JP6384800B2 - Method for producing glass beads for X-ray fluorescence analyzer - Google Patents
Method for producing glass beads for X-ray fluorescence analyzer Download PDFInfo
- Publication number
- JP6384800B2 JP6384800B2 JP2017021678A JP2017021678A JP6384800B2 JP 6384800 B2 JP6384800 B2 JP 6384800B2 JP 2017021678 A JP2017021678 A JP 2017021678A JP 2017021678 A JP2017021678 A JP 2017021678A JP 6384800 B2 JP6384800 B2 JP 6384800B2
- Authority
- JP
- Japan
- Prior art keywords
- glass bead
- platinum crucible
- heating
- manufacturing apparatus
- rpm
- 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.)
- Expired - Fee Related
Links
Images
Landscapes
- Sampling And Sample Adjustment (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
Description
本発明は、蛍光Ｘ線分析装置に使用するガラスビードの作製方法に関する。 The present invention relates to a method for producing a glass bead used in a fluorescent X-ray analyzer.
従来、無機物や酸化物等を分析する場合には、ガラスビードを作製して、これを蛍光Ｘ線分析装置により分析していた。蛍光Ｘ線分析装置に使用するガラスビードの作製方法は、試料を微粉末化し溶融剤及び剥離剤を混入して白金ルツボに入れ、高周波加熱装置や電気炉あるいはガス炉等で高温溶解攪拌し、そのまま凝固してガラスビードを作製していた。 Conventionally, when analyzing an inorganic substance, an oxide, etc., a glass bead was produced and analyzed by a fluorescent X-ray analyzer. A method for producing a glass bead used in a fluorescent X-ray analyzer is to finely pulverize a sample, mix a melting agent and a release agent, put in a platinum crucible, and perform high-temperature melting and stirring with a high-frequency heating device, an electric furnace, a gas furnace, etc. The glass beads were produced by solidification as they were.
従来、蛍光Ｘ線分析装置に使用するガラスビードの作製方法は、微粉末の分析資料を白金ルツボに入れ、これに溶融剤及び剥離剤を混入して高周波加熱装置や電気炉あるいはガス炉にて溶融攪拌し、冷却凝固してガラスビードを作製していた。
しかし、冷却凝固の過程において、剥離剤の表面張力等により真円形のガラスビードにならず、三日月形に変形凝固することが多々ある。
特許第４２９１３１８号においては、加熱機構と回転機構及び揺動機構を有するガラスビード作製装置にて白金ルツボに微粉末試料と溶融剤及び剥離剤を混入して加熱し、回転及び揺動手段によりガラスビードを作製している。
特開２００４−２２６２３１号においては、ガラスビード作製装置については明記されていないものの、ガラスビード作製装置によると思われる内容になっている。白金ルツボに微粉末試料と溶融剤及び剥離剤を混入して加熱し、回転及び揺動手段によりガラスビードを作製している。
また、実用新案登録第２５９６４７１号においても、加熱機構と回転機構及び揺動機構を有するガラスビード作製装置にて、白金ルツボに微粉末試料と溶融剤及び剥離剤を混入して加熱し、回転及び揺動手段によりガラスビードを作製している。
しかし、上記いずれの場合においても、剥離剤等による表面張力の増大により真円形のガラスビードに凝固せず、三日月形に変形凝固する場合が多々ある。そのため加熱終了後直ちに高温の白金ルツボを専用のトングスで持ち上げ、適当に揺らせながら冷却、真円形に凝固する作業をする必要がある。高温で危険な作業である。
本発明は、ガラスビード作製装置を用いて、溶融加熱終了後の冷却凝固の過程において剥離剤等による表面張力の増大による変形凝固を防止し、真円形の高品質のガラスビードを作製する方法を提案するものである。Conventionally, a method for producing a glass bead used in a fluorescent X-ray analyzer is to put a fine powder analysis material into a platinum crucible and mix a melting agent and a release agent in a high frequency heating apparatus, electric furnace or gas furnace. The glass beads were prepared by melting and stirring and cooling and solidifying.
