JP3276496B2 - Titration solution and method for producing the same - Google Patents
Titration solution and method for producing the sameInfo
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- JP3276496B2 JP3276496B2 JP34689993A JP34689993A JP3276496B2 JP 3276496 B2 JP3276496 B2 JP 3276496B2 JP 34689993 A JP34689993 A JP 34689993A JP 34689993 A JP34689993 A JP 34689993A JP 3276496 B2 JP3276496 B2 JP 3276496B2
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- mol
- titration
- solution
- solvent
- less
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Description
【０００１】[0001]
【産業上の利用分野】本発明は滴定を行うための標準溶
液およびその溶液を作製する方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a standard solution for performing a titration and a method for preparing the standard solution.
【０００２】[0002]
【従来の技術】滴定用標準溶液としては、溶媒として水
が用いられている。通常の中和滴定するには、水溶液を
用いても問題はほとんどない。2. Description of the Related Art Water is used as a solvent as a standard solution for titration. For ordinary neutralization titration, there is almost no problem even if an aqueous solution is used.
【０００３】しかしながら、近年、高精度、多目的な滴
定法として、電位差滴定法が多く使われるようになって
きている。However, in recent years, potentiometric titration has been increasingly used as a highly accurate and versatile titration method.
【０００４】この電位差滴定法は溶媒中の解離状態の差
を利用し、滴定を行う方法であるが、水溶媒中で解離状
態に差がないような物質を分離することは困難であっ
た。[0004] This potentiometric titration method is a method of performing titration utilizing a difference in dissociation state in a solvent, but it has been difficult to separate substances having no difference in dissociation state in an aqueous solvent.
【０００５】[0005]
【発明が解決しようとする課題】水溶媒中で解離状態に
差がないような物質を再現性良く、高精度に分析するた
めには、鉄と鋼、第７０年、第１１号において高張らに
よって開示されているように、電位差滴定において分析
し難い物資をあらかじめイオン交換膜を用い拡散透析さ
せ、その後、イオン選択電極を用い選択的に目的とする
物質をそれぞれのイオン電極で分析している。In order to analyze a substance having no difference in the dissociation state in a water solvent with high reproducibility and high accuracy, it is necessary to use Takazari et al. In Iron and Steel, 70th and 11th. As disclosed in U.S. Pat. .
【０００６】しかしながら、一度に多くの物質を分析す
るためには、その物質に対して選択性があるイオン電極
が必要となる。However, in order to analyze many substances at one time, an ion electrode having selectivity for the substances is required.
【０００７】また、あらかじめ、そのイオン選択性電極
に妨害を及ぼす物質をイオン交換膜などで除去する必要
がある。[0007] Further, it is necessary to remove in advance a substance that interferes with the ion-selective electrode with an ion-exchange membrane or the like.
【０００８】本発明では前記問題を解消するための滴定
用標準液を提供する。The present invention provides a standard solution for titration to solve the above-mentioned problem.
【０００９】[0009]
【課題を解決するための手段】本発明は、滴定用溶液と
して、溶質が５モル／リットル以上、１４モル／リット
ル以下に溶解している塩基性水溶液を用い、溶媒として
有機溶媒中に０．０５モル／リットル以上、２．００モ
ル／リットル以下となるように溶解させた溶液としたこ
とを特徴とする滴定用溶液である。また、本発明は、滴
定用溶液として、溶質が５モル／リットル以上、１４モ
ル／リットル以下に溶解している塩基性水溶液を、溶媒
として有機溶媒中に０．０５モル／リットル以上、２．
００モル／リットル以下に溶解させ調合することを特徴
とする滴定用溶液の作製方法である。SUMMARY OF THE INVENTION The present invention provides a titration solution and
And the solute is more than 5 mol / l, 14 mol / l
Using a basic aqueous solution dissolved below
More than 0.05 mol / l, 2.00
Liters / liter or less.
