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Fluorescence X-ray Spectrometer System ZSX Series - Rigaku

Fluorescence X-ray Spectrometer System ZSX Series - Rigaku

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The <strong>Rigaku</strong> Journal<br />

Vol. 16/ number 2/ 1999<br />

Product Information<br />

<strong>Fluorescence</strong> X-<strong>ray</strong> <strong>Spectrometer</strong> <strong>System</strong><br />

<strong>ZSX</strong> <strong>Series</strong><br />

The <strong>ZSX</strong>: Innovative XRF Technology-Accelerated.<br />

1 Introduction<br />

The <strong>ZSX</strong> is a revolutionary WDXRF system that<br />

combines innovative and powerful software with the<br />

best available hardware technology. <strong>ZSX</strong> software<br />

incorporates <strong>Rigaku</strong>'s long accumulated experience<br />

and expertise in X-<strong>ray</strong> spectrometry analysis with<br />

cutting edge technology. While the <strong>ZSX</strong> is built on<br />

solid, state-of­the-art technology, it features a simple<br />

user interface. The novice is guided along with templates<br />

that cover everything from sample preparation<br />

to control samples. And, the experienced XRF analyst<br />

can utilize the same interface to operate independently<br />

with a full suite of analytical capabilities. <strong>ZSX</strong> software<br />

