AU2004206033B2 - X-ray fluorescence flux composition - Google Patents
X-ray fluorescence flux composition Download PDFInfo
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- AU2004206033B2 AU2004206033B2 AU2004206033A AU2004206033A AU2004206033B2 AU 2004206033 B2 AU2004206033 B2 AU 2004206033B2 AU 2004206033 A AU2004206033 A AU 2004206033A AU 2004206033 A AU2004206033 A AU 2004206033A AU 2004206033 B2 AU2004206033 B2 AU 2004206033B2
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- Australia
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- composition
- proportion
- terbium
- weight
- flux
- Prior art date
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- 239000000203 mixture Substances 0.000 title claims description 64
- 230000004907 flux Effects 0.000 title claims description 52
- 238000004876 x-ray fluorescence Methods 0.000 title claims description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 42
- 229910052771 Terbium Inorganic materials 0.000 claims description 32
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 claims description 32
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 25
- 229910052796 boron Inorganic materials 0.000 claims description 25
- 229910052742 iron Inorganic materials 0.000 claims description 21
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 13
- 229910052744 lithium Inorganic materials 0.000 claims description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- 150000001875 compounds Chemical class 0.000 claims description 8
- 239000000377 silicon dioxide Substances 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
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 claims 5
- 230000004927 fusion Effects 0.000 claims 3
- 238000001506 fluorescence spectroscopy Methods 0.000 claims 1
- 239000002245 particle Substances 0.000 claims 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 18
- 229910052697 platinum Inorganic materials 0.000 description 9
- 229910001260 Pt alloy Inorganic materials 0.000 description 8
- 238000004458 analytical method Methods 0.000 description 7
- 229910017052 cobalt Inorganic materials 0.000 description 4
- 239000010941 cobalt Substances 0.000 description 4
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 235000012239 silicon dioxide Nutrition 0.000 description 4
- 230000003595 spectral effect Effects 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- ZOXJGFHDIHLPTG-BJUDXGSMSA-N Boron-10 Chemical class [10B] ZOXJGFHDIHLPTG-BJUDXGSMSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 239000012491 analyte Substances 0.000 description 1
- FFBHFFJDDLITSX-UHFFFAOYSA-N benzyl N-[2-hydroxy-4-(3-oxomorpholin-4-yl)phenyl]carbamate Chemical compound OC1=C(NC(=O)OCC2=CC=CC=C2)C=CC(=C1)N1CCOCC1=O FFBHFFJDDLITSX-UHFFFAOYSA-N 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 230000007717 exclusion Effects 0.000 description 1
- 238000007499 fusion processing Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910052747 lanthanoid Inorganic materials 0.000 description 1
- 150000002602 lanthanoids Chemical class 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000012768 molten material Substances 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000003502 terbium compounds Chemical class 0.000 description 1
- 229910003451 terbium oxide Inorganic materials 0.000 description 1
- SCRZPWWVSXWCMC-UHFFFAOYSA-N terbium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Tb+3].[Tb+3] SCRZPWWVSXWCMC-UHFFFAOYSA-N 0.000 description 1
- 238000004846 x-ray emission Methods 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical group [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
Description
Received 20 August 2004 Specification The following statement is a full description of this invention, including the best method of performing it known to me: 5 Title "X-RAY FLUORESCENCE FLUX COMPOSITION" 10 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 ore samples. 15 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 20 exclusion of any other integer or group of integers. Background 25 X-ray flux is produced by fusing at high temperatures ( approx. 1100 degrees C.) in platinum or platinum alloy crucibles, chemicals containing lithium and boron or chemicals containing lithium or 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 30 ratios of lithium tetraborate to lithium metaborate. The x-ray flux is then mixed with samples to be analyzed, e.g. iron ore, and melted in a platinum or platinum alloy mold. Alternatively, the mixture 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 35 into an x-ray fluorescence spectrograph machine for analysis. Previous difficulties Difficulties exist with the calibration of the x-ray fluorescence spectrograph such 40 that the concentration of target analyte in the disc can be determined with confidence. Hitherto, attempts have been made to add cobalt to the flux, to provide what is referred to as an internal standard, however this had a big disadvantage in the case of iron ore, as cobalt itself is present in iron ore and can therefore cause significant errors. Furthermore, cobalt reacts with platinum to 45 form an alloy and as all the equipment used in the x-ray analytical fusion process 1 - Received 20 August 2004/ consists of platinum or platinum alloys it is not practical. Due to these problems, the use of cobalt in such application has been abandoned. 