Vol. 12 No. 1 1995 41

THE RIGAKU JOURNAL VOL. 12 / NO.1 / 1995

ON-LINE MULTICHANNEL SIMULTANEOUS X-RAY SPECTROMETER SYSTEM

SIMULTIX 10S, SIMULTIX 11S

1. Introduction The Simultix 10S and Simultix 11S are new

version of the Simultix 10 and Simultix 11, re-spectively. They are equipped with an automatic sample loading mechanism at the sample inlet port. Samples from an automatic sample pretreat-ment device are automatically loaded onto a dedi-cated sample holder located at the sample loading mechanism. After the completion of analysis, the samples are automatically discharged from the dedicated holder. Because unattended analysis is performed in this way, manpower is saved and even faster analysis is feasible.

The following sample pretreatment devices are available: an ingot grinding/cutting system, crushing and shaping system, glass bead sampler, liquid dripping system, polymer hot press system and so on.

2. Features

(1) Manpower Saving by Using Various Sample Pretreatment Devices

a) Automatic bead sampler (electric furnace type, high frequency furnace type)

. . . Cement, slag, etc. b) Automatic powder sample preparator (ASP)

. . . Slag, sintered iron, etc. c) Automatic ingot grinder

. . . Pig iron, cast iron, etc. d) Automatic ingot cutter

. . . Copper alloy, aluminum alloy, etc. e) Liquid sample treatment device

. . . Electrolyte, plating solution f) Automatic polymer shape

. . . High polymer

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List of Sample Pretreatment Devices

(a) Automatic Glass Bead Sampler: Glass bead samples can be automatically pre-

pared by just adding spoonfuls of sample.

(d) Automatic Ingot Cutter: Nonferrous materials like aluminum, zinc, copper alloy, etc. may be cut into samples for analysis featur-ing high reproducibility. Automation of cutting and analysis is possible by combining this cutter with the Simultix.

(b) Automatic Sample Preparator (ASP): A briquette sample can be automatically prepared by just approx. 30 to 50 grams of powder sample. The sample is pulverized to 200 mesh. By combin-ing the ASP with the Simultrix, manpower savings can be made for the chain of work covering crush-ing, pressing and analysis.

(e) Liquid Sample Treatment Device: A sample suitable for analysis is automatically pre-pared. A prescribed amount of solution, e.g. electro-lyte, plating solution, etc. can be dropped onto a filter and dried. Control of the concentration of solution can be automated by combining the sampling system and the Simultix.

(c) Automatic Ingot Grinder: The automatic ingot grinder turn out samples fea-turing high reproducibility. Automation of grinding and analysis is possible by combining with the Simultix.

(f) Automatic Polymer Shaper: A maximum of 30 discs of polymer sample can I be automatically prepared by hot press when, approx. 6 grams of polymer is added per sample.

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(2) Analytical Range Newly developed goniometer and analyzing

crystals permit high-sensitivity and high-precision analysis covering Be through U. (3) Fast Operation

An automatic sample loading mechanism handles sample installation and removal to and from the sample holder automatically. (See 4. (1) Overall View.) Also, sample conveyance from the sample inlet port to the measurement position is made by a new one-step motion device, leading to substantial speed-up of operation. (4) Automatic Calibration of Analytical System

If a standard sample stocker (optional) is in-stalled, system calibration (PHA adjustment, stan-dardization) can be carried out automatically at the prescribed time by program run. (5) Safe Measurement of Powdery Samples and Filter Samples

The pumping speed and the lead speed can be set according to the type of sample to minimize

the potential scattering of powdery samples and filter samples. As a result, a long-term stable op-eration can be maintained. Further, a powder sample attachment (optional), if utilized, can sig-nificantly keep fine particles from mixing into valves and vacuum pumps. (6) Safe Maintenance

(1) The status of the analytical system can be known easily through regular display of its running condition. Besides, plentiful main-tenance functions are provided.

(2) In case of a trouble, the substance and cause of that abnormality are displayed to enable the operator to check and fix it promptly.

(3) A remote diagnostics function (optional) is provided to reduce the repair time.

The following are the major types of samples for measurement with the on-line type Simultix.

