JPS62238458A - Quantitative analysis of halogen - Google Patents
Quantitative analysis of halogenInfo
- Publication number
- JPS62238458A JPS62238458A JP8194786A JP8194786A JPS62238458A JP S62238458 A JPS62238458 A JP S62238458A JP 8194786 A JP8194786 A JP 8194786A JP 8194786 A JP8194786 A JP 8194786A JP S62238458 A JPS62238458 A JP S62238458A
- Authority
- JP
- Japan
- Prior art keywords
- sulfuric acid
- hydrogen halide
- halogen
- 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.)
- Granted
Links
- 229910052736 halogen Inorganic materials 0.000 title claims abstract description 24
- 150000002367 halogens Chemical class 0.000 title claims abstract description 15
- 238000004445 quantitative analysis Methods 0.000 title description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 54
- 239000012433 hydrogen halide Substances 0.000 claims abstract description 21
- 229910000039 hydrogen halide Inorganic materials 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 14
- 239000007789 gas Substances 0.000 claims abstract description 10
- 239000011261 inert gas Substances 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 5
- 150000002366 halogen compounds Chemical class 0.000 claims abstract description 4
- 239000003792 electrolyte Substances 0.000 claims abstract 4
- -1 halogen ions Chemical class 0.000 claims description 9
- 239000008151 electrolyte solution Substances 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 3
- 238000001461 argentometric titration Methods 0.000 claims 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 abstract description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 4
- 229910001873 dinitrogen Inorganic materials 0.000 abstract description 4
- 239000002904 solvent Substances 0.000 abstract description 3
- 238000004448 titration Methods 0.000 abstract description 3
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 abstract description 2
- 239000001632 sodium acetate Substances 0.000 abstract description 2
- 235000017281 sodium acetate Nutrition 0.000 abstract description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 abstract 1
- 229910052709 silver Inorganic materials 0.000 abstract 1
- 239000004332 silver Substances 0.000 abstract 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 3
- 239000000460 chlorine Substances 0.000 description 3
- 229910052801 chlorine Inorganic materials 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 238000005443 coulometric titration Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- UZFMOKQJFYMBGY-UHFFFAOYSA-N 4-hydroxy-TEMPO Chemical compound CC1(C)CC(O)CC(C)(C)N1[O] UZFMOKQJFYMBGY-UHFFFAOYSA-N 0.000 description 1
- 241000283986 Lepus Species 0.000 description 1
- HYJODZUSLXOFNC-UHFFFAOYSA-N [S].[Cl] Chemical compound [S].[Cl] HYJODZUSLXOFNC-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- ROAYSRAUMPWBQX-UHFFFAOYSA-N ethanol;sulfuric acid Chemical compound CCO.OS(O)(=O)=O ROAYSRAUMPWBQX-UHFFFAOYSA-N 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
- 238000005259 measurement Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 150000002896 organic halogen compounds Chemical class 0.000 description 1
- 150000004968 peroxymonosulfuric acids Chemical class 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
Landscapes
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
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ロゲンの定
量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 quantifying halogen, and more particularly to a method for quantifying halogen.
〈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> Halogen in an organic halogen compound is generally determined by burning a sample to convert the halogen in the sample into hydrogen halide, which is absorbed by an electrolytic solution and subjected to 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って定量することは一般に困難であ
る。まだ、試料を滴定装置に直接入れて滴定することも
、試料によっては困難な場合がある。<Problems to be Solved by the Invention> However, it is generally difficult to quantify halogen ions in inorganic compounds with sufficient accuracy using the above method. However, depending on the sample, it may be difficult to titrate the sample directly into a titration device.
従っ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・
・ロゲンの定量法が望まれている。Therefore, it can be applied to various samples containing halogen ions and halogens that can be hydrolyzed and converted to halogen ions.
・A quantitative method for rogens is desired.
