JPH06130051A - Fractional determination method of peracetic acid and hydrogen peroxide - Google Patents
Fractional determination method of peracetic acid and hydrogen peroxideInfo
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- JPH06130051A JPH06130051A JP4303215A JP30321592A JPH06130051A JP H06130051 A JPH06130051 A JP H06130051A JP 4303215 A JP4303215 A JP 4303215A JP 30321592 A JP30321592 A JP 30321592A JP H06130051 A JPH06130051 A JP H06130051A
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- Prior art keywords
- paa
- hydrogen peroxide
- aqueous solution
- concentration
- peracetic acid
- Prior art date
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Abstract
Description
【0001】[0001]
【産業上の利用分野】本発明は過酢酸、過酸化水素、酢
酸混合水溶液中の過酢酸(以下、PAAと略称する。)
と過酸化水素(以下、H2O2 と略称する。)を分別定
量する方法に関する。PAAは種々の目的に使用される
有用な薬剤である。例えば漂白剤、重合開始剤、殺菌
剤、酸化剤として使用されている。BACKGROUND OF THE INVENTION The present invention relates to peracetic acid in a mixed aqueous solution of peracetic acid, hydrogen peroxide and acetic acid (hereinafter abbreviated as PAA).
And hydrogen peroxide (hereinafter, abbreviated as H 2 O 2 ). PAA is a useful drug used for various purposes. For example, it is used as a bleaching agent, a polymerization initiator, a bactericide, and an oxidizing agent.
【0002】PAAの主な製造方法には、アセトアルデ
ヒドの直接酸化法とH2O2のアセチル化法の2通りの方
法がある。H2O2のアセチル化法においては、アセチル
化剤として、無水酢酸、塩化アセチル、ケテン等が使用
可能であるが、価格および爆発性の強いジアセチルパー
オキサイドが生成しにくいこと等から酢酸が使用され
る。There are two main methods for producing PAA: a direct oxidation method of acetaldehyde and an acetylation method of H 2 O 2 . In the acetylation method of H 2 O 2 , acetic anhydride, acetyl chloride, ketene, etc. can be used as the acetylating agent, but acetic acid is used because of the difficulty in producing diacetyl peroxide, which is highly priced and highly explosive. To be done.
【0003】重合開始剤や酸化剤等反応原料となる用途
のPAAは、主にアセトアルデヒドより合成されるが、
殺菌剤等比較的低濃度で使用される用途のPAAは、H
2O2と酢酸とから合成される場合が多い。H2O2と酢酸
からPAAと水ができる反応は平衡反応であるため、P
AA水溶液中には常に数パーセント以上のH2O2と酢酸
が存在する。このPAA使用時のPAA、H2O2の濃度
管理は重要であり、手分析、機器分析等により工程中の
PAA、H2O2の濃度を把握し、消費された分を追加注
入することにより一定の濃度に保つことが望ましい。PAA used as a reaction raw material such as a polymerization initiator or an oxidizing agent is mainly synthesized from acetaldehyde.
PAA used for relatively low concentration such as bactericide is H
It is often synthesized from 2 O 2 and acetic acid. Since the reaction of H 2 O 2 and acetic acid to form PAA and water is an equilibrium reaction,
A few percent or more of H 2 O 2 and acetic acid are always present in the AA aqueous solution. It is important to control the concentration of PAA and H 2 O 2 when using this PAA. It is necessary to grasp the concentration of PAA and H 2 O 2 in the process by manual analysis, instrumental analysis, etc., and to inject the consumed amount additionally. Therefore, it is desirable to maintain a constant concentration.
