JP2808982B2 - Method for analyzing impurities in sample liquid - Google Patents
Method for analyzing impurities in sample liquidInfo
- Publication number
- JP2808982B2 JP2808982B2 JP15000692A JP15000692A JP2808982B2 JP 2808982 B2 JP2808982 B2 JP 2808982B2 JP 15000692 A JP15000692 A JP 15000692A JP 15000692 A JP15000692 A JP 15000692A JP 2808982 B2 JP2808982 B2 JP 2808982B2
- Authority
- JP
- Japan
- Prior art keywords
- sample solution
- sample
- impurities
- reagent
- analyzing
- 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 - Lifetime
Links
Landscapes
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Description
【０００１】[0001]
【産業上の利用分野】本発明は、不揮発性の酸またはア
ルカリ試料液中の不純物金属成分の分析方法に関するも
のである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for analyzing an impurity metal component in a nonvolatile acid or alkali sample solution.
【０００２】[0002]
【従来の技術】従来、試料液中の不純物成分を分析する
際には、希釈後、分析機器で直接分析する方法と、何ら
かの前処理を行い主成分を除去した後、分析機器で分析
する方法が用いられている。前処理としては、加熱蒸
発、イオン交換樹脂などの固相への吸着、沈殿生成、共
沈などが主に用いられている。2. Description of the Related Art Conventionally, when analyzing an impurity component in a sample liquid, a method of directly analyzing with an analytical instrument after dilution, and a method of analyzing with an analytical instrument after removing a main component by performing some pretreatment. Is used. As the pretreatment, heat evaporation, adsorption to a solid phase such as an ion exchange resin, precipitation, coprecipitation, and the like are mainly used.
【０００３】[0003]
【発明が解決しようとする課題】しかしながら、試料液
が高濃度の不揮発性の酸やアルカリの場合、加熱気化に
よる主成分の除去は困難である。高濃度の酸やアルカリ
溶液からの固相への吸着は特定成分に対して起きても、
種々の成分を同時に濃縮することは困難である。沈殿生
成や共沈には多量の薬品添加が必要であり、添加薬品中
の不純物のため空試験値が高くなり、試料液中の微量成
分を分析する際には再現性が悪くなる。また、試料液
に、酸またはアルカリ試薬を加えて中和した後、種々の
高感度な分析に供する方法もあるが、酸またはアルカリ
試薬中の不純物が混入したり、あるいは中和操作の工程
で汚染される恐れがあった。However, when the sample solution is a high-concentration nonvolatile acid or alkali, it is difficult to remove the main component by heating and vaporizing. Even if adsorption to a solid phase from a highly concentrated acid or alkali solution occurs for a specific component,
It is difficult to simultaneously concentrate various components. Precipitation and coprecipitation require a large amount of chemicals to be added, and the blank value increases due to impurities in the added chemicals, and reproducibility deteriorates when analyzing trace components in the sample solution. There is also a method of subjecting a sample solution to neutralization by adding an acid or alkali reagent, and then subjecting the sample solution to various high-sensitivity analyses. There was a risk of contamination.
【０００４】本発明はこのような従来法の問題に対処す
るためになされたもので、不揮発性の高濃度の酸やアル
カリ溶液などの試料液中の種々の金属不純物を同時に濃
縮し、濃縮液を誘導結合プラズマ質量分析法や誘導結合
プラズマ発光分光分析法等の分析機器で当該試料液中の
微量金属不純物を汚染の心配なく、かつ高感度に定量す
る方法を提供することを目的とする。The present invention has been made to address such problems of the conventional method, and simultaneously concentrates various metal impurities in a sample solution such as a non-volatile high-concentration acid or alkali solution to form a concentrated solution. It is an object of the present invention to provide a method for quantifying trace metal impurities in a sample solution with high sensitivity without concern for contamination by an analytical instrument such as inductively coupled plasma mass spectrometry or inductively coupled plasma emission spectroscopy.