However, in the process of cooling and solidification, due to the surface tension of the release agent or the like, it does not become a true round glass bead but often deforms and solidifies in a crescent shape.
In Japanese Patent No. 4291318, a glass bead manufacturing apparatus having a heating mechanism, a rotation mechanism, and a swing mechanism is heated by mixing a fine powder sample, a melting agent, and a release agent in a platinum crucible, and rotating and swinging the glass. Making a bead.
In Japanese Patent Application Laid-Open No. 2004-226231, although the glass bead manufacturing apparatus is not specified, the contents are considered to be based on the glass bead manufacturing apparatus. A fine powder sample, a melting agent and a release agent are mixed in a platinum crucible and heated, and a glass bead is produced by rotating and swinging means.
Also in Utility Model Registration No. 2596471, a glass bead manufacturing apparatus having a heating mechanism, a rotation mechanism, and a rocking mechanism is heated by mixing a fine powder sample, a melting agent, and a release agent in a platinum crucible. A glass bead is produced by a swinging means.
However, in any of the above cases, the surface tension due to the release agent or the like is often not solidified into a perfect circular glass bead, but is often deformed and solidified into a crescent shape. Therefore, it is necessary to lift the high-temperature platinum crucible with a special tongs immediately after the heating, and to cool and solidify into a perfect circle while shaking it appropriately. It is dangerous work at high temperature.
The present invention provides a method for producing a round glass high-quality glass bead by using a glass bead production apparatus to prevent deformation solidification due to an increase in surface tension caused by a release agent or the like in the process of cooling and solidification after completion of melting and heating. It is what we propose.
請求項１の場合、ガラスビード作製装置の加熱機構に設置された耐熱ホルダーに、微粉末試料と溶融剤及び剥離剤を混入した白金ルツボを設置し、８００°Ｃ〜１２００°Ｃの決められた温度にて加熱溶融を行う。加熱終了後直ちに白金ルツボを揺動機構により１５度から３０度の間の適当な角度に傾け、同時に回転機構により３０ＲＰＭ〜６０ＲＰＭの適当な回転数にて回転させながら放冷却する。この状態で溶融試料は白金ルツボ底面を穏やかに移動しながら凝固していく。完全に凝固したら揺動機構の傾きを水平に戻し、回転を停止する。これにより品質の良い完全な円形のガラスビードが作製できる。
請求項２の場合、ガラスビード作製装置で白金ルツボを８００°Ｃ〜１２００°Ｃの決められた温度にて加熱溶融し、加熱終了後直ちに水平の白金ルツボを２００ＲＰＭ〜３００ＲＰＭの高速回転を２〜３秒間与えて試料が遠心力で外周に寄ったところで回転を停止する。すると高速回転の遠心力で外周に寄った溶融試料が回転終了と同時に中心に向かって移動し底面に均一に広がったところでそのまま凝固する。これにより品質の良い完全な円形のガラスビードができる。
請求項１の場合においても請求項２の場合においても、加熱装置は、高周波加熱炉の他に電気炉でもガス炉でも応用できる。In the case of claim 1, a platinum crucible mixed with a fine powder sample, a melting agent and a release agent is installed in a heat-resistant holder installed in a heating mechanism of a glass bead manufacturing apparatus, and a temperature of 800 ° C. to 1200 ° C. is determined. Heat melting at temperature . Immediately after the heating, the platinum crucible is tilted to an appropriate angle between 15 degrees and 30 degrees by the swing mechanism , and at the same time, the platinum crucible is allowed to cool while being rotated at an appropriate rotational speed of 30 RPM to 60 RPM by the rotating mechanism. In this state, the molten sample solidifies while gently moving on the bottom of the platinum crucible. When completely solidified, the tilt of the swing mechanism is returned to the horizontal position and the rotation is stopped. This makes it possible to produce a perfect circular glass bead of good quality.
