JPS63154945A - Analysis of glass - Google Patents
Analysis of glassInfo
- Publication number
- JPS63154945A JPS63154945A JP30248186A JP30248186A JPS63154945A JP S63154945 A JPS63154945 A JP S63154945A JP 30248186 A JP30248186 A JP 30248186A JP 30248186 A JP30248186 A JP 30248186A JP S63154945 A JPS63154945 A JP S63154945A
- Authority
- JP
- Japan
- Prior art keywords
- glass
- analysis
- sample
- hydrogen fluoride
- aqueous solution
- 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.)
- Pending
Links
- 239000011521 glass Substances 0.000 title claims abstract description 40
- 238000004458 analytical method Methods 0.000 title claims abstract description 27
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 42
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000002253 acid Substances 0.000 claims abstract description 8
- 239000007864 aqueous solution Substances 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 4
- ABTOQLMXBSRXSM-UHFFFAOYSA-N silicon tetrafluoride Chemical compound F[Si](F)(F)F ABTOQLMXBSRXSM-UHFFFAOYSA-N 0.000 claims description 9
- 230000008018 melting Effects 0.000 claims description 3
- 238000002844 melting Methods 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 abstract description 7
- 239000010703 silicon Substances 0.000 abstract description 7
- 238000005259 measurement Methods 0.000 abstract description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 4
- 239000010453 quartz Substances 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
- 229910052739 hydrogen Inorganic materials 0.000 abstract 2
- 239000001257 hydrogen Substances 0.000 abstract 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 abstract 2
- 239000000523 sample Substances 0.000 description 13
- 239000000243 solution Substances 0.000 description 9
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 7
- 239000012535 impurity Substances 0.000 description 7
- 239000013256 coordination polymer Substances 0.000 description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 5
- 238000002834 transmittance Methods 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- 239000004743 Polypropylene Substances 0.000 description 3
- 239000004809 Teflon Substances 0.000 description 3
- 229920006362 Teflon® Polymers 0.000 description 3
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- -1 polypropylene Polymers 0.000 description 3
- 229920001155 polypropylene Polymers 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 239000006199 nebulizer Substances 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 239000012488 sample solution Substances 0.000 description 2
- 238000004506 ultrasonic cleaning Methods 0.000 description 2
- 244000089486 Phragmites australis subsp australis Species 0.000 description 1
- 235000014676 Phragmites communis Nutrition 0.000 description 1
- 239000000538 analytical sample Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 235000013601 eggs Nutrition 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
Landscapes
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
Description
【発明の詳細な説明】 〔産業上の利用分野〕 本発明はガラスの分析方法に関する。[Detailed description of the invention] [Industrial application field] The present invention relates to a method for analyzing glass.
本発明は弗化水素を用いてガラスを溶解し１分析試料と
するガラスの工ＣＰ分析法において、ガラスを弗化水素
および四弗化ケイ素を加熱により蒸発させてから、■び
水または酸水溶液を添加して分析する。従来は弗化水素
酸溶液の、６４、工ＣＰ分析を行なっていたので分析精
度ｔ；あｈ″−らないという問題点を有してｔ、−＋７
２が、本発明を用いることにより、飛降的に分析積電を
向上させろことが可能となった。In the CP analysis method of glass, which uses hydrogen fluoride to melt glass and prepare one analysis sample, the present invention involves heating the glass to evaporate hydrogen fluoride and silicon tetrafluoride, and then Add and analyze. Conventionally, CP analysis of hydrofluoric acid solution was carried out, which had the problem that the analysis accuracy was not t, -+7.
2, by using the present invention, it has become possible to improve the analytical product in a flying manner.
近年１石英ガラス等の基板はハイテク分野に利用され、
要求されるガラス純変も牟々高水準となってきている。In recent years, substrates such as 1 quartz glass have been used in high-tech fields,
The required glass purity has also become extremely high.
しため１つて品ｉ管卵の面から亮精質の分析法を開発す
ることｈ；必要と言える。Therefore, it is necessary to develop a method for analyzing the quality of the spermatozoa from the perspective of the quality of the eggs.
従来のガラスの工ＣＰ分析は弗化水素酸だ溶解し定試料
を弗酸溶液のまま測定してｂた。Conventional CP analysis of glass involves dissolving the sample in hydrofluoric acid and measuring the sample as it is in the hydrofluoric acid solution.
しかし、前述の従来技術では次のような問題点を有する
。However, the above-mentioned conventional technology has the following problems.
