CN109187399A - A kind of method of Peracetic acid and content of hydrogen peroxide in quick measurement solution - Google Patents
A kind of method of Peracetic acid and content of hydrogen peroxide in quick measurement solution Download PDFInfo
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- CN109187399A CN109187399A CN201810813047.8A CN201810813047A CN109187399A CN 109187399 A CN109187399 A CN 109187399A CN 201810813047 A CN201810813047 A CN 201810813047A CN 109187399 A CN109187399 A CN 109187399A
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- peracetic acid
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- KFSLWBXXFJQRDL-UHFFFAOYSA-N Peracetic acid Chemical compound CC(=O)OO KFSLWBXXFJQRDL-UHFFFAOYSA-N 0.000 title claims abstract description 253
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 title claims abstract description 122
- 238000000034 method Methods 0.000 title claims abstract description 35
- 238000005259 measurement Methods 0.000 title claims description 35
- 239000000243 solution Substances 0.000 claims abstract description 51
- 238000002835 absorbance Methods 0.000 claims abstract description 33
- 238000006243 chemical reaction Methods 0.000 claims abstract description 25
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 claims abstract description 24
- 239000011609 ammonium molybdate Substances 0.000 claims abstract description 15
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims abstract description 15
- 229940010552 ammonium molybdate Drugs 0.000 claims abstract description 15
- 235000018660 ammonium molybdate Nutrition 0.000 claims abstract description 15
- 238000012417 linear regression Methods 0.000 claims abstract description 13
- 239000011259 mixed solution Substances 0.000 claims description 91
- 238000010521 absorption reaction Methods 0.000 claims description 28
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims description 16
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 14
- 238000004519 manufacturing process Methods 0.000 claims description 8
- 239000008363 phosphate buffer Substances 0.000 claims description 8
- 238000012360 testing method Methods 0.000 claims description 7
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 7
- 239000012498 ultrapure water Substances 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims description 4
- 229910052740 iodine Inorganic materials 0.000 claims description 4
- 239000011630 iodine Substances 0.000 claims description 4
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 229910052700 potassium Inorganic materials 0.000 claims description 3
- 239000011591 potassium Substances 0.000 claims description 3
- 238000001514 detection method Methods 0.000 abstract description 6
- 230000007613 environmental effect Effects 0.000 abstract description 5
- 239000002253 acid Substances 0.000 abstract description 4
- 235000013305 food Nutrition 0.000 abstract description 4
- 239000003054 catalyst Substances 0.000 abstract description 3
- 239000012086 standard solution Substances 0.000 abstract 2
- 238000011410 subtraction method Methods 0.000 abstract 1
- 229960002163 hydrogen peroxide Drugs 0.000 description 37
- 238000004448 titration Methods 0.000 description 8
- 239000003153 chemical reaction reagent Substances 0.000 description 7
- 239000001257 hydrogen Substances 0.000 description 7
- 229910052739 hydrogen Inorganic materials 0.000 description 7
- XMBWDFGMSWQBCA-UHFFFAOYSA-M iodide Chemical compound [I-] XMBWDFGMSWQBCA-UHFFFAOYSA-M 0.000 description 7
- 229940006461 iodide ion Drugs 0.000 description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 6
- 238000007254 oxidation reaction Methods 0.000 description 6
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 238000004737 colorimetric analysis Methods 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 3
- 150000002978 peroxides Chemical class 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 230000035945 sensitivity Effects 0.000 description 3
- 230000008033 biological extinction Effects 0.000 description 2
- 238000004061 bleaching Methods 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 238000004128 high performance liquid chromatography Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000002798 spectrophotometry method Methods 0.000 description 2
- 238000004659 sterilization and disinfection Methods 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 206010064571 Gene mutation Diseases 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 238000005273 aeration Methods 0.000 description 1
- 239000003899 bactericide agent Substances 0.000 description 1
- 239000007844 bleaching agent Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 239000000645 desinfectant Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005672 electromagnetic field Effects 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002795 fluorescence method Methods 0.000 description 1
- -1 has titration Chemical compound 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- ICIWUVCWSCSTAQ-UHFFFAOYSA-M iodate Chemical compound [O-]I(=O)=O ICIWUVCWSCSTAQ-UHFFFAOYSA-M 0.000 description 1
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 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
- VLAPMBHFAWRUQP-UHFFFAOYSA-L molybdic acid Chemical compound O[Mo](O)(=O)=O VLAPMBHFAWRUQP-UHFFFAOYSA-L 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 229910000403 monosodium phosphate Inorganic materials 0.000 description 1
