe maximum X-ray intensity. With the ZSX, the use
60 The Rigaku Journal
Fig. 2. Sensitivity Comparison Profiles in OffsetArrangement and Tandem Arrangement.
Fig. 3. Sensitivity Comparison by use of the r-2 stage.
of the r-2 stage makes it possible to performmeasurements at the maximum X-ray intensityposition even for small diameter samples. And, whenused with the CCD camera, this r-2 stage is especiallyeffective for mapping processing by CCD viewing aswell as for the analysis of a faulty portion on thesample.
Figure 4 shows the point analysis result of a rockby the use of the r-2 stage along with the CCD camera.
6. SoftwareThe ZSX software incorporates Rigaku's
longaccumulated experience and expertise in X-rayspectrometry analysis with cutting edge technology. It is so easy to use that even a novice can quickly use itcorrectly. The ZSX software configuration is shownbelow.
6.1. SQX(ScanQuantX)
Software for computation covering qualitativeanalysis through semiquantitative values.
6.2. EZ scan
Sophisticated SQX analysis can be performedwith five easy steps.
6.3. Application packages
Turnkey solutions for a variety of applications.These packages include standards set-up, optimalcalibration curves and program check standards.
6.4. Application templates
The user is guided along the analysis withtemplates that incorporate steps from samplepretreatment methods to measuring conditions upto control samples.
6.5. Universal standard samplesA database of commercially available standardreference samples is already in place. Noadditional data entry work is necessary.
6.6. Fixed-precision measurement
If a required precision is entered, the analysis iscarried out with the optimized measurement timefor each of the unknown samples.
6.7. Energy saving function
The X-ray output can be automatically reducedaccording to the amount of instrument idle time.
6.8. Automatic program run
This provides system ON/OFF, resumption afterpower failure, auto aging, PR gas flow control,etc.
6.9. Decision on material
Retrieval of standards is made, such as the JIS(Japanese Industrial Standard), for instance.
6. 10. E-mail transfer
The analysis result, an error message, or otherinformation can be e-mailed.
6. 11. Remote control
Remote-control operation can be made usingLAN.
6.12. Remote diagnosis
Diagnosis of the system status can be made fromthe Rigaku service station through e-mail.
6.13. Automatic selection of sample diameter
Automatic setting of the optimum area limitingdiaphragm is performed for a given samplediameter.
Vol. 16 No. 2 1999 61
Fig. 4. CCD Picture of Granite Sample and Comparison Chart.
62 The Rigaku Journal
Fig. 5. ZSX Software Configuration
ZSX100e ZSX101e ZSX100s ZSX101s
X-ray generator
Rated voltage & current
Voltage: 60 kV
Current: 150 mA (rkW spec.)
100 mA or 80 mA (ekW spec.)
(Upper limit of current value differs depending onthe tube type).
Voltage: 60 kV
Current: 80 mA
Max. Continuous Output 4 kW or 3 kW 3 kW
Stability "0.005% (for input variation "10%
Control Safety device (standard), energy saving run (standard), automatic program run (optional)
X-ray spectrometer assembly
X-ray tube
End window type
Single target: Rh, W, Mo (3kW)
Cr (2.4 kW)
Thin window type: Rh (3kW, 4kW)
Micro analysis handling type: Rh (4kW)
Dual target: Rh/Cr (3/2.4 kW), Rh/W (3/3 kW)
Side window type
Single target: Rh, Cr, W, Mo, Au (3kW)
Sample changer One sample feed, 12-turret, ASC48
Sample chamber
Sample inlet: Air lock system
Sample chamber inside turret: 2 positions with sample detector
Sample size: 51 mm N x 30 mm H max. (ZSX100e/100s)
51 mm N x 46 mm H max. (ZSX 101e/101s)
Stage Spinner or r-2 driving Spinner
Primary beam filter Select from Ti, Al, CU, Zr (2 kinds), and Fe One kind selectable from Ti, Al, Cu, Zr
7. Configuration, Specification
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ZSX100e ZSX101e ZSX100s ZSX101s
Area limiting diaphragm30 mm N fixed (no attenuator) or 35, 30, 25, 20, 10,3, 1, 0.5 mm N and attenuator exchanger
(For spinner or r-2 driving)
30 mm N fixed (no attenuator) or 35, 30, 25, 20, 10mm N (no attenuator exchanger)
(spinner)
Divergence slitStandard resolution, 1 kind, fixed or slit exchanger
Select from standard resolution, high resolution andultralight element use
Standard resolution, 1 kind, fixed or slit exchanger
Selection from standard resolution and highresolution
Receiving slit High resolution for SC (standard) high sensitivity for SC (optional), for F-PC (select for ZSX101e/101s)
Goniometer
2-22-22 3-axis independent drive system
Scan range: SC -1~118E (22)
F-PC 7~148E (22)
Scan speed: Max 1400E/min
Step angle: 1E/1000, 2E/1000, 5E/1000, 1E/100, 2E/100, 5E/100, 1E/100
Continuous scan: 0.1~240E /min (optional)
Crystal exchanger 10-crystal exchanger or 4-crystal exchanger
Analyzing crystalSelect from LIF(200) PET, Ge, TAP, RX-4, RX-9, RX-35, LiF (220)
Select from RX-40, RX-45, RX-60, RX-70, RX-80
Detector
For Ti~U: Scintillation counter (SC)
For Be~Zn: Gas-flow proportional counter (F-PC)
With center wire cleaner and gas density stabilizer
Vacuum system High-speed vacuum system (2 vacuum pumps), or general-purpose vacuum system (1 vacuum pump)
Temperature stabilizer Temperature for control: 36.5EC"0.1EC
OptionPowder sample attachment, automatic He substitution device, PR gas switching device, remote diagnosis,remote control, mapping device, sample observation mechanism