JP2005114505A - Method for determinating very small amount of selenium in glass - Google Patents
Method for determinating very small amount of selenium in glass Download PDFInfo
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- JP2005114505A JP2005114505A JP2003348067A JP2003348067A JP2005114505A JP 2005114505 A JP2005114505 A JP 2005114505A JP 2003348067 A JP2003348067 A JP 2003348067A JP 2003348067 A JP2003348067 A JP 2003348067A JP 2005114505 A JP2005114505 A JP 2005114505A
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Abstract
Description
本発明は、ガラス中の微量セレンの定量方法に関する。 The present invention relates to a method for determining a trace amount of selenium in glass.
セレンは人にとって必須元素であると同時に、過剰になると人体に害を及ぼすことが知られている。また、環境基準等でも規制がされており、このようなことからも、有害物質であるセレンの濃度を把握することは必要不可欠である。 It is known that selenium is an essential element for human beings and at the same time harms the human body when excessive. In addition, environmental standards are also regulated, and it is indispensable to grasp the concentration of selenium, which is a harmful substance, for these reasons.
微量セレンを分析する際、感度を向上させるため、試料量を多く分解する必要がある。 When analyzing a small amount of selenium, it is necessary to decompose a large amount of sample in order to improve sensitivity.
ガラス中の不純物の定量方法としては、セラミックス協会で定められている公定化学定量法があるが、その中にはセレンの分析方法は規定されていない。セレンと性質が酷似しているヒ素についてはフッ化水素酸、硝酸および硫酸の混酸による分解法(非特許文献1)、NaOH融解法(非特許文献2)などがある。フッ化水素酸、硝酸および硫酸の混酸による分解法ではAs(III)が十分に酸化されず、AsF3として揮散してしまう恐れがあるが、KMnO4を併用することによりAs(V)へ酸化が行われ揮散を防ぐことが出来る。この方法をセレンに適用し分析する場合、セレンが揮散してしまうと言った問題がある。 As a method for quantifying impurities in glass, there is an official chemical quantification method stipulated by the Ceramic Society, but no analysis method for selenium is defined therein. Arsenic having properties very similar to those of selenium includes a decomposition method using a mixed acid of hydrofluoric acid, nitric acid and sulfuric acid (Non-Patent Document 1), an NaOH melting method (Non-Patent Document 2), and the like. In the decomposition method using a mixed acid of hydrofluoric acid, nitric acid and sulfuric acid, As (III) is not sufficiently oxidized and may be volatilized as AsF3. We can prevent volatilization. When this method is applied to selenium and analyzed, there is a problem that selenium is volatilized.
NaOH融解法の場合は、ガラス試料量が多い場合、融解後コロイド状のケイ酸塩が生成し、このケイ酸塩中にセレンが吸着してしまうことが懸念される。このようなことから、ヒ素の定量法をセレンに適用することは出来ない。 In the case of the NaOH melting method, when the amount of the glass sample is large, there is a concern that colloidal silicate is generated after melting and selenium is adsorbed in the silicate. For this reason, the arsenic determination method cannot be applied to selenium.
一方、鉱石中のセレンの分析法は、硝酸と過塩素酸とで分解し、過塩素酸の白煙を発生させた後、テルルで共沈分離誘導結合プラズマ発光分光法(非特許文献3)または3,3−ジアミノペンジジン抽出吸光光度法で定量する方法が、JIS M 8134で規定されているが、この方法では、ガラス試料は分解することが出来ない。
本発明は、従来技術の問題点を解消し、試料の分解および分離等の前処理の過程でのセレンの揮散および吸着による損失を防ぎ、ガラス中のセレンを分析する方法を提供することを目的とする。 An object of the present invention is to provide a method for analyzing selenium in glass by solving the problems of the prior art, preventing loss due to volatilization and adsorption of selenium in the pretreatment process such as decomposition and separation of a sample. And
上記課題を解決するために、本発明はガラス試料をアルカリ融解し溶融物を得、該溶融物を塩酸で溶解し、さらにフッ化水素酸を加え、該溶融物中のコロイダルシリカを分解し溶液とし、放冷後、該溶液に共沈剤としてテルル溶液および還元剤を加え加熱することによりセレンを沈殿させ、セレンをろ過分離させ、該分離物を誘導結合プラズマ発光分光分析法により分析することを特徴とするガラス中セレンの分析方法である。 In order to solve the above problems, the present invention provides a solution in which a glass sample is alkali-melted to obtain a melt, the melt is dissolved with hydrochloric acid, hydrofluoric acid is further added, and colloidal silica in the melt is decomposed. After allowing to cool, a tellurium solution and a reducing agent are added to the solution as a coprecipitation agent and heated to precipitate selenium, the selenium is filtered and separated, and the separated product is analyzed by inductively coupled plasma emission spectrometry. This is a method for analyzing selenium in glass.