【0004】PAA、H2O2、酢酸混合水溶液中のPA
A、H2O2の分析方法には次のようなものがある。 (A)試料に希硫酸、ヨウ化カリウムを加え、遊離した
ヨードをチオ硫酸ナトリウム標準液で滴定して、PA
A、H2O2の合計量を測定する。次いで、別にサンプリ
ングした試料に希硫酸を加え過マンガン酸カリウム標準
液で滴定するか、フェロインを指示薬として硫酸第二セ
リウム標準液で滴定して、H2O2濃度を測定する。PA
AはPAA、H2O2の合計量からH2O2量を差し引いて
間接的に求める。PAA, H 2 O 2 , PA in acetic acid mixed aqueous solution
The methods for analyzing A and H 2 O 2 are as follows. (A) Dilute sulfuric acid and potassium iodide were added to the sample, and the liberated iodine was titrated with a sodium thiosulfate standard solution to obtain PA.
A, measure the total amount of H 2 O 2 . Then, dilute sulfuric acid is added to a sample sampled separately and titrated with a potassium permanganate standard solution, or titrated with a ceric sulfate standard solution using ferroin as an indicator to measure the H 2 O 2 concentration. PA
A is indirectly determined by subtracting the amount of H 2 O 2 from the total amount of PAA and H 2 O 2 .
【0005】(B)(A)の方法と同様にしてPAAと
H2O2の合計量を測定する。次いで、別にサンプリング
した試料に適量のジフェニルスルフィドを加え放置し、
PAAを還元した後、希硫酸、ヨウ化カリウムを加え、
遊離したヨードをチオ硫酸ナトリウム標準液で滴定して
H2O2濃度を測定する。PAAの濃度は、PAAとH2
O2の合計量からH2O2量を差し引いて間接的に求め
る。The total amount of PAA and H 2 O 2 is measured in the same manner as (B) and (A). Next, add an appropriate amount of diphenyl sulfide to the sample sampled separately and let it stand,
After reducing PAA, dilute sulfuric acid and potassium iodide were added,
The liberated iodine is titrated with a sodium thiosulfate standard solution to measure the H 2 O 2 concentration. The concentrations of PAA are PAA and H 2
From the total quantity of O 2 by subtracting the H 2 O 2 amount indirectly determined.
【0006】(C)(A)の方法と同様にしてPAAと
H2O2の合計量を測定する。次いで、別の試料に適量の
カタラーゼを加えてH2O2を分解させ、これに希硫酸、
ヨウ化カリウムを加えて遊離したヨードをチオ硫酸ナト
リウム標準液で滴定してPAA濃度を測定する。H2O2
濃度は、PAA、H2O2の合計量からPAA濃度を差し
引いて間接的に求める。The total amount of PAA and H 2 O 2 is measured in the same manner as in the methods (C) and (A). Then, an appropriate amount of catalase was added to another sample to decompose H 2 O 2 , and diluted sulfuric acid,
The iodine released by adding potassium iodide is titrated with a sodium thiosulfate standard solution to measure the PAA concentration. H 2 O 2
The concentration is indirectly determined by subtracting the PAA concentration from the total amount of PAA and H 2 O 2 .
【0007】(D)試料に希硫酸を加え、該試料を0℃
に冷却した後、過マンガン酸カリウム標準液で滴定して
H2O2を測定する。次に、同じく0℃に冷却された別の
試料にヨウ化カリウム溶液を加えて、遊離したヨウ素を
チオ硫酸ナトリウム溶液で滴定してPAAを測定する。(D) Dilute sulfuric acid was added to the sample, and the sample was heated to 0 ° C.
After cooling to room temperature, it is titrated with a potassium permanganate standard solution to measure H 2 O 2 . Next, a potassium iodide solution is added to another sample which is also cooled to 0 ° C., and free iodine is titrated with a sodium thiosulfate solution to measure PAA.
【0008】これらの方法において、(A)の方法は、
H2O2を測定する際に過マンガン酸カリウムが過酢酸や
酢酸の有機物とわずかづつ反応して消費されるためH2
O2濃度が高めに出る。従って、PAA濃度は低めとな
る。硫酸セリウム標準液で滴定した場合は多少改善され
るが、いずれにせよ金属イオンが触媒となり、PAAを
H2O2と酢酸に加水分解するので誤差が出る。Among these methods, the method (A) is
When measuring H 2 O 2 , potassium permanganate reacts with peracetic acid and organic substances of acetic acid little by little and is consumed, so H 2 O 2
The O 2 concentration becomes higher. Therefore, the PAA concentration is low. When titrated with a cerium sulfate standard solution, there is some improvement, but in any case, an error occurs because metal ions act as a catalyst and PAA is hydrolyzed into H 2 O 2 and acetic acid.