Type Sample size (mm) and shape after treatment Powder (iron ore) (Cement) (Slag) (Lime)

Pellet 4-7 t x 48-50 φ

Powder (iron ore) (Cement) (Slag)

Glass bead 3t x 35 φ

Ingot (pig iron, cast iron) (Aluminum) (Other nonferrous)

20-30t x 35-40 φ

Liquid Filter paper for dripping

3.2t x 48 φ

Chip-shape polymer 3t x 35 φ

3. Sample

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(2) Time Chart

1. A sample is mounted on IN-belt and conveyed to

the origin point. (IN-belt operation) 2. Pushing the sample to the inlet port from the origin

point. (transfer operation) 3. Conveyance from the inlet port to the analysis posi-

tion. Then after analysis, return to the inlet port again. (sample internal conveyance? analysis? take-out)

4. Sample discharge (arm OUT chute, vibrator operation)

(1) Overall View

4. Automatic Sample Loading Mechanism

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(3) Function of Each Part IN-belt : Carries a processed sample to a transfer mechanism consisting of an arm, stopper and

pusher. The sample diameter is then measured on the belt and if there is any sample whose diameter falls short of specification, the pusher is moved to the transfer retreat position and then the sample is discarded by driving of the IN-belt. Moreover, if another sample does not pass through the sample dia. counter within a cer-tain period after the IN-belt drive, it is regarded as an error.

Transfer : Carries a sample, which has been halted by a stopper, to each position with the aid of the pusher (arm). The transfer stop positions are called respectively the origin point, transfer retreat position, inlet port and sample discharge position in sequence from the bottom in the illustration.

Slot for discard: A bead sample or the like which is broken during conveyance will be discarded through the slots.

Leveler : A mechanism to load samples on the on-line sample holder, A cradle of the online sam-ple holder is vertically moved by the leveler in order to load on-line samples on the on-line sample holder. The leveler moving amount that depends on the sample thickness is mechanically fixed.

OUT chute: A sample-discharging device. After the sample is sent out to the discharge position, it is discharged through the chute, while being vibrated by a vibrator.

OUT belt : Carries the sample received from the chute to another position. This device is optional.

5. Configuration-Specifications

Hardware

Simultix 10S Simultix 11S Dimensions WxDxH mm 880x1300x1700 880x1100x1700

Analytical range 4Be ~ 92U X-ray generator Max. capacity

Max. voltage Max. current Stability Permissible line voltage varia-

tion

3 kW 60 kV 80 mA

Within ±0.01% for ±10% line deviation Rated value ±10%

X-ray tube Target Cooling system

Rh (AFX-76H) Distilled water recirculation system

(with ion exchange resin) No. of samples for loading Standard sample stocker

(optional) Sample irradiation Sample spin Atmosphere Vacuum system Max. sample size

8-samples turret (with automatic sample changer) 50 samples

Upper surface

60 rpm Air, vacuum, nitrogen (option), helium (option)

Direct-couple rotary pump/Pirani gauge (for vacuum level detection), with Automatic Pressure Control-ler (APC) 50.8 mm dia. X 25 mm thick (standard) 50.0 mm dia. X 30 mm thick (on-line)

No. of elements for simulta-neous analysis

Max. 30 elements (Optional: Max. 40)

Max. 16 elements

Sample chamber & spectrometric chamber

Temperature stabilizer Cabinet: 36.5±0.5°C Spectrometer: within 0.1°C (deviation)

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Fixed type Analyzing crystals: LiF, PET, RX4, Ge, NaCl, TAP, RX (synthetic) (synthetic multilayer film), etc. Curving system: Log spiral

Goniometer

Scanning type Programming system: Full angle continuous qualitative analysis/Element designated qualitative analy-sis/automatic identification analysis

Analyzing range: Heavy element 22Ti ~ 92U (analyzing crystal LiF) Light element 9F ~ 22Ti (analyzing crystal: TAP, PET, Ge with 3-crystal exchanger)

Detector

S-PC, SC F-PC: With gas density stabilizer and center wire

cleaner. Also with a buzzer alarm for gas pressure and flow rate.

Flow rate: Approx. 25 ml/min

Counting system/ System controller

Counting linearity Pulse height analyzer

S-PC: 4x106 cps/within 2% SC: 1x106 cps/within 2% F-PC: 4x106 cps/within 2% Automatic noise elimination circuit Automatic pulse height peak shift correcting circuit Automatic pulse height adjustment

Heat exchanger Distilled water recirculation system

Data Processing 32-bit multijob Mouse OS Printer CRT

O O OS/2 Dot matrix system (max. 132 characters/column) 15” color high resolution

Software FP software Automatic aging Theoretical matrix correction Automatic group selection Automatic measuring condition selection Automatic adjusting funtion (α, β, etc.) Calibration curve selection Calibration curve quantitation Automatic calibration curve correction Automatic bias correction Automatic identification analysis (qualitative analysis) Superposed drawing (qualitative analysis) Peak separation (qualitative analysis) Tabulation Transmission Self-diagnosis, health check Status display during analysis System maintenance Display of details at time of error Remote diagnostics

(O optional) O O O O O O (three curves) Linear, quadratic and cubic equations O (5 empirical interelement correction models) O O O (8 samples) O O O (O optional) O O O History (error, α, β, M values, self-diagnosis result,

number of analyses) O (O optional)