【０００５】[0005]
【課題を解決するための手段】本発明は、酸またはアル
カリ試料液中の金属不純物を定量することよりなる試料
液中の不純物分析方法において、試料液と該試料液を中
和する揮発性の試薬をそれぞれ別の広口の開口部を備え
た容器に入れ、該二種の容器を前記試薬に対して耐性の
ある密閉性の容器内に放置し、気相を介して中和試薬成
分を試料液に吸収させ試料液を中和させた後、該試料液
をキレート樹脂カラムに通し試料液中の金属不純物をカ
ラムに濃縮し、濃縮回収液中の金属不純物を定量するこ
とを特徴とする試料液中の不純物分析方法である。SUMMARY OF THE INVENTION The present invention relates to a method for analyzing impurities in a sample solution, which comprises quantifying metal impurities in an acid or alkali sample solution. The reagents are placed in separate containers each having a wide opening, and the two types of containers are left in a hermetically sealed container resistant to the reagents. The sample is characterized by being absorbed in a liquid and neutralizing the sample liquid, passing the sample liquid through a chelating resin column, concentrating the metal impurities in the sample liquid into the column, and quantifying the metal impurities in the concentrated and recovered liquid. This is a method for analyzing impurities in a liquid.
【０００６】[0006]
【作用】予め十分に洗浄した清浄な密閉容器内に試料液
と当該試料液を中和する揮発性の試薬を配置し、当該試
薬中の揮発性の試薬成分を容器の気相を介して当該試料
に吸収させ中和させることにより、当該試薬中の不純物
と中和操作による汚染の影響なく当該試料を中和でき
る。中和後の試料液をキレート樹脂カラムに通すことで
試料液中の金属不純物をカラムに濃縮し、濃縮後少量の
酸等の回収液で溶離し、回収液中の金属不純物を誘導結
合プラズマ質量分析法や誘導結合プラズマ発光分析法で
分析することにより、試料液中の金属不純物を同時に高
感度に定量できる。A sample solution and a volatile reagent for neutralizing the sample solution are arranged in a clean and sealed container which has been sufficiently washed beforehand, and the volatile reagent component in the reagent is passed through the gas phase of the container. By absorbing and neutralizing the sample, the sample can be neutralized without being affected by impurities in the reagent and contamination due to the neutralization operation. By passing the neutralized sample solution through a chelating resin column, metal impurities in the sample solution are concentrated on the column, and after concentration, eluted with a small amount of a recovery solution such as an acid. By analyzing by an analysis method or an inductively coupled plasma emission analysis method, metal impurities in a sample solution can be simultaneously quantified with high sensitivity.
【０００７】[0007]
【実施例】次に、本発明の実施例について説明する。図
１は、本発明の一実施例の概略構成図である。図１にお
いて、試料容器１には不純物含有のリン酸を、試薬容器
２にはアンモニア水を入れ、これら各容器をリン酸およ
びアンモニアに対して耐性のある材質からなる、予め内
部を十分洗浄し金属成分に関して清浄な密閉容器本体５
内に入れ、密閉容器蓋６をかぶせ一昼夜放置する。試薬
容器２内のアンモニアは気化し、気化したアンモニアは
試料容器１内のリン酸に吸収され、リン酸の中和反応が
起こる。中和後のリン酸に超純水を添加し塩を溶解し、
この溶液をキレート樹脂を充填したカラムに通して金属
成分を濃縮する。濃縮後、非沸騰蒸留により精製した硝
酸を用いて調製した２ｍｏｌ／ｄｍ3硝酸を当該キレー
トカラムに流す。カラムからの溶出液を捕集する。捕集
液を加熱濃縮した後、定容にし、誘導結合プラズマ質量
分析法や誘導結合プラズマ発光分光法により定量する。Next, an embodiment of the present invention will be described. FIG. 1 is a schematic configuration diagram of one embodiment of the present invention. In FIG. 1, phosphoric acid containing impurities is put in a sample container 1 and ammonia water is put in a reagent container 2, and the inside of each container is sufficiently washed beforehand with a material which is resistant to phosphoric acid and ammonia. Closed container body 5 clean with respect to metal components
And cover it with a closed container lid 6 and leave it overnight. The ammonia in the reagent container 2 is vaporized, and the vaporized ammonia is absorbed by the phosphoric acid in the sample container 1 and a neutralization reaction of the phosphoric acid occurs. Ultrapure water is added to the neutralized phosphoric acid to dissolve the salt,
The solution is passed through a column filled with a chelating resin to concentrate the metal components. After concentration, 2 mol / dm 3 nitric acid prepared using nitric acid purified by non-boiling distillation is passed through the chelate column. Collect the eluate from the column. After the collected solution is concentrated by heating, the volume is made constant and quantified by inductively coupled plasma mass spectrometry or inductively coupled plasma emission spectroscopy.
