Total Oxide X-Ray Analyzer ARL ADVANTX Series Sequential X-Ray Fluorescence Spectrometers

Product Description

Introduction
The T otal Oxide X-ray Analyzer (TOXA) is a complete analytical package which provides the possibility to analyze by Wavelength Dispersive X-Ray Fluorescence (WD-XRF) a very large variety of minerals, e.g. dolomite, limestone, bentonite, marl, sand, laterite, feldspar, bauxite, magnesite, firebrick, silica brick, sillimanite, rocks, slags, cement, iron ores, etc...(Fig. 1). WD-XRF allows measurement of up to 83 elements of the periodic table in samples of various forms and nature: solids or liquids, conductive or non-conductive. Advantages of XRF over other techniques are speed of analysis, generally easy sample preparation, very good stability, precision and wide dynamic range (from ppm levels to 100%). Clay Dolomite Limestone Bentonite Marl Sand Laterite Cement Slags Refractories

Nr. 514
Traditional ceramics Feldspar Bauxite Magnesite

Firebrick Silica brick Rocks Iron Ores Phosphates

Fig. 1: Various applications determined by the ARL TOXA Element CaO SiO2 Fe2O3 MgO Al2O3 K2O MnO Cr2O3 TiO2 P2O5 SO3 Na2O Range [%] ignited samples 0.02 - 94.4 0.35 - 99.7 0.025 - 94 0.01 - 97.3 0.16 - 89.2 0.006 - 15.4 0.005 - 8 0.002 - 17.4 0.011 - 3.8 0.014 - 40.0 0.015 - 3.7 0.045 - 10.4 Typical SEE [%] ignited samples 0.21 0.17 0.15 0.10 0.11 0.05 0.04 0.03 0.03 0.04 0.05 0.05

Calibration ranges and results

The types of oxides which can be addressed and their concentration ranges are shown in Table 1. The Standard Error of Estimate (SEE) is a measure of the accuracy of analysis. It is the average error between the certified concentration of the standard samples and the calibration curve for any particular oxide type. The limits of detection (LOD) determined with precision tests at low concentrations are listed in T able 2 for the various oxides. The analysis time per element can range from 4 to 40 seconds depending on the element and the precision required. A working curve is established for each element using the Multi-Variable-Regression incorporated in the WinXRF software package. Theoretical alpha factors are used for all matrix corrections. Loss on ignition values, which spread up to 47 % can be used for correction purposes in the multi-variable regression.

T able 1: Concentration ranges of the various oxide types with the Standard Er rors of Estimate achieved
Element Typical LOD Typical LOD on ARL on ARL ADVANTXP ADVANTX (3 sigma) (3 sigma) [ppm] [ppm] Element Typical LOD Typical LOD on ARL on ARL ADVANTXP ADVANTX (3 sigma) (3 sigma) [ppm] [ppm]

Sample preparation
Standard samples are dried prior to being fused. Standards are prepared from ignited or non-ignited powder as 35 mm diameter fused beads. In case of ignition it is carried out for 1 hour at 1050C. The fusion is made from 0.6 grams of sample, 6.6 grams of Fluorex 65 and 0.02 grams of LiBr (dilution 1:12) on a Claisse Fluxer machine.

MnO Cr2O3 TiO2 P2O5 SO3 Na2O

6 7 6 13 15 143

15 16 15 30 35 330

CaO SiO2 Fe2O3 MgO Al2O3 K2O

8 47 15 36 13 9

20 115 36 85 30 20

T able 2: Typical limits of detection in 100s obtained on various oxides (fusions with 1:12 dilution)

ARLApplied Research Laboratories S.A.

En Vallaire Ouest C, case postale, CH-1024 Ecublens, Switzerland Tel. (++41)(21) 694 71 11, Fax (++41)(21) 694 71 12 e-mail: marketing@arl.ch - Internet: http://www.arl.ch

Two types of sample preparation can be used: a. No calcination of samples ( quicker preparation for clean oxides). Loss on ignition is estimated by the software, therefore all elements must be measured for this automatic correction to work. If other elements/oxides than the 12 measured are present, the loss on ignition should be introduced through manual input in order to improve accuracy of analysis. Note that fusion from non-ignited samples can be fatal for the Pt-Au crucible in case small metallic particles are present in the sample. b. Fusion from ignited samples ( better accuracy and safer fusion). Samples are ignited at 1050C for 1 hour and their loss on ignition (LOI) is determined. Samples are prepared from ignited powder as 35 mm diameter fused beads. Ignited samples are easier and safer to fuse especially in the case where small metallic particles are present.

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Total Oxide X-ray Analyzer package

The package consists of the following items:

ARL ADVANTX SeriesWD-XRF spectrometer

calibrated for the analysis of the most common oxide materials as shown above (either ADVANTX, ADVANTXP or ADVANTXP+). Claisse Fluxy, fusion machine to transform oxide materials into glass beads. 1 Pt/Au crucible and 1 Pt/Au mould. Ultrasonic bath to help clean mould and crucible after use. 1 kg Fluorex-65 (66%Li2B4O7-34% LiBO2): fusion flux 50 gr LiBr fusion additive. A set of six stable and polished setting-up samples for maintenance of the calibration curves over time (A0 36057, A0 38173 and A0 35918). The pre-calibration of the instrument is carried out in the factory at Ecublens, Switzerland using standards prepared on a Claisse Fluxy machine. No standard samples are delivered with this pre-calibration.

The descriptions contained herein were cor rect at the time of printing and are subject to alteration without notice. All orders are accepted subject to our current Conditions of Sale, copies of wich are available on request. ARL-CH publication XRF-04-923-0500-CH-e

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