In the case of claim 2, the platinum crucible is heated and melted at a predetermined temperature of 800 ° C. to 1200 ° C. with a glass bead manufacturing apparatus, and immediately after the heating is completed, the horizontal platinum crucible is rotated at a high speed of 200 RPM to 300 RPM. Apply for 3 seconds and stop rotation when the sample approaches the outer periphery by centrifugal force. Then, the molten sample approaching the outer periphery by the centrifugal force of high-speed rotation moves toward the center at the end of rotation and solidifies as it is when it spreads uniformly on the bottom surface. This makes a perfect circular glass bead of good quality.
In both the case of claim 1 and the case of claim 2, the heating device can be applied to an electric furnace or a gas furnace in addition to a high-frequency heating furnace.
本発明の方法を用いると、変形や三日月形防止のための厳密な剥離剤の添加管理が不要になる。
また、変形や三日月形になる時に、専用のトングスで高温の白金ルツボを持ち上げて適当に揺らせながら冷却凝固して真円に固める、高温で危険な作業がなくなる。
連続のガラスビード作製装置に組み込むと、変形ガラスビードによる不良品はなくなる。When the method of the present invention is used, it is not necessary to strictly manage the addition of a release agent to prevent deformation and crescent shape.
Also, when it becomes deformed or crescent shaped, the high temperature platinum crucible is lifted with a special tongs, and it is cooled and solidified while being shaken appropriately.
When incorporated in a continuous glass bead manufacturing apparatus, defective products due to deformed glass beads are eliminated.
ガラスビードの作製方法を図１により説明する。
請求項１の場合、ガラスビード作製装置（１）の耐熱ホルダー（３）に、微粉末試料と溶融剤及び剥離剤を混入した白金ルツボ（４）を乗せて蓋（５）をし、加熱機構（２）により８００°Ｃ〜１２００°Ｃの決められた温度にて加熱溶融する。加熱機構（２）は内側に加熱コイル（７）を設置し、周りは絶縁断熱部材（８）で囲われている。加熱機構（２）の加熱温度制御は、誘導加熱回路部（９）により行う。
溶融加熱終了後、素早く揺動機構（１１）により加熱機構（２）及び白金ルツボ（４）を１５度から３０度の間の適当な角度に傾斜させ、回転機構（１０）により３０ＲＰＭ〜６０ＲＰＭの適当な回転を与え、回転放冷を数十秒間行い、この状態で凝固させる。凝固したら、揺動機構（１１）により加熱機構（２）を水平に戻し完了する。
この動作により、品質の良い完全な真円形のガラスビード（６）ができる。
試料は無機物、酸化物の微粉末とし、溶融剤は四ホウ酸リチウム、剥離剤は臭化リチウムなどが用いられる。
請求項２の場合、ガラスビード作製装置（１）及び加熱溶融過程は、請求項１と同様である。
加熱溶融終了直後に、水平状態の白金ルツボ（４）を回転機構（１０）により２００ＲＰＭ〜３００ＲＰＭの高速回転を２〜３秒間与えて試料が遠心力で外周に寄ったところで回転を止める。そのまま放冷で凝固を待つ。
溶融した試料は、高速回転の遠心力で外周に集まり、回転停止と共に中心に向かって流れ、数秒後には水平になり真円形のガラスビード（６）になり凝固してゆく・
完全に凝固すると、品質の良い完全な真円形のガラスビード（６）ができる。
上記請求項１及び請求項２の工程は、システムとしてガラスビード作製装置に組み込むことも可能である。
図２は、白金ルツボのガラスビードが三日月形になった状態の断面図であり、図３は、白金ルツボのガラスビードが三日月形になった状態の平面図である。図４は、白金ルツボのガラスビードが平滑状態の断面図である。A method for producing a glass bead will be described with reference to FIG.