- 210000004400 mucous membrane Anatomy 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 238000005375 photometry Methods 0.000 description 1
- JLKDVMWYMMLWTI-UHFFFAOYSA-M potassium iodate Chemical compound [K+].[O-]I(=O)=O JLKDVMWYMMLWTI-UHFFFAOYSA-M 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 210000002345 respiratory system Anatomy 0.000 description 1
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
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- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Plasma & Fusion (AREA)
- Engineering & Computer Science (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
Abstract
本发明公开了一种快速测定溶液中过氧乙酸和过氧化氢含量的方法，以钼酸铵为催化剂，以碘化钾为指示剂测定标准溶液中过氧乙酸与过氧化氢总浓度，以碘化钾为指示剂测定标准溶液中过氧乙酸浓度，分别拟合得到过氧乙酸与过氧化氢总浓度以及过氧乙酸浓度相对于各自吸光度值的标准曲线和线性回归方程，通过检测待测样品在相同条件下反应后的吸光度值即可算出待测样品中过氧乙酸与过氧化氢总含量和过氧乙酸含量，再通过差减法得出待测样品中过氧化氢含量，是一种操作简便、准确灵敏、绿色环保、经济实用的方法，可广泛用于环保、食品及医疗行业，对各种经过氧乙酸溶液氧化、漂白或消毒的样品中过氧乙酸和过氧化氢残余量进行快速而准确的检测。The invention discloses a method for rapidly determining the content of peracetic acid and hydrogen peroxide in a solution. Ammonium molybdate is used as a catalyst, potassium iodide is used as an indicator to measure the total concentration of peracetic acid and hydrogen peroxide in a standard solution, and potassium iodide is used as an indicator. The indicator measures the concentration of peracetic acid in the standard solution, and obtains the standard curve and linear regression equation of the total concentration of peracetic acid and hydrogen peroxide and the concentration of peracetic acid relative to their respective absorbance values by fitting respectively. The total content of peracetic acid and hydrogen peroxide and the content of peracetic acid in the sample to be tested can be calculated by lowering the absorbance value after the reaction, and then the content of hydrogen peroxide in the sample to be tested can be obtained by the subtraction method, which is a simple and accurate method. A sensitive, green, economical and practical method that can be widely used in the environmental protection, food and medical industries to quickly and accurately determine the residual peracetic acid and hydrogen peroxide in various samples that have been oxidized, bleached or sterilized by oxyacetic acid solutions. detection.
Description
Technical field
The invention belongs to peroxide detection technique fields, and in particular to a kind of quickly to measure Peracetic acid and mistake in solution
The method for aoxidizing hydrogen content quickly measures Peracetic acid and concentration of hydrogen peroxide in solution using potassium iodide as indicator.
Background technique
Peracetic acid has stronger oxidability, and reaction product is environmentally friendly, therefore Peracetic acid is in environmental protection, food
In product, medical treatment and dyeing, it is widely used as oxidant, disinfectant, bactericidal agent and bleaching agent.However Peracetic acid
With very strong corrosivity and certain toxicity, there is intense stimulus effect to eyes, skin, mucous membrane and the upper respiratory tract, in addition, people
Remaining Peracetic acid also results in human genetic material damage and gene mutation in body.Therefore, in peracetic acid soln
In use process, the monitoring of the variation of its residual volume is particularly important.Commercial peracetic acid soln is mostly by peroxidating
Hydrogen and acetic acid are made under conditions of strong acid is as catalyst, therefore usually contain hydrogenperoxide steam generator in peracetic acid soln, this
Many inconvenience are produced to the concentration of direct measurement peracetic acid soln.
Currently, the measuring method of content of hydrogen peroxide mainly has titration, chemoluminescence method, fluorescence method, infra-red method, divides
Light photometry, test paper colorimetric method, high performance liquid chromatography etc..Mainly there are iodimetric titration, permanganimetric method, cerimetry in titration
The accurate, high sensitivity Deng, titration measuring result, but there is also complicated for operation, disturbing factor is more, expends the deficiencies of of long duration；
Permanganimetric method result is accurate, but complicated for operation, is easily affected by other factors.Chemoluminescence method has high sensitivity, detection
The advantages that low, measurement result is accurate is limited, but equally exists the shortcomings such as minute length, cost of determination height.Test paper colorimetric method
Have many advantages, such as that easy to operate, finding speed is fast, such as patent ZL 201220408884.0 and ZL 87106131.7, but there is also
In place of the deficiencies of test paper preparation cost is higher, measurement result accuracy is poor.High performance liquid chromatography has high sensitivity, detection
The advantages that low, measurement result is accurate is limited, but detects instrument valuableness, leads to testing cost height.Spectrophotometry, which has, to be surveyed
Determine that result is reliable, finding speed is fast, operation relative ease, the instrument used is less expensive, i.e. the low advantage of testing cost, but mesh
It is preceding not have a kind of technology using peroxide and hydrogen peroxide in SIMULTANEOUS DETERMINATION solution.