【0009】(B)の方法は、かなり正確にPAA、H
2O2の濃度が測定できるので、現在のところ最も優れた
方法と考えられる。しかしながら、ジフェニルスルフィ
ドを添加してから十分程度放置して還元反応が完結する
のを待たなければならないので、この点自動分析装置に
適用しにくい欠点がある。The method (B) is quite accurate in PAA, H
Since the concentration of 2 O 2 can be measured, it is considered to be the most excellent method at present. However, since it is necessary to wait for the reduction reaction to complete by adding the diphenyl sulfide and allowing it to stand for a sufficient period of time, there is a drawback that this point is difficult to apply to an automatic analyzer.
【0010】(C)の方法は、PAA濃度が高い場合、
カタラーゼ活性が阻害され、H2O2が分解されなくな
り、測定不能となる。The method (C) is used when the PAA concentration is high,
Catalase activity is inhibited, H 2 O 2 is not decomposed, and measurement becomes impossible.
【0011】(D)の方法おいても、過マンガン酸カリ
ウム溶液によるH2O2分析では、前記の問題があるし、
チオ硫酸ナトリウムによるPAAの分析ではPAAがヨ
ウ化カリウム溶液ヨードを遊離して誤差となる。また、
0℃まで冷却して分析するのは容易ではない。Also in the method (D), the above-mentioned problems occur in the H 2 O 2 analysis using the potassium permanganate solution.
In the analysis of PAA with sodium thiosulfate, PAA liberates potassium iodide solution iodine, resulting in an error. Also,
It is not easy to analyze by cooling to 0 ° C.
【0012】従来の分析方法は、以上のような種々問題
点がある。尚、(A)〜(C)の方法は、PAA、H2
O2の濃度を求めるためにいずれか一方だけを直接分析
し、他は計算値として算出しているに過ぎないし、ま
た、いずれの方法もPAA、H2O2の濃度を求めるため
に2回サンプリングしなければならない。本発明者等
は、上記の欠点のない1回のサンプリングで直接PA
A、H2O2を正確に分析できる方法を鋭意研究した結
果、本発明を完成させた。The conventional analysis method has various problems as described above. The methods of (A) to (C) are the same as PAA, H 2
In order to obtain the concentration of O 2 , only one of them is directly analyzed and the other is calculated as a calculated value. In addition, both methods are performed twice to obtain the concentrations of PAA and H 2 O 2. Must be sampled. The inventors of the present invention can directly perform PA with one sampling without the above-mentioned drawbacks.
The present invention has been completed as a result of earnest research on a method capable of accurately analyzing A and H 2 O 2 .
【0013】[0013]
【課題を解決するための手段】即ち、本発明は、PA
A、H2O2、酢酸混合水溶液中のPAA、H2O2の分別
定量方法において、先ず、(1)PAAに対して少過剰
当量のヨウ化カリウム水溶液を混合水溶液に添加し、遊
離したヨードをチオ硫酸ナトリウム標準液で滴定してP
AA濃度を測定し、次いで、(2)H2O2に対して大過
剰のヨウ化カリウム水溶液、希硫酸、およびモリブデン
酸アンモニウム水溶液を添加し、再度遊離したヨードを
チオ硫酸ナトリウム標準液で滴定してH2O2濃度を測定
することを特徴とするPAA、H2O2、酢酸混合水溶液
中の過酢酸とH2O2の分別定量方法に関する。That is, the present invention provides a PA
In the method for fractionating and quantifying PAA and H 2 O 2 in A, H 2 O 2 and acetic acid mixed aqueous solution, first, (1) potassium iodide aqueous solution with a small excess equivalent to PAA was added to the mixed aqueous solution to release it. Titrate iodine with sodium thiosulfate standard solution to obtain P
The AA concentration was measured, and then (2) a large excess of potassium iodide aqueous solution, dilute sulfuric acid, and ammonium molybdate aqueous solution was added to H 2 O 2 , and the liberated iodine was titrated again with sodium thiosulfate standard solution. The present invention relates to a method for fractionating and quantifying peracetic acid and H 2 O 2 in a mixed aqueous solution of PAA, H 2 O 2 and acetic acid, which is characterized by measuring the H 2 O 2 concentration.
