JPS6141945A - Production of bead sample for component analysis - Google Patents
Production of bead sample for component analysisInfo
- Publication number
- JPS6141945A JPS6141945A JP16379984A JP16379984A JPS6141945A JP S6141945 A JPS6141945 A JP S6141945A JP 16379984 A JP16379984 A JP 16379984A JP 16379984 A JP16379984 A JP 16379984A JP S6141945 A JPS6141945 A JP S6141945A
- Authority
- JP
- Japan
- Prior art keywords
- bead
- ore
- temp
- stage
- melting
- 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.)
- Granted
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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)
- Sampling And Sample Adjustment (AREA)
- Investigating And Analyzing Materials By Characteristic Methods (AREA)
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野９
本発明は鉱物類の化学成分分析用ビード試料の製造方法
ｆこ関するものである。DETAILED DESCRIPTION OF THE INVENTION (Industrial Application Field 9) The present invention relates to a method for producing a bead sample for chemical component analysis of minerals.
（従来の技術〕
ＪＩＳ −Ｍ −８２０５ｔこ示すよう１こ、該鉱物類
を融剤やはぐり剤と混合して白金容器内で浴融撹拌後葡
却してガラス質のビード資料を製造する方法で、溶融物
が凝固する時ｔこ表面張力１こよってビード周縁部に上
反シ（まれに下皮シシの湾曲が生ずる。(Prior art) As shown in JIS-M-8205t, 1 is a method of manufacturing glassy bead materials by mixing the minerals with a fluxing agent and a peeling agent, stirring the mixture in a platinum container, and then discarding the mixture. When the molten material solidifies, the surface tension 1 causes an inversion (in rare cases, a curvature of the lower skin) at the bead periphery.
螢光Ｘ線分析法ではＸ１ｖ１５！照射距離が重要な管理
項目となる。例えば、上皮シ湾曲部の高さが０．６ｍｆ
こなるとＴ、Ｆｅの分析値が０．６％（ａｔ５０％Ｔ、
Ｆｅ％）低値となる。このため、特開昭５６−６０３３
７号に示すような上皮シ湾曲部を補正するようなスペー
サーを用いるか、或いは一般的１こ行われているビード
下面を分析する方法が行なわれている。X1v15 in fluorescent X-ray analysis! Irradiation distance is an important control item. For example, the height of the epithelial curve is 0.6 mf.
In this case, the analysis value of T and Fe is 0.6% (at50%T,
Fe%) becomes a low value. For this reason, JP-A-56-6033
A spacer such as that shown in No. 7 is used to correct the curved portion of the epithelium, or a commonly used method is to analyze the underside of the bead.
（発明が解決しようとする問題点）
％開昭５６−６０３３７号の如くスペーサーを用いる方
法は効果的であるが、Ｘ線強度がスペーサーの分だけ弱
くなυ微量成分析１こは不利になる。又、従来技術の他
の一つであるビード下面を分析する方法は常に白金容器
の底面を平らに保たなければならないが、加熱冷却の繰
り返しで歪が生ずるため白金容器の底面を平らに保つこ
とは困難である。(Problems to be Solved by the Invention) Although the method using a spacer as in Patent Publication No. 56-60337 is effective, the X-ray intensity is weaker due to the spacer, which is disadvantageous for υ trace component analysis. . In addition, in the method of analyzing the bottom surface of the bead, which is another conventional technique, the bottom surface of the platinum container must be kept flat at all times, but since distortion occurs due to repeated heating and cooling, it is difficult to keep the bottom surface of the platinum container flat. That is difficult.
本発明は前記したビード試料の周縁近傍に発生する上反
り状、下皮り状の湾曲の発生を防止することを目的とす
るものである。The object of the present invention is to prevent the above-mentioned curvature or curvature that occurs near the periphery of the bead sample from occurring.