Summary of the invention
The present invention in order to solve cumbersome, measurement result error complicated for operation existing for existing determining peroxy-acetic acid method it is big,
The problems such as minute is long, cost of determination is high and cannot measure Peracetic acid and concentration of hydrogen peroxide simultaneously, proposes one
Kind is easy, accurately and quickly measures the spectrophotometry of Peracetic acid and content of hydrogen peroxide in solution.
The technical solution adopted by the present invention to solve the technical problems is:
A kind of method of Peracetic acid and content of hydrogen peroxide in measurement solution, comprising:
Step 1: production Peracetic acid and hydrogen peroxide total concentration standard curve: by sulfuric acid solution, ammonium molybdate solution and
Excessive liquor kalii iodide, which is added in ultrapure water, forms mixed solution A 1, measures suction of the mixed solution A 1 at specific absorption wavelength
Shading value, and school zero；The Peracetic acid standard sample of same volume V1 various concentration gradient is added into a series of mixed solution As 1
Product obtain a series of mixed solution B1；After 1 color stability of solution B to be mixed, mixed solution B1 is measured in the specific absorption wave
The absorbance value of strong point, is denoted as a1；Using a1 as ordinate, with the total concentration of Peracetic acid and hydrogen peroxide in mixed solution B1
For abscissa, standard curve and its equation of linear regression are established；Wherein, in the mixed solution B1, the concentration of ammonium molybdate is not low
In 97.2 μm of ol L-1, the concentration of potassium iodide is not less than 96mmol L-1；
Step 2: it makes the standard curve of peroxyacetic acid concentration: phosphate buffer and excessive liquor kalii iodide is added
Mixed solution A 2 is formed in ultrapure water, measures absorbance value of the mixed solution A 2 at specific absorption wavelength, and school zero；To a system
The Peracetic acid standard sample of same volume V2 various concentration gradient is added in column mixed solution A 2, obtains a series of mixed solutions
B2；After 2 color stability of solution B to be mixed, absorbance value of the mixed solution B2 at the specific absorption wavelength is measured, is denoted as
a2；Using a2 as ordinate, using the peroxyacetic acid concentration in mixed solution B2 as abscissa, standard curve and its linear is established
Regression equation；Wherein, the phosphate buffer density is 0.2~0.6mol L-1, pH value is 5.0~6.0；The mixed solution
In B2, the concentration of potassium iodide is not less than 48mmol L-1；
Step 3: Peracetic acid and hydrogen peroxide total content in measurement sample to be tested: production and mixed solution in step 1
The identical mixed solution C 1 of A1 measures absorbance value of the mixed solution C 1 at specific absorption wavelength, and school zero；To mixing
The Peracetic acid sample to be tested of V1 volume is added in solution C 1, obtains mixed solution D1；After 1 color stability of solution D to be mixed,
Absorbance value of the mixed solution D1 at the specific absorption wavelength is measured, b1 is denoted as；B1 value is substituted into linear obtained by step 1
In regression equation, the total concentration of Peracetic acid and hydrogen peroxide in mixed solution D1 is calculated, further according to the Peracetic acid of addition
Peracetic acid and peroxidating in sample to be tested is calculated in relationship between sample to be tested volume V1 and mixed solution D1 total volume
The total concentration of hydrogen；
Step 4: Peracetic acid content in sample to be tested: production with mixed solution A 2 is identical in step 2 mixes
Solution C 2 measures absorbance value of the mixed solution C 2 at specific absorption wavelength, and school zero；V2 body is added into mixed solution C 2
Long-pending Peracetic acid sample to be tested, obtains mixed solution D2；After 2 color stability of solution D to be mixed, mixed solution D2 is measured in institute
The absorbance value at specific absorption wavelength is stated, b2 is denoted as；B2 value is updated in equation of linear regression obtained by step 2, is calculated
The concentration of Peracetic acid in mixed solution D2, it is overall further according to the Peracetic acid sample to be tested volume V2 and mixed solution D2 of addition
The concentration of Peracetic acid in sample to be tested is calculated in relationship between product.
In one embodiment: in the step 1, a series of quantity n >=5 of mixed solution As 1.
In one embodiment: in the step 1, Peracetic acid and hydrogen peroxide in a series of obtained mixed solution B1
Total concentration is respectively 0,9~11,19~21,29~31,49~51,69~71 μm of ol L-1。
In one embodiment: in the step 1, the sulfuric acid solution concentration used is 1.88~6.26mol L-1, ammonium molybdate is molten
Liquid concentration is 20~30mmol L-1, liquor kalii iodide concentration is 0.5~1.0mol L-1。
In one embodiment: in the step 2, a series of quantity n >=5 of mixed solution As 2.