In the case of claim 1, a platinum crucible (4) mixed with a fine powder sample, a melting agent and a release agent is placed on the heat-resistant holder (3) of the glass bead manufacturing apparatus (1), and the lid (5) is placed thereon, and the heating mechanism It is heated and melted at a predetermined temperature of 800 ° C. to 1200 ° C. according to (2). The heating mechanism (2) is provided with a heating coil (7) on the inside, and is surrounded by an insulating heat insulating member (8). The heating temperature control of the heating mechanism (2) is performed by the induction heating circuit section (9).
After the end of melting and heating, the heating mechanism (2) and the platinum crucible (4) are quickly tilted to an appropriate angle between 15 degrees and 30 degrees by the rocking mechanism (11), and 30 RPM to 60 RPM by the rotating mechanism (10). Appropriate rotation is given, rotation cooling is performed for several tens of seconds, and solidification is performed in this state. Once solidified, the heating mechanism (2) is returned to the horizontal position by the swing mechanism (11) to complete.
By this operation, a perfect round glass bead (6) with good quality can be obtained.
The sample is an inorganic substance or fine oxide powder, the melting agent is lithium tetraborate, and the release agent is lithium bromide.
In the case of claim 2, the glass bead manufacturing apparatus (1) and the heating and melting process are the same as those of claim 1.
Immediately after the completion of heating and melting, the platinum crucible (4) in a horizontal state is subjected to high speed rotation of 200 RPM to 300 RPM for 2 to 3 seconds by the rotation mechanism (10) , and the rotation is stopped when the sample approaches the outer periphery by centrifugal force . Allow to cool and wait for coagulation.
The molten sample gathers on the outer periphery due to the centrifugal force of high-speed rotation, flows toward the center when rotation stops, and becomes horizontal and becomes a perfect circular glass bead (6) in a few seconds, and then solidifies.
When completely solidified, a perfect round glass bead (6) of good quality is produced.
The processes of claims 1 and 2 can be incorporated into a glass bead manufacturing apparatus as a system.
FIG. 2 is a cross-sectional view of a platinum crucible glass bead in a crescent shape, and FIG. 3 is a plan view of a platinum crucible glass bead in a crescent shape. FIG. 4 is a cross-sectional view of a platinum crucible with a smooth glass bead.
１ ガラスビード作製装置
２ 加熱機構
３ 耐熱ホルダー
４ 白金ルツボ
５ 蓋
６ ガラスビード
７ 加熱コイル
８ 絶縁断熱部材
９ 誘導加熱回路部
１０ 回転機構
１１ 揺動機構
１１ａ 大プーリ
１１ｂ 小プーリ
１１ｃ ベルト
１１ｄ 揺動モーターDESCRIPTION OF SYMBOLS 1 Glass bead preparation apparatus 2
Claims (2)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2017021678A JP6384800B2 (en) | 2017-01-23 | 2017-01-23 | Method for producing glass beads for X-ray fluorescence analyzer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2017021678A JP6384800B2 (en) | 2017-01-23 | 2017-01-23 | Method for producing glass beads for X-ray fluorescence analyzer |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2018119940A JP2018119940A (en) | 2018-08-02 |
| JP6384800B2 true JP6384800B2 (en) | 2018-09-05 |
Family
ID=63045106
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2017021678A Expired - Fee Related JP6384800B2 (en) | 2017-01-23 | 2017-01-23 | Method for producing glass beads for X-ray fluorescence analyzer |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP6384800B2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108918563A (en) * | 2018-08-08 | 2018-11-30 | 唐山瑞丰钢铁（集团）有限公司 | Preparation method for the sample of manganese silicon phosphorus content in X-ray fluorescence method measurement silicomangan |
