JPH0718802B2 - End point detector for phase separation titration - Google Patents
End point detector for phase separation titrationInfo
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- JPH0718802B2 JPH0718802B2 JP61209338A JP20933886A JPH0718802B2 JP H0718802 B2 JPH0718802 B2 JP H0718802B2 JP 61209338 A JP61209338 A JP 61209338A JP 20933886 A JP20933886 A JP 20933886A JP H0718802 B2 JPH0718802 B2 JP H0718802B2
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- Prior art keywords
- titration
- phase
- organic solvent
- end point
- phase separation
- Prior art date
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Description
【発明の詳細な説明】 〔産業上の利用分野〕 本発明はイオン性界面活性剤の分相滴定用終点検出装置
に関する。TECHNICAL FIELD The present invention relates to an end point detection device for phase separation titration of ionic surfactants.
分相滴定は水及び水不溶性有機溶媒とからなる不均一系
を被滴定液とし、これを水溶液で滴定する方法である。
滴定終点は、滴定に関与する化合物（分相指示薬）が有
機相に抽出されて着色或いは変色するが、逆に水相に転
溶して脱色する過程を観察して求めるが、通常、水相と
有機相で分相指示薬はその色調を異にするため終点の判
定には熟練を要する。また分相滴定法は、滴定液を滴下
する毎に、共栓付滴定用シリンダーの激しい振とうを必
要とし、更に特に界面活性剤を含む系では乳化のために
二相が分離するまでに時間がかかること等から、他の滴
定法に比べて測定に時間と労力が要求されている。The phase separation titration is a method in which a heterogeneous system consisting of water and a water-insoluble organic solvent is used as a liquid to be titrated, and this is titrated with an aqueous solution.
The titration end point is obtained by observing the process in which the compound involved in the titration (phase separation indicator) is extracted into the organic phase and is colored or discolored. Since the phase-separation indicator has different color tones in the organic phase, skill is required to determine the end point. In addition, the phase separation titration method requires vigorous shaking of the titration cylinder with a stopper each time the titrant is dropped, and especially in a system containing a surfactant, it takes time until the two phases are separated due to emulsification. Therefore, it takes more time and labor for measurement than other titration methods.
そこで、被検イオン性界面活性剤及び該界面活性剤と錯
体を形成する分相滴定指示薬を含み、水及び水不溶性有
機溶媒からなる不均一系を被滴定液とする滴定系から、
有機溶媒相のみを抽出することのできる多孔性薄膜を通
して有機溶媒相のみを連続的に抜出し、その光吸収を測
定し、滴定系に循環させながら、被検イオン性界面活性
剤と逆の電荷を有する界面活性剤を滴定液として分相滴
定を行う際に、多孔性薄膜を該多孔性薄膜の外面におけ
る垂線が略水平になるように配した有機溶媒抽出部を通
して有機溶媒相を抜き出すことを特徴とするイオン性界
面活性剤の測定方法が先に開発され、報告されている
（特開昭57−106860号）。Therefore, from a titration system that contains a test ionic surfactant and a phase-separation titration indicator that forms a complex with the surfactant, and a heterogeneous system consisting of water and a water-insoluble organic solvent as a liquid to be titrated,
Only the organic solvent phase is continuously extracted through a porous thin film that can extract only the organic solvent phase, the light absorption is measured, and the charge opposite to that of the ionic surfactant to be detected is circulated in the titration system. When phase separation titration is carried out using a surfactant having a titration liquid, the organic solvent phase is extracted through an organic solvent extraction section in which the porous thin film is arranged such that the perpendicular line on the outer surface is substantially horizontal. The method for measuring ionic surfactants has been previously developed and reported (JP-A-57-106860).
