CN108414670A - The detection method of hydrogen peroxide in a kind of water sample - Google Patents
The detection method of hydrogen peroxide in a kind of water sample Download PDFInfo
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- CN108414670A CN108414670A CN201810223672.7A CN201810223672A CN108414670A CN 108414670 A CN108414670 A CN 108414670A CN 201810223672 A CN201810223672 A CN 201810223672A CN 108414670 A CN108414670 A CN 108414670A
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- hydrogen peroxide
- water sample
- leacheate
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- 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
- G01N30/96—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 using ion-exchange
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- 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
- G01N30/62—Detectors specially adapted therefor
- G01N30/74—Optical detectors
Abstract
Hydrogen peroxide is a kind of common industrial chemicals, has the multiple uses such as oxidation, bleaching and disinfection.Therefore, in sample hydrogen peroxide it is accurate, facilitate detection practical application it is significant.But existing hydrogen peroxide detection method operation is relatively cumbersome, time-consuming, and needs additional addition chemical substance that could obtain detection signal with hydroperoxidation, makes troubles to the actual use of detection method.Here, the present invention provides a kind of detection methods accurately measuring hydrogen peroxide in water sample by ion chromatograph.This method is without additionally adding other chemical substances into water sample, so easy to operate and strong interference immunity.The specific present invention makes hydrogen peroxide be converted into ionic condition in alkaline leacheate first, then hydrogen peroxide ions are detached with other ions and neutral substance using ion chromatographic column, the hydrogen peroxide of ionic condition is converted by molecular state by suppressor again, finally carries out quantitative detection with UV detector.
Description
Technical field
The present invention relates to the detection of hydrogen peroxide, the detection method of hydrogen peroxide in especially a kind of water sample.
Background technology
Hydrogen peroxide is a kind of common industrial chemicals, has the multiple uses such as oxidation, bleaching.The detection of hydrogen peroxide exists
The multiple fields such as Food Science, industrial flow, Environmental Chemistry are all concerned.The detection technique packet of hydrogen peroxide in existing water sample
It includes：Titration, spectrophotometry, fluorescence method, chemoluminescence method, electrochemical process and liquid chromatography etc..These methods are in reality
Can encounter some problems in use, such as it is cumbersome, time-consuming, needs additional addition various medicaments, be unfavorable for practice.
Peroxidating in a kind of water sample is disclosed in Chinese invention patent application prospectus CN 201310154581.X
The graphene and hydrogen peroxide indicator tetramethyl biphenyl of chitosan dispersion are added in party's normal direction water sample for the detection method of hydrogen
Then amine detects the concentration of hydrogen peroxide in water sample by measuring absorbance of the water sample at 652nm.This method can be accurate
Detection water sample in concentration of hydrogen peroxide, but need additionally to add a variety of chemical reagent, measurement process is relatively cumbersome.And if
In sample with other colour developings, oxidisability or reproducibility chaff interferent, test result will appear deviation.Wangkai hero etc. passes through Asia
Sulfate analyzes hydrogen peroxide with the method for sulfate radical is measured with ion chromatography after hydroperoxidation, but this method is indirect
Measurement method, other oxidisability or reducing substances can form interference in method, or obstruction persulfate and hydrogen peroxide it is anti-
It answers, or is directly reacted with hydrogen peroxide, lead to detection error.
Invention content
Problems to be solved by the invention
The detection method operation of hydrogen peroxide is relatively cumbersome in existing water sample, time-consuming and needs additional addition medicament,
It makes troubles to practical application.
Here, it is an object of the invention to：On the basis of adding any reagent not into sample, realize that hydrogen peroxide exists
Accurate detection in water sample.
The means solved the problems, such as
Ion chromatography is a kind of chromatographic process for being detached and being detected using measured matter ion characteristic, under conventional sense
Hydrogen peroxide exists with neutral molecule state in water, therefore the not yet useful chromatography of ions directly detects hydrogen peroxide in water sample
Report.
The present invention controls existence of the hydrogen peroxide in water sample by adjusting the variation of pH in reaction process, passes through
The difference property of hydrogen peroxide ions state and molecular state is detached and is detected.Relative theory is：Allow hydrogen peroxide first
Ionic condition is fully converted into alkali ion chromatogram eluate, then by anion chromatographic column by hydrogen peroxide ions with
Other ions and neutral substance separation, then gone back to the hydrogen peroxide of ionic condition for molecular state by suppressor, finally use
UV detector detects the hydrogen peroxide detached.