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On-line Multichannel Simultaneous X-ray Spectrometer system

-- External Dimensions –

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Specifications

Automatic Bead Sampler

• Sample Feeder Kind of sample Sample grain size Weighting Sample turret Flux feed Crucible turret

Cement, slag, various materials 100 µm, residue: Below 35% Minimum unit: 0.1 mg 12-sample turret 1000 cc container Screw feeder, automatic two-stage switchover system for feed amount (with shutter mechanism), Patent pending Flux ratio: 1 ~ 20 6-crucible turret

• Heating Section Heating system Output Heating temperature Temperature control Number for simultane-

ous fusing Heating time Stirring system

(High frequency furnace type) High frequency heating Max. 3 kW 500°C - 1250°C Work coil current control system ±10°C 1 piece Advanced burning: 0-60 min Fusion : 1-120 min Precession oscillation by rotation and

tilting (Patent pending)

(Electric furnace type) Electric resistance heating Max. 3 kW 1000°C - 1200°C PID control 3 pieces Advanced burning: 0-60 min Fusion : 1-120 min Rotation and tilting

• Bead Take-out & Conveyor Section Decision with crucible Decision by referring to crucible weight before and after bead making Decision with bead Decision on sticking and crack by the vacuum degree at time of take-out By vacuum adsorption Refusion function Refusion is possible after detection of sticking. Bead stocker 12-sample stocker • Utility Power supply require-

ment Grounding Cooling water Dimensions Weight

(high frequency furnace type) Single phase 200 V ± within 10%, 50 A Single phase 100 V ±within 10%, 5A Dedicated independent grounding: One Flow rate 1.3 lit/min Water pressure: 0.08 – 0.3 Mpa 0.8-3.0 kgf/cm2 Water temp.: Above 5°C and Below 35°C Water quality: City water or equivalent 1565(W) x 1300(D) x 1620(H) mm 850 kg

(Electric furnace type) Single phase 200 V± 10%, 50A Single phase 100 V± 10%, 1A One (grounding resistance: 100 Ω or less)

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Automatic Powder sample Preparator ASP • Crusher

Kind of sample Sample amount Sample grain size Grain size after crushing Crushing system Collection rate Cross contamination level Cleaning method Iron removing method

Slag, sintered ore, etc. Approx. 30-50 kg Max. 15 mm (with a coarse crusher for 10 to 300 mm) 200 mesh, Pass: 95% or more Coarse crushing: Jaw crusher Fine crushing: Disc mill 95% or more Less than 2% (Less than 0.2% is possible by flushing by forthcoming sample.) Air cleaning Electromagnetic drum (Patent pending)

• Pressure Shaper Pressure shaper

Punch for pressurizing

Max. 500 kN 50 tf, oil pressure system With a device to decide on the minimum amount of sample 2 units, with cleaner

• Utility Power supply requirement Grounding Dust collection duct Dimensions, weight

3-phase 200V ± within 10%, 50 A 3-phase 200V ± within 10%, 30 A (for dust collector) 3-phase 200V ± within 10%, 30 A (for compressor) One (grounding resistance: 100 Ω or less) Required Coarse crusher : 1300 (W) x 1850 (D) x 1970 (H) mm, 1000 kg Pressure shaper: 1220 (W) x 1300 (D) x 1900 (H) mm, 400 kg Cup feeder: 620 (W) x 780 (D) x 700 (H) mm, 100 kg Compressor: 1420 (W) x 420 (D) x 1000 (H) mm, 180 kg Dust collector: 650 (W) x 850 (D) x 2000 (H) mm, 100 kg

* The coarse crusher is not required when the max. grain size is below 15 mm.

Automatic Ingot Cutter • Cutter Kind of sample Sample processing time Cutting condition Tool

Copper alloy, aluminum alloy, etc. Within one min (for one-side grind-ing) Program control Throw-away tip/holder, 4 cutting edges

• Utility Power supply re-quirement Grounding Dimensions, weight

3-phase 200 V± within 10%, 20 A Single phase 100 V ± within 10%, 5 A One (grounding resistance: 100 Ω or less) 1647 (W) x 1530 (D) x 1935 (H) mm, 1600 kg

Automatic Ingot Grinder • Grinder Kind of sample Sample processing time Grinding condition Whetstone Dresser Cooling method

Pig iron, cast iron, etc. Within one min (for pig iron one-side grinding) Program control Cup type whetstone Air dresser Air cooling

• Utility Power supply re-quirement Grounding Dimensions, weight

3-phase 200 V± within 10%, 20 A Single phase 100 V ± within 10%, 5 A One (grounding resistance: 100 Ω or less) 1060 (W) x 850 (D) x 1475 (H) mm, 500 kg