しかしながら、上記の方法は、有機溶媒相のみを強制的
かつ連続的に取り出すために多孔性薄膜及びポンプを必
要とするものであり、これらの耐久性に問題があつた。
また、滴定中に空気を吸い込み、滴定を中断しなければ
ならないという欠点もあった。更に、滴定系中の有機溶
媒相をパイプを用いて検出装置に送るものであるため、
滴定系の現実の中和と検出系での判定が異なるというタ
イム・ラグの問題もあつた。However, the above method requires a porous thin film and a pump to forcibly and continuously take out only the organic solvent phase, and there is a problem in durability of these.
Further, there is a drawback that air must be sucked in during the titration to interrupt the titration. Furthermore, since the organic solvent phase in the titration system is sent to the detection device using a pipe,
There was also the problem of time lag, where the actual neutralization of the titration system and the judgment of the detection system were different.
したがつて、簡便に分相滴定をおこなうことのできる方
法及びその装置の開発が望まれていた。Therefore, there has been a demand for the development of a method and an apparatus capable of easily performing phase separation titration.
かかる現状において本発明者は、広く種々の界面活性剤
に応用でき、終点の判定が容易で精度も高く、かつ短時
間で界面活性剤の測定ができる分相滴定法の開発を目指
して鋭意研究した結果、乳化系から有機溶媒相のみを選
択的に通過せしめる多孔性膜と、該多孔性膜からなる外
面を有する検知室中に光路を有する、発光部及び受光部
を組み合せ、一定の条件で使用することによりこの目的
が達成されることを見出し本発明を完成した。Under the present circumstances, the present inventor has diligently studied for the purpose of developing a phase-separation titration method that can be widely applied to various surfactants, can easily determine the end point and has high accuracy, and can measure the surfactant in a short time. As a result, a porous membrane that selectively allows only the organic solvent phase to pass from the emulsified system, and an optical path in the detection chamber having an outer surface made of the porous membrane, a light emitting unit and a light receiving unit are combined under certain conditions. The present invention has been completed by finding that this object can be achieved by using it.
すなわち、本発明は被滴定液に浸漬可能で、有機溶媒相
のみを選択的に流通せしめる多孔性膜からなる外面を有
する検知室と、該検知室中に光路を有する発光部及び受
光部を設けてなる分相滴定用終点検出装置を提供するも
のである。That is, the present invention provides a detection chamber having an outer surface made of a porous film that can be immersed in a liquid to be titrated and selectively allows only an organic solvent phase to flow, and a light emitting unit and a light receiving unit having an optical path in the detection chamber. The present invention provides an end point detection device for phase separation titration.
以下、本発明の分相滴定用終点検知装置（以下「検出装
置」という）について、その実施例を示す図面挙げて説
明する。Hereinafter, an end point detection device for phase-separation titration (hereinafter referred to as “detection device”) of the present invention will be described with reference to the drawings showing an embodiment thereof.
第１図、第２図及び第３図は、本発明検出装置の断面図
である。各図中、２は検知室であり、基体１を切り欠き
設けられている。この検知室２は多孔性膜３を通じて外
部と連絡している。また、４は発光部、５は受光部であ
り、発光部４で発生した光は、光路ａを通つて受光部５
に到達する。分相滴定時において、本発明検出装置は滴
定系に浸漬され、多孔性膜３が有機溶媒相のみを選択的
に通過せしめるので、検知室２は有機溶媒相により満さ
れる。1, 2 and 3 are sectional views of the detection device of the present invention. In each figure, 2 is a detection chamber, in which the base 1 is cut out. The detection chamber 2 communicates with the outside through the porous membrane 3. Further, 4 is a light emitting unit, 5 is a light receiving unit, and the light generated by the light emitting unit 4 passes through the optical path a and is received by the light receiving unit 5.
To reach. At the time of phase-separation titration, the detection device of the present invention is immersed in the titration system to allow the porous membrane 3 to selectively pass only the organic solvent phase, so that the detection chamber 2 is filled with the organic solvent phase.