| CN114518377B (en) * | 2022-04-20 | 2022-06-24 | 南京中科特检机器人有限公司 | Fuse piece system of intelligent robot for x-ray fluorescence analysis |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6141948A (en) * | 1984-08-06 | 1986-02-28 | Nippon Steel Corp | Production of bead sample for component analysis |
| JPS63210758A (en) * | 1987-02-27 | 1988-09-01 | Aichi Steel Works Ltd | Fluorescent x-ray analysis of metal |
| JPH0280326A (en) * | 1988-09-06 | 1990-03-20 | Shinagawa Refract Co Ltd | Glass bead sample preparing device and its utilization |
| JP2596471Y2 (en) * | 1992-12-16 | 1999-06-14 | 日本サーモニクス 株式会社 | X-ray fluorescence sample preparation equipment |
| JP2004226231A (en) * | 2003-01-23 | 2004-08-12 | Murata Mfg Co Ltd | Method of manufacturing glass bead for fluorescent x-ray analysis |
| JP4322598B2 (en) * | 2003-08-29 | 2009-09-02 | Ｔｄｋ株式会社 | Evaluation sample preparation method, analysis method, electronic component material production method, and evaluation sample preparation apparatus |
| DE102012109248A1 (en) * | 2012-09-28 | 2014-04-03 | Fluxana GmbH & Co. KG | Preparation of analysis samples |
-
2017
- 2017-01-23 JP JP2017021678A patent/JP6384800B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JP2018119940A (en) | 2018-08-02 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP6384800B2 (en) | Method for producing glass beads for X-ray fluorescence analyzer | |
| KR102071164B1 (en) | Method and apparatus for producing a slurry slurry | |
| KR20190108105A (en) | Casting method | |
| CN105358955A (en) | Method and device for producing a tablet | |
| JP6651644B2 (en) | Continuous semi-solid die casting manufacturing method and manufacturing system | |
| CN104846219A (en) | Preparation device and preparation method of metal semi-solid billets | |
| EP1745873B1 (en) | Method and device for removing slag | |
| CN104439202B (en) | System used for casting alloy and method for machining casting | |
| JP2005118783A (en) | Metal-mold casting device in casting equipment | |
| CN104209488B (en) | Vacuum centrifugal casting method and device thereof | |
| JP2002026405A (en) | Thermoelectric material, and method and device for manufacturing it | |
| WO2016180362A1 (en) | Cutting and breaking device for homogenizing and refining metallic melts and rheological forming method | |
| KR101974334B1 (en) | Method for manufacturing glassbead | |
| JP5536290B1 (en) | Method for producing sulfur solidified body and apparatus for producing sulfur solidified body | |
| CN102798567A (en) | High-frequency sample wafer fusing machine | |
| JP2007010501A (en) | Glass bead manufacturing device and method | |
| JPS62240845A (en) | Apparatus for preparing sample for fluorescent x-ray analysis | |
| JP2008222523A (en) | Method of manufacturing glass gob | |
| JP2004226231A (en) | Method of manufacturing glass bead for fluorescent x-ray analysis | |
| CN209773411U (en) | Material mixing and casting mechanism based on tin-copper alloy target production device | |
| JP6459375B2 (en) | Centrifugal casting method of metal material | |
| KR101719725B1 (en) | Vacuum casting apparatus for producing turbo charger wheel and spark plug of internal combustion engine | |
| JPS6319302Y2 (en) | ||
| JPH05123829A (en) | Treatment of molten steel | |
| CN111601673A (en) | Stirring device for semi-solid metal slurry and method and system for producing semi-solid metal slurry using the same |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| TRDD | Decision of grant or rejection written | ||
| A01 | Written decision to grant a patent or to grant a registration (utility model) |
Free format text: JAPANESE INTERMEDIATE CODE: A01 Effective date: 20180724 |
|
| A61 | First payment of annual fees (during grant procedure) |
Free format text: JAPANESE INTERMEDIATE CODE: A61 Effective date: 20180727 |
|
| R150 | Certificate of patent or registration of utility model |
Ref document number: 6384800 Country of ref document: JP Free format text: JAPANESE INTERMEDIATE CODE: R150 |
|
| LAPS | Cancellation because of no payment of annual fees |