く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堆出すこと、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谷過程を経ること
によジハロゲンを精度よく定量することができる。According to the present invention, a sample containing a halogen compound is supplied to a sulfuric acid bath to generate hydrogen halide, and an inert gas is passed through the bath to generate hydrogen halide. Dihalogen can be quantified with high precision by going through the process of causing hydrogen halide to be entrained in the gas and deposited from the bath, and quantifying the amount of hydrogen halide entrained in the gas.
本発明の詳細な説明するに、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、６θチ以上の濃
度のもの、好ましくは７ｊ’チ以上のに酸を用いる。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、／θ０％髄
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、かつ試料によっては発泡するなど問題か
ある。特に好ましい硫酸浴は、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, first, a sample is supplied into a sulfuric acid bath. The sulfuric acid bath usually uses an acid having a concentration of 6θ or higher, preferably 7j' or higher. If the sulfuric acid concentration in the sulfuric acid bath is low, it is difficult to release hydrogen halide from the sulfuric acid bath quickly. On the other hand, /θ0% marrow acid also has a high viscosity, so it is difficult to release hydrogen halide quickly, and there are problems such as foaming depending on the sample. A particularly preferred sulfuric acid bath is one prepared by dissolving in sulfuric acid an organic solvent that can be uniformly mixed therewith, such as an alcohol or a 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か、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／−につき７〜１０４７分
の流量で！〜／θ分間流通させればより０
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
フィーで定量できる。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鎖部定法によりミ
！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滴定す
る方式（特願昭６６−１６７３ｇ）を採用するのが好ま
しい。As the inert gas to be passed through the sulfuric acid bath, dry nitrogen gas is usually used, or any other gas may be used as long as it does not affect the subsequent quantitative determination of halogen. Inert gas is typically at a flow rate of 7 to 1047 minutes per sulfuric acid bath/-! The hydrogen halide taken out from the sulfuric acid bath along with the inert gas can be quantitatively determined by any known method. For example, it can be absorbed with an absorption liquid and quantified by titration or ion chromatography. Preferably, an inert gas containing hydrogen halide is blown into an electrolytic bath housed in an electrolytic cell of a coulometric titration device to absorb the hydrogen halide into the electrolytic bath, and then the halogen ions in the bath are removed by a chain reaction method. By Mi! Titrate. At this time, if the halogen content of the sample is minute, it is preferable to adopt a method in which halogen ions are accumulated in an electrolytic bath and then titrated (Japanese Patent Application No. 1673/1983).
実施例／
塩素硫黄分析装置ＴＳＸ−／θ（三菱化成工業株式会社
裂品）のクーロメータ部と電解セル及び洗気びん（２よ
ρＸ３００Ｈ）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／、３３９／ｌを含む
♂ｊ％酢酸を用い、洗気びんには容積比で≦二／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: The apparatus shown in the figure was assembled using the coulometer part of a chlorine-sulfur analyzer TSX-/θ (manufactured by Mitsubishi Chemical Industries, Ltd.), an electrolytic cell, and an air washing bottle (2×300H). As the electrolytic solution in the electrolytic cell, ♂j% acetic acid containing 339/l of sodium acetate was used, and in the air washing bottle, a sulfuric acid-ethanol mixture with a volume ratio of ≦2/l was used so that the liquid height was 200 mm. Contained.
窒素ガスをダθ０ゴ／ ｎ１ｉｎで流しなから試料を硫
酸浴に入れた。引続き窒素ガスを約７０分間流したのち
、電解溶中のハロゲンイオンを鎖部定した結果を第１表
に示す。The sample was placed in a sulfuric acid bath while nitrogen gas was flowing at a rate of θ0/n1 in. After continuing to flow nitrogen gas for about 70 minutes, the halogen ions in the electrolytic solution were determined and the results are shown in Table 1.
第１表
実施例コ
実施例／の装置を用い、（ＯＨ３）３ＳｉＣｆ−エタノ
ール溶液（Ａ）、（ＣＨ３０）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っ
た。結果を第２表に示す。Using the apparatus shown in Table 1, Example 1, measurements were carried out using (OH3)3SiCf-ethanol solution (A), (CH30)4Si-ethanol solution (B), and a mixed solution of both as samples. The results are shown in Table 2.