本発明において、滴定系中の有機溶媒相を検知室２に導
入するに当つては、何ら特別な力を用いず、多孔性膜３
からの拡散力のみに依存する。したがつて、検知室２は
小容量であることが好ましく、特に2cm2以下であること
が好ましい。また、多孔性膜３も滴定系から有機溶媒相
のみを分離、通過せしめ、しかもその通過速度の速いも
のが好ましく、具体的には、ポリフツ化エチレン樹脂、
ポリフツ化プロピレン樹脂等のフツ素樹脂製の多孔性薄
膜が適当であり、その孔径は10〜100μ、好ましくは10
〜60μであり、厚さは約0.1〜1mm程度が適当である。更
に、発光部４において発光される光は、連続光であつて
も単色光であつても良いが、検知に用いる光の波長は分
相滴定において用いられる分相指示薬により定められ
る。In the present invention, when the organic solvent phase in the titration system is introduced into the detection chamber 2, no special force is used and the porous membrane 3 is used.
Depends only on the diffusing power from. Therefore, the detection chamber 2 preferably has a small volume, and particularly preferably 2 cm 2 or less. Further, the porous membrane 3 is also preferably one which allows only the organic solvent phase to be separated and passed from the titration system, and has a high passage speed, specifically, a polyfluorinated ethylene resin,
A porous thin film made of a fluorine resin such as a polyfluorinated propylene resin is suitable, and its pore size is 10 to 100 μ, preferably 10
Appropriate thickness is about 0.1 to 1 mm. Further, the light emitted from the light emitting unit 4 may be continuous light or monochromatic light, but the wavelength of the light used for detection is determined by the phase separation indicator used in the phase separation titration.
第１図に示した本発明の検出装置は、発光部４で発光し
た光をグラスフアイバー6A及びレンズ７を通じて検知室
２中に導き、反射鏡８で反射させた後再度２中を通過せ
しめ、グラスフアイバー6Bを通じて受光部５に到達せし
め、吸光度を測定するものである。この装置によれば、
検知室２の容積を増大させずに２中の光路ａが長くなる
ので、検出感度の向上が図れる。The detection device of the present invention shown in FIG. 1 guides the light emitted from the light emitting portion 4 into the detection chamber 2 through the glass fiber 6A and the lens 7, reflects it by the reflecting mirror 8 and then passes through the inside 2 again. The light is made to reach the light receiving section 5 through the glass fiber 6B and the absorbance is measured. According to this device,
Since the optical path a in 2 is lengthened without increasing the volume of the detection chamber 2, the detection sensitivity can be improved.
第２図に示した本発明の検出装置は、発光部４で発生し
た光をグラスフアイバー6A及びレンズ７を通して検知室
２に導き、そのままグラスフアイバー6Bから受光部５に
到着せしめるものである。The detector of the present invention shown in FIG. 2 guides the light generated in the light emitting section 4 to the detection chamber 2 through the glass fiber 6A and the lens 7 and allows the light to reach the light receiving section 5 from the glass fiber 6B as it is.
なお、第１図及び第２図のいずれの検出装置においても
レンズ７は必須なものでなく、これを取り去ることもで
きる。It should be noted that the lens 7 is not essential in any of the detection devices shown in FIGS. 1 and 2 and can be removed.
第３図に示した本発明の検出装置は、発光部４として発
光ダイオードを用い、発光部５として受光素子を用いた
ものである。受光素子としては、フオトダイオード、フ
オトトランジスター等が用いられる。この検出装置にお
いて、発光ダイオード及び受光素子は用いる分相指示薬
によつて適宜選択される。The detection device of the present invention shown in FIG. 3 uses a light emitting diode as the light emitting section 4 and a light receiving element as the light emitting section 5. As the light receiving element, a photo diode, a photo transistor or the like is used. In this detection device, the light emitting diode and the light receiving element are appropriately selected depending on the phase separation indicator used.
叙上の本発明検出装置によつて、分相滴定の終定が定め
られるのは、次の原理に基くものである。The above-mentioned detection device of the present invention determines the end of the phase separation titration based on the following principle.