5 Inventive Idea The inventors have found that the rare earth element terbium, a specific lanthanide in the yttrium group of elements, has hitherto unsuspected x-ray fluorescence properties such that when fused together with lithium and boron 10 compounds to form x-ray flux, it is useful as an internal standard for the quantitative determination of iron in iron ore and iron containing compounds when such ore or compounds are fused with the x-ray flux. Thus in accordance with this aspect of the invention there is presented an x-ray fluorescence flux composition for the quantitative determination of iron in iron ore and iron 15 containing compounds, having an ionic moiety of terbium. Best Mode(s) for Carrying Out the Invention The embodiment involves the addition of terbium or terbium containing 20 compounds plus silicon dioxide to the lithium and boron containing chemicals before fusing to make the flux. The addition of terbium or terbium compounds is added such that the percentage of terbium in the finished flux is from 0.5 to 15% by weight. 25 Silicon dioxide is also added to the lithium, boron and terbium containing compounds before fusing to give a percentage of silicon dioxide in the finished flux of 2 to 7% by weight. A batch of flux is made up by adding to 100 grams of lithium tetraborate and 30 lithium metaborate in the proportion of 1.2 parts to 2.2 parts respectively or a mixture of chemicals which when fused gives the equivalent of fusing the directly aforementioned mixture, 13.095 grams of terbium oxide (Tb 4 0 7 ) and 5.95 grams of silicon dioxide (SiO 2 ). These ingredients are combined and mixed, and placed in a platinum or platinum alloy crucible and are fused at 1100 degrees C. The 35 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 composition. In use, a known quantity of iron ore is combined with a known quantity of the finished flux composition, such that the amount of ore relative to the amount of 40 elemental terbium present in the flux composition is known. Typically from 1:4 to 1:20 by weight ratio ore to flux is usually satisfactory, depending upon the ore type and grade. For typical iron ore deposits which are usually of a reasonably high grade, 1 gram of ore is added to 7 grams of flux, and melted in a platinum or platinum alloy mold. Alternatively, the ore and flux is melted in a platinum or 45 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 2 Received 20 August 2004 spectrograph machine for analysis. The amount of iron present is determined by analysis of the spectral lines and comparison with the spectral lines of terbium. It has been found that terbium has an x-ray fluorescence wavelength close to iron, such that the matrix effect or interference effect is effectively the same as for iron. 5 Further, the terbium and iron spectral lines are similarly affected by other elements usually present in iron ore samples. Consequently, by examining the ratios of the intensity of the wavelength of terbium to iron, the amount of iron in the disc and subsequently in the sample, can be easily and accurately determined mathematically. Furthermore, the flux composition provides a failsafe 10 analytical technique, in that should the spectral lines for terbium not be present, the analysis can be considered to have failed. 3
Claims (29)
1. A flux composition comprising lithium values and boron values as a borate of lithium, together with terbium such that the ionic moiety of terbium is present in proportion of at least 0.05% by weight of boron values in said composition and such flux being specifically used for the quantitative 10 determination of iron in iron ore by x-ray fluorescence spectrography.
2. The flux composition of claim 1 where the ionic moiety of terbium is present in proportion of at least 1.0% by weight of boron values in the said composition. 15
3. The flux composition of claim 1 where the ionic moiety of terbium is present in proportion of at least 2.0% by weight of boron values in the said composition. 20
4. The flux composition of claim 1 where the ionic moiety of terbium is present in proportion of at least 4.0% by weight of boron values in the said composition.
