JPS6363966A - Method for measuring concentration of chloride using silver hexacyanoferrate (iii) - Google Patents
Method for measuring concentration of chloride using silver hexacyanoferrate (iii)Info
- Publication number
- JPS6363966A JPS6363966A JP61208613A JP20861386A JPS6363966A JP S6363966 A JPS6363966 A JP S6363966A JP 61208613 A JP61208613 A JP 61208613A JP 20861386 A JP20861386 A JP 20861386A JP S6363966 A JPS6363966 A JP S6363966A
- Authority
- JP
- Japan
- Prior art keywords
- iii
- hexacyanoferrate
- silver
- chloride
- concn
- 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
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 title claims abstract description 23
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 20
- 239000004332 silver Substances 0.000 title claims abstract description 20
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 19
- YAGKRVSRTSUGEY-UHFFFAOYSA-N ferricyanide Chemical compound [Fe+3].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] YAGKRVSRTSUGEY-UHFFFAOYSA-N 0.000 title claims abstract description 16
- 238000000034 method Methods 0.000 title claims description 36
- -1 hexacyanoferrate (III) ion Chemical class 0.000 claims abstract description 8
- 238000006467 substitution reaction Methods 0.000 claims abstract description 5
- 150000002500 ions Chemical class 0.000 claims description 14
- 238000002848 electrochemical method Methods 0.000 claims description 5
- 238000000691 measurement method Methods 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 238000004832 voltammetry Methods 0.000 claims description 2
- 238000005660 chlorination reaction Methods 0.000 claims 1
- 239000000126 substance Substances 0.000 claims 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 abstract description 18
- 239000011780 sodium chloride Substances 0.000 abstract description 9
- 238000004458 analytical method Methods 0.000 abstract description 8
- 238000011088 calibration curve Methods 0.000 abstract description 4
- 239000011521 glass Substances 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 239000011159 matrix material Substances 0.000 abstract description 2
- 239000004568 cement Substances 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- UETZVSHORCDDTH-UHFFFAOYSA-N iron(2+);hexacyanide Chemical compound [Fe+2].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] UETZVSHORCDDTH-UHFFFAOYSA-N 0.000 description 6
- 238000005259 measurement Methods 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 2
- 238000002798 spectrophotometry method Methods 0.000 description 2
- 239000003115 supporting electrolyte Substances 0.000 description 2
- 238000004448 titration Methods 0.000 description 2
- ZFWAHZCOKGWUIT-UHFFFAOYSA-N 1-anilino-3-phenyliminourea Chemical compound C=1C=CC=CC=1N=NC(=O)NNC1=CC=CC=C1 ZFWAHZCOKGWUIT-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000000840 electrochemical analysis Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- GBZANUMDJPCQHY-UHFFFAOYSA-L mercury(ii) thiocyanate Chemical compound [Hg+2].[S-]C#N.[S-]C#N GBZANUMDJPCQHY-UHFFFAOYSA-L 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 235000010344 sodium nitrate Nutrition 0.000 description 1
- 239000004317 sodium nitrate Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
Landscapes
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、環境化学、食品化学、医療化学等の技術分野
において利用される塩化物の濃度測定方法に関するもの
である。DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to a method for measuring chloride concentration used in technical fields such as environmental chemistry, food chemistry, and medical chemistry.
従来の塩化物の濃度の実用的測定法としては、モール法
、ナルハルト法、ファヤンス法等の容量分析法が簡便で
ある為に、多用されている。As a conventional practical method for measuring chloride concentration, volumetric analysis methods such as the Mohr method, Narhardt method, and Fayance method are often used because they are simple.
機器分析法としてはチオシアン酸水銀（ＩＩ）法、ジフ
ェニルカルバゾン法などの吸光光度法が用いられている
。As instrumental analysis methods, spectrophotometric methods such as mercury(II) thiocyanate method and diphenylcarbazone method are used.
電気分析法としてはイオン電極法、電気導電率法、ボー
ラログラフ法などが使用されている。The ion electrode method, electrical conductivity method, boularographic method, etc. are used as the electrical analysis method.