すなわち、前述したように検知室２は、多孔質膜３を通
過した被滴定液中の有機溶媒相で満たされているが、検
知室２中の有機溶媒相及び被滴定液中の有機溶媒相は多
孔性膜３を介して拡散するので、被滴定液を撹拌するこ
とにより検知室２中の有機溶媒相と被滴定液中の有機溶
媒相とは同様の状態に保たれるものであり、分相滴定の
終点においては、分相指示薬が水相から有機溶媒相に抽
出されて着色若しくは変色するか、有機溶媒相から水相
に転溶して脱色するため、有機溶媒相全体の色調も変化
する。したがつて、検知室２中の有機溶媒相の色調も変
化するため、発光部４から検知室２中に入射した光も有
機溶媒相の変化の影響を受け、受光部５において有機溶
媒相から出射された光の吸光度の変化が測定され、すな
わち分相滴定の終点が検出されるのである。That is, although the detection chamber 2 is filled with the organic solvent phase in the liquid to be titrated that has passed through the porous membrane 3 as described above, the organic solvent phase in the detection chamber 2 and the organic solvent phase in the liquid to be titrated are Is diffused through the porous film 3, so that by stirring the liquid to be titrated, the organic solvent phase in the detection chamber 2 and the organic solvent phase in the liquid to be titrated are kept in the same state. At the end point of the phase separation titration, the phase separation indicator is extracted from the aqueous phase to the organic solvent phase to be colored or discolored, or is transferred from the organic solvent phase to the aqueous phase for decolorization, and therefore the color tone of the entire organic solvent phase is also changed. Change. Therefore, since the color tone of the organic solvent phase in the detection chamber 2 also changes, the light incident from the light emitting unit 4 into the detection chamber 2 is also affected by the change in the organic solvent phase, and the light receiving unit 5 changes from the organic solvent phase to the light. The change in the absorbance of the emitted light is measured, that is, the end point of the phase separation titration is detected.
本発明の検出装置を用いる分析方法の機構をアニオン性
界面活性剤を、分相滴定指示薬及びカチオン性界面活性
剤を滴定液として用いて分析する場合を例にとつて更に
詳しく説明すれば次の通りである。The mechanism of the analysis method using the detection device of the present invention will be described in more detail with reference to an anionic surfactant, an example in which a phase-separation titration indicator and a cationic surfactant are used as titrants. On the street.
水及び水不溶性有機溶媒からなる被滴定液中に、アニオ
ン性界面活性剤（An -）と指示薬（In +）を加えると、ア
ニオン性界面活性剤の一部と指示薬が錯体を形成し、有
機相に入る（有機相着色）。In water and the titrant consisting of water-insoluble organic solvent, an anionic surfactant (A n -) Adding an indicator of (I n +), a portion indicator anionic surfactant form a complex , Enter the organic phase (organic phase coloring).
An -aq＋In +aq→〔An−In〕org 過剰に存在するアニオン性界面活性剤は、滴定液から供
給されるカチオン性界面活性剤（Ct +）と錯体を形成し
て有機溶媒相に移るが、これは無色である。A n - aq + I n + aq → [A n − I n ] org An excess of anionic surfactant forms an organic compound by forming a complex with the cationic surfactant (C t + ) supplied from the titration solution. Transfer to the solvent phase, which is colorless.
An -aq＋Ct +aq→〔An−Ct〕org さらにカチオン性界面活性剤を加えていき、終点近くに
なると、有機溶媒相中のアニオン性界面活性剤と指示薬
との錯体が、カチオン性界面活性剤により複分解され
て、指示薬が水相中に転溶する。A n - aq + C t + aq → [A n − C t ] org By further adding a cationic surfactant, and near the end point, the complex of the anionic surfactant and the indicator in the organic solvent phase becomes a cation. The indicator is trans-dissolved in the aqueous phase by being meta-decomposed by the organic surfactant.
