JPH0715468B2 - Halogen determination method - Google Patents
Halogen determination methodInfo
- Publication number
- JPH0715468B2 JPH0715468B2 JP61081947A JP8194786A JPH0715468B2 JP H0715468 B2 JPH0715468 B2 JP H0715468B2 JP 61081947 A JP61081947 A JP 61081947A JP 8194786 A JP8194786 A JP 8194786A JP H0715468 B2 JPH0715468 B2 JP H0715468B2
- Authority
- JP
- Japan
- Prior art keywords
- sulfuric acid
- halogen
- hydrogen halide
- bath
- gas
- 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
- 229910052736 halogen Inorganic materials 0.000 title claims description 26
- 150000002367 halogens Chemical class 0.000 title claims description 15
- 238000000034 method Methods 0.000 title claims description 11
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 48
- 239000012433 hydrogen halide Substances 0.000 claims description 15
- 229910000039 hydrogen halide Inorganic materials 0.000 claims description 15
- 239000007789 gas Substances 0.000 claims description 8
- 239000011261 inert gas Substances 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000008151 electrolyte solution Substances 0.000 claims description 5
- 238000004448 titration Methods 0.000 claims description 5
- 239000003960 organic solvent Substances 0.000 claims description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 3
- 229910052709 silver Inorganic materials 0.000 claims description 3
- 239000004332 silver Substances 0.000 claims description 3
- 150000002366 halogen compounds Chemical class 0.000 claims description 2
- -1 halogen ions Chemical class 0.000 description 10
- 239000000243 solution Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 3
- 229910001873 dinitrogen Inorganic materials 0.000 description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 238000005443 coulometric titration Methods 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 1
- HYJODZUSLXOFNC-UHFFFAOYSA-N [S].[Cl] Chemical compound [S].[Cl] HYJODZUSLXOFNC-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 238000003869 coulometry Methods 0.000 description 1
- ROAYSRAUMPWBQX-UHFFFAOYSA-N ethanol;sulfuric acid Chemical compound CCO.OS(O)(=O)=O ROAYSRAUMPWBQX-UHFFFAOYSA-N 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 238000004255 ion exchange chromatography Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 150000002896 organic halogen compounds Chemical class 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000001632 sodium acetate Substances 0.000 description 1
- 235000017281 sodium acetate Nutrition 0.000 description 1
Landscapes
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Description
【発明の詳細な説明】 ＜産業上の利用分野＞ 本発明はハロゲンの定量法に関するものである。詳しく
は本発明は試料中のハロゲンイオン及び加水分解してハ
ロゲンイオンに転換し得るハロゲンの定量法に関するも
のである。DETAILED DESCRIPTION OF THE INVENTION <Field of Industrial Application> The present invention relates to a method for quantifying halogen. More specifically, the present invention relates to a method for quantifying halogen ions in a sample and halogen that can be hydrolyzed and converted into halogen ions.
＜従来技術＞ 有機ハロゲン化合物中のハロゲンの定量は、試料を燃焼
させて試料中のハロゲンをハロゲン化水素に転換し、こ
れを電解液で吸収して電量滴定する方法が一般に行なわ
れている。<Prior Art> The quantitative determination of halogen in an organic halogen compound is generally performed by burning a sample, converting the halogen in the sample into hydrogen halide, and absorbing this with an electrolytic solution to perform coulometric titration.
＜発明が解決しようとする問題点＞ しかし、上記の方法により無機化合物中のハロゲンイオ
ンを十分な精度をもつて定量することは一般に困難であ
る。また、試料を滴定装置に直接入れて滴定すること
も、試料によつては困難な場合がある。<Problems to be Solved by the Invention> However, it is generally difficult to quantify the halogen ion in the inorganic compound with sufficient accuracy by the above method. In addition, it may be difficult for some samples to put the sample directly into the titration device for titration.
従つてハロゲンイオン及び加水分解してハロゲンイオン
に転換し得るハロゲンを含む各種の試料に適用し得るハ
ロゲンの定量法が望まれている。Therefore, a halogen determination method applicable to various samples containing halogen ions and halogens that can be hydrolyzed and converted into halogen ions is desired.
＜問題点を解決するための手段＞ 本発明によれば、ハロゲン化合物を含む試料を硫酸及び
これと均一に混合し得る有機溶媒とから成る硫酸浴中に
供給してハロゲン化水素を生成させること、該浴中に不
活性ガスを流通させて生成したハロゲン化水素を該ガス
に同伴させて該浴から取出すこと、該ガスに同伴された
ハロゲン化水素量を定量することの各過程を経ることに
よりハロゲンを精度よく定量することができる。<Means for Solving Problems> According to the present invention, a sample containing a halogen compound is supplied to a sulfuric acid bath containing sulfuric acid and an organic solvent capable of being uniformly mixed with the sample to generate hydrogen halide. , Passing through an inert gas in the bath, taking out hydrogen halide produced by entraining the gas in the bath, and quantifying the amount of hydrogen halide entrained in the gas The halogen can be quantified with high accuracy.