（１） 弗化水素酸溶液のため、樗変の高いクォーツ
系のトーチが使用できず、テフロン系のトーチを使用し
なければならない。(1) Because of the hydrofluoric acid solution, a quartz-based torch with a high degree of translucency cannot be used, and a Teflon-based torch must be used.
（２） 弗化水素だガラスを溶解するため、弗化水素
酸をガラスの数倍量添加せねばならず、実際の不純物製
電よりも低い濃度の試料を測定しなければならないので
精度がおちる。(2) Hydrogen fluoride: In order to dissolve the glass, it is necessary to add several times the amount of hydrofluoric acid to the glass, and it is necessary to measure a sample with a lower concentration than the actual impurity production, which reduces accuracy. .
（３） ガラスの主成分定るケイ素ｆｌｔ犬量に溶解
しているため、ケイ素の発光ピークが非常に大弾くなり
、バックグラウンドめ；安定しなかったり、ケイ素のピ
ークにかぐれてしまい、測定できない元素もでてくる。(3) Because the main component of glass is silicon, which is dissolved in a fixed amount, the emission peak of silicon becomes very loud and becomes background; There are some elements that cannot be done.
（４） 弗化水素酸と四弗化ケイ素の溶液の粘性は比
較的犬鍍いため、■ＣＰネブライザーからの吸収が安定
しにくい。(4) Since the viscosity of a solution of hydrofluoric acid and silicon tetrafluoride is relatively low, absorption from ■CP nebulizer is difficult to stabilize.
本発明のガラスの工ａｐ分析法は１分析試料を弗化水素
酸を甲いて溶解しｔ後、弗化水素および四弗化ケイ素を
加熱により蒸発させてから水あるいは酸水溶液を添加し
て分析試料とすることを特徴とする、
〔作用〕
本発明の上記の構成によれば１次のような理由により分
析精首を飛踵的如向上することができる、（１） 弗
化水素を含まない系での分析ｈ１できろため、精度の高
いクォーツ系のトーチが使用できる、（２） ガラス
を溶解させろために余分に添加した弗化水素酸を蒸発に
より除去できるため、ガラスの不純物濃叶と−（ロ）じ
不純物ＩＩＦの系をつくり、試料とすることができる。The glass engineering analysis method of the present invention involves dissolving an analytical sample in hydrofluoric acid, evaporating hydrogen fluoride and silicon tetrafluoride by heating, and then adding water or an acid aqueous solution for analysis. [Function] According to the above-described structure of the present invention, the precision of analysis can be dramatically improved for the following reasons: (1) Hydrogen fluoride is not included. (2) Since the extra hydrofluoric acid added to melt the glass can be removed by evaporation, the concentration of impurities in the glass can be removed. A system of the same impurity IIF can be created and used as a sample.
（３） ガラスの主成分たるケイ素は弗化水素に溶解
して四弗化ケイ素になるが、これは沸点が氷点下にある
ので加熱により容易に除去で弾る。したがって、ケイ素
りｔ存在しない系とすること六；で鎗バックグラウンド
に影響を及ぼさない。した１１１’、つて弗化水素溶液
試料の場合、ケイ素のピークにかくれてしまい、測定不
能でもった元素（例えば、ニッケル）でも測定ｂ；容易
にできろ。(3) Silicon, the main component of glass, dissolves in hydrogen fluoride to form silicon tetrafluoride, which has a boiling point below the freezing point and can be easily removed by heating. Therefore, by making the system free of silicon, the background will not be affected. In the case of a 111' hydrogen fluoride solution sample, even elements (such as nickel) that cannot be measured because they are hidden behind the silicon peak can be easily measured.
（４）弗化水素酸と四弗化ケイ素の系から、水または酸
水溶液の系に替わるため、粘性ｈ；近くなり、工ＣＰネ
ブライザーからの試料吸入ｈ′−安定し、精度向上に寄
与する。(4) Since the system of hydrofluoric acid and silicon tetrafluoride is replaced by the system of water or acid aqueous solution, the viscosity becomes closer to h', which stabilizes the sample intake from the CP nebulizer and contributes to improved accuracy. .
実施例１゜
工Ｃフｔトマスク基板のＮｊ にニッケル）純貧と紫外
透過率の相関を求める定めに分析を行なりｔ、。Example 1 An analysis was carried out to determine the correlation between pure impurity (Nj of nickel) and ultraviolet transmittance of a C foot mask substrate.