【0014】PAA、H2O2が酸性下でヨウ化カリウム
からヨウ素を遊離する反応は以下の式で示される。 CH3COOOH+ 2I- + 2H+ = CH3COOH+H2O +I2 H2O2 + 2I- + 2H+ = 2H2O+I2 これらの2つの反応は一般に硫酸酸性下で行われるが、
酢酸酸性下でも反応は進行する。両者の反応速度は異な
り、PAAとヨウ化カリウムとの反応は速く、H2O2と
ヨウ化カリウムとの反応は遅い。特に酢酸酸性下で硫酸
が存在しない場合はこの差が大きくなる。しかし、大過
剰当量のヨウ化カリウムが存在するとH2O2との反応も
徐々に進み、PAAとH2O2を分別して測定することは
難しかった。The reaction of PAA and H 2 O 2 to release iodine from potassium iodide under acidic condition is shown by the following formula. CH 3 COOOH + 2I - + 2H + = CH 3 COOH + H 2 O + I 2 H 2 O 2 + 2I - + 2H + = 2H 2 O + I 2 is two reactions which are generally carried out under sulfuric acid,
The reaction proceeds even under acidic acetic acid. The reaction rates of the two are different, the reaction between PAA and potassium iodide is fast, and the reaction between H 2 O 2 and potassium iodide is slow. This difference becomes large especially in the absence of sulfuric acid under acidic acetic acid. However, in the presence of a large excess of potassium iodide, the reaction with H 2 O 2 gradually progressed, and it was difficult to measure PAA and H 2 O 2 separately.
【0015】ところが、硫酸の非存在下で、PAAに対
して少過剰当量のヨウ化カリウムを添加したところ、P
AAのみがヨウ化カリウムと反応し、ヨードを遊離する
ことが分かった。このヨードをチオ硫酸ナトリウム標準
液で滴定することによって、H2O2の影響を全く受けず
にPAAを定量することができる。また、このPAAを
測定した後の液に希硫酸、過酸化水素に対して過剰当量
のヨウ化カリウム溶液、及び反応触媒としてモリブデン
酸アンモニウム液を添加して、再度ヨードを遊離させ、
そのヨードをチオ硫酸ナトリウム標準液で滴定すること
によってH2O2を定量することができる。However, when a small excess of potassium iodide was added to PAA in the absence of sulfuric acid, P
It has been found that only AA reacts with potassium iodide, liberating iodine. By titrating this iodine with a sodium thiosulfate standard solution, PAA can be quantified without being affected by H 2 O 2 . Further, dilute sulfuric acid, an excess equivalent potassium iodide solution with respect to hydrogen peroxide, and ammonium molybdate solution as a reaction catalyst are added to the solution after measuring the PAA to release iodine again,
H 2 O 2 can be quantified by titrating the iodine with a sodium thiosulfate standard solution.