第２表
回収率はＡ、Ｂの測定値の平均値から算出、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／ ００ ｐｐｍの（ＯＨ，）、５ｉＯｊ −！
タノール溶液又はＮａ（Ｊ！−水溶液を７００μ！注入
した以外は実施例／と全く同様にして塩素の定量を行な
った。結果を第３表に示す。The recovery rate in Table 2 is calculated from the average value of the measured values of A and B. Example 3 The sulfuric acid bath in the air washing bottle was changed, and the sample was (OH,) with a chlorine concentration of /00 ppm, 5iOj -!
Chlorine was determined in exactly the same manner as in Example except that 700 μ! of a tanol solution or Na(J!-aqueous solution) was injected. The results are shown in Table 3.
第３表
：［Ｈ，Ｓｏ、と溶媒との容積比
＊２試料中の塩素の回収率
く効 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。Table 3: [Effect on the recovery rate of chlorine in the sample by volume ratio of H, So, and solvent *2] According to the present invention, halogen ions and hydrolyzable halogens in the sample, that is, in the sulfuric acid bath, Halogens that can be converted into halogen ions can be quantified with high accuracy.
図は本発明を実施する装置の７例である、／ 電解セル
２ クーロメーター３ スターラー グ
硫酸浴
！ ガス流量計 ６ ニードル弁
７ 試料導入口
特許出願人 三菱化成工業株式会社
代 理 人 弁理士 長谷用 −
ほか／名The figure shows seven examples of apparatus for carrying out the invention: / electrolytic cell 2 coulometer 3 stirrer
Sulfuric acid bath! Gas flow meter 6 Needle valve 7 Sample inlet Patent applicant Mitsubishi Chemical Industries, Ltd. Agent Patent attorney Hase - Others/names
Claims (4)
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) Supplying a sample containing a halogen compound into a sulfuric acid bath to generate hydrogen halide; passing an inert gas through the bath to entrain the generated hydrogen halide with the gas and removing it from the bath; A method for quantifying halogen that involves the steps of extracting the gas and measuring the amount of hydrogen halide entrained in the gas.
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) The hydrogen halide in the gas is absorbed into the electrolyte by bringing the gas containing hydrogen halide into contact with the electrolyte,
2. The method for quantifying halogen according to claim 1, wherein halogen ions in the electrolytic solution are determined by argentometric titration.
溶媒とから成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 method for quantifying halogen according to claim 1 or 2, wherein the sulfuric acid bath comprises sulfuric acid and an organic solvent that can be uniformly mixed with the sulfuric acid.
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。(4) The method for quantifying halogen according to claim 1 or 2, wherein the sulfuric acid bath is prepared by mixing sulfuric acid with alcohol.
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 true JPS62238458A (en) | 1987-10-19 |
| JPH0715468B2 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) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006177800A (en) * | 2004-12-22 | 2006-07-06 | Tokuyama Corp | Trace chlorine ion concentration analysis method |
| JP2007286032A (en) * | 2006-03-22 | 2007-11-01 | Dia Instr:Kk | Apparatus for analyzing chlorine |
| JP2008082808A (en) * | 2006-09-27 | 2008-04-10 | Dia Instr:Kk | Analyzer |
Citations (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
Patent Citations (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 |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006177800A (en) * | 2004-12-22 | 2006-07-06 | Tokuyama Corp | Trace chlorine ion concentration analysis method |
| JP4617153B2 (en) * | 2004-12-22 | 2011-01-19 | 株式会社トクヤマ | Trace chlorine ion concentration analysis method |
| JP2007286032A (en) * | 2006-03-22 | 2007-11-01 | Dia Instr:Kk | Apparatus for analyzing chlorine |
| JP2008082808A (en) * | 2006-09-27 | 2008-04-10 | Dia Instr:Kk | Analyzer |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0715468B2 (en) | 1995-02-22 |
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