The detection method of hydrogen peroxide, is detached and is examined by ion chromatograph in a kind of water sample of the present invention
It surveys, is analyzed using quantified by external standard method, specific steps include：
(1) operating condition for setting ion chromatograph ensures that the water sample containing hydrogen peroxide is passing through ion chromatography column
When be ionic condition, and be fully converted back into as molecular state after by suppressor.
(2) Standard Stock solutions for configuring hydrogen peroxide, are reconfigured Hydrogen peroxide standard solution, utilize ion chromatography chromatography
Instrument is detached and is detected, the peak area or peak heights of the ultraviolet detector response of record standard solution；Peroxide is drawn with external standard method
Concentration ----peak area or concentration --- peak heights standard curve for changing hydrogen, to obtain peroxide standard curve regression equation；
(3) take water sample to be measured, analyzed with ion chromatograph, record the sample UV detector peak area or peak
Highly, the content of hydrogen peroxide in water sample is obtained according to standard curve regression equation calculation obtained by step (1).
The ion chromatograph operating condition, including ion chromatographic column, column oven, suppressor, UV detector, leacheate
Etc. setting.
The chromatographic column column oven temperature be 20-40 degrees Celsius in the range of when, in the identical situation of other conditions
Lower analysis, smaller on the separating degree of sample, peak shape, symmetry etc. influence, hydrogen peroxide can realize good separation.
As a kind of preferred embodiment measuring the method for hydrogen peroxide in water sample of the present invention, the chromatographic column column oven
Temperature is 30 degrees Celsius.
The leacheate need to ensure that the pH value of leacheate is more than the acid ionization constant of hydrogen peroxide under normal temperature and pressure, that is, elute
The pH value of liquid is greater than 11.6.
As a kind of preferred embodiment measuring the method for hydrogen peroxide in water sample of the present invention, the leacheate can select
Select the mixing leacheate etc. of potassium hydroxide leacheate, sodium hydroxide leacheate or sodium bicarbonate and sodium carbonate.
When the eluent concentration is in the range of 10-40mmol/L, analyzed in the case where other conditions are identical,
It has a certain impact to the separating degree, peak shape, symmetry etc. of sample, but can realize effective measurement.
As a kind of preferred embodiment measuring the method for hydrogen peroxide in water sample of the present invention, the leacheate selects hydrogen
Potassium oxide leacheate, a concentration of 10mmol/L.
As a kind of preferred embodiment measuring the method for hydrogen peroxide in water sample of the present invention, the water sample sample size is
100μL。
When the UV detector selects wavelength as in the range of 200-230nm, in the identical situation of other conditions
Lower analysis has a certain impact to the peak shape of sample, baseline noise etc..
As a kind of preferred embodiment measuring the method for hydrogen peroxide in water sample of the present invention, the UV detector choosing
It is 210nm with wavelength.
The suppressor is electrochemical membrane suppressor.
The present invention is a kind of to be measured in water sample in the procedure of hydrogen peroxide, and concentration of hydrogen peroxide ----peak area is dense
Degree ----Height Standard curve is drawn using external standard method, obtains standard curve regression equation, when measuring water sample, according to ultraviolet detection
The peak area or height that device measurement obtains, are calculated the content of hydrogen peroxide in water sample.
The present invention is to be put forward for the first time directly to detect hydrogen peroxide using ion chromatograph, compared with technology before,
Without additionally adding any chemical agent to water sample, hydrogen peroxide other any substances of also getting along well chemically react this method,
Therefore it is easy to use, anti-interference is stronger, can more accurately measure tested substance.
Description of the drawings
Fig. 1 is the typical ion chromatography figure of present invention detection hydrogen peroxide
Fig. 2 is the chromatography of ions figure for the influence that different eluent concentrations detect hydrogen peroxide
The chromatography of ions figure of influences of the Fig. 3 for fluorine ion and glycolic in the presence of common to hydrogen peroxide detection
Fig. 4 is the chromatography of ions figure that hydrogen peroxide detects in actual water sample
Fig. 5 is to use AS-15 chromatographic column testing result figures
Fig. 6 is to use AZ chromatographic columns and 10mmol/L sodium hydroxide leacheate testing result figures
Fig. 7 is to be detected using the mixing leacheate of AZ chromatographic columns and 1.9mmol/L sodium bicarbonates and 3.2mmol/L sodium carbonate
Result figure
Fig. 8 is different ultraviolet wavelength testing result figures
Specific implementation mode
A kind of method measuring hydrogen peroxide in water sample of the present invention, is detached and is detected by ion chromatograph, used
Quantified by external standard method is analyzed, and without additional addition medicament, easy to use, strong interference immunity, precision are high, and concrete principle is as follows：
The separation process of hydrogen peroxide in water sample
Acid ionization constant of the hydrogen peroxide under normal temperature and pressure conditions, i.e. pKa=11.6, when the pH of water sample is more than 11.6
When, hydrogen peroxide mainly exists in the form of an ion.Therefore, when ion chromatograph selection pH be more than 11.6 strong basicity leacheate,
When such as potassium hydroxide leacheate, hydrogen peroxide mainly exists in the form of an ion after entering ion chromatograph, therefore can pass through
Anion chromatographic column is detached.