【0016】[0016]
【実施例】以下に実施例をあげて本発明を詳細に説明す
る。 実施例1 市販PAA、H2O2、酢酸混合水溶液(商品名オキシペ
ール060(PAA6%品),日本パーオキサイド株式
会社製)を200ml三角フラスコに約0.3g精秤
し、純水100mlと1Mヨウ化カリウム溶液を0.6
〜1.0ml(6%PAA 0.3gと0.48mlが反
応当量)加え、遊離したヨードを0.1Nチオ硫酸ナト
リウム標準溶液により無色になるまで滴定した。(Am
l) さらに、(1+9)硫酸10ml、1Mヨウ化カ
リウム溶液10ml、5%モリブデン酸アンモニウム溶
液1滴を加え、再度遊離したヨードを0.1Nチオ硫酸
ナトリウム標準溶液で滴定し、液が淡黄色になった時に
0.5%デンプン溶液を1ml加え滴定を続け、無色と
なった点を終点とした。(Bml) PAA、H2O2濃度は下記の式により計算した。 PAA(%)=0.38×f×A/S H2O2(%)=0.17×f×B/S f : 0.1Nチオ硫酸ナトリウム標準液のファクタ
ー S : 試料採取量(g) 1Mヨウ化カリウム溶液の添加量を0.6ml、0.8m
l、1.0mlとし、それぞれ3回ずつ分析したときの
PAA、H2O2濃度(%)は下記の表のようになった。EXAMPLES The present invention will be described in detail below with reference to examples. Example 1 About 0.3 g of commercially available PAA, H 2 O 2 and acetic acid mixed aqueous solution (trade name Oxyper 060 (PAA 6% product), manufactured by Nippon Peroxide Co., Ltd.) was precisely weighed in a 200 ml Erlenmeyer flask, and 100 ml of pure water and 1M were added. Add potassium iodide solution to 0.6
˜1.0 ml (0.3 g of 6% PAA and 0.48 ml of reaction equivalent) was added, and the liberated iodine was titrated with 0.1N sodium thiosulfate standard solution until it became colorless. (Am
l) Further, 10 ml of (1 + 9) sulfuric acid, 10 ml of 1M potassium iodide solution, 1 drop of 5% ammonium molybdate solution were added, and the liberated iodine was titrated with 0.1N sodium thiosulfate standard solution to give a pale yellow solution. When it became, 1 ml of 0.5% starch solution was added and the titration was continued. (Bml) PAA and H 2 O 2 concentrations were calculated by the following formula. PAA (%) = 0.38 × f × A / S H 2 O 2 (%) = 0.17 × f × B / S f: Factor S of 0.1N sodium thiosulfate standard solution S: Sampling amount (g ) The amount of 1M potassium iodide solution added was 0.6 ml, 0.8 m
The following table shows the concentrations (%) of PAA and H 2 O 2 when the amount was 1, 1.0 ml, and the analysis was performed 3 times each.
【0017】 対象 KI添加量(ml) 1回目 2回目 3回目 −−−−−−−−−−−−−−−−−−−−−−−−−−−−−−−−−− PAA 0.6 6.12 6.05 6.01 PAA 0.8 6.11 6.05 6.05 PAA 1.0 6.06 6.06 6.07 −−−−−−−−−−−−−−−−−−−−−−−−−−−−−−−−−− H2O2 0.6 8.00 8.06 7.99 H2O2 0.8 7.96 7.99 7.99 H2O2 1.0 7.96 7.96 7.97Target KI addition amount (ml) 1st time 2nd time 3rd time -------------------------------------- PAA 0.6 6.12 6.05 6.01 PAA 0.8 6.11 6.05 6.05 PAA 1.0 6.0 6.0 6.0 6.07 -------------- −−−−−−−−−−−−−−−−−−−−−−− H 2 O 2 0.6 8.00 8.06 7.99 H 2 O 2 0.8 7.967 .99 7.9 H 2 O 2 1.0 7.96 7.96 7.97
【0018】実施例2 市販PAA、H2 O2 、酢酸混合水溶液(商品名オキシ
ペール150(PAA15%品),日本パーオキサイド
株式会社製)を200ml三角フラスコに約0.1g精
秤し、純水100mlと1Mヨウ化カリウム溶液1ml
を加え、実施例1と同様にしてPAA、H2 O2 濃度
(%)を3回測定した。Example 2 About 0.1 g of commercially available PAA, H 2 O 2 and acetic acid mixed aqueous solution (trade name Oxypal 150 (PAA 15% product), manufactured by Nippon Peroxide Co., Ltd.) was precisely weighed in a 200 ml Erlenmeyer flask, and pure water was added. 100 ml and 1 M potassium iodide solution 1 ml
Was added, and PAA and H 2 O 2 concentrations (%) were measured three times in the same manner as in Example 1.