This is a titration solution characterized by the following. The present invention also provides a titration solution comprising a basic aqueous solution in which a solute is dissolved in an amount of 5 mol / L or more and 14 mol / L or less in an organic solvent as a solvent in an amount of 0.05 mol / L or more.
This is a method for preparing a titration solution, which is prepared by dissolving the solution at a concentration of not more than 00 mol / liter.
【００１０】[0010]
【作用】以下、本発明の作用を詳細に説明する。The operation of the present invention will be described below in detail.
【００１１】本発明では滴定用標準液として、溶質とし
て塩基を有する物質を溶媒として有機溶媒中に分散させ
ている。In the present invention, as a standard solution for titration, a substance having a base as a solute is dispersed in an organic solvent as a solvent.
【００１２】溶媒として、有機溶媒を用いているところ
が従来の滴定用標準液との大きな違いである。The use of an organic solvent as the solvent is a major difference from the conventional standard solution for titration.
【００１３】溶媒として有機溶媒と規定したのは、メタ
ノール、エタノール、アセトン等の溶媒は水に比べ比誘
電率が低く、化学便覧によると、２５℃においてそれぞ
れ３２．６３、２４．３、２０．７である。水は２５℃
において７８．５である。The solvent is defined as an organic solvent because solvents such as methanol, ethanol, and acetone have a lower dielectric constant than water, and according to Chemical Handbook, 32.63, 24.3, 20. 7 Water is 25 ℃
Is 78.5.
【００１４】このため、同じ酸性物質が溶媒中で解離す
る場合、溶媒の活性度の高い水の方が解離し易いことが
判る。For this reason, when the same acidic substance is dissociated in a solvent, it is understood that water having high activity of the solvent is more easily dissociated.
【００１５】一方、比誘電率の低い溶媒中では解離が起
こり難くなり、水中で解離状態の近接している物質でも
比誘電率の低い溶媒中では分離することが可能となる。
第１表にその一例を示す。On the other hand, dissociation is less likely to occur in a solvent having a low relative dielectric constant, and it is possible to separate even substances that are close to each other in a dissociated state in water in a solvent having a low relative dielectric constant.
Table 1 shows an example.
【００１６】ここで、ｐＫａとは解離定数Ｋａの対数を
とったものであり、ｐＫａと表示する。Here, pKa is the logarithm of the dissociation constant Ka, and is expressed as pKa.
【００１７】弗酸は水溶媒中ではｐＫａが３．２であ
り、酢酸はｐＫａが４．８であり、その差が１．６程度
しか無いが、エタノール溶媒中では弗酸が７．２、酢酸
が１０．２となり、３．０程度にも広がる。Hydrofluoric acid has a pKa of 3.2 in an aqueous solvent, acetic acid has a pKa of 4.8, and the difference is only about 1.6, whereas hydrofluoric acid has a pKa of 7.2 in an ethanol solvent. Acetic acid becomes 10.2 and spreads to about 3.0.
【００１８】このため、従来、水溶媒中では分離するこ
とができなかった物質をこの滴定用標準液を用いること
によって、分離することを可能とした。For this reason, it has become possible to separate substances which could not be separated in a water solvent by using this standard solution for titration.
【００１９】本発明において、溶質として水溶液と規定
したのは有機溶媒中に溶解し難い物質において、滴定用
標準溶液を作製する場合、直接有機溶媒中に溶解させ
ず、水溶液として溶解させた後、有機溶媒中に分散させ
るためである。In the present invention, an aqueous solution is defined as a solute in a substance which is hardly soluble in an organic solvent. When a standard solution for titration is prepared, the substance is not directly dissolved in the organic solvent but is dissolved in an aqueous solution. This is for dispersing in an organic solvent.
【００２０】また、溶質が溶解している水溶液の下限を
５モル／リットルと規定したのは、５モル／リットル以
下になると、その後、有機溶媒中に０．０５モル／リッ
トル以上、２．００モル／リットル以下の濃度に分散さ
せる場合、有機溶媒よりも水溶媒の濃度の影響の方が大
きくなり、正確な分析ができなくなるためである。Further, the lower limit of the aqueous solution in which the solute is dissolved is defined as 5 mol / l. This is because, in the case of dispersing at a concentration of mol / liter or less, the influence of the concentration of the aqueous solvent is larger than that of the organic solvent, and accurate analysis cannot be performed.