H2O2→HO2 -+H+pH>11.6
The detection of hydrogen peroxide in water sample
Ion chromatograph equipped with electrochemical membrane suppressor, when sample passes through suppressor, sample pH can return neutrality
Or it is acid.Therefore, after the inhibited device of the aqueous sample stream containing hydrogen peroxide, since pH value becomes neutral or acid from strong basicity,
Hydrogen peroxide can be again gone back to by ionic state as molecule neutral state；This neutral state cannot by the conductivity of ion chromatography into
Row detection, but can be detected by UV detector.
HO2 -+H+→H2O2pH<11.6
Illustrate the present invention with reference to specific embodiment.
Embodiment is only applicable to that the present invention will be described in detail, does not limit the scope of the invention in any form.
Embodiment 1
Used ion chromatography condition is：Ion chromatograph is Tosoh company IC2010；Guard column is Dai An companies AG-
15；Analytical column is Dai An companies AS-15 chromatographic columns；Chromatographic column column oven temperature is 30 degrees Celsius；Suppressor is to contain vast electrochemistry
Membrane suppressor SHY-A- III, detector are Shimadzu SPD 20A UV detector, and it is 210nm which, which selects wavelength,；Leaching
Washing lotion selects potassium hydroxide leacheate, a concentration of 10mmol/L；Elution flow velocity is 0.5mL/min；Sample injection volume is 100
μL。
Specific steps include：
(1) Hydrogen peroxide standard solution storing solution is configured
30% hydrogen peroxide (analysis is pure) 33.3333g to 1000ml volumetric flasks are weighed, the peroxide of 10g/L is obtained after constant volume
Change hydrogen standard solution S1.
30% hydrogen peroxide (analysis is pure) 3.3333g to 1000ml volumetric flasks are weighed, the peroxidating of 1g/L is obtained after constant volume
Hydrogen standard solution S2.
30% hydrogen peroxidase 10 .3333g to 1000ml volumetric flasks are weighed, the Hydrogen peroxide standard of 100mg/L is obtained after constant volume
Solution S 3.
(2) Hydrogen peroxide standard solution is configured
S1 standard solution storing solution 1ml, 2ml, 3ml, 4ml, 5ml to five 1000ml volumetric flasks are taken respectively, after constant volume
To standard solution A1, B1, C1, D1, F1, corresponding concentration is respectively the mistake of 10mg/L, 20mg/L, 30mg/L, 40mg/L, 50mg/L
Hydrogen oxide standard solution.
S2 standard solution storing solution 1ml, 3ml, 5ml, 7ml, 10ml to five 1000ml volumetric flasks are taken respectively, after constant volume
To standard solution A2, B2, C2, D2, F2, corresponding concentration is respectively the peroxidating of 1mg/L, 3mg/L, 5mg/L, 7mg/L, 1mg/L
Hydrogen standard solution.
S3 standard solution storing solution 0.03ml, 1ml, 3ml, 5ml, 7ml, 10ml to five 1000ml volumetric flasks are taken respectively,
Obtain standard solution A3, B3, C3, D3, F3, G3 after constant volume, corresponding concentration be respectively 0.03mg/L, 0.1mg/L, 0.3mg/L,
The Hydrogen peroxide standard solution of 0.5mg/L, 0.7mg/L, 1mg/L.
(3) Specification Curve of Increasing
By the ion chromatography of standard solution A1, B1, C1, D1, F1 above-mentioned condition-UV detector technology analysis, record
Peak area of the sample in UV detector；Concentration-peak area standard curve is drawn, the mistake that concentration range is 10-50mg/L is obtained
The regression equation of the standard curve of hydrogen oxide.
By the ion chromatography of standard solution A2, B2, C2, D2, F2 above-mentioned condition, record sample is in UV detector
Peak area；Concentration-peak area standard curve is drawn, the standard curve for the hydrogen peroxide that concentration range is 1-10mg/L is obtained
Regression equation.