5. The flux composition of claim 1 where the ionic moiety of terbium is 25 present in proportion of at least 6.0% by weight of boron values in the said composition.
6. The flux composition of claim 1 where the ionic moiety of terbium is present in proportion of at least 8.0% by weight of boron values in the said 30 composition.
7. The flux composition of claim 1 where the ionic moiety of terbium is present in proportion of at least 10.0% by weight of boron values in the said composition. 35
8. The flux composition of claim I where the ionic moiety of terbium is present in proportion of up to 100.0% by weight of boron values in the said composition. 40
9. The flux composition of claim 1 where the ionic moiety of terbium is present in proportion of up to 90.0% by weight of boron values in the said composition.
10. The flux composition of claim 1 where the ionic moiety of terbium is 45 present in proportion of up to 80.0% by weight of boron values in the said composition. 4 Received 20 August 2004
11. The flux composition of claim 1 where the ionic moiety of terbium is present in proportion of up to 70.0% by weight of boron values in the said composition. 5
12. The flux composition of claim 1 where the ionic moiety of terbium is present in proportion of up to 60.0% by weight of boron values in the said composition. 10
13. The flux composition of claim 1 where the ionic moiety of terbium is present in proportion of up to 50.0% by weight of boron values in the said composition.
14. The flux composition of claim 1 where the ionic ionic moiety of terbium is 15 present in proportion of up to 40.0% by weight of boron values in the said composition.
15. The flux composition of claim 1 where the ionic moiety of terbium is present in proportion of up to 30.0% by weight of boron values in the said 20 composition.
16. The flux composition of claim 1 where the ionic moiety of terbium is present in proportion of up to 20.0% by weight of boron values in the said composition. 25
17. The flux composition of claim I where the ionic moiety of terbium is present in proportion of at from 45% to 50% by weight of boron values in the said composition. 30
18. The flux composition of claim 1 where the ionic moiety of terbium is present in proportion of about 48.2% by weight of boron values in the said composition. 35
19. The flux composition of any one of the claims 1 to 18 where silica is added in proportion of at least 1% by weight of the said composition.
20. The flux composition of any one of the claims 1 to 18 where silica is added 40 in proportion of from 2% to 7% by weight of the said composition.
21. The flux composition of claim 1 where the borate of lithium may be entirely lithium tetraborate. 45
22. The flux composition of claim 1 where the borate of lithium may be entirely lithium meta-borate. 5 Received 20 August 2004
23. The 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. 5
24. The flux composition of claim I where the borate of lithium comprises a mixture of lithium tetraborate and lithium meta-borate in the proportion of 1.2:2.2 respectively. 10
25. The flux composition of claim 1 where the lithium may be provided from any lithium containing compound and the boron may be provided from any boron containing compound.
26. The flux composition of claim 1 comprises finely divided particles of a 15 fusion of compounds of any one of the claims 1 to 25.
27. A known quantity of the flux compositions of any one of the claims 1 to 26 is mixed with a predetermined sample of iron ore, fusing the said ore and flux composition to form a fusion thereof, and performing x-ray 20 fluorescence spectroscopy on the said fusion.