塩化物の濃度測定法に関し、従来用いられている容量法
、吸光光度法等は、試料の調整に習熟した技術を要する
ことから現場における管理分析法としては難点がある。Conventionally used methods for measuring chloride concentration, such as the volumetric method and the spectrophotometric method, are difficult to use as controlled analysis methods in the field because they require experienced techniques for sample preparation.
また、電気分析法としてのイオン電極法、電気導電率法
等による塩化物の濃度測定方法は簡便ではあるが、共存
する他のイオン種の影響を受は易くその選択性および精
度に問題があり、ボーラログラフ法においては水銀を用
いる点等で問題がある。In addition, although chloride concentration measurement methods such as the ion electrode method and the electrical conductivity method as electroanalytical methods are simple, they are easily influenced by other coexisting ionic species and have problems in selectivity and accuracy. However, there are problems with the boularographic method, such as the use of mercury.
ところで、今日において、容量分析法、機器分析法、電
気分析法の長所を組み合わせた測定法はまだ無い。Nowadays, there is still no measurement method that combines the advantages of capacitive analysis, instrumental analysis, and electroanalysis.
本発明は、現場における管理分＋Ｊ′ｒ法として利用で
きる塩化物イオンの選択性に秀れた塩化物の濃度測定方
法の開発を堤案するものである。The present invention proposes the development of a method for measuring chloride concentration with excellent selectivity for chloride ions, which can be used as an on-site control + J'r method.
本発明は、容量分析法、機器分析法、電気分析法の長所
を組み合わせた計測化が可能な塩化物の濃度測定方法を
提供するもので、ヘキサシアノ鉄（ＩＩＩ）酸銀と塩化
物イオンとの置換反応により生成するヘキサシアノ鉄（
ＩＩＩ）酸イオンを測定することを特徴とするものであ
る。The present invention provides a method for measuring the concentration of chloride that combines the advantages of volumetric analysis, instrumental analysis, and electroanalysis. Iron hexacyano produced by substitution reaction (
III) It is characterized by measuring acid ions.
またヘキサシアノ鉄（ＩＩＩ）酸イオンの測定にイオン
Ｔｉ１ｔ極法、ボルタンメトリー法、電気導電率測定法
、ボーラログラフ法などの電気化学的測定法を用いる。Furthermore, electrochemical measurement methods such as the ion Ti1t electrode method, voltammetry method, electrical conductivity measurement method, and boularographic method are used to measure hexacyanoferrate (III) ions.
また固形状のヘキサシアノ鉄（１）酸銀あるいは微粉体
のヘキサシアノ鉄（ＩＩＩ）酸銀あるいはアルミナ、シ
リカ、を紙粉末等の保持材中に保持させたヘキサシアノ
鉄（ＩＩＩ）酸銀を用いる。Further, solid silver hexacyanoferrate (1) or finely powdered silver hexacyanoferrate (III), or silver hexacyanoferrate (III) in which alumina or silica is held in a holding material such as paper powder, is used.
ここで用いるヘキサシアノ鉄（１）酸銀は、塩化物イオ
ンと定量的に置換反応を起こし、安定なヘキサシアノ鉄
（Ｉ［ｌ）酸イオンを遊離する。The silver hexacyanoferrate(1) used here undergoes a quantitative substitution reaction with chloride ions to liberate stable hexacyanoferrate(I[l) ions.
Ａｇａ［Ｆ ｅ（ＣＮ）ｅ】＋ ３０ Ｑ−＝ ３ Ａ
ｇＣＱ↓＋Ｆｅ（ＣＮＮ１３
従って、ヘキサシアノ鉄（ＩＩＩ）酸イオンの濃度を定
量することによって、塩化物イオンの濃度を定量するこ
とが可能となる。Aga[F e(CN)e]+ 30 Q-= 3 A
gCQ↓+Fe(CNN13) Therefore, by quantifying the concentration of hexacyanoferrate (III) ions, it becomes possible to quantify the concentration of chloride ions.