〔An−In〕org＋Ct +aq→〔An−Ct〕org＋In +aq この時点で有機溶媒相は脱色されるので、吸光度を測定
することにより終点を知ることができる。吸光度は、指
示薬の種類により有機溶媒相の可視部吸収、紫外部吸収
を測定すれば良い。[A n −I n ] org + C t + aq → [A n −C t ] org + I n + aq Since the organic solvent phase is decolored at this point, the end point can be known by measuring the absorbance. The absorbance may be determined by measuring the visible part absorption and the ultraviolet absorption of the organic solvent phase depending on the kind of the indicator.
本発明検出装置を用いる分析方法が適用されるイオン性
界面活性剤には、アニオン性界面活性剤、カチオン性界
面活性剤及び両性界面活性剤が含まれる。The ionic surfactant to which the analysis method using the detection device of the present invention is applied includes an anionic surfactant, a cationic surfactant and an amphoteric surfactant.
アニオン性界面活性剤には、脂肪酸塩（石けん）、ポリ
オキシエチレンアルキルエーテルカルボキシレート等の
カルボン酸型界面活性剤；アルキルベンゼンスルホン酸
塩（ABS、LAS）、アルカンスルホン酸塩（SAS或いはパ
ラフインスルホン酸塩）、ジアルキルスルホこはく酸
塩、α−スルホ脂肪酸塩、ヒドロキシアルカンスルホン
酸塩、アルケンスルホン酸塩（AOS或いはα−オレフイ
ンスルホン酸塩）等のスルホン酸型界面活性剤；アルキ
ル硫酸エステル塩、ポリオキシアルキレンアルキルフエ
ニルエーテル硫酸エステル塩等の硫酸エステル塩型界面
活性剤；アルキルリン酸エステル塩、ポリオキシエチレ
ンアルキルエーテルリン酸エステル塩等のリン酸エステ
ル塩型界面活性剤等がある。Anionic surfactants include carboxylic acid type surfactants such as fatty acid salts (soap) and polyoxyethylene alkyl ether carboxylates; alkylbenzene sulfonates (ABS, LAS), alkane sulfonates (SAS or paraffin sulfonate). Salts), dialkyl sulfosuccinates, α-sulfo fatty acid salts, hydroxyalkane sulfonates, alkene sulfonates (AOS or α-olefin sulfonates), and other sulfonic acid type surfactants; alkyl sulfate ester salts, poly There are sulfate ester type surfactants such as oxyalkylene alkylphenyl ether sulfate ester salts; and phosphate ester salt type surfactants such as alkyl phosphate ester salts and polyoxyethylene alkyl ether phosphate ester salts.
カチオン性界面活性剤には、テトラアルキルアンモニウ
ム塩、アルキルピリジニウム塩等の第４級アンモニウム
塩がある。Cationic surfactants include quaternary ammonium salts such as tetraalkyl ammonium salts and alkyl pyridinium salts.
また両性界面活性剤には、N,N,N−トリアルキル−Ｎ−
カルボキシアルキルアンモニウムベタイン、N,N,N−ト
リアルキル−Ｎ−スルホアルキルアンモニウムベタイン
（スルホベタイン）、トリアルキルアミンオキシド等が
ある。Further, the amphoteric surfactant includes N, N, N-trialkyl-N-
Examples thereof include carboxyalkyl ammonium betaine, N, N, N-trialkyl-N-sulfoalkyl ammonium betaine (sulfobetaine), trialkylamine oxide and the like.