By the ion chromatography of standard solution A3, B3, C3, D3, F3, G3 above-mentioned condition, record sample is in ultraviolet inspection
Survey the peak area of device；Concentration-peak height standard curve is drawn, the standard for obtaining the hydrogen peroxide that concentration range is 0.1-1mg/L is bent
The regression equation of line.
| Concentration range (mg/L) | Slope | Intercept | R2 |
| 0.03--1 | 37065±425 | 1334±67 | 0.9952 |
| 1--10 | 41610±268 | 8070±659 | 0.9996 |
| 10--50 | 45598±329 | 29428±4508 | 0.9998 |
(4) concentration of hydrogen peroxide in water sample is tested
Prepare the mistake of 20mg/L, 2mg/L, 0.2mg/L concentration respectively with hydrogen peroxide standard solution storing solution S1, S2, S3
Hydrogen oxide water sample with above-mentioned ion chromatography condition analysis, and brings the regression equation of peak area standard curve into respectively, calculates water sample
The concentration of middle hydrogen peroxide.Each water sample measures five times.
| Theoretical concentration (mg/L) | Peak area | Actual concentrations | Mean value | Accuracy | Relative standard deviation | Accuracy % |
| 20 | 832806 | 19.66502 | 19.94536 | 0.139637 | 0.007001 | 99.72 |
| 2 | 73241 | 1.943857 | 1.957363 | 0.036205 | 0.018497 | 97.86 |
| 0.2 | 5331 | 0.175048 | 0.181168 | 0.009758 | 0.053862 | 90.58 |
Embodiment 2
Used ion chromatography condition is identical as 1 conditional of embodiment.
Specification Curve of Increasing process is identical with embodiment 1.
Different time rainwater sample R1, R2 are collected, with 0.45 μm of membrane filtration.With the standard solution configured in embodiment 1
Rainwater solution R11, R12, R21 of hydrogen peroxide external standard is added in S2 and the configuration of rainwater sample.Wherein R11 is in rainwater sample R1
In be added to the sample of 0.5mg/L hydrogen peroxide, wherein R12 is the sample that 1mg/L hydrogen peroxide is added in rainwater sample R1
Product, wherein R21 are the sample for adding 1mg/L hydrogen peroxide again in rainwater sample R2.
The content of hydrogen peroxide in R1, R2, R11, R12, R21 is measured with ion chromatography respectively.
The results are shown in Figure 4.It is carried out pair with the method that the method for the present invention measures hydrogen peroxide with Hash company of the U.S. in Fig. 4
Than measuring R1, R2, R11, R12, R21 this 5 kinds of water samples respectively, and compare to result.Hash company is surveyed with spectrophotometry
The method for measuring hydrogen peroxide in water sample, method number LIT2214, concrete operation step are：10ml water samples are taken to add 3 drop, 20% iodate
Potassium solution and 3 drop ammonium molybdate solutions, shake up；A DPD reagent packet is added after 6 minutes in reaction；Using ultraviolet specrophotometer,
530nm reads the absorbance of sample.Before measurement, configuration standard solution obtains standard song by drawing the standard curve of this method
Line.When measuring water sample, by measuring water sample in the absorbance of 530nm, it is updated in standard curve, mistake in sample is calculated
Aoxidize hydrogen content.As a result show that the data that two methods are obtained are almost consistent.
Embodiment 3
Used ion chromatography condition is：Ion chromatograph is that Tosoh company IC2010 guard columns are Dai An companies AG-
15；Analytical column is Dai An companies AS-15 chromatographic columns, Tosoh company AZ chromatographic columns；Chromatographic column column oven temperature is 30 degrees Celsius；Suppression
Device processed is to contain vast electrochemical membrane suppressor SHY-A- III；Detector is Shimadzu SPD 20A UV detector, UV detector choosing
It is 200-230nm with wavelength；Two kinds of leacheates, one kind are a concentration of 10mmol/L sodium hydroxides leacheate, and another kind is
The mixing leacheate of 1.9mmol/L sodium bicarbonates and 3.2mmol/L sodium carbonate；Sample injection volume is 100 μ L.
(1) select leacheate for 10mmol/L sodium hydroxide leacheates, it is 210nm, flow velocity that UV detector, which selects wavelength,
When 0.5ml/min, respectively use AS-15 chromatographic columns and AZ chromatographic columns, test the hydrogen peroxide containing 50mg/L water sample, as a result as Fig. 5,
Shown in Fig. 6.
(2) select leacheate for the mixing leacheate of 1.9mmol/L sodium bicarbonates and 3.2mmol/L sodium carbonate, flow velocity
When 0.5ml/min, AZ chromatographic columns test the water sample of the hydrogen peroxide containing 50mg/L, and the results are shown in Figure 7.
