AU2007202703A1

AU2007202703A1 - X-ray flux composition

Info

Publication number: AU2007202703A1
Application number: AU2007202703A
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: AU2007202703B2

Description

Specification for Patent Application Title: "X-Ray Flux Composition" 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 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 materials, and in particular to a flux composition for x-ray fluorescence spectroscopy analysis of minerals, ores and other materials.

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. 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. At this stage, the x-ray flux can have additions of oxidizing agents such as sodium nitrate or lithium nitrate or other mold releasing agents.

The x-ray flux is then mixed with the samples to be analyzed and subsequently melted in a platinum or platinum alloy mold. Alternatively, the x-ray flux plus sample is melted 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 Difficulties exist with previous manufacture because of the production of substantial amounts of water vapor in the reaction which when combined with the flux fumes formed in the reaction form a very corrosive atmosphere, which subsequently causes rapid deterioration of the furnace or melting apparatus linings and heating elements, thus causing premature breakdown of the melting equipment.

N Further, because large quantities of water are generated in the reaction which have to be converted to steam as the flux melts, large quantities of electrical or 5 gas energy are needed to drive off the water vapor as the reaction continues before the chemical reaction can proceed to completion.

Inventive Idea The inventor has found that the compound boron oxide (B 2 0 3 which was hitherto not known to be suitable as a starting substance for x-ray flux N manufacture, can be used as the specific boron donating substance in the manufacture of such x-ray flux. When this compound is used, the amount of water formed in the flux reaction is eliminated or substantially diminished depending on the lithium compound used thus significantly diminishing the corrosive effect on the furnace or melting apparatus. Also, the amount of energy input needed to complete the reaction is substantially reduced. Further, the processing time to produce a given quantity of x-ray flux by using boron oxide is approximately halved, as a consequence of not having to drive off water formed in the reaction which is the case with other boron compounds such as boric acid which is currently used.

Best Mode(s) for Carrying Out the Invention The embodiment involves the addition boron oxide (B 2 0 3 to the lithium containing chemicals before fusing to make the flux. The addition of boron oxide is added such that the percentage of boron in the finished flux is from 1.0 to by weight.

Sodium nitrate, lithium nitrate, or other oxidizing compounds, can also be also added to the lithium compounds and boron oxide after fusing to give a percentage of sodium nitrate, lithium nitrate, or other oxidizing compounds, in the finished flux 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 samples, so they can be analyzed.

A batch of flux is made up by adding various amounts of boron oxide to lithium containing compounds to make the flux. For a flux equivalent to lithium tetraborate and lithium metaborate in the proportion of 1.2 parts to 2.2 parts respectively, boron oxide is added to a lithium containing compound in the ratio of 1.05 parts of boron oxide to 1.0 part of a lithium compound containing 1 atom of lithium or 0.5 parts of a lithium compound containing 2 atoms of lithium. These ingredients are combined and mixed, and placed in a platinum or platinum alloy crucible and are fused at 1100 degrees C. The fused mix, which forms a liquid glass, is allowed to cool and reduced in size to a coarse material or a powder to produce the finished flux.

In use, a known quantity of the minerals, ore or other materials to be analyzed is combined with a known quantity of the finished flux, such that the amount of minerals, ore or other material relative to the amount of finished flux is known.

This mixture is melted at high temperature. Typically from 1:4 to 1:30 by weight minerals, ore or other material to finished flux is usually satisfactory, depending upon the substance or ore type and grade. For typical ore deposits in Australia, 1 gram of ore is added to 7 grams of finished flux with or without a percentage of sodium nitrate or lithium nitrate and melted in a platinum or platinum alloy mold.

Alternatively, the ore and finished flux is melted in a platinum or platinum alloy crucible and poured into a mold. The mold is cooled and the contents form a glass-like disc which is then placed into an x-ray fluorescence spectrograph machine for analysis. The amount of elements present is determined by analysis of the spectral lines.

Claims

1. An x-ray flux composition comprising lithium from lithium compounds and boron oxide, which when melted together give a finished x-ray flux product as a borate of lithium where all or part of the boron in the finished x-ray flux is obtained specifically from boron oxide with the boron being present in proportion by weight of at least 1.0% in the finished x-ray flux with such finished x-ray flux used for the quantitative or qualitative determination of elements in samples of minerals, ores or other material to be analyzed by x-ray fluorescence spectrography.

2. The x-ray flux composition of claim 1 where the boron is proportion of at least 2.0% by weight in the said composition.

3. The x-ray flux composition of claim 1 where the boron is proportion of at least 4.0% by weight in the said composition.

4. The x-ray flux composition of claim 1 where the boron is proportion of at least 6.0% by weight in the said composition. The x-ray flux composition of claim 1 where the boron is proportion of at least 8.0% by weight in the said composition

6. The x-ray flux composition of claim 1 where proportion of at least 10.0% by weight in the said

7. The x-ray flux composition of claim 1 where proportion of at least 20.0% by weight in the said

8. The x-ray flux composition of claim 1 where proportion of at least 40.0% by weight in the said

9. The x-ray flux composition of claim 1 where proportion of at least 60.0% by weight in the said The x-ray flux composition of claim 1 where proportion of at least 80.0% by weight in the said

11. The x-ray flux composition of claim 1 where proportion of at least 90.0% by weight in the said the boron is composition. the boron is composition the boron is composition the boron is composition the boron is composition the boron is composition present in present in present in present in present in present in present in present in present in present in

12. The x-ray flux composition of claim 1 where the borate of lithium may be entirely lithium tetraborate.

13. The x-ray flux composition of claim 1 where the borate of lithium may be Ci entirely lithium meta-borate. 5 14. The x-ray flux composition of claim 1 where the borate of lithium comprises a mixture of lithium tetraborate and lithium meta-borate in a range of proportions from 1:10 to 10:1. The x-ray flux composition of claim 1 where the borate of lithium 10 comprises a mixture of lithium tetraborate and lithium meta-borate in the proportion of 1.2:2.2 respectively.

16. The x-ray flux composition of claim 1 where the lithium may be provided from any lithium containing compound. 0 c 17. The x-ray flux composition of claim 1 comprises finely divided particles of a fusion of compounds of any one of the claims 1 to

18. The x-ray flux composition of claim 1 comprises finely divided particles of a fusion of compounds of any one of the claims 1 to

19. A known quantity of the x-ray flux compositions of any one of the claims 1 to 17 is mixed and fused with a predetermined sample of minerals, ore or other material and an x-ray fluorescence spectroscopy is performed on the said fusion. The said minerals, ore or other materials and said x-ray flux composition of any one of the claims 1 to 19 are mixed in weight proportion from 1:1 to 1:50 respectively.