本発明で使用されるイオン性界面活性剤と錯体を形成し
て着色あるいは変色する分相滴定指示薬としては、メチ
レンブルー、メチルグリーン、トルイジンブルー、フク
シン、ニユートラルレツド、ポータミンフアーストレツ
ドBNL、ジミジウムブロマイド、アゾールＡ、ブロムフ
エノールブルー、メチルオレンジ、エリスロシン、ブロ
ムチモールブルー、ブロムクレゾールパープル、オレン
ジII、ジクロルフルオレツセイン、エオシン、エリスロ
シン、ジスルフインブルー、テトラブロモフエノールフ
タレインエチルエステルカリウム塩等がある。Examples of the phase separation titration indicator that forms a complex with an ionic surfactant to be used in the present invention and that is colored or discolored include methylene blue, methyl green, toluidine blue, fuchsin, neutral red, and portamine fares tread BNL, Dimidium bromide, azole A, bromphenol blue, methyl orange, erythrosine, bromthymol blue, bromcresol purple, orange II, dichlorofluorescein, eosin, erythrosine, disulfin blue, tetrabromophenolphthalein ethyl ester potassium There is salt etc.
被滴定液とする水不溶性有機溶媒としては、ベンゼン、
トルエン、キシレン、酢酸エチル等の比重が１より小さ
な溶媒でも良いが、クロロホルム、塩化メチレン、パー
クロロエチレン、モノクロロベンゼン、四塩化炭素等の
比重が１より大きい塩素化炭化水素系溶媒が好ましく、
特にクロロホルムは生成する錯体を良く溶かし最も好ま
しい溶媒である。The water-insoluble organic solvent used as the titrant is benzene,
A solvent having a specific gravity of less than 1 such as toluene, xylene, ethyl acetate may be used, but a chlorinated hydrocarbon solvent having a specific gravity of more than 1 such as chloroform, methylene chloride, perchloroethylene, monochlorobenzene, carbon tetrachloride is preferable,
In particular, chloroform is the most preferable solvent because it dissolves the formed complex well.
滴定液は、被検イオン性界面活性剤と逆の電荷を有する
界面活性剤の水溶液とする。即ち、アニオン性界面活性
剤の分析を行う場合はカチオン性界面活性剤溶液を、逆
にカチオン性界面活性剤の分析を行う場合はアニオン性
界面活性剤溶液をそれぞれ滴定液として行う。この場
合、被検イオン性界面活性剤と逆の電荷を有するイオン
性界面活性剤を過剰に加えておき、被検イオン性界面活
性剤と同じ電荷を有する活性剤で滴定するいわゆる逆滴
定で行うこともできる。両性界面活性剤は、pHの違いに
よりアニオン性界面活性剤として挙動したりカチオン性
界面活性剤として挙動したりするので、例えば酸を加え
てpHを低くしてある場合にはカチオン性界面活性剤を分
析する場合に準じて行うことができる。The titrant is an aqueous solution of a surfactant having a charge opposite to that of the test ionic surfactant. That is, when an anionic surfactant is analyzed, a cationic surfactant solution is used as a titration liquid, and conversely, when a cationic surfactant is analyzed, an anionic surfactant solution is used as a titration liquid. In this case, an ionic surfactant having a charge opposite to that of the test ionic surfactant is added in excess, and titration is performed with an active agent having the same charge as the test ionic surfactant. You can also Amphoteric surfactants behave as anionic or cationic surfactants depending on the difference in pH, so for example, if the pH is lowered by adding an acid, the cationic surfactants Can be carried out according to the case of analysis.
本発明によればこれまで手で振とうして行つていたイオ
ン性界面活性剤の分相滴定を、自動化することができる
と共に、終点の判定が容易で精度が高く、かつ短時間で
行うことができることとなつた。According to the present invention, the phase separation titration of the ionic surfactant, which has been performed by shaking by hand, can be automated, and the end point can be easily determined with high accuracy and can be performed in a short time. I was able to do it.
また、ポンプ等を用いないため、ポンプ、多孔性膜の耐
久性の問題、空気の混入の問題等も解消される。Further, since the pump or the like is not used, the problem of durability of the pump and the porous membrane, the problem of air inclusion, etc. are solved.