【0019】 対象 1回目 2回目 3回目 −−−−−−−−−−−−−−−−−−−−−−−−−−−− PAA 15.01 15.03 15.01 H2O2 22.49 22.48 22.50Subject 1st time 2nd time 3rd time ---------- PAA 15.01 15.03 15.01 H 2 O 2 22.49 22.48 22.50
【0020】実施例3 オキシペール150 0.1102gを200mlビー
カーに秤り取り、これに純水100mlと1Mヨウ化カ
リウム溶液1mlを加えた後、酸化還元電位計の電極を
入れ、0.1Nチオ硫酸ナトリウム標準溶液(f=1.0
12)を滴下しながら電位を測定した。電位が急激に低
下したところで(1+9)硫酸10mlと1Mヨウ化カ
リウム溶液10ml、5%モリブデン酸アンモニウム溶
液1滴を加えて、さらに測定を続けたときの0.1Nチ
オ硫酸ナトリウム標準溶液滴下量と電位との関係は次の
通りであった。Example 3 0.1102 g of Oxipale 150 was weighed in a 200 ml beaker, 100 ml of pure water and 1 ml of 1M potassium iodide solution were added thereto, and then an electrode of an oxidation-reduction potentiometer was put in the 0.1N thiosulfuric acid. Sodium standard solution (f = 1.0
The potential was measured while dropping 12). When the potential dropped sharply, 10 ml of (1 + 9) sulfuric acid and 10 ml of 1M potassium iodide solution were added, and 1 drop of 5% ammonium molybdate solution was added. The relationship with the potential was as follows.
【0021】[0021]
【表1】 [Table 1]
【0022】電位が最初に急激に低下した0.1Nチオ
硫酸ナトリウム標準溶液の滴下量4.3mlよりPAA
の濃度を算出すると15.0%となった。また、次に電
位が急激に低下したときの0.1Nチオ硫酸ナトリウム
標準溶液の滴下量18.7mlより4.3mlを差し引い
た値、14.4mlよりH2O2濃度を算出すると22.5
%となった。From the dropping amount of 4.3 ml of 0.1N sodium thiosulfate standard solution in which the potential dropped sharply from the beginning, PAA was used.
The concentration was calculated to be 15.0%. The value obtained by subtracting 4.3 ml from the dropwise addition amount of 18.7 ml of 0.1N sodium thiosulfate standard solution when the potential dropped sharply next time, and the H 2 O 2 concentration calculated from 14.4 ml were 22.5 ml.
It became%.
【0023】比較例1 オキシペール060を約0.3gずつ200ml三角フ
ラスコ2個に精秤し、一方には純水100ml、(1+
9)硫酸10mlを添加し、0.1N過マンガン酸カリ
ウム標準溶液で滴定し、H2O2濃度を測定した。またも
う一方には純水100ml、(1+9)硫酸10ml、
1Mヨウ化カリウム溶液10ml、モリブデン酸アンモ
ニウム溶液1滴を加え、0.1Nチオ硫酸ナトリウム標
準溶液で滴定して総過酸化物量を測定した。この値より
H2O2分を差し引いてPAA濃度とした。 それぞれ3
回ずつ分析した結果は下記の表の通りであった。Comparative Example 1 Oxypal 060 was precisely weighed in two 200 ml Erlenmeyer flasks, each containing about 0.3 g, and 100 ml of pure water was added to one of the flasks (1+
9) 10 ml of sulfuric acid was added and titrated with a 0.1N potassium permanganate standard solution to measure the H 2 O 2 concentration. On the other hand, 100 ml of pure water, 10 ml of (1 + 9) sulfuric acid,
10 ml of 1M potassium iodide solution and 1 drop of ammonium molybdate solution were added, and the total amount of peroxide was measured by titrating with 0.1N sodium thiosulfate standard solution. The H 2 O 2 content was subtracted from this value to obtain the PAA concentration. 3 each
The results of each analysis are shown in the table below.