本発明は、以上説明した方法により、試料の分解および分離等の前処理過程での揮発および吸着によるセレンの損失なく、ガラス中のセレンを分析することができる。 The present invention can analyze selenium in glass without loss of selenium due to volatilization and adsorption in the pretreatment process such as decomposition and separation of the sample by the method described above.
以下に各過程を図1に基づいて詳細に説明する。
サンプル:ガラスの種類として、石英ガラス,ソーダガラス,ソーダライムガラス等が挙げられる。
(分解方法)
まず、試料をはかり取り、約10倍量の過酸化ナトリウムを加えブンゼンバーナーで加熱し溶解する(ステップS10)。水の入ったビーカーにるつぼを入れ、塩を溶解した後、塩酸を加えて加熱する。放冷後、さらにフッ化水素酸を加えて加熱することによりコロイダルシリカを分解し、試料を完全分解する(ステップS11)。
(共沈方法)
テルル溶液;10g/lテルル溶液 (4N塩酸性)
還元剤:還元剤としては塩化スズ,硫酸ヒドラジニウム,塩化ヒドラジニウムなどがあるが、塩化ヒドラジニウムが好ましい。
Each process will be described in detail below with reference to FIG.
Sample: Examples of glass types include quartz glass, soda glass, and soda lime glass.
(Disassembly method)
First, a sample is weighed, about 10 times the amount of sodium peroxide is added, and heated with a Bunsen burner to dissolve (step S10). Put a crucible in a beaker containing water, dissolve the salt, add hydrochloric acid and heat. After allowing to cool, hydrofluoric acid is further added and heated to decompose the colloidal silica, and the sample is completely decomposed (step S11).
(Co-precipitation method)
Tellurium solution; 10 g / l tellurium solution (4N hydrochloric acid)
Reducing agent: Examples of the reducing agent include tin chloride, hydrazinium sulfate, and hydrazinium chloride, with hydrazinium chloride being preferred.
放冷後、試料溶液にテルル溶液および塩化ヒドラジニウムを加え、180〜200°Cで2時間程度加熱し、セレンを還元し共沈させる(ステップS12)。
(分離方法)
5種Bのろ紙を用いてろ過(ステップS13)後、希塩酸で沈殿をよく洗浄し、ろ液は廃棄する。受けのビ−カーを取替え、熱王水を少量ずつ加え、沈殿を溶解する(ステップS14)。純水でろ紙をよく洗浄した後、ろ液を湯煎器上で乾固させる(ステップS15)。
(定量方法)
乾固後、残渣を王水で溶解し(ステップS16)、純水を加えて定容して試料溶液とする。この溶液を、誘導結合プラズマ発光分光分析法で定量する(ステップS17)。
After standing to cool, a tellurium solution and hydrazinium chloride are added to the sample solution and heated at 180 to 200 ° C. for about 2 hours to reduce and coprecipitate selenium (step S12).
(Separation method)
After filtration using Step 5 B filter paper (step S13), the precipitate is thoroughly washed with dilute hydrochloric acid, and the filtrate is discarded. The receiving beaker is replaced, hot aqua regia is added little by little, and the precipitate is dissolved (step S14). After thoroughly washing the filter paper with pure water, the filtrate is dried on a water bath (step S15).
(Quantitative method)
After drying to dryness, the residue is dissolved in aqua regia (step S16), and pure water is added to make a constant volume to obtain a sample solution. This solution is quantified by inductively coupled plasma optical emission spectrometry (step S17).
2種類のソーダライムガラス試料を乳鉢で粉砕し、該試料0.5gをジルコニウムるつぼにはかり取り、セレンをそれぞれ1mgおよび0.1mg添加した。 Two types of soda lime glass samples were ground in a mortar, 0.5 g of the sample was weighed into a zirconium crucible, and 1 mg and 0.1 mg of selenium were added, respectively.
融剤として、過酸化ナトリウムを5g加えてブンゼンバーナーで加熱し融解した。 As a flux, 5 g of sodium peroxide was added and heated with a Bunsen burner to melt.
放冷後、水80mlおよび塩酸50mlの入った樹脂製ビーカー中にジルコニウムるつぼを入れホットプレートで加熱して塩を溶解した。放冷後、ジルコニウムるつぼを取り出し、フッ化水素酸を5ml加えて、加熱溶解した。 After allowing to cool, a zirconium crucible was placed in a resin beaker containing 80 ml of water and 50 ml of hydrochloric acid, and heated with a hot plate to dissolve the salt. After allowing to cool, the zirconium crucible was taken out, 5 ml of hydrofluoric acid was added and dissolved by heating.