ヘキサシアノ鉄（ＩＩＩ）酸銀は、常温では溶解度は極
めて小さく、塩化物イオンが存在しない場合には、その
溶解度積以上には解離しない。Silver hexacyanoferrate (III) has extremely low solubility at room temperature, and in the absence of chloride ions, does not dissociate beyond its solubility product.
例１ この発明の実施例を図Ｉに示す。 Example 1 An example of the present invention is shown in FIG.
粉末状のヘキサシアノ鉄（ＩＩＩ）酸銀を粉末濾紙（３
００メツシユ）と混合し、内径４ズスのガラス管につめ
、両端に濾紙をつめたキャピラリーを作る。このキャピ
ラリーの一方を０〜１％濃度の塩化ナトリウム溶液に浸
し、他方をハンディポンプにつなぎ塩化ナトリウム溶液
を吸引する。Powdered silver hexacyanoferrate(III) was filtered through powder filter paper (3
00 mesh) and packed into a glass tube with an inner diameter of 4 sq. to make a capillary with filter paper packed at both ends. One end of this capillary is immersed in a 0-1% concentration sodium chloride solution, and the other end is connected to a handy pump to suck out the sodium chloride solution.
ハンディポンプ側に集まった溶液を、公知のポーラグラ
フを用いて、その溶液中のヘキサシアノ鉄（ＩＩＩ）酸
イオンにもとづく電流を測定する。A current based on hexacyanoferrate (III) ions in the solution collected on the hand pump side is measured using a known polar graph.
観測された電流値を塩化ナトリウム溶液の濃度に対して
プロットすると図２の検量線か得られた。ヘキサンアノ
鉄（１）酸イオンにもとづくτｕ流と塩化ナトリウム溶
液の間には直線関係か見られ、この方法によって塩化物
の定量ができることを示している。When the observed current values were plotted against the concentration of the sodium chloride solution, the calibration curve shown in FIG. 2 was obtained. A linear relationship was observed between the τu flow based on the hexaneanoferrate (1) ion and the sodium chloride solution, indicating that chloride can be determined by this method.
例２ 図３のように金属製のカップの底に、ヘキサンア
ノ鉄（［Ｉ）酸銀を濾紙層中に保持させた円形濾紙と、
硝酸ナトリウム等の支持電解質を含有させた円形濾紙を
重ねて置き、その下側に三電極の電流検出のセンサーを
溶液が保持される空間を保って装着させる。電流検出セ
ンサーは、直径１ｍ１１１の金線から成る作用電極に、
ステンレスの対極および電位の安定した参照電極を一体
化したものである。金属カップの内側には０〜１％濃度
の塩化ナトリウムを含むセメントペースト（水セメント
比５５％）を入れ、下側の濾紙層を通過した溶液中のヘ
キサシアノ鉄（ＩＩＩ）酸イオンの濃度を電流検出セン
サーを用いて測定する。電流の測定には、公知のポルタ
ンメトリックアナライザーを用いた。観測された電流と
セメントペースト中の塩化ナトリウムの濃度をプロット
すると図４のような直線関係が得られ、セメントペース
ト中の塩化物の測定に使えることが分かる。Example 2 As shown in Figure 3, a circular filter paper in which silver hexaneanoferrate ([I) acid is held in the filter paper layer is placed at the bottom of a metal cup,
Circular filter papers containing a supporting electrolyte such as sodium nitrate are placed one on top of the other, and a three-electrode current detection sensor is attached to the bottom of the paper, keeping a space in which the solution is retained. The current detection sensor has a working electrode made of gold wire with a diameter of 1 m111,
It integrates a stainless steel counter electrode and a reference electrode with stable potential. A cement paste containing 0-1% sodium chloride (water-cement ratio 55%) is placed inside the metal cup, and the concentration of hexacyanoferrate (III) ions in the solution that has passed through the lower filter paper layer is measured by electric current. Measure using a detection sensor. A known portanmetric analyzer was used to measure the current. When the observed current and the concentration of sodium chloride in cement paste are plotted, a linear relationship as shown in Figure 4 is obtained, indicating that this can be used to measure chloride in cement paste.
