CN116559342A - Method for simultaneously quantifying concentration of peroxyacetic acid and hydrogen peroxide in kinetics - Google Patents
Method for simultaneously quantifying concentration of peroxyacetic acid and hydrogen peroxide in kinetics Download PDFInfo
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- CN116559342A CN116559342A CN202310526441.4A CN202310526441A CN116559342A CN 116559342 A CN116559342 A CN 116559342A CN 202310526441 A CN202310526441 A CN 202310526441A CN 116559342 A CN116559342 A CN 116559342A
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- paa
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- tppo
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- KFSLWBXXFJQRDL-UHFFFAOYSA-N Peracetic acid Chemical compound CC(=O)OO KFSLWBXXFJQRDL-UHFFFAOYSA-N 0.000 title claims abstract description 128
- 238000000034 method Methods 0.000 title claims abstract description 27
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract 2
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 30
- FIQMHBFVRAXMOP-UHFFFAOYSA-N triphenylphosphane oxide Chemical compound C=1C=CC=CC=1P(C=1C=CC=CC=1)(=O)C1=CC=CC=C1 FIQMHBFVRAXMOP-UHFFFAOYSA-N 0.000 claims description 21
- 239000000126 substance Substances 0.000 claims description 8
- 238000004128 high performance liquid chromatography Methods 0.000 claims description 5
- 238000011002 quantification Methods 0.000 claims description 4
- AYEKOFBPNLCAJY-UHFFFAOYSA-O thiamine pyrophosphate Chemical compound CC1=C(CCOP(O)(=O)OP(O)(O)=O)SC=[N+]1CC1=CN=C(C)N=C1N AYEKOFBPNLCAJY-UHFFFAOYSA-O 0.000 claims 5
- 239000002904 solvent Substances 0.000 claims 1
- RIOQSEWOXXDEQQ-UHFFFAOYSA-N triphenylphosphine Chemical compound C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 RIOQSEWOXXDEQQ-UHFFFAOYSA-N 0.000 abstract description 30
- 238000001514 detection method Methods 0.000 abstract description 8
- 230000001590 oxidative effect Effects 0.000 abstract description 8
- 230000008569 process Effects 0.000 abstract description 8
- 238000004659 sterilization and disinfection Methods 0.000 abstract description 7
- 239000007800 oxidant agent Substances 0.000 abstract description 5
- 239000003344 environmental pollutant Substances 0.000 abstract description 4
- 231100000719 pollutant Toxicity 0.000 abstract description 4
- -1 4-methyl anisole sulfide Chemical compound 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 238000004364 calculation method Methods 0.000 abstract 1
- 239000007795 chemical reaction product Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 39
- JGSARLDLIJGVTE-MBNYWOFBSA-N Penicillin G Chemical compound N([C@H]1[C@H]2SC([C@@H](N2C1=O)C(O)=O)(C)C)C(=O)CC1=CC=CC=C1 JGSARLDLIJGVTE-MBNYWOFBSA-N 0.000 description 5
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 5
- 229910052700 potassium Inorganic materials 0.000 description 5
- 239000011591 potassium Substances 0.000 description 5
- 229910021642 ultra pure water Inorganic materials 0.000 description 5
- 239000012498 ultrapure water Substances 0.000 description 5
- 229930182555 Penicillin Natural products 0.000 description 4
- 239000000356 contaminant Substances 0.000 description 4
- 229940049954 penicillin Drugs 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 239000000645 desinfectant Substances 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 244000005700 microbiome Species 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000008055 phosphate buffer solution Substances 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000002238 attenuated effect Effects 0.000 description 1
- 239000007844 bleaching agent Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/067—Preparation by reaction, e.g. derivatising the sample
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Measuring Or Testing Involving Enzymes Or Micro-Organisms (AREA)
Abstract
The invention belongs to the field of environmental chemistry, and relates to a method for detecting instantaneous peracetic acid (PAA) and hydrogen peroxide (H) in dynamics 2 O 2 ) Concentration method. The invention uses Triphenylphosphine (TPP) and PAA and H 2 O 2 The reaction universality and the selectivity of 4-methyl anisole sulfide (MTS) and PAA are taken as theoretical basis, and the PAA and H are quantified in the dynamic reaction by the concentration difference of reaction products 2 O 2 The concentration detection and calculation method provides basis for researching the concentration detection of the oxidant in the water treatment processes such as disinfection, pollutant conversion and the like.
