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AU2010249195B1 - Lithium X-Ray flux composition - Google Patents

Lithium X-Ray flux composition Download PDF

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Publication number
AU2010249195B1
AU2010249195B1 AU2010249195A AU2010249195A AU2010249195B1 AU 2010249195 B1 AU2010249195 B1 AU 2010249195B1 AU 2010249195 A AU2010249195 A AU 2010249195A AU 2010249195 A AU2010249195 A AU 2010249195A AU 2010249195 B1 AU2010249195 B1 AU 2010249195B1
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Australia
Prior art keywords
lithium
ray flux
flux composition
borate
ray
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AU2010249195A
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David Brown
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X Ray Flux Pty Ltd
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X Ray Flux Pty Ltd
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Priority to AU2010249195A priority Critical patent/AU2010249195B1/en
Publication of AU2010249195B1 publication Critical patent/AU2010249195B1/en
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Abstract

Abstract 5 In the x-ray fluorescence analysis of minerals, ores and other materials, chemicals containing lithium and boron are melted together at high temperatures to produce lithium borate compounds which are then cooled and reduced in size to a powder or coarse material. Such material is known as x-ray flux and is usually represented or specified in the final commercial product as ratios of 10 lithium tetraborate to lithium metaborate. The x-ray flux is melted with samples of materials to be analyzed and cast into discs which are then analyzed by an x-ray fluorescence spectrograph. In this invention, lithium carbonate (Li 2 CO3 ) has been used wholly or in part as the source of lithium in the manufacture of an x-ray flux when such flux is mixed 15 and melted with minerals, ores or other materials to be analyzed.

Description

Specification for Patent Application Title: "Lithium X-Ray Flux Composition" Applicant: X-Ray Flux Pty Ltd 88 Guthrie St., Osborne Park, West Australia 6017 Country: Australia Type: Standard Number: Date: 3 December 2010 IP Australia 0 7 DEC 2010 PP Australia 3 0 MAY 20I Title RECEIVED CM "LITHIUM X-RAY FLUX COMPOSITION 5 Specification The following statement is a full description of this invention, including the best method of performing it known to me: 10 Field of the Invention This invention relates to the analysis of materials, and in particular to a method of flux manufacture for x-ray fluorescence spectroscopy analysis of minerals, ores 15 and other materials. Description Throughout the description, unless the context requires otherwise, the word 20 "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. 25 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 30 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 35 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. 40 Previous difficulties Difficulties exist with previous manufacture because of the production of substantial amounts of water in the reaction which when combined with the flux 45 fumes formed in the reaction form a very corrosive atmosphere, which subsequently causes rapid deterioration of the furnace or melting apparatus 1 linings and heating elements, thus causing premature breakdown of the melting equipment. Further, because quantities of water are generated in the reaction which have to be converted to steam as the flux melts, large quantities of electrical or gas 5 energy are needed to drive off the water vapor as the reaction continues before the chemical reaction can proceed to completion. Inventive Idea 10 The inventor has found that the compound lithium carbonate (Li 2
CO
3 ) by itself or in combination with lithium hydroxide (LiOH.H 2 0), can be used together with boric acid as the starting substances for x-ray flux manufacture. The lithium carbonate or lithium hydroxide either separately or together are the specific lithium donating substances in the manufacture of such x-ray flux. The water that 15 is generated is eliminated in the fusion reaction eliminating the need to further dehydrogenate the finished product thereby enabling the finished product to be produced in one manufacturing step. Best Mode(s) for Carrying Out the Invention 20 The embodiment involves the addition lithium carbonate (Li 2 CO3) or lithium hydroxide (LiOH.H20) or a combination of both to boric acid before fusing to make the flux. The addition of lithium compounds are added such that the percentage of lithium in the finished flux is from 0.5 to 90% by weight. 25 Sodium nitrate, lithium nitrate, or other oxidizing compounds, can also be also added to the melted and cooled lithium borate compound 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 30 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 lithium carbonate or lithium hydroxide or a mixture of both to boric acid to make the flux. For a flux 35 equivalent to lithium tetraborate and lithium metaborate in the proportion of 1.2 parts to 2.2 parts respectively, lithium carbonate is added to a boron containing compound in the ratio of 0.5 lithium carbonate to 1.88 parts of a boric acid, for lithium hydroxide 1 part is added for 1.88 parts of boric acid.. These ingredients are combined and mixed, and placed in a platinum or platinum alloy crucible and 40 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 45 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. 2 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 5 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 10 of the spectral lines. 3

Claims (9)