紫外透過率を測定した工Ｃフォトマスク基板から線質分
析用試料として５ｇのガラスを切り出した。切り出ｉ、
たガラス片をアセトンに浸し、１０分間超音波洗浄をし
た。次にガラス片８−純水でよく洗浄したあと、１規定
塩酸水溶液中に浸し、１０分間放電して表面に寸着した
ゴミや、油分を除去した、再びガラス片を純水でよく洗
浄しｆｃあと、よく洗浄され之ポリプロピレン製のビン
に入れ、密閉した。次にガラス片の重さの５倍量の５０
悌弗化水素酸（ｇｂ−ｓｓ グレード）を添加し、密閉
し＋ ６０ ’Ｃの栢温槽中に一昼夜密閉して放曾した
ところ、ガラス片は完全に溶解し７ｔ６得られ次試料溶
液を充分に洗浄したテフロン製ビーカーに移し替え、オ
イルバス中で１５０℃にホールドシて弗化水素酸および
四弗化ケイ素を蒸発させて除去した。約２時間で弗化水
素および四弗化ケイ素は完全に蒸発し、あとだ若干のガ
ラスに含まれていた不純物ｈ；残留した。残留物に１規
定の硝酸を添加し、加熱しなｈ；ら溶解した。不純物の
硝酸溶液を充分に洗浄されたポリプロピレン製容器にと
り、秤量しながら１Ｎ硝酸溶液を更廻添加し、溶液の重
量が、最初のガラス片と同様になるようにし之。−
以上の手煩で作成した分析サンプルを工ＣＰ（工ｏｎ
ＣｏｕｐＨｅｄ Ｐｌａｓｍａ ）分析機にて分析し之
。5 g of glass was cut out as a sample for radiation quality analysis from the C photomask substrate whose ultraviolet transmittance was measured. Cutout i,
The glass pieces were immersed in acetone and subjected to ultrasonic cleaning for 10 minutes. Next, glass piece 8 - After thoroughly washing with pure water, immersing it in a 1N hydrochloric acid aqueous solution and discharging it for 10 minutes to remove dirt and oil that had adhered to the surface. Wash the glass piece thoroughly with pure water again. After fc, it was thoroughly washed, placed in a polypropylene bottle, and sealed. Next, 50, which is 5 times the weight of the glass piece
When hydrofluoric acid (GB-SS grade) was added, the glass was sealed and allowed to stand overnight in a heat bath at +60'C, the glass pieces were completely dissolved and a sample solution of 7t6 was obtained. The mixture was transferred to a thoroughly washed Teflon beaker and held at 150° C. in an oil bath to evaporate and remove hydrofluoric acid and silicon tetrafluoride. Hydrogen fluoride and silicon tetrafluoride were completely evaporated in about 2 hours, leaving behind some impurities contained in the glass. 1N nitric acid was added to the residue and dissolved while heating. A nitric acid solution containing impurities was placed in a thoroughly cleaned polypropylene container, and while being weighed, 1N nitric acid solution was added until the weight of the solution was the same as that of the original glass piece. − The analysis sample created through the above steps is
Analyzed using a CoupHed Plasma analyzer.
トーチはクォーツ系のものを用いアルゴンプラズマに、
て行なった。糾明分析結果と紫外透過率の関係を第１表
に示す。The torch is quartz-based and uses argon plasma.
I did it. Table 1 shows the relationship between the clear analysis results and the ultraviolet transmittance.
第１表 Ｎｉ純変と紫外透過嘉の測定
第１表かられかるようＫ ＮｉＩ’ｔ ２６０ ｎｍ
で紫外吸収のピークをもち、ピークの大きさｆ＋”＝
Ｎｉの量に依存していることが拓かる。Table 1 Measurement of Ni purity and ultraviolet transmission
It has an ultraviolet absorption peak at , and the peak size is f+”=
It is revealed that it depends on the amount of Ni.
比較例１゜
実施例１と同じサンプルを弗酸系にて純質分析を行なっ
之。Comparative Example 1 The same sample as in Example 1 was analyzed for purity using a hydrofluoric acid system.