In one embodiment: in the step 2, the concentration of Peracetic acid is respectively in a series of obtained mixed solution B2
0,9~11,19~21,29~31,39~41,49~51,59~61,69~71 μm of ol L-1。
In one embodiment: in the step 2, the concentration of the liquor kalii iodide used is 0.5~1.0mol L-1。
In one embodiment: in the step 1, the color stability time is 1~3 minute, and reaction temperature is 5~25 DEG C.
In one embodiment: in the step 2, the color stability time is 0.25~1.5 minute, and reaction temperature is 5~25
℃。
In one embodiment: the range of the specific absorption wavelength is 325~425nm.
The technical program compared with the background art, it has the following advantages:
The present invention quickly aoxidizes the I that iodide ion generates brown using ammonium molybdate catalysis Peracetic acid and hydrogen peroxide- 3, according to
The I of generation- 3Absorbance value at specific absorption wavelength calculates the total concentration of Peracetic acid and hydrogen peroxide in solution；It utilizes
In the case where the catalysis of no ammonium molybdate, the speed of Peracetic acid oxidation iodide ion is far longer than hydrogen peroxide oxidation iodide ion
The characteristic of speed, Peracetic acid quickly aoxidize the I that iodide ion generates brown- 3, further according to the I for generating brown- 3, in specific absorption
Absorbance value at wavelength calculates the concentration of Peracetic acid in solution；The dense of hydrogen peroxide in solution is obtained further according to minusing
Degree.
The present invention has volume of water sample and pharmacy response dosage compared with national standard (GB 19104-2008) described titration
Less, (without cumbersome titration operation) easy to operate, the advantages that finding speed is fast；Compared with chemoluminescence method and chromatography, tool
Have the advantages that cost of determination low (without using expensive chemiluminescence medicament and chromatograph), finding speed are fast；With test paper colorimetric
Method is compared, and has the advantages that measurement result is accurate, minimum detection limit is low etc..
In addition, the present invention does not need expensive instrument and equipment and reagent, it is only necessary to a common ultraviolet-uisible spectrophotometer
Measurement can be met to require, cost of determination is greatly reduced, be conducive to popularization and application of the invention.The method of the present invention can be used extensively
In environmental protection, food and medical industry, to Peracetic acid and mistake in the sample of the oxidation of various peracetic acid solns, bleaching or disinfection
Hydrogen oxide residual volume carries out quick, easy and accurate detection.
Detailed description of the invention
Present invention will be further explained below with reference to the attached drawings and examples.
Fig. 1 is the canonical plotting of Peracetic acid and hydrogen peroxide total concentration that the embodiment of the present invention obtains.
Fig. 2 is the canonical plotting for the peroxyacetic acid concentration that the embodiment of the present invention obtains.
Specific embodiment
The contents of the present invention are illustrated below by embodiment:
Embodiment:
The method that one kind of the present embodiment quickly measures Peracetic acid and content of hydrogen peroxide in solution, it is by following step
It is rapid to carry out:
Step 1: production measurement Peracetic acid and hydrogen peroxide total concentration standard curve:
1, the sulfuric acid solution of 0.05mL, the ammonium molybdate solution of 0.01mL and 0.4mL liquor kalii iodide are added to ultrapure water
In, mixed solution A 1 is obtained, absorbance value of the mixed solution A 1 at specific absorption wavelength, and school zero are measured；Among the present embodiment,
Specific absorption wavelength is 350nm；
2, the peracetic acid soln standard of same volume (V1=0.1mL) various concentration gradient is added into mixed solution A 1
Sample obtains a series of mixed solution B1, total reaction volume 2.5mL；
3,5~25 DEG C reaction 1~3 minute after, oxidative color-developing stablize, measurement reaction after mixed solution B1 in specific absorption wave
The absorbance value of strong point, is denoted as a1；
4, using a1 as ordinate, using Peracetic acid in mixed solution B1 and the total concentration of hydrogen peroxide as abscissa,
Establish standard curve and its equation of linear regression.
