AU2007202706A1

AU2007202706A1 - X-ray flux composition mixture

Info

Publication number: AU2007202706A1
Application number: AU2007202706A
Authority: AU
Inventors: David Brown
Original assignee: X Ray Flux Pty Ltd
Current assignee: X Ray Flux Pty Ltd
Priority date: 2007-05-04
Filing date: 2007-06-13
Publication date: 2008-11-20
Anticipated expiration: 2027-06-13
Also published as: AU2007202706B2

Description

Specification for Patent Application Title: "X-Ray Flux Composition Mixture" Applicant: Country: Type: Number: X-Ray Flux Pty Ltd 88 Guthrie St., Osborne Park, West Australia 6017 Australia Standard Date: 12 June 1007 Title "X-RAY FLUX COMPOSITION MIXTURE Specification The following statement is a full description of this invention, including the best method of performing it known to me: Field of the Invention This invention relates to the analysis of samples or ores and in particular to an xray flux composition mixture for the x-ray fluorescence spectroscopy analysis of such samples or ores. The aforesaid composition mixture specifically contains boron oxide as one component of the combined sample or ore plus x-ray flux composition mixture before fusion and analysis.

Description Throughout the description, unless the context requires otherwise, the word "comprise" or variations such as "comprises" or "comprising", will be understood to imply the inclusion of a stated integer or group of integers but not to the exclusion of any other integer or group of integers.

Background X-ray flux is produced by fusing at high temperatures approximately 1100 degrees C. in platinum or platinum alloy crucibles, chemicals containing lithium and boron. The molten material is then cooled and reduced in size to a powder or coarse material by grinding or crushing. The resultant material is x-ray flux and is usually represented or specified in the final commercial product as ratios of lithium tetraborate to lithium metaborate.

The x-ray flux is then mixed with samples of materials or ores to be analyzed and a second fusion is carried out in a platinum or platinum alloy mold. Alternatively, the x-ray flux/sample mixture is fused in a platinum or platinum alloy crucible and poured into a platinum or platinum alloy mold. The mold is cooled and the result is a glass like disc which is then placed into an x-ray fluorescence spectrograph machine for analysis.

Previous difficulties Previous practice for the analysis of samples or ores involves two distinct time consuming sequential mixing and melting or fusing steps, with pick up of contaminating materials from the size reduction by grinding or crushing of material involved post melting in the first step. The first step of mixing and fusion involves mixing a boron containing compound with a lithium containing compound and fusing or melting the mixture at about 1100 degrees centigrade in a platinum or platinum alloy crucible or apparatus to form a molten x-ray flux. The molten x-ray flux is then poured into a cooling tray and the resultant cooled x-ray flux is reduced to a fine powder or granules by grinding or crushing. During this size reduction process in the first step, there is a pick up of contaminating materials from the grinding or crushing equipment used. The second step of mixing and fusion involves mixing of the powder or granular previously produced x-ray flux together with samples or ores to be analyzed and fusing or melting the resultant mixture at high temperature in platinum or platinum alloy crucibles or molds to form a liquid. This liquid is melted in a crucible and then poured into a mold to form a disc and the resultant disc is analyzed by an x-ray spectrograph.

Inventive Step The inventor has found that it was hitherto unknown that specifically boron oxide can be fused at high temperature with lithium containing compounds plus samples or ores to be analyzed in platinum or platinum alloy crucibles or molds in a single melting step to form a fused disc consisting of the borate of lithium plus sample. Thus in accordance with this aspect of the invention there is presented a boron oxide/ lithium compound x-ray flux composition mixture that can be fused or melted with samples or ores to be analysed in a single step or process and the resultant fusion after cooling, which consists of a glass solution containing the target analyte ions from the sample or ore together with lithium and boron ions all evenly dispersed in a glass matrix, analyzed by x-ray fluorescence spectroscopy to give an accurate analysis of the sample or ore. The use of the aforesaid mixture eliminates approximately one half of the normal preparatory process and enables a time reduction for sample or ore analysis to be decreased by approximately 50% and further, the pick up of contamination material is eliminated by not having to use crushing or grinding equipment.

Best Mode(s) for Carrying Out the Invention The embodiment involves mixing boron oxide and lithium containing compounds or compound together to make the x-ray flux composition mixture which is subsequently mixed with the sample or ore to be analyzed and then melted or fused to make a fused disc.

Sodium nitrate, lithium nitrate, or other oxidizing compounds, can also be also added to the mixture before fusing to give a percentage of sodium nitrate, lithium nitrate, or other oxidizing compounds, in the mixture before fusion, of 1 to 25% by weight. Sodium nitrate, lithium nitrate, or other oxidizing compounds are added if required, to oxidize sulphides when they are present in the sample or ore, so they can be analyzed.

A batch of x-ray flux composition mixture is made up by mixing boron oxide with lithium containing compounds or compound such that the resultant boron/lithium mixture is equivalent to the ratio of 1.2 parts to 2.2 parts respectively of lithium S tetraborate to lithium metaborate when fused with the sample or ore. These c ingredients are combined and mixed with the sample or ore to be analyzed and Splaced in a platinum or platinum alloy crucible and are fused at 1100 degrees C.

The fused mix, which forms a liquid glass, is poured into a mold and allowed to cool to form a disc.

_In use, a known quantity of sample or ore is combined with a known quantity of the said x-ray flux composition mixture, such that the amount of sample or ore to the said x-ray flux composition mixture is known. This resultant combined mixture is melted at high temperature. Typically from 1:2 to 1:40 by weight ratio sample or ore to said x-ray flux composition mixture is usually satisfactory, c depending upon the sample or ore type. Typically 0.6 gram of sample or ore is added to approximately 10 grams of the said x-ray flux composition mixture optionally containing a percentage of sodium nitrate or lithium nitrate, and melted 0 15 in a platinum or platinum alloy mold. Alternatively, the sample or ore and said x- 0 ray flux composition mixture is melted in a platinum or platinum alloy crucible and poured into a mold. The mold is cooled, the contents forming a glass-like disc which is then placed into an x-ray fluorescence spectrograph machine for analysis. The amount of impurities present is determined by analysis of the spectral lines.

Claims

1. An x-ray flux composition mixture containing boron and lithium, comprising specifically boron oxide and lithium compounds or compound such that when mixed together with samples or ores to be analyzed can be fused in a single melting step prior to analysis and such x-ray flux composition mixture being specifically used for the quantitative determination of elemental substances in samples or ores to be analyzed by x-ray fluorescence spectrography.

2. The x-ray flux composition mixture of claim 1 where the contained boron oxide and lithium comprises a mixture of boron oxide and lithium in a range of proportions from 1:10 to 30:1 respectively.

3. The x-ray flux composition mixture of claim 1 where the boron oxide and lithium compounds or compound comprises a mixture equivalent to, after fusing, to 100% lithium tetraborate, 100% lithium metaborate, or any proportional ratio between these two compounds.

4. The x-ray flux composition mixture of claim 1 where the lithium may be provided from any lithium containing compound.

The x-ray composition mixture of claim 1 where the boron may be provided wholly or in part from boron oxide

6. The said samples or ores to be analyzed and the x-ray flux composition mixture of any one of the claims 1 to 5 are mixed in weight proportion between 1% and 50% respectively.