実施例１と同じサンプル２． Ｏ、ｌｉ＋を切り出し、
アセトンに浸し、１０分間超音波洗浄を［７念。次にガ
ラス片を純水でよ〈洗浄したあと、１規定塩酸水溶液中
に浸し、１０分間放買して表面に寸着したゴミや、油分
を除去した。再びガラス片をよく洗浄したあと、よく洗
浄されたポリプロピレン製容器にガラス片を移し替え之
。５０４弗化水素酸（Ｆ、Ｌ−ｓＳグレード）をガラス
片の５倍１ｋ（１００Ｃ）添加した。密閉して６０℃の
恒温槽で一昼夜放置］、たところ、ガラス片は完全に溶
解した。試料に更に５倍量の純水を添加し、トータルで
１００倍量して、工ＣＰ４＋析慢で分析を行なった。線
質分析結果と紫外透過率の関係を第２表に示す。測定は
テフロン系トーチで行なつ之。Sample 2. Same as Example 1. Cut out O, li+,
Soak in acetone and perform ultrasonic cleaning for 10 minutes [7 times]. Next, after washing the glass piece with pure water, it was immersed in a 1N aqueous hydrochloric acid solution for 10 minutes to remove dirt and oil that had settled on the surface. After washing the glass pieces thoroughly again, transfer them to a well-washed polypropylene container. 504 hydrofluoric acid (F, L-sS grade) was added at 1k (100C) 5 times the amount of the glass piece. The glass pieces were completely dissolved after the glass was sealed and left in a constant temperature bath at 60° C. for a day and a night. Five times the amount of pure water was further added to the sample, making the total amount 100 times the amount, and analysis was performed using CP4+ analysis. Table 2 shows the relationship between the radiation quality analysis results and the ultraviolet transmittance. Measurements were performed using a Teflon torch.
紳変測定値はサンプル溶液ｈｔガラス重ｔに対して１０
倍あることから、実測値の１０倍としである。第２表か
られかるとおり、ガラスのＮｉ純電と紫外透過率の間に
相間は見出せない。また、値のでないものと、でるもの
の差が極端である。以上のことから、弗酸系の測定では
純質測定結果があまり精Ｉの良いものではなかったと推
測され７ｔ。The measured value is 10 for the sample solution h and glass weight t.
Since it is twice as large, it is assumed to be 10 times the actual measurement value. As can be seen from Table 2, no correlation can be found between the Ni pure electricity and the ultraviolet transmittance of the glass. Also, the difference between those with no value and those with value is extreme. From the above, it can be inferred that the purity measurement results for hydrofluoric acid were not very accurate.7t.
以上述べて般ｔように発明によれば、工ＣＰによるガラ
ス中の不純物の定量において、ガラスを溶解しｔ後、弗
化水素卦よび四弗化ケイ素を加熱により蒸発させてから
水あるいは酸水溶液を添加して分析試料とすることによ
り、分析精度を大巾に向上させることｈ′−で芦、ガラ
スの品質管理等に大きな貢献をするものである。As described above, according to the invention, in the determination of impurities in glass by CP, after melting the glass, hydrogen fluoride and silicon tetrafluoride are evaporated by heating, and then water or acid aqueous solution is added. By adding h'- to the analysis sample, the accuracy of analysis can be greatly improved, which will greatly contribute to the quality control of reeds and glass.
以 上that's all
Claims (1)
ＩＣＰ分析法において、ガラスを溶解した後、弗化水素
および四弗化ケイ素を加熱により蒸発させてから水ある
いは酸水溶液を添加して分析試料とすることを特徴とす
るガラスの分析方法。In the ICP analysis method of glass as a sample by melting glass using hydrogen fluoride, after melting the glass, hydrogen fluoride and silicon tetrafluoride are evaporated by heating, and then water or an acid aqueous solution is added. A method for analyzing glass, characterized in that it is used as an analysis sample.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP30248186A JPS63154945A (en) | 1986-12-18 | 1986-12-18 | Analysis of glass |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP30248186A JPS63154945A (en) | 1986-12-18 | 1986-12-18 | Analysis of glass |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS63154945A true JPS63154945A (en) | 1988-06-28 |
Family
ID=17909471
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP30248186A Pending JPS63154945A (en) | 1986-12-18 | 1986-12-18 | Analysis of glass |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63154945A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02259563A (en) * | 1989-03-31 | 1990-10-22 | Shin Etsu Handotai Co Ltd | Method for determining concentration of metal impurity in cz single crystal silicon |
| CN101776607A (en) * | 2009-12-30 | 2010-07-14 | 中国科学院上海硅酸盐研究所 | Method for analyzing total arsenic in glass |
| CN103439313A (en) * | 2013-08-16 | 2013-12-11 | 成都光明光电股份有限公司 | Method for testing content of compound in glass |
-
1986
- 1986-12-18 JP JP30248186A patent/JPS63154945A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02259563A (en) * | 1989-03-31 | 1990-10-22 | Shin Etsu Handotai Co Ltd | Method for determining concentration of metal impurity in cz single crystal silicon |
| CN101776607A (en) * | 2009-12-30 | 2010-07-14 | 中国科学院上海硅酸盐研究所 | Method for analyzing total arsenic in glass |
| CN103439313A (en) * | 2013-08-16 | 2013-12-11 | 成都光明光电股份有限公司 | Method for testing content of compound in glass |
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