Illustrate:
Wherein, used reagent: ammonium molybdate solution concentration is 24.3mmol L-1(in overall reaction system ammonium molybdate
Concentration is 97.2 μm of ol L-1Or more when, absorbance value is almost unchanged, i.e., does not influence absorbance；Molybdic acid in overall reaction system
Ammonium concentration is 97.2 μm of ol L-1When the corresponding ammonium molybdate solution volume being added be 0.01mL)；The dense sulphur that sulfuric acid solution is 98%
Acid is formed according to the volume ratio of water for the dilution proportion of 1:2~1:9, is diluted among the present embodiment according to 1:9, concentration is
1.88mol L-1, 0.05mL is added, strong acid condition needed for guaranteeing reaction；The concentration of liquor kalii iodide is 0.6mol L-1(
The concentration of potassium iodide is 96mmol L in overall reaction system-1Or more when, absorbance value is almost unchanged, i.e., does not influence extinction
Degree；Iodate potassium concn is 96mmol L in overall reaction system-1When the corresponding liquor kalii iodide volume being added be 0.4mL).
Used peracetic acid soln standard sample, to be purchased from the Yunnan Industry Development Area Yang Lin Shan Dian pharmaceutcal corporation, Ltd
The Peracetic acid reagent containing certain hydrogen peroxide that Peracetic acid A, the B stoste bought is prepared passes through national standard (GB first
Titration in 19104-2008) determines Peracetic acid, the concentration of hydrogen peroxide in Peracetic acid reagent, and (titration 3 times, makes even
Mean value), and using this concentration as normal concentration, which is prepared to obtain used peracetic acid soln
Standard sample, similarly hereinafter.
The various concentration gradient refer in mixed solution B1 Peracetic acid and the total concentration of hydrogen peroxide be respectively 0,
10、20、 30、50、70μmol L-1。
Step 2: peroxyacetic acid concentration standard curve in production measurement peracetic acid soln:
1, the phosphate buffer of 0.05mL, 0.2mL liquor kalii iodide are added into ultrapure water, obtain mixed solution A 2, surveyed
Determine absorbance value of the mixed solution A 2 at specific absorption wavelength, and school zero；Among the present embodiment, specific absorption wavelength is
350nm；
2, the peracetic acid soln standard of same volume (V2=0.2mL) various concentration gradient is added into mixed solution A 2
Sample obtains a series of mixed solution B2, total reaction volume 2.5mL；
3,5~25 DEG C reaction 0.25~1.5 minute after, oxidative color-developing stablize, measurement reaction after mixed solution B2 specific
Absorbance value at absorbing wavelength, is denoted as a2；
4, using a2 as ordinate, using peroxyacetic acid concentration in mixed solution B2 as abscissa, establish standard curve and
Its equation of linear regression.
Illustrate:
Wherein, used reagent: phosphate buffer density is 0.5mol L-1, pH 5.5, the preparation of phosphate buffer
Method are as follows: prepare 0.5mol L respectively first-1Disodium hydrogen phosphate and 0.5mol L-1Sodium dihydrogen phosphate, then by two kinds
Reagent mixing adjusts pH=5.5 using pH meter；The concentration of liquor kalii iodide is 0.6mol L-1(in overall reaction system iodine
The concentration for changing potassium is 48mmol L-1Or more when, absorbance value is almost unchanged, i.e., does not influence absorbance；In overall reaction system
Iodate potassium concn is 48mmol L-1When the corresponding liquor kalii iodide volume being added be 0.2mL).
The various concentration gradient refer to the concentration of Peracetic acid in mixed solution B2 be respectively 0,10,20,30,40,
50、 60、70μmol L-1。
Step 3: Peracetic acid, content of hydrogen peroxide in measurement sample:
1, the sulfuric acid solution of 0.05mL, the ammonium molybdate solution of 0.01mL and 0.4mL liquor kalii iodide are added to ultrapure water
In, mixed solution C 1 is obtained, absorbance value of the mixed solution C 1 at specific absorption wavelength, and school zero are measured；
2, sample to be tested (known Peracetic acid and the peroxidating of V1 volume (V1=0.1mL) are added into mixed solution C 1
Hydrogen total concentration is 1250 μm of ol L-1, peroxyacetic acid concentration be 525 μm of ol L-1Peracetic acid soln), mixed solution D1 is formed,
Total reaction volume is 2.5mL, after color stability, absorbance of the mixed solution D1 at specific absorption wavelength after measurement reaction
Value, is denoted as b1；
3, b1 value is substituted into equation of linear regression obtained by step 1, calculates Peracetic acid and peroxide in mixed solution D1
The total concentration for changing hydrogen, further according to the relationship between the Peracetic acid sample to be tested volume (V1) and mixed solution D1 total volume of addition
The total concentration of Peracetic acid and hydrogen peroxide in sample to be tested is calculated.