contains the most advanced FP program available<br />

and its EZ scan program allows rapid measurement<br />

of unknown samples with no prior setup.<br />

The <strong>ZSX</strong> hardware incorporates the best available<br />

technology for high-sensitivity and high-resolution<br />

measurements. Its design incorporates modular components<br />

that allow a wide variety of configu-rations.<br />

This design means that the <strong>ZSX</strong> is capable of<br />

hardware upgrades on site. The <strong>ZSX</strong> can be configured<br />

with normal (tube above) or inverted (tube below)<br />

optics and high-powered side or end window X-<strong>ray</strong><br />

tubes. Its flexible layout means that valuable laboratory<br />

space can be saved by remote location of the<br />

X-<strong>ray</strong> generator and heat exchanger.<br />

<strong>ZSX</strong> Options include an R-Theta sample stage, a<br />

CCD camera and mapping capability for easy and<br />

rapid surface mapping for contamination testing.<br />

Micro-area analysis is possible down to 0.5 mm; and,<br />

with the exclusive high focus end window tube and<br />

high sensitivity optical system, there is a 10X increase<br />

in intensity when compared to existing micro area<br />

analysis systems offered.<br />

The optional X-Y automatic sample changer<br />

provides quick and reliable sample transport with or<br />

without sample cups. Applications Packages that<br />

provide turnkey solutions to applications problems,<br />

such as steels, brass, oils, refractories and cement, are<br />

also available.<br />

2. Features<br />

(1) A new 3-axis (2-22-22) goniometer makes it<br />

possible to select a detector arrangement according to<br />

the analysis objective, specifically, high-sensitivity<br />

analysis or high-resolution analysis.<br />

(2) Accurate mapping and point analysis can be<br />

realized with the use of a CCD camera. This enables<br />

the operator to identify faulty portions of the sample<br />

58 The <strong>Rigaku</strong> Journal


with CCD viewing and to specify the location of<br />

analysis simply by a click of the mouse.<br />

(3) A new r-2 stage is employed to allow<br />

microarea analysis with optimized conditions. In<br />

mapping and point analysis, there is no effect from the<br />

unevenness of radiation from the X-<strong>ray</strong> tube or from<br />

reflection with the analyzing crystal.<br />

(4) The <strong>ZSX</strong> produces wavelength dispersive X-<br />

<strong>ray</strong> fluorescence analysis with a measurable sample<br />

diameter down to 50 :m.<br />

(5) A variety of X-<strong>ray</strong> tubes are available<br />

including a 30 :m thin window X-<strong>ray</strong> tube featuring<br />

high sensitivity for light elements and an X-<strong>ray</strong> tube<br />

optimal for small diameter samples.<br />

(6) A t<strong>ray</strong> system incorporated in the ASC<br />

(automatic sample changer) facilitates the control and<br />

conveyance of samples.<br />

(7) The revolutionary software package contains a<br />

full suite of analysis capabilities with a simple,<br />

straightforward user interface.<br />

(8) Windows NT Operating <strong>System</strong>.<br />

3. Application Field<br />

Application fields and specific examples are listed<br />

below.<br />

Applications Examples<br />

Electronics and<br />

magnetic<br />

Chemical industry<br />

Ceramics<br />

Steel<br />

Nonferrous metals<br />

Mining<br />

Petroleum, coal<br />

Environmental analysis<br />

Other<br />

4. Optical <strong>System</strong><br />

LSI, memory disk, CRT parts, magnetic<br />

materials<br />

Catalyst, polymer, pharma ceuticals,<br />

fertilizer, pigment, paint, oil & fat,<br />

detergent, cosmetics<br />

Silicon nitride, alumina, glass,<br />

refractories, enamel, cement<br />

Special steel, surface treat ment steel<br />

plate, ferroalloy, cast iron, cast steel,<br />

iron ores, plating liquid<br />

Aluminum, shape memory alloy, copper<br />

alloy, precious metal, Ni alloy, solder,<br />

plating liquid<br />

Ore, rock, volcanic ash<br />

Grease, lubricant, cutting oil, kerosene,<br />

heavy oil<br />

Waste water, seawater, river water, airborne<br />

dust, in- dustrial wastes<br />

Soil , rock, plant, organisms, foodstuff<br />

Fig. 1 shows the optical system of the <strong>ZSX</strong>. When<br />

a sample is irradiated with the primary X-<strong>ray</strong> beam<br />

from an X-<strong>ray</strong> tube, fluorescent X-<strong>ray</strong>s whose<br />

Fig. 1. New Optics of <strong>ZSX</strong><br />

Vol. 16 No. 2 1999 59


wavelengths are characteristic of the elements in the<br />

sample will transpire. These secondary X-<strong>ray</strong>s then<br />

undergo spectral processing with the analyzing crystal<br />

and are detected by the detector (SC, F-PC). The <strong>ZSX</strong><br />

Fig. 2. Sensitivity Comparison Profiles in Offset<br />

Arrangement and Tandem Arrangement.<br />

is equipped with a 3-axis (2-22-22) independent<br />

driving goniometer. This allows for the selection of<br />

the offset arrangement for high-resolution analysis or<br />

for the tandem arrangement for high-sensitivity<br />

analysis (SC+F-PC arranged in series).<br />

The SC detector can be equipped with an optional<br />

high-sensitivity slit. This can be installed in addition<br />

to the standard high-resolution slit. This allows an<br />

optimal combination to meet the desired analytical<br />

requirement. Fig. 2 shows a sensitivity comparison<br />

chart for the tandem arrangement. The sample<br />

chamber employs a double vacuum system. A<br />

preliminary vacuum chamber is also provided to<br />

enable evacuation for a subsequent sample while<br />

measurement of the current sample is occurring.<br />

5. r-2 Sample Stage and CCD Point Analysis<br />

Figure 3 depicts the X-<strong>ray</strong> intensity distribution<br />

that takes place with the primary X-<strong>ray</strong>s. The<br />

conventional design enables the maximum X-<strong>ray</strong><br />

intensity to be obtained with a standard diameter<br />

sample. However, for small diameter samples, the<br />

measurement will occur at a position deviating from<br />

the maximum X-<strong>ray</strong> intensity. With the <strong>ZSX</strong>, the use<br />