【０００８】[0008]
【発明の効果】以上説明したように、本発明の不純物分
析方法を用いれば、高濃度の不揮発性酸やアルカリ中の
金属不純物の分析において、主成分を汚染の危険なく除
去し、低マトリックスの溶液にすることで、種々の高感
度な分析法の適用が可能になり、試料液中の金属不純物
を高感度に定量できる。As described above, according to the impurity analysis method of the present invention, the main component is removed without risk of contamination in the analysis of high-concentration non-volatile acids and metal impurities in alkalis. By using a solution, various highly sensitive analytical methods can be applied, and metal impurities in a sample solution can be quantified with high sensitivity.
【図１】本発明による不純物分析方法の説明図である。FIG. 1 is an explanatory diagram of an impurity analysis method according to the present invention.
１ 試料容器 ２ 試薬容器 ５ 密閉容器本体 ６ 密閉容器蓋 Reference Signs List 1 sample container 2 reagent container 5 closed container body 6 closed container lid
Claims (1)
を定量することよりなる試料液中の不純物分析方法にお
いて、試料液と該試料液を中和する揮発性の試薬をそれ
ぞれ別の広口の開口部を備えた容器に入れ、該二種の容
器を前記試薬に対して耐性のある密閉性の容器内に放置
し、気相を介して中和試薬成分を試料液に吸収させ試料
液を中和させた後、該試料液をキレート樹脂カラムに通
し試料液中の金属不純物をカラムに濃縮し、濃縮回収液
中の金属不純物を定量することを特徴とする試料液中の
不純物分析方法。In a method for analyzing impurities in a sample solution, which comprises quantifying metal impurities in an acid or alkali sample solution, a sample solution and a volatile reagent for neutralizing the sample solution are separately opened at different wide openings. The two types of containers are left in a hermetically sealed container that is resistant to the reagent, and the neutralizing reagent component is absorbed into the sample solution via the gas phase, and the sample solution is placed in the container. A method for analyzing impurities in a sample liquid, comprising passing the sample liquid through a chelate resin column, concentrating the metal impurities in the sample liquid into the column, and quantifying the metal impurities in the concentrated and recovered liquid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP15000692A JP2808982B2 (en) | 1992-05-19 | 1992-05-19 | Method for analyzing impurities in sample liquid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP15000692A JP2808982B2 (en) | 1992-05-19 | 1992-05-19 | Method for analyzing impurities in sample liquid |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH05322875A JPH05322875A (en) | 1993-12-07 |
| JP2808982B2 true JP2808982B2 (en) | 1998-10-08 |
Family
ID=15487415
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP15000692A Expired - Lifetime JP2808982B2 (en) | 1992-05-19 | 1992-05-19 | Method for analyzing impurities in sample liquid |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2808982B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10309937B2 (en) | 2016-02-03 | 2019-06-04 | Samsung Electronics Co., Ltd. | Method for detecting impurities in ammonium hydroxide |
-
1992
- 1992-05-19 JP JP15000692A patent/JP2808982B2/en not_active Expired - Lifetime
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10309937B2 (en) | 2016-02-03 | 2019-06-04 | Samsung Electronics Co., Ltd. | Method for detecting impurities in ammonium hydroxide |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH05322875A (en) | 1993-12-07 |
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