【００２１】また、上限として１４モル／リットルを規
定したのは、１４モル／リットル以上になると、溶質の
飽和溶解量に近くなるため、溶解させることが困難にな
り正確な滴定用の標準溶液を調合できなくなるためであ
る。Further, the upper limit of 14 mol / l is defined as that when the concentration is 14 mol / l or more, the amount of the solute becomes close to the saturated dissolution amount, so that it is difficult to dissolve the solute. This is because they cannot be mixed.
【００２２】本発明において、溶質を溶解させた水溶液
を有機溶媒中に分散させた溶液濃度の下限として、０．
０５モル／リットルを規定したのは、０．０５モル／リ
ットル以下になると滴定する場合に滴定用標準溶液が大
量に必要となるため、工業的には不経済であるためであ
る。In the present invention, the lower limit of the concentration of a solution in which an aqueous solution in which a solute is dissolved is dispersed in an organic solvent is 0.1.
The reason why the molar amount is set to 05 mol / l is that when the amount is 0.05 mol / l or less, a large amount of a standard solution for titration is required for titration, which is industrially uneconomical.
【００２３】また、標準溶液濃度のばらつきが大きくな
るためである。また、上限として、２．００モル／リッ
トルを規定したのは、２．００モル／リットル以上にな
ると、滴定標準溶液中の水濃度が高くなるため、水溶媒
中での解離定数に差がない物質の分離が困難になるため
である。Another reason is that the dispersion of the standard solution concentration becomes large. The upper limit of 2.00 mol / l is defined as that when the concentration is 2.00 mol / l or more, the water concentration in the standard solution for titration becomes higher, so that there is no difference in the dissociation constant in the aqueous solvent. This is because it becomes difficult to separate substances.
【００２４】実施例１に弗酸、酢酸、硝酸の混合溶液を
本発明滴定標準溶液にて電位差滴定した例を示す。Example 1 shows an example in which a mixed solution of hydrofluoric acid, acetic acid and nitric acid was subjected to potentiometric titration with the standard solution for titration of the present invention.
【００２５】実施例１に示されているように、本発明の
滴定標準溶液を用いると従来分離できなかった酸成分を
精度良く分析できる。As shown in Example 1, the use of the titration standard solution of the present invention enables accurate analysis of acid components which could not be separated conventionally.
【００２６】[0026]
【実施例】試料溶液として、５０ｗｔ％の弗酸、７０ｗ
ｔ％の硝酸、１００ｗｔ％の酢酸を用いて、実施例１に
示すような比率に調合をした。EXAMPLE As a sample solution, 50 wt% hydrofluoric acid, 70 w
Using t% nitric acid and 100 wt% acetic acid, the ratio was prepared as shown in Example 1.
【００２７】試料溶液を十分に撹拌した後、試料溶液を
５０ｃｃ、マイクロピペットを用いてサンプリングし、
電位差滴定を行った。After sufficiently stirring the sample solution, 50 cc of the sample solution was sampled using a micropipette.
Potentiometric titration was performed.
【００２８】滴定標準溶液は水酸化ナトリウムを水溶媒
に溶解させ、１０モル／リットルとし、この溶液をエタ
ノール溶媒中に分散させ、０．１０モル／リットルのエ
タノール溶媒滴定溶液を調合した。The titration standard solution was prepared by dissolving sodium hydroxide in an aqueous solvent to a concentration of 10 mol / l, dispersing this solution in an ethanol solvent, and preparing a 0.10 mol / l ethanol solvent titration solution.
【００２９】比較のため、従来の方法としては、０．１
モル／リットルの水酸化ナトリウムの水溶液を滴定標準
溶液としたものでも電位差滴定を行った。For comparison, the conventional method is 0.1
Potentiometric titration was also performed using an aqueous solution of sodium hydroxide (mol / liter) as a titration standard solution.