【0024】 対象 1回目 2回目 3回目 −−−−−−−−−−−−−−−−−−−−−−−−−−−− PAA 5.57 5.74 5.81 H2O2 8.21 8.13 8.10Subject 1st time 2nd time 3rd time ---------- PAA 5.57 5.74 5.8 1 H 2 O 2 8.21 8.13 8.10
【0025】比較例2 オキシペール060を約0.3gずつ200ml三角フ
ラスコ2個に精秤し、一方には純水100ml、(1+
9)硫酸10mlを加え、0℃に冷却し0.1N過マン
ガン酸カリウム標準溶液で滴定してH2O2の濃度を測定
した。もう一方には純水100mlを加えて0℃に冷却
した後、1Mヨウ化カリウム溶液10mlを加えて、遊
離したヨードを0.1Nチオ硫酸ナトリウム標準溶液で
滴定してPAA濃度を測定した。3回ずつ分析した結果
は下記の表の通りであった。COMPARATIVE EXAMPLE 2 About 0.3 g of Oxypal 060 was precisely weighed in two 200 ml Erlenmeyer flasks, and one of them was 100 ml of pure water, (1+
9) 10 ml of sulfuric acid was added, cooled to 0 ° C., and titrated with a 0.1N potassium permanganate standard solution to measure the concentration of H 2 O 2 . After adding 100 ml of pure water to the other and cooling to 0 ° C., 10 ml of a 1M potassium iodide solution was added, and the liberated iodine was titrated with a 0.1N sodium thiosulfate standard solution to measure the PAA concentration. The results of three times analysis are shown in the table below.
【0026】 対象 1回目 2回目 3回目 −−−−−−−−−−−−−−−−−−−−−−−−−−−− PAA 7.26 6.55 7.46 H2O2 8.31 8.34 8.33Subject 1st time 2nd time 3rd time ---------- PAA 7.26 6.55 7.46 H 2 O 2 8.31 8.34 8.33
【0027】[0027]
【発明の効果】本発明によれば、PAA、H2O2、酢酸
混合水溶液中のPAA、及びH2O2の濃度を、1回のサ
ンプリングで両者を正確に分析することが可能である。
また、本発明方法は、酸化還元電位計等で自動分析を行
う際に、便利に利用できる方法である。According to the present invention, PAA, H 2 O 2, PAA acetate mixed aqueous solution, and the concentration of H 2 O 2, it is possible to accurately analyze both in one sampling .
Further, the method of the present invention is a method that can be conveniently used when performing automatic analysis with an oxidation-reduction potentiometer or the like.
─────────────────────────────────────────────────────
─────────────────────────────────────────────────── ───
【手続補正書】[Procedure amendment]
【提出日】平成5年2月15日[Submission date] February 15, 1993
【手続補正1】[Procedure Amendment 1]
【補正対象書類名】明細書[Document name to be amended] Statement
【補正対象項目名】0011[Correction target item name] 0011
【補正方法】変更[Correction method] Change
【補正内容】[Correction content]
【0011】(D)の方法おいても、過マンガン酸カリ
ウム溶液によるH2O2分折では、前記の問題がある
し、チオ硫酸ナトリウムによるPAAの分析ではPAA
がヨウ化カリウム溶液からヨードを遊離して誤差とな
る。また、0℃まで冷却して分折するのは容易ではな
い。Also in the method (D), H 2 O 2 fractionation with a potassium permanganate solution has the above-mentioned problems, and PAA analysis with sodium thiosulfate causes PAA.
Will release iodine from the potassium iodide solution, resulting in an error. Moreover, it is not easy to cool to 0 ° C. and to perform the folding.