Description
Technical Field
The invention belongs to the field of environmental chemistry, and provides a method for detecting the concentration of instantaneous peroxyacetic acid and hydrogen peroxide. The invention mainly describes the quantitative detection mode of the concentration-changing peroxyacetic acid and hydrogen peroxide in the dynamic reaction, and can provide basis for researching the concentration detection of the oxidant in the disinfection and pollutant conversion processes.
Background
Peracetic acid (PAA) is a common peroxide of the formula CH 3 COOOH. PAA is a pungent, odoriferous, oxidative, colorless liquid that is commonly used as a disinfectant and bleach due to its oxidizing ability. The solution containing PAA as main active ingredient also contains acetic acid and hydrogen peroxide (H 2 O 2 )。H 2 O 2 Similar to the chemical nature of PAA, the chemical formula contains a peroxy bond, and thus has selective oxidation to thioether bond-containing contaminants. PAA as disinfectant needs to be in proper concentration condition to exert the disinfection effect to the maximum extent and at the same time not to happenHas influence on human health, process equipment and ecological environment. After disinfectant is added, the effective components PAA and H 2 O 2 Will rapidly interact with contaminants and microorganisms in aqueous solutions, where PAA and H 2 O 2 The concentration of (c) will also decrease over time. Thus study of PAA and H in kinetics 2 O 2 The concentration is of great importance for improving the disinfection efficiency.
In conventional PAA and H 2 O 2 In the concentration detection method, the detection reagent 4-methyl anisole sulfide (MTS) of PAA can be formed into corresponding oxidation product MTSO by PAA, and H 2 O 2 Triphenylphosphine (TPP) and H as detection reagents 2 O 2 Generating TPPO by reaction, and back calculating PAA and H in the solution according to the concentration of MTSO and TPPO 2 O 2 Concentration. But due to PAA and H 2 O 2 The difference in oxidizing power makes it necessary to add MTS and TPP sequentially, and the difference in time interval therebetween makes the conventional method incapable of detecting PAA and H in real time 2 O 2 Is a concentration of (3). For example in the determination of H 2 O 2 A time difference of 10min before concentration was required to allow the PAA to react completely with MTS, thereby quenching H within 10min of PAA 2 O 2 The concentration is also attenuated by the action of contaminants and microorganisms, thereby allowing H 2 O 2 Deviations in concentration occur.
In order to solve the error of real-time quantification caused by time difference, the invention provides a method for accurately quantifying PAA and H in dynamics 2 O 2 Concentration method. At the sampling time of the kinetic reaction, MTS was added to the first solution to quantify the PAA concentration for 10min before TPP was added to quantify H 2 O 2 Concentration; the TPP is directly added into the second part of solution to obtain PAA and H 2 O 2 Is used (total oxidant concentration). Finally, the total oxidant concentration and the PAA concentration are analyzed by adopting a differential method to obtain H 2 O 2 Provides basis for researching concentration change of each substance in the dynamic process.
Disclosure of Invention
The invention aims to provide a method for simply, conveniently, efficiently and accurately synchronizing dynamicsQuantitative PAA and H 2 O 2 The concentration method provides a guarantee for optimizing the disinfection process and accurately analyzing the concentration relation of each substance.
The invention provides a new method for solving the problems at the present stage, which mainly comprises the following steps:
1) To the first part contains PAA and H 2 O 2 To a second portion containing PAA and H at the same time as the MTS solution was added to the solution (sample A) 2 O 2 To the solution (sample B) of TPP solution was added.