（問題点を解決するための手段〕
本発明は粉末鉱物類を融剤とともに白金容器内で加熱融
解してビード試料を製造する方法１こ於いて、溶融撹拌
工程、該鉱物類の凝固温度＋１０℃〜５００℃の範囲内
の所定温度で５秒以上保持する平面成形工程、冷却工程
を順次経ることを特徴とする成分分析用ビード試料製造
方法にある。(Means for Solving the Problems) The present invention provides a method 1 for manufacturing a bead sample by heating and melting powdered minerals together with a flux in a platinum container, in which the melting and stirring step is performed at a solidification temperature of the minerals + 10%. A method for producing a bead sample for component analysis, characterized by sequentially carrying out a flat molding step of holding at a predetermined temperature within the range of 500° C. for 5 seconds or more, and a cooling step.
（作用〕
本発明における前記溶融撹拌工程、平面形成工程及び冷
却工程の各々の条件限定にもとすく作用１こついて以下
１こ述べる。(Function) The following is a description of one effect of limiting the conditions for each of the melting and stirring step, the plane forming step, and the cooling step in the present invention.
■溶融撹拌工程
該粉末鉱物を融剤で溶融し、均一に撹拌するものである
。(2) Melting and stirring process The powdered mineral is melted with a flux and stirred uniformly.
■平面成形工程
ビード上面の周縁近傍の上皮シ又は下反りの湾曲は、凝
固直前の溶融物の表面張力によって左右され、この表面
張力は溶融物の温度によって大きく異なる。ビード上面
を平面状に形成される温度が凝固温反＋１０℃〜５００
℃の範囲中にあることは本発明者が種々の実験と検討を
重ねて見いだしたものであり、鉄鉱石類に於いては凝固
点＋２５０℃を超えると周縁近傍部に上反りの湾曲が生
じ、）χ固点＋５０℃以下では上皮シ又は下皮シの湾曲
となり好ましくない。(2) Plane forming process The curvature of the epithelium or downward curvature near the periphery of the upper surface of the bead is influenced by the surface tension of the molten material just before solidification, and this surface tension varies greatly depending on the temperature of the molten material. The temperature at which the top surface of the bead is formed into a flat shape is the solidification temperature +10℃~500℃.
The inventor of the present invention has discovered through various experiments and studies that the iron ore is within the range of 250°C above the freezing point, and an upward curvature occurs near the periphery of the iron ore. ) Below χ solid point +50°C, the epithelium or hypodermis becomes curved, which is not preferable.
なお、平面が形成される温度は融剤の種類、添加するは
くυ剤及び白金容器の側壁角度によって異なるので、ビ
ード製造条件毎に最適湿度を選定する。保持する時間は
上反り部分が表面張力の変化によってゼロ１こなるまで
、通常１０秒以ユ必要である。Note that the temperature at which the flat surface is formed varies depending on the type of flux, the added foil, and the side wall angle of the platinum container, so the optimum humidity is selected for each bead production condition. The holding time is usually 10 seconds or more until the warped portion becomes zero-1 due to a change in surface tension.
■冷却工程
平面形成工程温度温まで放冷する。はぐり性の悪い粉末
鉱物類のビードを作成する場合には特開昭５７−６１９
３８に示すように凝固点直下で所定時間保持する方法が
あるが、不法では放冷のみで良好なはくシ性を示す。■ Cooling process Plane forming process Allow to cool to temperature. When making beads of powdered minerals with poor peelability, please refer to Japanese Patent Application Laid-Open No. 57-619.
As shown in No. 38, there is a method of holding the material just below the freezing point for a predetermined period of time, but illegally, it shows good adhesive properties only by allowing it to cool.
（実施例）
樹、下鉄鉱石類で本発明を実施した一例１こついて説明
する。(Example) An example 1 in which the present invention was implemented using iron ores will be explained.
鉄鉱石類０．５ｇを融剤（ホウ酸ナトリウム）５ｇと酸
化剤（ＫＩＯ，） ０．０５ ｇを白金容器に入れ、第
１図に示すごとく高周波炉で溶融撹拌工程９５０℃×４
分間、千面形成工程８００℃×１分間加熱して放冷する
ヒートパターンで、１００個のビード試料を作成した結
果、全ての試料が良好な平面になった。それｆこ比較し
て第２図１ご示す従来技術のヒートパターンでは全ての
ビードに上皮シの湾曲が生じた。0.5 g of iron ore, 5 g of flux (sodium borate) and 0.05 g of oxidizing agent (KIO) were placed in a platinum container, and melted and stirred in a high frequency furnace at 950°C x 4 times as shown in Figure 1.