4, the phosphate buffer of 0.05mL and excessive liquor kalii iodide are added into ultrapure water, obtain mixed solution C 2,
Measure absorbance value of the mixed solution C 2 at specific absorption wavelength, and school zero；
5, sample to be tested (known Peracetic acid and the peroxidating of V2 volume (V2=0.2mL) are added into mixed solution C 2
Hydrogen total concentration is 1250 μm of ol L-1, peroxyacetic acid concentration be 525 μm of ol L-1Peracetic acid soln), formed mixed solution
D2, total reaction volume 2.5mL, after color stability, extinction of the mixed solution D2 at specific absorption wavelength after measurement reaction
Angle value is denoted as b2；
6, b2 value is updated in equation of linear regression obtained by step 2, calculates the dense of Peracetic acid in mixed solution D2
Degree, further according to the relationship between the Peracetic acid sample to be tested volume (V2) and mixed solution D2 total volume of addition be calculated to
The concentration of Peracetic acid in sample.
7, concentration of hydrogen peroxide=Peracetic acid and hydrogen peroxide total concentration-peroxyacetic acid concentration in sample to be tested.
The standard curve of the resulting Peracetic acid of the present embodiment and the total concentration of hydrogen peroxide is as shown in Figure 1, gained is linear
Regression formula is as follows:
Therefore, Peracetic acid and the total concentration calculation formula of hydrogen peroxide are as follows in water sample:
[Peracetic acid+hydrogen peroxide]Sample=VAlways÷VSample× [Peracetic acid+hydrogen peroxide]Reaction
=2.5 0.1 × (A of ÷350÷0.02507)
The A that the present embodiment measures350It is 1.268, substitutes into above-mentioned formula and Peracetic acid and peroxidating in water sample is calculated
Hydrogen total concentration is 1264.46 μm of ol L-1, measurement deviation 1.14% illustrates that this measuring method is accurate and reliable.
The standard curve of the concentration of the resulting hydrogen peroxide of the present embodiment is as shown in Fig. 2, gained linear regression formula is as follows:
Therefore, the concentration calculation formula of Peracetic acid is as follows in water sample:
[Peracetic acid]Sample=VAlways÷VSample× [Peracetic acid]Reaction
=2.5 0.2 × (A of ÷350÷0.02501)
The A that the present embodiment measures350It is 1.069, peroxyacetic acid concentration in water sample, which is calculated, in substitution above-mentioned formula is
534.29 μmol L-1, measurement deviation 1.74% illustrates that this measuring method is accurate and reliable.
[hydrogen peroxide]Sample=[Peracetic acid+hydrogen peroxide]Sample[Peracetic acid]Sample=1264.46-534.29=
730.17μmol L-1, measurement deviation 0.7% illustrates that this measuring method is accurate and reliable.
The present embodiment generates elemental iodine, iodine using ammonium molybdate catalysis Peracetic acid and hydrogen peroxide and potassium iodide fast reaction
Simple substance generates I with excessive iodide ion again- 3, then its absorbance value is measured under specific wavelength；And surveying peroxyacetic acid concentration
When, using under conditions of no catalyst, the speed of Peracetic acid oxidation iodide ion be far longer than hydrogen peroxide oxidation iodine from
The characteristic of the speed of son, Peracetic acid quickly aoxidize the I that iodide ion generates brown- 3, further according to the I for generating brown- 3, specific
Absorbance value at absorbing wavelength calculates the concentration of Peracetic acid in solution.Method is simple and easy, does not need additionally to carry out again
Ultraviolet irradiation, microwave irradiation, electron beam irradiation, ultrasonic cavitation, aeration, additional electromagnetic field and heating, minute is short, measurement knot
Fruit error is small, does not also need expensive instrument and equipment and reagent, it is only necessary to the ultraviolet-uisible spectrophotometer of a relative low price
Measurement can be met to require, reduce cost of determination.Measuring method can be widely used in environmental protection, food and medical industry, to each
Peracetic acid, content of hydrogen peroxide carry out quick, environmental protection, effectively detect in sample of the kind through oxidation, bleaching or disinfection.
The above is only the preferred embodiment of the present invention, the range implemented of the present invention that therefore, it cannot be limited according to, i.e., according to
Equivalent changes and modifications made by the invention patent range and description, should still be within the scope of the present invention.