2) After 10min of reaction, the TPP solution was added to the first solution and reacted for 30min, during which time the second solution remained stationary.
3) The MTSO and TPPO concentrations in the first solution and the TPPO concentration in the second solution were measured by HPLC.
4) H is accurately obtained by the following chemical relationship 2 O 2 Concentration.
Sample a:
c[MTSO] A ＝c[PAA]
c[TPPO] A ＝c[H 2 O 2 ]
sample B:
c[TPPO] B ＝c[H 2 O 2 ]+c[PAA]
c[H 2 O 2 ]＝c[TPPO] B -c[MTSO] A
the beneficial effects are that:
the invention has the beneficial effects that: can simultaneously and accurately quantify PAA and H in the dynamic reaction process 2 O 2 The concentration provides technical guidance for further research of the disinfection process.
Drawings
FIG. 1 measurement of PAA and H according to the invention 2 O 2 Standard curve experimental results of concentration.
FIG. 2 measurement of PAA and H in kinetics of the invention 2 O 2 Experimental results of concentration.
Detailed Description
The invention is further illustrated by the following examples and figures. The following examples simulate water pollution treatmentsThe process, and the potassium penicillin is taken as representative target pollutant to study PAA and H in the degradation kinetics of the potassium penicillin 2 O 2 Concentration variation. The examples of the present invention are intended to better understand the present invention to those skilled in the art, and are not intended to limit the present invention in any way.
Example 1
The present example is based on PAA and H obtained by an improved method 2 O 2 The standard curve of concentration illustrates the method of use of the invention, and the specific steps are as follows:
1) Preparing the concentration of 10mmol L -1 MTS solution in acetonitrile and 10mmol L -1 TPP solution in acetonitrile.
2) The theoretical concentration ranges are 0, 20, 40, 60, 80, 100 mu mol L -1 Two portions each of the PAA solutions.
3) To a first sample (sample A) containing 0.1mL of PAA solution, 0.1mL of MTS solution and 0.3mL of ultrapure water were added. To a second sample (sample B) containing 0.1mL of PAA solution, 0.1mL of TPP solution and 0.3mL of ultrapure water were added simultaneously.
4) After dark reaction of the two samples for 10min, 0.1mL of TPP solution and 0.4mL of acetonitrile solution were added to sample A. To sample B was added simultaneously 0.5mL of acetonitrile solution.
5) After a dark reaction for 30min, the concentrations of MTSO and TPPO in the two samples were measured using HPLC.
6) Obtaining PAA and H in solution by chemical relation in samples A and B 2 O 2 Concentration:
sample a:
c[MTSO] A ＝c[PAA]
c[TPPO] A ＝c[H 2 O 2 ]
sample B:
c[TPPO] B ＝c[H 2 O 2 ]+c[PAA]
c[H 2 O 2 ]＝c[TPPO] B -c[MTSO] A
the invention detects PAA and H 2 O 2 The standard curve experiment results of the concentration are shown in fig. 1.
Example 2
This example selects potassium penicillin as the target contaminant and studies the binding kinetics to illustrate the method of use of the invention, as follows:
1) Preparing the concentration of 10mmol L -1 MTS solution in acetonitrile, 10mmol L -1 TPP solution in acetonitrile, 10mmol L -1 Penicillin potassium solution (10 mM phosphate buffer solution, pH 8) and 2mmol L -1 PAA solution.
2) To a 30mL brown bottle was added 0.2mL of potassium penicillin solution, phosphate buffer solution (final 10mM, pH 8) and ultrapure water to a solution volume of 19mL. 1mL of PAA solution was added to start the reaction. Two samples were taken at reaction 30, 60, 180, 300, 600s, respectively.
3) To a first sample (sample A) containing 0.1mL of PAA solution, 0.1mL of MTS solution and 0.3mL of ultrapure water were added. To a second sample (sample B) containing 0.1mL of PAA solution, 0.1mL of TPP solution and 0.3mL of ultrapure water were added simultaneously.