本発明は以下の様な効果を有する。 The present invention has the following effects.
１１共存する物のイオン種からの優れた塩化物選択性が
期待できることになる。This means that excellent chloride selectivity can be expected from the ionic species of coexisting compounds.
２、従来の塩化物の電気化学的測定法ではイオン電極性
以外に直接的な測定法が無かったが、本発明によるとボ
ルタンメトリー的な測定法が可能となり、その応用範囲
が飛躍的に増大する３、電気化学的測定方法の簡便さを
もって水溶液の塩化物のポールタンメトリー的な測定が
可能となる。2. Conventional electrochemical measurement methods for chlorides did not have a direct measurement method other than ion polarity, but the present invention enables voltammetric measurement, dramatically expanding its range of applications. 3. The simplicity of the electrochemical measurement method makes it possible to measure chloride in an aqueous solution using pole tammetry.
４、従来のイオン電極法においては、共存する他のイオ
ン種は、イオン雰囲気に影響を与え測定誤差を増大させ
たが、本発明においては、共存イオン種は、イオン強度
の増大をもたらし測定には有利となり従来より秀れた測
定精度を有する。4. In the conventional ion electrode method, coexisting ion species affect the ion atmosphere and increase measurement errors, but in the present invention, coexisting ion species cause an increase in ion intensity and increase measurement errors. is advantageous and has superior measurement accuracy compared to conventional methods.
５、置換反応で生成したヘキサシアノ鉄（ＩＩＩ）酸銀
イオンは安定で限界電流領域が広いことから固体電極を
用いた電気化学的方法により容易に定量分析が可能とな
り、管理分析法として秀れた塩化物の測定方法となる。5. The silver hexacyanoferrate(III) ion produced by the substitution reaction is stable and has a wide limiting current range, so it can be easily quantitatively analyzed by electrochemical methods using solid electrodes, making it an excellent control analysis method. This is a method for measuring chloride.
第１図は本発明の実施例による測定キャピラリーを示す
図であり、１はヘキサシアノ鉄（ＩＩＩ）酸銀を含むマ
トリックス、２は濾紙、３はアスピレータ−・＼の吸引
通路である。
第２図は第１図のキャピラリーを用いて測定した場合の
検量線である。
第３図は本発明の実施例によるセメントペースト中の塩
化物定量のための測容器であり、４はフィルター、５は
ヘキサシアノ鉄（Ｉｆ［）酸銀を保持させたが低層、６
は支持電解質を保持させたが紙層、７はセメントペース
トが入るコンテナー、８は作用電極、９は参照電極、ｌ
Ｏは対極、１１は置換液の流出孔である。
第４図は第３図の測容器を用いて測定した場合の検量線
である。
昭和６１年９月４日
出願人 山 １） 明 文
発明者 山 １） 明 文
［？’Ｊ ａ−Ｃ： ｌ コ ／
％セメントペースト中FIG. 1 is a diagram showing a measurement capillary according to an embodiment of the present invention, in which 1 is a matrix containing silver hexacyanoferrate (III), 2 is a filter paper, and 3 is a suction passage of an aspirator. FIG. 2 is a calibration curve measured using the capillary shown in FIG. 1. FIG. 3 shows a measuring vessel for quantifying chloride in cement paste according to an embodiment of the present invention; 4 is a filter; 5 is a low layer containing silver hexacyanoferrate (If[);
is a paper layer holding a supporting electrolyte, 7 is a container containing cement paste, 8 is a working electrode, 9 is a reference electrode, l
O is a counter electrode, and 11 is an outflow hole for the replacement liquid. FIG. 4 is a calibration curve when measured using the measuring container shown in FIG. 3. September 4, 1986 Applicant: Yama 1) Akira Bun Inventor: Yama 1) Akira Bun [? 'J a-C: l ko /
% in cement paste
Claims (1)
換反応により生成するヘキサシアノ鉄（III）酸イオン
を測定することを特徴とするヘキサシアノ鉄（III）酸
銀を用いる塩化物の濃度測定方法。 ２ ヘキサシアノ鉄（III）酸イオンの測定にイオン電
極法、ボルタンメトリー法、電気導電率測定法、ボーラ
ログラフ法などの電気化学的測定法を用いる特許請求の
範囲第１項記載のヘキサシアノ鉄（III）酸銀を用いる
塩化物の濃度測定方法。 ３ 固形状のヘキサシアノ鉄（III）酸銀あるいは微粉
体のヘキサシアノ鉄（III）酸銀あるいはアルミナ、シ
リカ、ろ紙粉末等の保持材中に保持させたヘキサシアノ
鉄（III）酸銀を用いる特許請求の範囲の第１項記載の
ヘキサシアノ鉄（III）酸銀を用いる塩化物の濃度測定