Claims (10)
1. a kind of method of Peracetic acid and content of hydrogen peroxide in measurement solution, it is characterised in that: include:
Step 1: the standard curve of production Peracetic acid and hydrogen peroxide total concentration: by sulfuric acid solution, ammonium molybdate solution and excess
Liquor kalii iodide be added in ultrapure water and form mixed solution A 1, measure absorbance of the mixed solution A 1 at specific absorption wavelength
Value, and school zero；The Peracetic acid standard sample of same volume V1 various concentration gradient is added into a series of mixed solution As 1, obtains
To a series of mixed solution B1；After 1 color stability of solution B to be mixed, mixed solution B1 is measured at the specific absorption wavelength
Absorbance value, be denoted as a1；It is cross with Peracetic acid in mixed solution B1 and the total concentration of hydrogen peroxide using a1 as ordinate
Coordinate establishes standard curve and its equation of linear regression；Wherein, in the mixed solution B1, the concentration of ammonium molybdate is not less than
97.2μmol L-1, the concentration of potassium iodide is not less than 96mmol L-1；
Step 2: it makes the standard curve of peroxyacetic acid concentration: phosphate buffer and excessive liquor kalii iodide being added ultrapure
Mixed solution A 2 is formed in water, measures absorbance value of the mixed solution A 2 at specific absorption wavelength, and school zero；It is mixed to a series of
The Peracetic acid standard sample that same volume V2 various concentration gradient is added in solution A 2 is closed, a series of mixed solution B2 are obtained；
After 2 color stability of solution B to be mixed, absorbance value of the mixed solution B2 at the specific absorption wavelength is measured, a2 is denoted as；With
A2 establishes standard curve and its linear regression side using the peroxyacetic acid concentration in mixed solution B2 as abscissa as ordinate
Journey；Wherein, the phosphate buffer density is 0.2~0.6mol L-1, pH value is 5.0~6.0；In the mixed solution B2, iodine
The concentration for changing potassium is not less than 48mmol L-1；
Step 3: Peracetic acid and hydrogen peroxide total content in measurement sample to be tested: production is complete with mixed solution A 1 in step 1
Exactly the same mixed solution C 1 measures absorbance value of the mixed solution C 1 at specific absorption wavelength, and school zero；To mixed solution
The Peracetic acid sample to be tested of V1 volume is added in C1, obtains mixed solution D1；After 1 color stability of solution D to be mixed, measurement is mixed
Absorbance value of the solution D 1 at the specific absorption wavelength is closed, b1 is denoted as；B1 value is substituted into linear regression side obtained by step 1
Cheng Zhong calculates the total concentration of Peracetic acid and hydrogen peroxide in mixed solution D1, waits for test sample further according to the Peracetic acid of addition
The total of Peracetic acid and hydrogen peroxide in sample to be tested is calculated in relationship between product volume V1 and mixed solution D1 total volume
Concentration；
Step 4: Peracetic acid content in sample to be tested: production and the identical mixed solution of mixed solution A 2 in step 2
C2 measures absorbance value of the mixed solution C 2 at specific absorption wavelength, and school zero；V2 volume is added into mixed solution C 2
Peracetic acid sample to be tested obtains mixed solution D2；After 2 color stability of solution D to be mixed, mixed solution D2 is measured in the spy
Determine the absorbance value at absorbing wavelength, is denoted as b2；B2 value is updated in equation of linear regression obtained by step 2, mixing is calculated
The concentration of Peracetic acid in solution D 2, further according to addition Peracetic acid sample to be tested volume V2 and mixed solution D2 total volume it
Between relationship the concentration of Peracetic acid in sample to be tested is calculated.
2. the method for Peracetic acid and content of hydrogen peroxide in measurement solution according to claim 1, it is characterised in that: institute
It states in step 1, a series of quantity n >=5 of mixed solution As 1.
3. the method for Peracetic acid and content of hydrogen peroxide in measurement solution according to claim 1, it is characterised in that: institute
It states in step 1, Peracetic acid and the total concentration of hydrogen peroxide are respectively 0,9~11,19 in a series of obtained mixed solution B1
~21,29~31,49~51,69~71 μm of ol L-1。
4. the method for Peracetic acid and content of hydrogen peroxide in measurement solution according to claim 1, it is characterised in that: institute
It states in step 1, the sulfuric acid solution concentration used is 1.88~6.26mol L-1, ammonium molybdate solution concentration is 20~30mmol L-1, liquor kalii iodide concentration is 0.5~1.0mol L-1。
5. the method for Peracetic acid and content of hydrogen peroxide in measurement solution according to claim 1, it is characterised in that: institute
It states in step 2, a series of quantity n >=5 of mixed solution As 2.
6. the method for Peracetic acid and content of hydrogen peroxide in measurement solution according to claim 1, it is characterised in that: institute
State in step 2, in a series of obtained mixed solution B2 the concentration of Peracetic acid be respectively 0,9~11,19~21,29~31,
39~41,49~51,59~61,69~71 μm of ol L-1。
7. the method for Peracetic acid and content of hydrogen peroxide in measurement solution according to claim 1, it is characterised in that: institute
It states in step 2, the concentration of the liquor kalii iodide used is 0.5~1.0mol L-1。
8. the method for Peracetic acid and content of hydrogen peroxide in measurement solution according to claim 1, it is characterised in that: institute
It states in step 1, the color stability time is 1~3 minute, and reaction temperature is 5~25 DEG C.