As a result of creating 100 bead samples using a heat pattern of heating at 800° C. for 1 minute and cooling for 1 minute, all samples had good flat surfaces. In comparison, in the conventional heat pattern shown in FIG. 2, all beads had epithelial curvature.
なお、平面形成工程の最適温度は、融剤の種類及び添加
するはくり剤の種類や量によって異なるが、融剤にホウ
酸ナトリウム５ｇｘはくシ剤にヨウ素酸カリウム０．０
５ｇ用いた場合の平面形成工程温度とビード周縁部の湾
曲は第３図１こ示すごとく８００℃が最適である。The optimum temperature for the plane forming process varies depending on the type of flux and the type and amount of the peeling agent added, but the temperature should be 5 g of sodium borate for the flux and 0.0 g of potassium iodate for the foil.
When 5g is used, the optimum temperature for the flat surface forming process and the curvature of the bead periphery are 800°C as shown in FIG. 3.
（発明の効果〕
本発明によれば溶融撹拌工程後の冷却過程１こ平面形成
工程を設け、平面形成に最適な温度に保持することで、
ビード上面の湾曲が防止でき、螢光Ｘ線分析に最適など
−ド試料が得られる。(Effect of the invention) According to the present invention, by providing a plane forming step in the cooling process after the melting and stirring step and maintaining the temperature at the optimum temperature for forming the plane,
Curving of the upper surface of the bead can be prevented, and an ideal sample for fluorescent X-ray analysis can be obtained.
第１図は本発明によるヒートパターンであり、第２図は
特開昭５７−６１９３８によるヒートパターンである。
第３図はビード平面形成工程の温度を９００℃、８００
℃、 ７００℃、 ６００℃と変化させた場合の湾
曲状況を示す図で、（イ）は断面図、（ロ）は平面図で
ある。FIG. 1 shows a heat pattern according to the present invention, and FIG. 2 shows a heat pattern according to Japanese Patent Application Laid-Open No. 57-61938. Figure 3 shows the temperatures of the bead plane forming process at 900°C and 800°C.
700° C., 700° C., and 600° C., in which (a) is a cross-sectional view and (b) is a plan view.
Claims (1)
ード試料を製造する方法に於いて、溶融撹拌工程、該鉱
物類の凝固温度＋１０℃〜５００℃の範囲内の所定温度
で５秒以上保持する平面成形工程、冷却工程を順次経る
ことを特徴とする成分分析用ビード試料製造方法。In a method of manufacturing a bead sample by heating and melting powdered minerals together with a flux in a platinum container, the melting and stirring step is performed at a predetermined temperature within the range of the solidification temperature of the mineral +10°C to 500°C for 5 seconds or more. A method for producing a bead sample for component analysis, characterized by sequentially carrying out a holding flat forming process and a cooling process.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16379984A JPS6141945A (en) | 1984-08-06 | 1984-08-06 | Production of bead sample for component analysis |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16379984A JPS6141945A (en) | 1984-08-06 | 1984-08-06 | Production of bead sample for component analysis |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6141945A true JPS6141945A (en) | 1986-02-28 |
| JPH0327061B2 JPH0327061B2 (en) | 1991-04-12 |
Family
ID=15780920
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP16379984A Granted JPS6141945A (en) | 1984-08-06 | 1984-08-06 | Production of bead sample for component analysis |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6141945A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004069758A1 (en) * | 2003-01-06 | 2004-08-19 | Lang, G | Flux for producing beads for x-fluorescent analysis and method for producing said flux |
-
1984
- 1984-08-06 JP JP16379984A patent/JPS6141945A/en active Granted
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004069758A1 (en) * | 2003-01-06 | 2004-08-19 | Lang, G | Flux for producing beads for x-fluorescent analysis and method for producing said flux |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0327061B2 (en) | 1991-04-12 |
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