1. A method of producing an x-ray flux composition solely as a borate of lithium where the lithium comes specifically from lithium carbonate or lithium hydroxide or a combination of both and the boron comes solely from boric acid which together when melted at temperatures over 800 10 degrees C in an open container and exposed to air forms in one single processing step the final anhydrous x-ray flux composition to obtain specific ratios of lithium to boron from 1:2 to 1:1 which is used specifically for the quantitative or qualitative determination of elements in samples of minerals, ores or other material to be analyzed by x-ray fluorescence 15 spectrography.
2. The method of producing the x-ray flux composition as in claim 1 where the lithium is present in proportion by weight of at least 0.5%. 20
3. The method of producing the x-ray flux composition as in claim 1 where the lithium is present in proportion of at least 90.0% by weight in the said composition
4. The method of producing the x-ray flux composition as in claim 1 where 25 the borate of lithium may be entirely lithium tetraborate.
5. The method of producing the x-ray flux composition as in claim 1 where the borate of lithium may be entirely lithium meta-borate. 30
6. The method of producing the x-ray flux composition as in 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.
7. The method of producing the x-ray flux composition as in claim 1 where 35 the borate of lithium comprises a mixture equivalent to lithium tetraborate and lithium meta-borate in the proportion of 1.2:2.2 respectively.
8. A known quantity of the x-ray flux compositions produced as in any one of the claims I to 7 is mixed and fused with a predetermined sample of 40 minerals, ore or other material and an x-ray fluorescence spectroscopy is performed on the said fusion.
9. The said minerals, ore or other materials and said x-ray flux composition of any one of the claims 1 to 8 are mixed in weight proportion from 1:1 to 45 1:50 respectively. 4
AU2010249195A 2010-12-07 2010-12-07 Lithium X-Ray flux composition Ceased AU2010249195B1 (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102507287A (en) * 2011-11-21 2012-06-20 山东省地质科学实验研究院 Sample preparation flux for fluorite sample in X ray fluorescence spectrum analysis
EP2750849A4 (en) * 2011-08-30 2015-08-26 Spex Sample Prep Llc PREPARATION OF INORGANIC SAMPLES BY FUSION
EP2966039A1 (en) * 2014-07-08 2016-01-13 PANalytical B.V. Preparation of samples for XRF using flux and platinum crucible
CN106706387A (en) * 2016-12-20 2017-05-24 武汉科技大学 Preparation method of fluxing agent coverage piece
CN114235546A (en) * 2021-12-14 2022-03-25 清远南玻节能新材料有限公司 Silica sand composite fluxing agent and detection method of silica sand
CN114460117A (en) * 2022-03-16 2022-05-10 清远南玻节能新材料有限公司 Method for detecting component content of aluminum hydroxide product
CN115389489A (en) * 2022-08-04 2022-11-25 江苏沙钢集团淮钢特钢股份有限公司 Method for detecting element content in iron ore

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2957749A (en) * 1958-01-16 1960-10-25 American Potash & Chem Corp Manufacture of lithium tetraborate
GB990765A (en) * 1963-05-31 1965-04-28 Gnesja Abramovna Asinovskaja Fluxes
JPS5433299A (en) * 1977-08-20 1979-03-10 Agency Of Ind Science & Technol Preparation of lithium borate
JPS6296315A (en) * 1985-10-18 1987-05-02 Honjiyou Chem Kk Production of lithium borate
EP0306276B1 (en) * 1987-08-31 1997-05-14 Ngk Insulators, Ltd. Method for vitrifying powdery and granular materials
WO2004065949A1 (en) * 2003-01-21 2004-08-05 X-Ray Flux Pty Ltd X-ray fluorescence flux composition
WO2007076562A1 (en) * 2006-01-05 2007-07-12 X-Ray Flux Pty Ltd Nickel flux composition
AU2007216909A1 (en) * 2006-10-17 2008-05-01 X-Ray Flux Pty Ltd Copper X-ray flux composition
AU2007202703B2 (en) * 2007-05-04 2009-01-15 X-Ray Flux Pty Ltd X-ray flux composition

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2957749A (en) * 1958-01-16 1960-10-25 American Potash & Chem Corp Manufacture of lithium tetraborate
GB990765A (en) * 1963-05-31 1965-04-28 Gnesja Abramovna Asinovskaja Fluxes
JPS5433299A (en) * 1977-08-20 1979-03-10 Agency Of Ind Science & Technol Preparation of lithium borate
JPS6296315A (en) * 1985-10-18 1987-05-02 Honjiyou Chem Kk Production of lithium borate
EP0306276B1 (en) * 1987-08-31 1997-05-14 Ngk Insulators, Ltd. Method for vitrifying powdery and granular materials
WO2004065949A1 (en) * 2003-01-21 2004-08-05 X-Ray Flux Pty Ltd X-ray fluorescence flux composition
WO2007076562A1 (en) * 2006-01-05 2007-07-12 X-Ray Flux Pty Ltd Nickel flux composition
AU2007216909A1 (en) * 2006-10-17 2008-05-01 X-Ray Flux Pty Ltd Copper X-ray flux composition
AU2007202703B2 (en) * 2007-05-04 2009-01-15 X-Ray Flux Pty Ltd X-ray flux composition

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2750849A4 (en) * 2011-08-30 2015-08-26 Spex Sample Prep Llc PREPARATION OF INORGANIC SAMPLES BY FUSION
AU2012302126B2 (en) * 2011-08-30 2017-01-12 Spex Sample Prep Llc Preparation of inorganic samples by fusion
CN102507287A (en) * 2011-11-21 2012-06-20 山东省地质科学实验研究院 Sample preparation flux for fluorite sample in X ray fluorescence spectrum analysis
EP2966039A1 (en) * 2014-07-08 2016-01-13 PANalytical B.V. Preparation of samples for XRF using flux and platinum crucible
US10107551B2 (en) 2014-07-08 2018-10-23 Malvern Panalytical B.V. Preparation of samples for XRF using flux and platinum crucible
CN106706387A (en) * 2016-12-20 2017-05-24 武汉科技大学 Preparation method of fluxing agent coverage piece
CN106706387B (en) * 2016-12-20 2019-02-12 武汉科技大学 A kind of preparation method of flux cover sheet
CN114235546A (en) * 2021-12-14 2022-03-25 清远南玻节能新材料有限公司 Silica sand composite fluxing agent and detection method of silica sand
CN114460117A (en) * 2022-03-16 2022-05-10 清远南玻节能新材料有限公司 Method for detecting component content of aluminum hydroxide product
CN114460117B (en) * 2022-03-16 2023-06-06 清远南玻节能新材料有限公司 Method for detection of composition content of aluminum hydroxide products
CN115389489A (en) * 2022-08-04 2022-11-25 江苏沙钢集团淮钢特钢股份有限公司 Method for detecting element content in iron ore

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