なお、本発明の検出装置においては、多孔性膜を通じて
の有機溶媒相の移動が律速となるため、一定の速度で滴
定をおこなうことが望ましい。In the detection device of the present invention, since the movement of the organic solvent phase through the porous membrane is rate-determining, it is desirable to perform titration at a constant rate.
次に本発明の分相滴定用検出装置を用いる分相滴定につ
いて、実施例を挙げ説明する。Next, the phase separation titration using the phase separation titration detection device of the present invention will be described with reference to examples.
実施例１（アニオン性界面活性剤の定量） A.使用試薬 （１）1/200Nベンゼトニウムクロライド水溶液ハイアミ
ン1622（米国Rohm＆Hass社製）2.35gを秤量し、水を加
えて１リツトルとする。なお、力価は一次標準スルホコ
ハク酸ジ２−エチルヘキシルナトリウムを用いて定め
た。Example 1 (Quantification of anionic surfactant) A. Reagents used (1) 2.35 g of 1/200 N benzethonium chloride aqueous solution Hyamine 1622 (manufactured by Rohm & Hass, USA) is weighed, and water is added to make 1 liter. The titer was determined using the primary standard sodium di2-ethylhexyl sulfosuccinate.
（２）メチレンブルー溶液 メチレンブルー（JIS K8897特級）0.03g、濃硫酸6.8g、
硫酸ナトリウム（無水）50gに水を加えて１リツトルと
する。(2) Methylene blue solution Methylene blue (JIS K8897 special grade) 0.03 g, concentrated sulfuric acid 6.8 g,
Water is added to 50 g of sodium sulfate (anhydrous) to make 1 liter.
（３）クロロホルム 試薬特級を使用する。(3) Chloroform Use special grade reagent.
B.使用機器 （１）分相滴定用検出装置 第１図に示すのと同一の型式の装置であり、その検知室
容積は0.7cm3、この検知室に設けられた多孔性膜はポリ
フツ化エチレン製（孔系60μ、厚さ0.3mm）である。B. Equipment used (1) Phase-division titration detection device This is the same type of device as shown in Fig. 1. Its detection chamber volume is 0.7 cm 3 , and the porous membrane provided in this detection chamber is made of polyfutation. Made of ethylene (pore system 60μ, thickness 0.3mm).
（２）発光部及び受光部 発光部及び受光部として京都電子社製PTA−118を用い
た。また、測定波長は630nmである。(2) Light emitting unit and light receiving unit PTA-118 manufactured by Kyoto Electronics Co., Ltd. was used as a light emitting unit and a light receiving unit. The measurement wavelength is 630 nm.
C.操作法 アニオン性界面活性剤量が0.3〜0.4gとなるように試料
を精秤し、純水に溶解し、正確に200mlとする。この溶
液10mlを正確に150ml容量のビーカーにとり、メチレン
ブルー溶液25ml、純水40ml及びクロロホルム25mlを加え
る。ビーカーに撹拌子を入れ、磁気撹拌機により撹拌
（1200rpm）をおこなう。このビーカー中に分相滴定用
検出装置を浸漬し、発光部及び受光部を調節して基準吸
光度（吸光度＝０）を定める。次いで、1/200Nベンゼト
ニウムクロライド溶液を用い、0.3ml/minの割合で滴下
して滴定を行つた。終点は吸光度で記録して滴定曲線中
の変曲点を中心とした直線部分を基準吸光部（吸光度＝
０）に外挿した交点である。次式によりアニオン性界面
活性剤の含量を求めた。C. Procedure The sample is precisely weighed so that the amount of anionic surfactant is 0.3 to 0.4 g, dissolved in pure water, and made exactly 200 ml. Exactly 10 ml of this solution is placed in a beaker having a volume of 150 ml, and 25 ml of methylene blue solution, 40 ml of pure water and 25 ml of chloroform are added. Put a stir bar in the beaker and stir (1200 rpm) with a magnetic stirrer. The detector for phase-phase titration is immersed in this beaker, and the light-emitting part and the light-receiving part are adjusted to determine the reference absorbance (absorbance = 0). Then, using a 1/200 N benzethonium chloride solution, titration was performed by dropping at a rate of 0.3 ml / min. The end point is recorded by absorbance, and the straight line portion centered on the inflection point in the titration curve is used as the reference absorbance (absorbance =
It is the intersection point extrapolated to 0). The content of the anionic surfactant was calculated by the following formula.