28. The said ore and said flux composition of claim 27 are mixed in weight proportion from 1:1 to 1:40. 25
29. The said ore and said flux composition of any one of the claims 1 to 28 are mixed in weight proportion between 4% to 25% respectively. 6
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| AU2004206033A AU2004206033B2 (en) | 2003-01-21 | 2004-01-02 | X-ray fluorescence flux composition |
Applications Claiming Priority (6)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| AU2003900222A AU2003900222A0 (en) | 2003-01-21 | 2003-01-21 | Flux composition |
| AU2003900222 | 2003-01-21 | ||
| AU2003903310 | 2003-06-30 | ||
| AU2003903310A AU2003903310A0 (en) | 2003-06-30 | 2003-06-30 | Flux composition |
| AU2004206033A AU2004206033B2 (en) | 2003-01-21 | 2004-01-02 | X-ray fluorescence flux composition |
| PCT/AU2004/000001 WO2004065949A1 (en) | 2003-01-21 | 2004-01-02 | X-ray fluorescence flux composition |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| AU2004206033A1 AU2004206033A1 (en) | 2004-08-05 |
| AU2004206033B2 true AU2004206033B2 (en) | 2009-05-14 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| AU2004206033A Expired AU2004206033B2 (en) | 2003-01-21 | 2004-01-02 | X-ray fluorescence flux composition |
Country Status (1)
| Country | Link |
|---|---|
| AU (1) | AU2004206033B2 (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2500910A1 (en) * | 1975-01-11 | 1976-12-09 | Siemens Ag | Luminescent terbium-activated lithium beryllium borate glass - avoiding discoloration on long exposure to UV X-rays or electrons |
| US4889707A (en) * | 1988-01-29 | 1989-12-26 | The Curators Of The University Of Missouri | Composition and method for radiation synovectomy of arthritic joints |
| JPH09257673A (en) * | 1996-03-26 | 1997-10-03 | Fuji Electric Co Ltd | Analysis of vanadium oxide ceramic |
| US6358531B1 (en) * | 1999-02-01 | 2002-03-19 | The Curators Of The University Of Missouri | Method for preparing porous shells or gels from glass particles |
-
2004
- 2004-01-02 AU AU2004206033A patent/AU2004206033B2/en not_active Expired
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2500910A1 (en) * | 1975-01-11 | 1976-12-09 | Siemens Ag | Luminescent terbium-activated lithium beryllium borate glass - avoiding discoloration on long exposure to UV X-rays or electrons |
| US4889707A (en) * | 1988-01-29 | 1989-12-26 | The Curators Of The University Of Missouri | Composition and method for radiation synovectomy of arthritic joints |
| JPH09257673A (en) * | 1996-03-26 | 1997-10-03 | Fuji Electric Co Ltd | Analysis of vanadium oxide ceramic |
| US6358531B1 (en) * | 1999-02-01 | 2002-03-19 | The Curators Of The University Of Missouri | Method for preparing porous shells or gels from glass particles |
Non-Patent Citations (2)
| Title |
|---|
| Eddy, et. aI., "A Flux for Fusion of Samples in Analysis by X-Ray Fluorescence Spectroscopy, X-RAY SPECTROSCOPY, Vol. 17 (1988), pp. 17-18. * |
| Zamechek, "Determination of elemental compositor of zeolitic materials," in VERIFIED SYNTHESIS OF ZEOLITIC MATERIALS, 2nd Revised Edition (Harry X Robson, editor), Elsevier, 2001; pages 51-53 * |
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| Publication number | Publication date |
|---|---|
| AU2004206033A1 (en) | 2004-08-05 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| MK1 | Application lapsed section 142(2)(a) - no request for examination in relevant period | ||
| NB | Applications allowed - extensions of time section 223(2) |
Free format text: THE TIME IN WHICH TO REQUEST EXAMINATION HAS BEEN EXTENDED TO 07 JUN 2007. |
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| FGA | Letters patent sealed or granted (standard patent) | ||
| MK14 | Patent ceased section 143(a) (annual fees not paid) or expired | ||
| NA | Applications received for extensions of time, section 223 |
Free format text: AN APPLICATION TO EXTEND THE TIME FROM 02 JAN 2012 TO 02 AUG 2012 IN WHICH TO PAY A RENEWAL FEE HAS BEEN FILED . |
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| NB | Applications allowed - extensions of time section 223(2) |
Free format text: THE TIME IN WHICH TO PAY A RENEWAL FEE HAS BEEN EXTENDED TO 02 AUG 2012 . |
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| MK14 | Patent ceased section 143(a) (annual fees not paid) or expired |