方法。[Scope of Claims] 1. Chlorination using silver hexacyanoferrate (III), characterized in that hexacyanoferrate (III) ions produced by a substitution reaction between silver hexacyanoferrate (III) and chloride ions are measured. How to measure the concentration of a substance. 2. Hexacyanoferrate (III) acid according to claim 1, which uses an electrochemical measurement method such as an ion electrode method, a voltammetry method, an electrical conductivity measurement method, or a boularographic method to measure hexacyanoferrate (III) acid ions. Method for measuring chloride concentration using silver. 3. Patent claims using solid silver hexacyanoferrate (III), fine powder silver hexacyanoferrate (III), or silver hexacyanoferrate (III) held in a holding material such as alumina, silica, filter paper powder, etc. A method for measuring chloride concentration using silver hexacyanoferrate(III) according to item 1 of the scope.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61208613A JPH0638078B2 (en) | 1986-09-04 | 1986-09-04 | Method for measuring chloride ion concentration using silver hexacyanoferrate (III) |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61208613A JPH0638078B2 (en) | 1986-09-04 | 1986-09-04 | Method for measuring chloride ion concentration using silver hexacyanoferrate (III) |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6363966A true JPS6363966A (en) | 1988-03-22 |
| JPH0638078B2 JPH0638078B2 (en) | 1994-05-18 |
Family
ID=16559117
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61208613A Expired - Lifetime JPH0638078B2 (en) | 1986-09-04 | 1986-09-04 | Method for measuring chloride ion concentration using silver hexacyanoferrate (III) |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0638078B2 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02249376A (en) * | 1989-03-22 | 1990-10-05 | Sharp Corp | Video tape recorder |
| WO2009001602A1 (en) * | 2007-06-25 | 2008-12-31 | Sai Corporation | Gas-filled capillary and sample placement method |
| RU2707580C1 (en) * | 2018-08-10 | 2019-11-28 | Российская Федерация, От Имени Которой Выступает Министерство Промышленности И Торговли Российской Федерации | Method for quantitative determination of chlorides in concentrate of tetramethylammonium hydroxide |
-
1986
- 1986-09-04 JP JP61208613A patent/JPH0638078B2/en not_active Expired - Lifetime
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02249376A (en) * | 1989-03-22 | 1990-10-05 | Sharp Corp | Video tape recorder |
| WO2009001602A1 (en) * | 2007-06-25 | 2008-12-31 | Sai Corporation | Gas-filled capillary and sample placement method |
| JP4521788B2 (en) * | 2007-06-25 | 2010-08-11 | Ｓａｉ株式会社 | Gas-filled capillary and sample filling method |
| JPWO2009001602A1 (en) * | 2007-06-25 | 2010-08-26 | Ｓａｉ株式会社 | Gas-filled capillary and sample filling method |
| RU2707580C1 (en) * | 2018-08-10 | 2019-11-28 | Российская Федерация, От Имени Которой Выступает Министерство Промышленности И Торговли Российской Федерации | Method for quantitative determination of chlorides in concentrate of tetramethylammonium hydroxide |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0638078B2 (en) | 1994-05-18 |
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