AU2007202706B2 - X-ray flux composition mixture - Google Patents
X-ray flux composition mixture Download PDFInfo
- Publication number
- AU2007202706B2 AU2007202706B2 AU2007202706A AU2007202706A AU2007202706B2 AU 2007202706 B2 AU2007202706 B2 AU 2007202706B2 AU 2007202706 A AU2007202706 A AU 2007202706A AU 2007202706 A AU2007202706 A AU 2007202706A AU 2007202706 B2 AU2007202706 B2 AU 2007202706B2
- Authority
- AU
- Australia
- Prior art keywords
- lithium
- boron
- ray flux
- composition mixture
- flux composition
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Ceased
Links
- 239000000203 mixture Substances 0.000 title claims description 53
- 230000004907 flux Effects 0.000 title claims description 27
- 229910052796 boron Inorganic materials 0.000 claims description 16
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 15
- 150000001875 compounds Chemical class 0.000 claims description 15
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 14
- 229910052744 lithium Inorganic materials 0.000 claims description 14
- 229910052810 boron oxide Inorganic materials 0.000 claims description 11
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims description 11
- 238000004458 analytical method Methods 0.000 claims description 10
- 238000002844 melting Methods 0.000 claims description 6
- 230000008018 melting Effects 0.000 claims description 6
- PSHMSSXLYVAENJ-UHFFFAOYSA-N dilithium;[oxido(oxoboranyloxy)boranyl]oxy-oxoboranyloxyborinate Chemical compound [Li+].[Li+].O=BOB([O-])OB([O-])OB=O PSHMSSXLYVAENJ-UHFFFAOYSA-N 0.000 claims description 5
- HZRMTWQRDMYLNW-UHFFFAOYSA-N lithium metaborate Chemical compound [Li+].[O-]B=O HZRMTWQRDMYLNW-UHFFFAOYSA-N 0.000 claims description 5
- 239000000654 additive Substances 0.000 claims description 3
- 238000004876 x-ray fluorescence Methods 0.000 claims description 3
- 150000002642 lithium compounds Chemical class 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 20
- 229910001260 Pt alloy Inorganic materials 0.000 description 10
- 229910052697 platinum Inorganic materials 0.000 description 10
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 description 8
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- 238000002156 mixing Methods 0.000 description 7
- 230000004927 fusion Effects 0.000 description 6
- 238000000227 grinding Methods 0.000 description 5
- 238000000034 method Methods 0.000 description 4
- 235000010344 sodium nitrate Nutrition 0.000 description 4
- 239000004317 sodium nitrate Substances 0.000 description 4
- 239000011521 glass Substances 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000001816 cooling Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000005549 size reduction Methods 0.000 description 2
- 238000004846 x-ray emission Methods 0.000 description 2
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 description 1
- 239000012491 analyte Substances 0.000 description 1
- -1 boron ions Chemical class 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007717 exclusion Effects 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000012768 molten material Substances 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 239000011369 resultant mixture Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/223—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/07—Investigating materials by wave or particle radiation secondary emission
- G01N2223/076—X-ray fluorescence
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
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 N Title "X-RAY FLUX COMPOSITION MIXTURE" 00 S 5 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 the sole source of boron in 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 lithium tetraborate, lithium metaborate or ratios of lithium tetraborate to lithium metaborate.
The x-ray flux is then mixed with samples of materials or ores to be analyzed and other additives if needed 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 N 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 0 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 consisting of the equivalent of lithium tetraborate, lithium metaborate or a mixture equivalent thereof. The molten x-ray flux is then poured into a cooling tray and Nthe 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 N 10 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 Oother additives if needed 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 used as the sole source of boron in x-ray flux and fused at high temperature with lithium containing compounds not containing boron 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 using boron oxide as the sole source of boron that can be fused or melted with samples or ores to be analyzed 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 solely boron oxide and lithium containing compounds or compound which do not contain boron 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 N 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 not containing boron such that the resultant boron/lithium mixture is equivalent to the ratio of 1.2 parts to 2.2 parts respectively of lithium tetraborate to lithium metaborate when fused with the sample or ore. These ingredients are combined and mixed with the sample or ore to be analyzed 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 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 the said x-ray flux composition mixture is usually satisfactory, 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 in a platinum or platinum alloy mold. Alternatively, the sample or ore and said xray 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 (6)
1. An x-ray flux composition mixture containing boron and lithium, comprising specifically boron oxide as the sole source of boron and lithium Ncompounds or compound not containing boron such that when mixed r together with samples or ores to be analyzed and other additives if N 10 needed, 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 Oby x-ray fluorescence spectrography.
2. The x-ray flux composition mixture of claim 1 where the contained boron oxide and lithium from compounds not containing boron 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 not containing boron.
The x-ray composition mixture of claim 1 where the boron is provided wholly 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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| AU2007202706A AU2007202706B2 (en) | 2007-05-04 | 2007-06-13 | X-ray flux composition mixture |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| AU2007902367 | 2007-05-04 | ||
| AU2007902367A AU2007902367A0 (en) | 2007-05-04 | X-Ray Flux Composition Mixture | |
| AU2007202706A AU2007202706B2 (en) | 2007-05-04 | 2007-06-13 | X-ray flux composition mixture |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| AU2007202706A1 AU2007202706A1 (en) | 2008-11-20 |
| AU2007202706B2 true AU2007202706B2 (en) | 2009-02-05 |
Family
ID=40099478
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| AU2007202706A Ceased AU2007202706B2 (en) | 2007-05-04 | 2007-06-13 | X-ray flux composition mixture |
Country Status (1)
| Country | Link |
|---|---|
| AU (1) | AU2007202706B2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106706387B (en) * | 2016-12-20 | 2019-02-12 | 武汉科技大学 | A kind of preparation method of flux cover sheet |
| CN111982951B (en) * | 2020-08-31 | 2023-05-16 | 广东韶钢松山股份有限公司 | Method for processing sample and measuring element content |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6296315A (en) * | 1985-10-18 | 1987-05-02 | Honjiyou Chem Kk | Production of lithium borate |
| FR2849650A1 (en) * | 2003-01-06 | 2004-07-09 | Gerard Lang | Borate glass used as flux in making beads used in X-ray fluorescence analysis, contains small percentage of germanium oxide |
| WO2004065949A1 (en) * | 2003-01-21 | 2004-08-05 | X-Ray Flux Pty Ltd | X-ray fluorescence flux composition |
-
2007
- 2007-06-13 AU AU2007202706A patent/AU2007202706B2/en not_active Ceased
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6296315A (en) * | 1985-10-18 | 1987-05-02 | Honjiyou Chem Kk | Production of lithium borate |
| FR2849650A1 (en) * | 2003-01-06 | 2004-07-09 | Gerard Lang | Borate glass used as flux in making beads used in X-ray fluorescence analysis, contains small percentage of germanium oxide |
| WO2004065949A1 (en) * | 2003-01-21 | 2004-08-05 | X-Ray Flux Pty Ltd | X-ray fluorescence flux composition |
Non-Patent Citations (1)
| Title |
|---|
| URL: http://www.spectrumplus.com/flux.htm (Nov. 2006) * |
Also Published As
| Publication number | Publication date |
|---|---|
| AU2007202706A1 (en) | 2008-11-20 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| FGA | Letters patent sealed or granted (standard patent) | ||
| MK14 | Patent ceased section 143(a) (annual fees not paid) or expired |