MW:アニオン性界面活性剤の平均分子量 f:滴定液の力価 アニオン性界面活性剤としてドデシル硫酸ナトリウムを
使用し、繰り返し定量分析を行つた場合の測定値を第１
表に示す。 MW: average molecular weight of the anionic surfactant f: titer of titrant The measured value when sodium dodecyl sulfate was used as the anionic surfactant and repeated quantitative analysis was performed.
Shown in the table.
実施例２（検出部の容量と分析時間） 実施例１に示した条件下に於いて、検知室の容量を変え
た場合の正確な結果を得るための所要滴定時間を測定し
た。その結果を第２表に示す。 Example 2 (Capacity of the detection part and analysis time) Under the conditions shown in Example 1, the titration time required to obtain accurate results when the capacity of the detection chamber was changed was measured. The results are shown in Table 2.
第１図は、反射型の本発明検出装置を示す断面図であ
る。 第２図は、通過型の本発明検出装置を示す断面図であ
る。 第３図は、発光部に発光ダイオードを、受光部に受光素
子を用いた本発明検出装置を示す断面図である。FIG. 1 is a sectional view showing a reflection type detection device of the present invention. FIG. 2 is a cross-sectional view showing the passage type detection device of the present invention. FIG. 3 is a cross-sectional view showing a detection device of the present invention using a light emitting diode for a light emitting portion and a light receiving element for a light receiving portion.
Claims (1)
選択的に流通せしめる多孔性膜からなる外面を有する検
知室２と、該検知室２中に光路を有する発光部４及び受
光部５を設けてなる分相滴定用終点検出装置。1. A detection chamber 2 having an outer surface made of a porous film which can be immersed in a liquid to be titrated and which selectively allows only an organic solvent phase to flow, a light emitting section 4 having an optical path in the detection chamber 2, and a light receiving unit. An end point detection device for phase separation titration, which is provided with a part 5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61209338A JPH0718802B2 (en) | 1986-09-05 | 1986-09-05 | End point detector for phase separation titration |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61209338A JPH0718802B2 (en) | 1986-09-05 | 1986-09-05 | End point detector for phase separation titration |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6365345A JPS6365345A (en) | 1988-03-23 |
| JPH0718802B2 true JPH0718802B2 (en) | 1995-03-06 |
Family
ID=16571294
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61209338A Expired - Lifetime JPH0718802B2 (en) | 1986-09-05 | 1986-09-05 | End point detector for phase separation titration |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0718802B2 (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2642522B1 (en) * | 1989-01-31 | 1991-05-10 | Elf Aquitaine | IN SITU OPTICAL DENSITY MEASURING APPARATUS FOR A CLOSER |
| US4892383A (en) * | 1989-02-17 | 1990-01-09 | Fiberchem Inc. | Reservoir fiber optic chemical sensors |
| US5059790A (en) * | 1990-03-30 | 1991-10-22 | Fiberchem, Inc. | Reservoir fiber optic chemical sensors |
| JP7115937B2 (en) * | 2018-08-31 | 2022-08-09 | 花王株式会社 | Methods for estimating physical properties of aqueous samples |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5526413A (en) * | 1978-08-15 | 1980-02-25 | Toshiba Corp | Waveform analyzing unit |
| JPS57106860A (en) * | 1980-12-23 | 1982-07-02 | Kao Corp | Method for measuring surface active agent |
-
1986
- 1986-09-05 JP JP61209338A patent/JPH0718802B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6365345A (en) | 1988-03-23 |
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