(3) select leacheate for 10mmol/L sodium hydroxide leacheates, it is 200-230nm that UV detector, which selects wavelength,
When flow velocity 0.5ml/min, AS-15 chromatographic columns are used respectively, test the water sample of the hydrogen peroxide containing 50mg/L, the results are shown in Figure 8
Bibliography
1. father-in-law builds, Wang Zhenbing.The detection method China of hydrogen peroxide, 201310154581.X [P] in a kind of water sample
.2013.04.27。
2. wangkai is male, Xu Lijun, Yao Ming, Zhu Yan.Ion chromatograph flow injection Means of Electrical Conductivity hydrogen peroxide [J] points
Analysis chemistry, 2003,31 (5):555-558.
Claims (8)
1. the detection method of hydrogen peroxide, includes the following steps in a kind of water sample：
(1) operating condition for setting ion chromatograph ensures that the water sample containing hydrogen peroxide is when by ion chromatography column
Ionic condition, and be fully converted back into as molecular state after by suppressor；
(2) configure hydrogen peroxide Standard Stock solutions, be reconfigured Hydrogen peroxide standard solution, using ion chromatography chromatograph into
Row separation and detection, the peak area or peak heights of the ultraviolet detector response of record standard solution；Hydrogen peroxide is drawn with external standard method
Concentration ----peak area or concentration --- peak heights standard curve, to obtain peroxide standard curve regression equation；
(3) take water sample to be measured, analyzed with ion chromatograph, record the sample UV detector peak area or peak height
Degree obtains the content of hydrogen peroxide in water sample according to standard curve regression equation calculation obtained by step (1).
2. method according to claim 1, wherein the ion chromatograph operating condition, including ion chromatographic column, column oven,
The setting of suppressor, UV detector, leacheate etc..
3. according to claim 1,2 the methods, which is characterized in that the suppressor is electrochemical membrane suppressor.
4. according to claim 1,2 the methods, which is characterized in that the column oven temperature is 20-40 degrees Celsius.
5. according to claim 1,2 the methods, which is characterized in that the leacheate need to ensure that the pH value of leacheate is more than room temperature
The acid ionization constant of hydrogen peroxide under normal pressure, the i.e. pH value of leacheate are greater than 11.6.
6. according to the method described in claim 5, it is characterized in that, the leacheate can select potassium hydroxide leacheate, hydrogen
The mixing leacheate etc. of sodium oxide molybdena leacheate or sodium bicarbonate and sodium carbonate.
7. according to the method described in claim 1,2, which is characterized in that it is 200-230nm that the UV detector, which selects wavelength,.
8. according to the detection method of hydrogen peroxide in a kind of water sample according to claim 1 described in claim 1 to 7,
It is characterized in that, the concentration range that can measure hydrogen peroxide in water sample is 0.03mg/L-50mg/L.It, can if sample concentration is excessively high
It is measured by diluting.
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| CN201810223672.7A CN108414670A (en) | 2018-03-19 | 2018-03-19 | The detection method of hydrogen peroxide in a kind of water sample |
| PCT/CN2018/000170 WO2019178710A1 (en) | 2018-03-19 | 2018-05-09 | Method for detecting hydrogen peroxide in water sample |
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| CN201810223672.7A CN108414670A (en) | 2018-03-19 | 2018-03-19 | The detection method of hydrogen peroxide in a kind of water sample |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115636396A (en) * | 2022-10-18 | 2023-01-24 | 厦门大学 | Hydrogen peroxide generation method |
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| US20230060851A1 (en) * | 2021-09-01 | 2023-03-02 | Cardioquip, Llc | System and method for in-line optical sensing of hydrogen peroxide |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103234933B (en) * | 2013-04-27 | 2014-12-24 | 厦门大学 | Detection method of hydrogen peroxide in water sample |
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- 2018-05-09 WO PCT/CN2018/000170 patent/WO2019178710A1/en active Application Filing
Non-Patent Citations (3)
| Title |
|---|
| MINGRUI SONG 等: "A Facile, Nonreactive Hydrogen Peroxide (H2O2) Detection Method Enabled by Ion Chromatography with UV Detector", 《ANALYTICAL CHEMISTRY》 * |
| 牟世芬 刘克纳: "《离子色谱方法及应用》", 30 September 2000, 化学工业出版社 * |
| 谢协忠 主编: "《水分析化学 第2版》", 28 February 2014, 中国电力出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115636396A (en) * | 2022-10-18 | 2023-01-24 | 厦门大学 | Hydrogen peroxide generation method |
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Application publication date: 20180817 |