【００３０】従来の方法では、全く分離できない場合や
硝酸のみが設定値と分析値が一致したが、弗酸、酢酸は
分離不可能であった。In the conventional method, the set value and the analysis value of only nitric acid could not be separated or hydrofluoric acid and acetic acid could not be separated.
【００３１】一方、本発明の滴定標準溶液を用いた場合
は硝酸、弗酸、酢酸の分離がなされ、設定値とも良く一
致する。On the other hand, when the titration standard solution of the present invention is used, nitric acid, hydrofluoric acid, and acetic acid are separated, and the values agree well with the set values.
【００３２】[0032]
【表１】 [Table 1]
【００３３】[0033]
【表２】 [Table 2]
【００３４】[0034]
【発明の効果】本発明は従来分析することが困難であっ
た水溶媒中での物質の滴定を、溶媒として有機溶媒を用
いることにより可能とし、精度良く、迅速に、簡便に行
える滴定用標準溶液およびその調合方法を提供するもの
である。The present invention makes it possible to titrate a substance in an aqueous solvent, which has been difficult to analyze conventionally, by using an organic solvent as a solvent. A solution and a method for preparing the solution are provided.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 垂永 伸二 山口県光市大字島田3434番地 ニッテツ 電子株式会社内 (56)参考文献 特開 昭63−65367（ＪＰ，Ａ) (58)調査した分野(Int.Cl.7，ＤＢ名) G01N 27/26 341 G01N 1/00 102 G01N 31/16 ＪＩＣＳＴファイル（ＪＯＩＳ)────────────────────────────────────────────────── ─── Continued on the front page (72) Inventor Shinji Tarunaga 3434 Shimada, Hikari-shi, Yamaguchi Pref. Nittetsu Electronics Co., Ltd. (Int.Cl. 7 , DB name) G01N 27/26 341 G01N 1/00 102 G01N 31/16 JICST file (JOIS)
Claims (2)
トル以上、１４モル／リットル以下に溶解している塩基
性水溶液を用い、溶媒として有機溶媒中に０．０５モル
／リットル以上、２．００モル／リットル以下となるよ
うに溶解させた溶液としたことを特徴とする滴定用溶
液。1. A titration solution comprising:5 mol / L solute
Base dissolved above Torr and below 14 mol / L
Using an aqueous solution, 0.05 mol in an organic solvent as a solvent
/ L or more and 2.00 mol / l or less
SolutionTitration characterized by the followingFor melting
liquid.
トル以上、１４モル／リットル以下に溶解している塩基
性水溶液を、溶媒として有機溶媒中に０．０５モル／リ
ットル以上、２．００モル／リットル以下に溶解させ調
合することを特徴とする滴定用溶液の作製方法。2. A titration solution comprising a basic aqueous solution in which a solute is dissolved in an amount of 5 mol / L or more and 14 mol / L or less is used as a solvent in an organic solvent at a concentration of 0.05 mol / L or more and 2.00 mol / L or less. Dissolve and adjust to less than mol / l
A method for preparing a titration solution, comprising:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP34689993A JP3276496B2 (en) | 1993-12-27 | 1993-12-27 | Titration solution and method for producing the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP34689993A JP3276496B2 (en) | 1993-12-27 | 1993-12-27 | Titration solution and method for producing the same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH07190982A JPH07190982A (en) | 1995-07-28 |
| JP3276496B2 true JP3276496B2 (en) | 2002-04-22 |
Family
ID=18386580
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP34689993A Expired - Fee Related JP3276496B2 (en) | 1993-12-27 | 1993-12-27 | Titration solution and method for producing the same |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3276496B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5636833B2 (en) * | 2010-09-07 | 2014-12-10 | 日本化成株式会社 | Method of analyzing nitric acid in mixed acid solution containing nitric acid |
-
1993
- 1993-12-27 JP JP34689993A patent/JP3276496B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH07190982A (en) | 1995-07-28 |
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