Fig. 3. Sensitivity Comparison by use of the r-2 stage.<br />

60 The <strong>Rigaku</strong> Journal


Fig. 4. CCD Picture of Granite Sample and Comparison Chart.<br />

of the r-2 stage makes it possible to perform<br />

measurements at the maximum X-<strong>ray</strong> intensity<br />

position even for small diameter samples. And, when<br />

used with the CCD camera, this r-2 stage is especially<br />

effective for mapping processing by CCD viewing as<br />

well as for the analysis of a faulty portion on the<br />

sample.<br />

Figure 4 shows the point analysis result of a rock<br />

by the use of the r-2 stage along with the CCD camera.<br />

6. Software<br />

The <strong>ZSX</strong> software incorporates <strong>Rigaku</strong>'s<br />

longaccumulated experience and expertise in X-<strong>ray</strong><br />

spectrometry analysis with cutting edge technology. It<br />

is so easy to use that even a novice can quickly use it<br />

correctly. The <strong>ZSX</strong> software configuration is shown<br />

below.<br />

6.1. SQX(ScanQuantX)<br />

Software for computation covering qualitative<br />

analysis through semiquantitative values.<br />

6.2. EZ scan<br />

Sophisticated SQX analysis can be performed<br />

with five easy steps.<br />

6.3. Application packages<br />

Turnkey solutions for a variety of applications.<br />

These packages include standards set-up, optimal<br />

calibration curves and program check standards.<br />

6.4. Application templates<br />

The user is guided along the analysis with<br />

templates that incorporate steps from sample<br />

pretreatment methods to measuring conditions up<br />

to control samples.<br />

6.5. Universal standard samples<br />

A database of commercially available standard<br />

reference samples is already in place. No<br />

additional data entry work is necessary.<br />

6.6. Fixed-precision measurement<br />

If a required precision is entered, the analysis is<br />

carried out with the optimized measurement time<br />

for each of the unknown samples.<br />

6.7. Energy saving function<br />

The X-<strong>ray</strong> output can be automatically reduced<br />

according to the amount of instrument idle time.<br />

6.8. Automatic program run<br />

This provides system ON/OFF, resumption after<br />

power failure, auto aging, PR gas flow control,<br />

etc.<br />

6.9. Decision on material<br />

Retrieval of standards is made, such as the JIS<br />

(Japanese Industrial Standard), for instance.<br />

6. 10. E-mail transfer<br />

The analysis result, an error message, or other<br />

information can be e-mailed.<br />

6. 11. Remote control<br />

Remote-control operation can be made using<br />

LAN.<br />

6.12. Remote diagnosis<br />

Diagnosis of the system status can be made from<br />

the <strong>Rigaku</strong> service station through e-mail.<br />

6.13. Automatic selection of sample diameter<br />

Automatic setting of the optimum area limiting<br />

diaphragm is performed for a given sample<br />

diameter.<br />

Vol. 16 No. 2 1999 61


Fig. 5. <strong>ZSX</strong> Software Configuration<br />

7. Configuration, Specification<br />

X-<strong>ray</strong> generator<br />

<strong>ZSX</strong>100e <strong>ZSX</strong>101e <strong>ZSX</strong>100s <strong>ZSX</strong>101s<br />

Rated voltage & current<br />

Voltage: 60 kV<br />

Current: 150 mA (rkW spec.)<br />

100 mA or 80 mA (ekW spec.)<br />

(Upper limit of current value differs depending on<br />

the tube type).<br />

Voltage: 60 kV<br />

Current: 80 mA<br />

Max. Continuous Output 4 kW or 3 kW 3 kW<br />

Stability "0.005% (for input variation "10%<br />

Control<br />

Safety device (standard), energy saving run (standard), automatic program run (optional)<br />

X-<strong>ray</strong> spectrometer assembly<br />

X-<strong>ray</strong> tube<br />

Sample changer<br />

End window type<br />

Single target: Rh, W, Mo (3kW)<br />

Cr (2.4 kW)<br />

Thin window type: Rh (3kW, 4kW)<br />

Micro analysis handling type: Rh (4kW)<br />

Dual target: Rh/Cr (3/2.4 kW), Rh/W (3/3 kW)<br />

One sample feed, 12-turret, ASC48<br />

Side window type<br />

Single target: Rh, Cr, W, Mo, Au (3kW)<br />

Sample chamber<br />

Sample inlet: Air lock system<br />

Sample chamber inside turret: 2 positions with sample detector<br />

Sample size: 51 mm N x 30 mm H max. (<strong>ZSX</strong>100e/100s)<br />

51 mm N x 46 mm H max. (<strong>ZSX</strong> 101e/101s)<br />

Stage Spinner or r-2 driving Spinner<br />

Primary beam filter Select from Ti, Al, CU, Zr (2 kinds), and Fe One kind selectable from Ti, Al, Cu, Zr<br />

62 The <strong>Rigaku</strong> Journal


<strong>ZSX</strong>100e <strong>ZSX</strong>101e <strong>ZSX</strong>100s <strong>ZSX</strong>101s<br />

Area limiting diaphragm<br />

Divergence slit<br />

30 mm N fixed (no attenuator) or 35, 30, 25, 20, 10,<br />

3, 1, 0.5 mm N and attenuator exchanger<br />

(For spinner or r-2 driving)<br />

Standard resolution, 1 kind, fixed or slit exchanger<br />

Select from standard resolution, high resolution and<br />

ultralight element use<br />

30 mm N fixed (no attenuator) or 35, 30, 25, 20, 10<br />

mm N (no attenuator exchanger)<br />

(spinner)<br />

Standard resolution, 1 kind, fixed or slit exchanger<br />

Selection from standard resolution and high<br />

resolution<br />

Receiving slit<br />

Goniometer<br />

Crystal exchanger<br />

Analyzing crystal<br />

Detector<br />

Vacuum system<br />

Temperature stabilizer<br />

Option<br />

High resolution for SC (standard) high sensitivity for SC (optional), for F-PC (select for <strong>ZSX</strong>101e/101s)<br />

2-22-22 3-axis independent drive system<br />

Scan range: SC -1~118E (22)<br />

F-PC 7~148E (22)<br />

Scan speed: Max 1400E/min<br />

Step angle: 1E/1000, 2E/1000, 5E/1000, 1E/100, 2E/100, 5E/100, 1E/100<br />

Continuous scan: 0.1~240E /min (optional)<br />

10-crystal exchanger or 4-crystal exchanger<br />

Select from LIF(200) PET, Ge, TAP, RX-4, RX-9, RX-35, LiF (220)<br />

Select from RX-40, RX-45, RX-60, RX-70, RX-80<br />

For Ti~U: Scintillation counter (SC)<br />

For Be~Zn: Gas-flow proportional counter (F-PC)<br />

With center wire cleaner and gas density stabilizer<br />

High-speed vacuum system (2 vacuum pumps), or general-purpose vacuum system (1 vacuum pump)<br />

Temperature for control: 36.5EC"0.1EC<br />

Powder sample attachment, automatic He substitution device, PR gas switching device, remote diagnosis,<br />

remote control, mapping device, sample observation mechanism<br />

Vol. 16 No. 2 1999 63

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