本発明を詳細に説明するに、本発明では先ず試料を硫酸
浴中に供給する。硫酸浴としては通常、60％以上の濃度
のもの、好ましくは75％以上の硫酸を用いる。硫酸浴中
の硫酸濃度が低いと、硫酸浴からのハロゲン化水素の放
出がすみやかに行なわれ難い。一方、100％硫酸も粘度
が高いのでハロゲン化水素の放出がすみやかに行なわれ
難く、かつ試料によつては発泡するなど問題がある。本
発明の硫酸浴は、硫酸にこれと均一に混合し得る有機溶
媒、例えばアルコールやカルボン酸を溶解して調製した
ものである。これらの有機溶媒は硫酸浴の粘度を低下さ
せてハロゲン化水素の放出を容易とする。To explain the present invention in detail, in the present invention, a sample is first fed into a sulfuric acid bath. As the sulfuric acid bath, one having a concentration of 60% or more, preferably 75% or more is used. When the sulfuric acid concentration in the sulfuric acid bath is low, it is difficult to release hydrogen halide from the sulfuric acid bath promptly. On the other hand, since 100% sulfuric acid also has a high viscosity, it is difficult to release hydrogen halide quickly, and there are problems such as foaming depending on the sample. The sulfuric acid bath of the present invention is prepared by dissolving in sulfuric acid an organic solvent capable of being mixed uniformly with sulfuric acid, such as alcohol or carboxylic acid. These organic solvents reduce the viscosity of the sulfuric acid bath and facilitate the release of hydrogen halide.
硫酸浴中に流通させる不活性ガスとしては、通常は乾燥
した窒素ガスが用いられるが、後続するハロゲンの定量
に影響を与えないものであれば他のガスでも差支えな
い。不活性ガスは通常、硫酸浴1mlにつき１〜10ml/分の
流量で５〜10分間流通させればよい。As the inert gas passed through the sulfuric acid bath, dry nitrogen gas is usually used, but any other gas may be used as long as it does not affect the subsequent quantitative determination of halogen. The inert gas may be passed through the sulfuric acid bath at a flow rate of 1 to 10 ml / min for 5 to 10 minutes.
不活性ガスに同伴されて硫酸浴から取出されたハロゲン
化水素の定量は、公知の任意の方法で行なうことができ
る。例えば吸収液で吸収して滴定やイオンクロマトグラ
フイーで定量できる。好ましくは、電量滴定装置の電解
セルに収容した電解浴中にハロゲン化水素を同伴した不
活性ガスを吹込んで、電解浴中にハロゲン化水素を吸収
させ、次いで浴中のハロゲンイオンを銀滴定法により電
量滴定する。この際、試料のハロゲン含有量が微量なら
ば、電解浴中にハロゲンイオンを蓄積させてから適定す
る方式（特願昭55−15736）を採用するのが好ましい。The quantification of the hydrogen halide taken out from the sulfuric acid bath while being entrained by the inert gas can be carried out by any known method. For example, it can be quantified by titration or ion chromatography after absorbing with an absorbing solution. Preferably, an inert gas accompanied by hydrogen halide is blown into the electrolytic bath contained in the electrolysis cell of the coulometric titrator to absorb the hydrogen halide in the electrolytic bath, and then the halogen ion in the bath is subjected to the silver titration method. Coulometric titration with. At this time, if the halogen content of the sample is very small, it is preferable to adopt a method (Japanese Patent Application No. 55-15736) in which halogen ions are accumulated in the electrolytic bath and then determined appropriately.
実施例１ 塩素硫黄分析装置TSX−10（三菱化成工業株式会社製
品）のクーロメータ部と電解セル及び洗気びん（25φ×
300H）を用いて図の如き装置を組立てた。電解セルの電
解液としては酢酸ソーダ1.35g/lを含む85％酢酸を用
い、洗気びんには容積比で6:1の硫酸−エタノール混合
液を液高が200mmとなるように収容した。Example 1 Coulometer part of chlorine-sulfur analyzer TSX-10 (product of Mitsubishi Kasei Kogyo Co., Ltd.), electrolytic cell, and air bottle (25φ ×)
300H) was used to assemble a device as shown. As the electrolytic solution of the electrolytic cell, 85% acetic acid containing 1.35 g / l of sodium acetate was used, and a sulfuric acid-ethanol mixed solution having a volume ratio of 6: 1 was housed in the flushing bottle so that the liquid height was 200 mm.
窒素ガスを400ml/minで流しながら試料を硫酸浴に入れ
た。引続き窒素ガスを約10分間流したのち、電解浴中の
ハロゲンイオンを銀適定した結果を第１表に示す。The sample was placed in a sulfuric acid bath while flowing nitrogen gas at 400 ml / min. After continuously flowing nitrogen gas for about 10 minutes, the halogen ions in the electrolytic bath were titrated to silver, and the results are shown in Table 1.