4) After dark reaction of the two samples for 10min, 0.1mL of TPP solution and 0.4mL of acetonitrile solution were added to sample A. To sample B was added simultaneously 0.5mL of acetonitrile solution.
5) After a dark reaction for 30min, the concentrations of MTSO and TPPO in the two samples were measured using HPLC.
6) Obtaining PAA and H in solution by chemical relation in samples A and B 2 O 2 Concentration:
sample a:
c[MTSO] A ＝c[PAA]
c[TPPO] A ＝c[H 2 O 2 ]
sample B:
c[TPPO] B ＝c[H 2 O 2 ]+c[PAA]
c[H 2 O 2 ]＝c[TPPO] B -c[MTSO] A
conventional and modified methods for kinetic measurement of PAA and H 2 O 2 The experimental results of the concentrations are shown in FIG. 2.
The implementation result of the scheme is as follows:
from the experimental results of FIGS. 1 and 2, it can be seen that the improved method is used for detecting PAA and H 2 O 2 Concentration stability while the present invention verifies from theoretical and practical point of view simultaneous quantification of PAA and H in kinetics 2 O 2 The feasibility of concentration, and further provides technical support for the detection of the concentration of the oxidant in the process of disinfection and pollutant treatment to be researched.
It should be understood that the embodiments and examples discussed herein are for illustrative purposes only and that modifications or changes in light thereof will be suggested to persons skilled in the art and are to be included within the purview of this application and are to be included within the scope of the appended claims.
Claims (3)
1. A method for simultaneously quantifying the concentration of peroxyacetic acid and hydrogen peroxide in kinetics, which mainly comprises the following steps:
step one: MTS and TPP solutions were formulated.
Step two: to the first part contains PAA and H 2 O 2 To a second portion containing PAA and H at the same time as the MTS solution was added to the solution (sample A) 2 O 2 To the solution (sample B) of TPP solution was added.
Step two: after 10min of reaction, the TPP solution was added to the first solution and reacted for 30min, during which time the second solution remained stationary.
Step three: the MTSO and TPPO concentrations in the first solution and the TPPO concentration in the second solution were measured by HPLC.
Step four: h is accurately obtained by the following chemical relationship 2 O 2 Concentration.
Sample a:
c[MTSO] A ＝c[PAA]
c[TPPO] A ＝c[H 2 O 2 ]
sample B:
c[TPPO] B ＝c[H 2 O 2 ]+c[PAA]
c[H 2 O 2 ]＝c[TPPO] B -c[MTSO] A 。
2. a method for simultaneous kinetic quantification of peroxyacetic acid and hydrogen peroxide concentration according to claim 1, characterized essentially by: the mobile phase at the MTSO and TPPO concentrations was acetonitrile and water using high performance liquid chromatography.
3. A method for simultaneous kinetic quantification of peroxyacetic acid and hydrogen peroxide concentration according to claim 1, characterized essentially by: in step one, both MTS and TPP were acetonitrile as solvents, and the MTS and TPP solutions were 10mmol in concentration.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310526441.4A CN116559342A (en) | 2023-05-11 | 2023-05-11 | Method for simultaneously quantifying concentration of peroxyacetic acid and hydrogen peroxide in kinetics |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310526441.4A CN116559342A (en) | 2023-05-11 | 2023-05-11 | Method for simultaneously quantifying concentration of peroxyacetic acid and hydrogen peroxide in kinetics |
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| CN116559342A true CN116559342A (en) | 2023-08-08 |
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| CN202310526441.4A Pending CN116559342A (en) | 2023-05-11 | 2023-05-11 | Method for simultaneously quantifying concentration of peroxyacetic acid and hydrogen peroxide in kinetics |
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| CN (1) | CN116559342A (en) |
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- 2023-05-11 CN CN202310526441.4A patent/CN116559342A/en active Pending
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