【手続補正2】[Procedure Amendment 2]
【補正対象書類名】明細書[Document name to be amended] Statement
【補正対象項目名】0021[Correction target item name] 0021
【補正方法】変更[Correction method] Change
【補正内容】[Correction content]
【0021】[0021]
【表1】 [Table 1]
Claims (1)
の過酢酸と過酸化水素の分別定量方法において、先ず、 (1)過酢酸に対して少過剰当量のヨウ化カリウム水溶
液を混合水溶液に添加し、遊離したヨードをチオ硫酸ナ
トリウム標準液で滴定して過酢酸濃度を測定し、 次いで、 (2)過酸化水素に対して大過剰のヨウ化カリウム水溶
液、希硫酸、およびモリブデン酸アンモニウム水溶液を
添加し、再度遊離したヨードをチオ硫酸ナトリウム標準
液で滴定して過酸化水素濃度を測定する ことを特徴とする過酢酸、過酸化水素、酢酸混合水溶液
中の過酢酸と過酸化水素の分別定量方法。1. A method of fractionating and quantifying peracetic acid and hydrogen peroxide in a mixed aqueous solution of peracetic acid, hydrogen peroxide and acetic acid, which comprises firstly: (1) mixing an aqueous solution of potassium iodide in a small excess amount with respect to peracetic acid; And the liberated iodine was titrated with sodium thiosulfate standard solution to measure the peracetic acid concentration, and then (2) a large excess of potassium iodide aqueous solution with respect to hydrogen peroxide, dilute sulfuric acid, and ammonium molybdate. An aqueous solution is added, and the liberated iodine is titrated with a sodium thiosulfate standard solution to measure the hydrogen peroxide concentration. Fractional quantification method.
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JP30321592A JP3170526B2 (en) | 1992-10-16 | 1992-10-16 | Differential determination of peracetic acid and hydrogen peroxide |
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JP30321592A JP3170526B2 (en) | 1992-10-16 | 1992-10-16 | Differential determination of peracetic acid and hydrogen peroxide |
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JPH06130051A true JPH06130051A (en) | 1994-05-13 |
JP3170526B2 JP3170526B2 (en) | 2001-05-28 |
Family
ID=17918269
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JP2006528774A (en) * | 2003-07-22 | 2006-12-21 | ステリス インク | Vaporized hydrogen peroxide visual detection device |
WO2007035987A1 (en) | 2005-09-27 | 2007-04-05 | Siemens Water Technologies Corp. | Chemical cleaning agent and process for cleaning filtration membranes |
WO2008133321A1 (en) * | 2007-04-25 | 2008-11-06 | Saraya Co., Ltd. | Method for measurement of concentration of peroxycarboxylic acid, and apparatus for the method |
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TWI237035B (en) | 1998-07-24 | 2005-08-01 | Polyplastics Co | Polyacetal copolymer |
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JP2001158850A (en) | 1999-12-02 | 2001-06-12 | Polyplastics Co | Branched polyacetal resin composition |
WO2001042326A1 (en) | 1999-12-10 | 2001-06-14 | Polyplastics Co., Ltd. | Polyacetal copolymer |
KR101942784B1 (en) | 2017-02-06 | 2019-01-28 | 한국수자원공사 | Method and Test Kit For Dectecting Concentration of Hydrogen Peroxide |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2006528774A (en) * | 2003-07-22 | 2006-12-21 | ステリス インク | Vaporized hydrogen peroxide visual detection device |
WO2007035987A1 (en) | 2005-09-27 | 2007-04-05 | Siemens Water Technologies Corp. | Chemical cleaning agent and process for cleaning filtration membranes |
WO2008133321A1 (en) * | 2007-04-25 | 2008-11-06 | Saraya Co., Ltd. | Method for measurement of concentration of peroxycarboxylic acid, and apparatus for the method |
CN102037959A (en) * | 2010-12-29 | 2011-05-04 | 广东环凯微生物科技有限公司 | Method for preparing stable peracetic acid disinfectant |
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