実施例２ 実施例１の装置を用い、（CH3）3SiCl−エタノール溶液
（Ａ）、（CH3O）4Si−エタノール溶液（Ｂ）および両
者の混合溶液を試料として測定を行なつた。結果を第２
表に示す。 Example 2 Using the apparatus of Example 1, measurement was performed using (CH 3 ) 3 SiCl-ethanol solution (A), (CH 3 O) 4 Si-ethanol solution (B) and a mixed solution of both as samples. . Second result
Shown in the table.
回収率はＡ、Ｂの測定値の平均値から算出。 The recovery rate was calculated from the average value of the measured values of A and B.
実施例３ 洗気びんに入れる硫酸浴を変え、かつ試料として塩素濃
度が100ppmの（CH3）3SiCl−エタノール溶液又はNaCl−
水溶液を100μｌ注入した以外は実施例１と全く同様に
して塩素の定量を行なつた。結果を第３表に示す。Example 3 A sulfuric acid bath put in an air purifying bottle was changed, and (CH 3 ) 3 SiCl-ethanol solution or NaCl-having a chlorine concentration of 100 ppm as a sample was used.
Chlorine was quantified in the same manner as in Example 1 except that 100 μl of the aqueous solution was injected. The results are shown in Table 3.
＜効 果＞ 本発明によれば、試料中のハロゲンイオン及び加水分解
性のハロゲン、すなわち硫酸浴中でハロゲンイオンに転
換しうるハロゲンを精度よく定量することができる。 <Effect> According to the present invention, the halogen ion in the sample and the hydrolyzable halogen, that is, the halogen that can be converted into the halogen ion in the sulfuric acid bath, can be accurately quantified.
図は本発明を実施する装置の１例である。 １……電解セル、２……クーロメーター ３……スターラー、４……硫酸浴 ５……ガス流量計、６……ニードル弁 ７……試料導入口 The figure is an example of an apparatus for carrying out the present invention. 1 ... Electrolysis cell, 2 ... Coulometer, 3 ... Stirrer, 4 ... Sulfuric acid bath, 5 ... Gas flow meter, 6 ... Needle valve, 7 ... Sample inlet
Claims (3)
と均一に混合し得る有機溶媒とから成る硫酸浴中に供給
してハロゲン化水素を生成させること、該浴中に不活性
ガスを流通させて生成したハロゲン化水素を該ガスに同
伴させて該浴から取出すこと、該ガスに同伴されたハロ
ゲン化水素量を測定することの各過程を経るハロゲンの
定量法。1. A sample containing a halogen compound is fed into a sulfuric acid bath consisting of sulfuric acid and an organic solvent capable of being uniformly mixed therewith to produce hydrogen halide, and an inert gas is passed through the bath. A method for quantifying halogen, which comprises the steps of: taking out the hydrogen halide produced by the gas and taking it out from the bath; and measuring the amount of the hydrogen halide carried by the gas.
液と接触させてガス中のハロゲン化水素を電解液中に吸
収し、電解液中のハロゲンイオンを銀滴定により定量す
ることを特徴とする特許請求の範囲第１項記載のハロゲ
ンの定量法。2. A method in which a gas containing hydrogen halide is brought into contact with an electrolytic solution to absorb the hydrogen halide in the gas into the electrolytic solution, and the halogen ion in the electrolytic solution is quantified by silver titration. The method for quantifying halogen according to claim 1.
整したものであることを特徴とする特許請求の範囲第１
項又は第２項記載のハロゲンの定量法。3. The sulfuric acid bath is prepared by mixing sulfuric acid with alcohol to prepare a sulfuric acid bath.
Item 2. A method for quantifying halogen according to Item 2 or Item 2.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61081947A JPH0715468B2 (en) | 1986-04-09 | 1986-04-09 | Halogen determination method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61081947A JPH0715468B2 (en) | 1986-04-09 | 1986-04-09 | Halogen determination method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS62238458A JPS62238458A (en) | 1987-10-19 |
| JPH0715468B2 true JPH0715468B2 (en) | 1995-02-22 |
Family
ID=13760695
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61081947A Expired - Lifetime JPH0715468B2 (en) | 1986-04-09 | 1986-04-09 | Halogen determination method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0715468B2 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4617153B2 (en) * | 2004-12-22 | 2011-01-19 | 株式会社トクヤマ | Trace chlorine ion concentration analysis method |
| JP4816420B2 (en) * | 2006-03-22 | 2011-11-16 | 株式会社三菱化学アナリテック | Chlorine analyzer |
| JP4811221B2 (en) * | 2006-09-27 | 2011-11-09 | 株式会社三菱化学アナリテック | Analysis equipment |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5596453A (en) * | 1979-01-18 | 1980-07-22 | Mitsubishi Chem Ind Ltd | Method and device for measuring quantity of chlorine in aqueous solution |
| JPS58153163A (en) * | 1982-03-09 | 1983-09-12 | Mitsubishi Chem Ind Ltd | Determining method for total organic halogenated matter in liquid |
-
1986
- 1986-04-09 JP JP61081947A patent/JPH0715468B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPS62238458A (en) | 1987-10-19 |
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