放冷後、10g/lテルル溶液(0.4N塩酸性)0.2ml、及び塩化ヒドラジニウム5.0gを加え攪拌した後、ホットプレートで180°Cで2時間加熱した。 After allowing to cool, 0.2 ml of a 10 g / l tellurium solution (0.4N hydrochloric acid) and 5.0 g of hydrazinium chloride were added and stirred, and then heated on a hot plate at 180 ° C. for 2 hours.
放冷後、5種Bのろ紙を用いて試料をろ過し、沈殿を(1十100)塩酸でよく洗浄した後ろ液は廃棄した。受けを50ml石英ビーカーに換え、ろ紙上に熱王水10mlを少量ずつ滴下し、沈殿を溶解した。溶解後、ろ紙を純水でよく洗浄した後、石英ビーカーを湯煎器上で加熱、蒸発乾固させた。 After allowing to cool, the sample was filtered using 5 type B filter paper, and the back solution was thoroughly washed with (10100) hydrochloric acid and discarded. The receiver was changed to a 50 ml quartz beaker, and 10 ml of hot aqua regia was dropped little by little on the filter paper to dissolve the precipitate. After dissolution, the filter paper was thoroughly washed with pure water, and then a quartz beaker was heated on a water bath and evaporated to dryness.
乾固後、硝酸0.2ml及び塩酸0.6mlを加え室温にて塩を溶解した。溶解後、純水を加え10mlに定容し、誘導結合プラズマ発光分光分析法により、セレンを定量した。 After drying, 0.2 ml of nitric acid and 0.6 ml of hydrochloric acid were added to dissolve the salt at room temperature. After dissolution, pure water was added to make a constant volume of 10 ml, and selenium was quantified by inductively coupled plasma emission spectrometry.
測定には196.090nmの波長を使用した。 A wavelength of 196.090 nm was used for the measurement.
ソーダライムガラスにセレンを1mg添加した試料では回収率99%、セレンを0.1mg添加した試料では97%という高い回収が得られ、セレンの揮発および吸着による損失なく定量することができた。 A sample with 1 mg of selenium added to soda lime glass had a recovery rate of 99%, and a sample with 0.1 mg of selenium obtained a high recovery of 97%.
Claims (2)
A glass sample is melted with an alkaline flux using a zirconium crucible, and the resulting melt is dissolved by adding hydrochloric acid and hydrofluoric acid. After standing to cool, a tellurium solution is added to the resulting solution as a coprecipitant. The method of analyzing selenium in glass is characterized by precipitating selenium by adding a reducing agent and heating, further filtering and separating selenium, and then analyzing the obtained separated product by inductively coupled plasma emission spectrometry .
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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WO2007138768A1 (en) * | 2006-05-26 | 2007-12-06 | Nippon Mining & Metals Co., Ltd. | Zirconium crucible for analytical sample melting, method of preparing analytical sample and method of analysis |
JP2009047543A (en) * | 2007-08-20 | 2009-03-05 | Nikko Kinzoku Kk | Zirconium crucible |
CN107643281A (en) * | 2017-09-29 | 2018-01-30 | 通标标准技术服务有限公司 | Industrial silicon dirt content test method |
CN111398399A (en) * | 2020-03-31 | 2020-07-10 | 广西壮族自治区地质矿产测试研究中心 | Method for determining silver by inductively coupled plasma mass spectrometry |
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2003
- 2003-10-07 JP JP2003348067A patent/JP2005114505A/en active Pending
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
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WO2007138768A1 (en) * | 2006-05-26 | 2007-12-06 | Nippon Mining & Metals Co., Ltd. | Zirconium crucible for analytical sample melting, method of preparing analytical sample and method of analysis |
JPWO2007138768A1 (en) * | 2006-05-26 | 2009-10-01 | 日鉱金属株式会社 | Zirconium crucible for melting analysis sample, method for preparing analysis sample and analysis method |
JP2011090010A (en) * | 2006-05-26 | 2011-05-06 | Jx Nippon Mining & Metals Corp | Zirconium crucible for melting analytical sample, method of preparing analytical sample, and method of analysis |
JP4968649B2 (en) * | 2006-05-26 | 2012-07-04 | Jx日鉱日石金属株式会社 | Zirconium crucible for melting analysis sample, method for preparing analysis sample and analysis method |
JP2009047543A (en) * | 2007-08-20 | 2009-03-05 | Nikko Kinzoku Kk | Zirconium crucible |
CN107643281A (en) * | 2017-09-29 | 2018-01-30 | 通标标准技术服务有限公司 | Industrial silicon dirt content test method |
CN111398399A (en) * | 2020-03-31 | 2020-07-10 | 广西壮族自治区地质矿产测试研究中心 | Method for determining silver by inductively coupled plasma mass spectrometry |
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