9. the method for Peracetic acid and content of hydrogen peroxide in measurement solution according to claim 1, it is characterised in that: institute
It states in step 2, the color stability time is 0.25~1.5 minute, and reaction temperature is 5~25 DEG C.
10. the method for Peracetic acid and content of hydrogen peroxide in measurement solution according to claim 1, it is characterised in that:
The range of the specific absorption wavelength is 325~425nm.
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| CN110501330A (en) * | 2019-09-18 | 2019-11-26 | 四川轻化工大学 | Method for rapidly detecting content of hydrogen peroxide |
| CN111189980A (en) * | 2020-01-16 | 2020-05-22 | 郑州笨农农业科技有限公司 | Method for detecting and monitoring concentration of species of disinfectant |
| CN111380828A (en) * | 2020-04-28 | 2020-07-07 | 今麦郎饮品股份有限公司 | Method for detecting residual quantity of hydrogen peroxide in water |
| CN111504926A (en) * | 2020-05-19 | 2020-08-07 | 华中科技大学 | A kind of assay method of peracetic acid content |
| CN111678879A (en) * | 2020-01-05 | 2020-09-18 | 天津大学 | A kind of method that utilizes KI to measure peroxyformic acid and coexisting hydrogen peroxide in water sample |
| CN113218902A (en) * | 2021-05-10 | 2021-08-06 | 宁波万泽微测环境科技股份有限公司 | Online automatic monitoring method and device for residual concentration of hydrogen peroxide |
| CN113340834A (en) * | 2021-06-11 | 2021-09-03 | 成都市排水有限责任公司 | Method for rapidly determining content of sodium acetate in industrial-grade sodium acetate solution |
| CN113959822A (en) * | 2021-10-29 | 2022-01-21 | 珠海市丽拓生物科技股份有限公司 | Diluent and oxidant for determining urine iodine content by peroxyacetic acid oxidation method and application |
| CN116559342A (en) * | 2023-05-11 | 2023-08-08 | 天津大学 | A Kinetic Method for the Simultaneous Quantification of Peracetic Acid and Hydrogen Peroxide Concentrations |
| CN118303400A (en) * | 2024-03-21 | 2024-07-09 | 浙江医之友环境科技有限公司 | Preparation method of peroxyacetic acid disinfectant with concentration indication function |
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| CN110501330A (en) * | 2019-09-18 | 2019-11-26 | 四川轻化工大学 | Method for rapidly detecting content of hydrogen peroxide |
| CN111678879A (en) * | 2020-01-05 | 2020-09-18 | 天津大学 | A kind of method that utilizes KI to measure peroxyformic acid and coexisting hydrogen peroxide in water sample |
| CN111189980A (en) * | 2020-01-16 | 2020-05-22 | 郑州笨农农业科技有限公司 | Method for detecting and monitoring concentration of species of disinfectant |
| CN111380828A (en) * | 2020-04-28 | 2020-07-07 | 今麦郎饮品股份有限公司 | Method for detecting residual quantity of hydrogen peroxide in water |
| CN111504926A (en) * | 2020-05-19 | 2020-08-07 | 华中科技大学 | A kind of assay method of peracetic acid content |
| CN113218902A (en) * | 2021-05-10 | 2021-08-06 | 宁波万泽微测环境科技股份有限公司 | Online automatic monitoring method and device for residual concentration of hydrogen peroxide |
| CN113340834A (en) * | 2021-06-11 | 2021-09-03 | 成都市排水有限责任公司 | Method for rapidly determining content of sodium acetate in industrial-grade sodium acetate solution |
| CN113340834B (en) * | 2021-06-11 | 2023-05-16 | 成都市排水有限责任公司 | Method for rapidly determining sodium acetate content in industrial sodium acetate solution |
| CN113959822A (en) * | 2021-10-29 | 2022-01-21 | 珠海市丽拓生物科技股份有限公司 | Diluent and oxidant for determining urine iodine content by peroxyacetic acid oxidation method and application |
| CN113959822B (en) * | 2021-10-29 | 2024-02-20 | 珠海市丽拓生物科技股份有限公司 | Diluent and oxidant for measuring iodine content in urine by peroxyacetic acid oxidation method and application |
| CN116559342A (en) * | 2023-05-11 | 2023-08-08 | 天津大学 | A Kinetic Method for the Simultaneous Quantification of Peracetic Acid and Hydrogen Peroxide Concentrations |
| CN118303400A (en) * | 2024-03-21 | 2024-07-09 | 浙江医之友环境科技有限公司 | Preparation method of peroxyacetic acid disinfectant with concentration indication function |
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