CN116893244A - Method for rapidly detecting hydrogen peroxide content in industrial hydrogen peroxide - Google Patents
Method for rapidly detecting hydrogen peroxide content in industrial hydrogen peroxide Download PDFInfo
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- CN116893244A CN116893244A CN202310928927.0A CN202310928927A CN116893244A CN 116893244 A CN116893244 A CN 116893244A CN 202310928927 A CN202310928927 A CN 202310928927A CN 116893244 A CN116893244 A CN 116893244A
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- hydrogen peroxide
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- sodium thiosulfate
- molybdate
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- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 title claims abstract description 126
- 238000000034 method Methods 0.000 title claims abstract description 34
- 239000000243 solution Substances 0.000 claims abstract description 54
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 claims abstract description 36
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims abstract description 36
- 235000019345 sodium thiosulphate Nutrition 0.000 claims abstract description 36
- 239000012086 standard solution Substances 0.000 claims abstract description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229920002472 Starch Polymers 0.000 claims abstract description 15
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 235000019698 starch Nutrition 0.000 claims abstract description 15
- 239000008107 starch Substances 0.000 claims abstract description 15
- 239000008367 deionised water Substances 0.000 claims abstract description 14
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 14
- 238000001514 detection method Methods 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 238000010790 dilution Methods 0.000 claims abstract description 9
- 239000012895 dilution Substances 0.000 claims abstract description 9
- 239000000523 sample Substances 0.000 claims abstract description 9
- 239000012488 sample solution Substances 0.000 claims abstract description 6
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 claims description 12
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 8
- 238000004448 titration Methods 0.000 claims description 7
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 5
- 239000011609 ammonium molybdate Substances 0.000 claims description 5
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 5
- 229940010552 ammonium molybdate Drugs 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 239000012153 distilled water Substances 0.000 claims description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 4
- PODWXQQNRWNDGD-UHFFFAOYSA-L sodium thiosulfate pentahydrate Chemical compound O.O.O.O.O.[Na+].[Na+].[O-]S([S-])(=O)=O PODWXQQNRWNDGD-UHFFFAOYSA-L 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 239000003054 catalyst Substances 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 2
- NMHMDUCCVHOJQI-UHFFFAOYSA-N lithium molybdate Chemical compound [Li+].[Li+].[O-][Mo]([O-])(=O)=O NMHMDUCCVHOJQI-UHFFFAOYSA-N 0.000 claims description 2
- 229910052700 potassium Inorganic materials 0.000 claims description 2
- 239000011591 potassium Substances 0.000 claims description 2
- 239000011684 sodium molybdate Substances 0.000 claims description 2
- 235000015393 sodium molybdate Nutrition 0.000 claims description 2
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims 2
- 239000012286 potassium permanganate Substances 0.000 description 8
- 238000010561 standard procedure Methods 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- FZERHIULMFGESH-UHFFFAOYSA-N N-phenylacetamide Chemical compound CC(=O)NC1=CC=CC=C1 FZERHIULMFGESH-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- 229910052684 Cerium Inorganic materials 0.000 description 1
- 229960001413 acetanilide Drugs 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 1
- 238000004737 colorimetric analysis Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 238000002795 fluorescence method Methods 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Molecular Biology (AREA)
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention relates to a rapid detection method for hydrogen peroxide content in industrial hydrogen peroxide, which comprises the steps of transferring a prepared sample solution into a container, adding molybdate, hydrochloric acid solution and potassium iodide solution, fully mixing, placing in a dark place for a period of time, adding deionized water for dilution, titrating with a calibrated sodium thiosulfate standard solution until the standard solution is just colorless, adding a starch solution, continuing titrating until blue just disappears, and calculating the hydrogen peroxide content according to the concentration of the sodium thiosulfate standard solution, the dosage of the sodium thiosulfate standard solution and the volume of the sample, wherein the blue is not returned within 30 seconds, and the end point is obtained. Compared with the prior art, the method for measuring the hydrogen peroxide content in the industrial hydrogen peroxide can be fast, simple and convenient and has high safety.
Description
Technical Field
The invention relates to the technical field of industrial hydrogen peroxide content determination, in particular to a rapid detection method for hydrogen peroxide content in industrial hydrogen peroxide.
Background
Industrial hydrogen peroxide is widely applied in the fields of industry, catalysis, biology, medicine and the like. Currently, the method for measuring the hydrogen peroxide content mainly comprises a titration method, a chemiluminescence method, a fluorescence method, an infrared method, a spectrophotometry method, a test paper colorimetry method, a high performance liquid chromatography method and the like. The titration method mainly includes iodine method, potassium permanganate method, cerium method, etc. The potassium permanganate method is the national standard method GB/T1616-2014, and the measurement principle is that hydrogen peroxide and potassium permanganate undergo oxidation-reduction reaction in an acidic medium. However, the industrial product hydrogen peroxide often contains organic substances such as acetanilide and the like as a stabilizer, and the substances consume potassium permanganate and influence the accuracy of the result. Because potassium permanganate belongs to a controlled preparation, the potassium permanganate is inconvenient to purchase, and has strong oxidizing property and certain corrosiveness, fire and even explosion are easy to occur, and certain potential safety hazard exists.
The titration by using the iodometry has the advantages of less side reaction and high accuracy, but has the problem of slower reaction speed, and if the reaction time is insufficient, the accuracy of the result can be influenced. Therefore, there is a need to provide a method for rapidly, simply and safely measuring the hydrogen peroxide content in industrial hydrogen peroxide.
Disclosure of Invention
The invention aims to provide a rapid detection method for the hydrogen peroxide content in industrial hydrogen peroxide.
The aim of the invention can be achieved by the following technical scheme: a method for quickly detecting the content of hydrogen peroxide in industrial hydrogen peroxide includes such steps as loading the solution of specimen in container, adding molybdate, hydrochloric acid solution and potassium iodide solution, fully mixing, putting it in dark for a period of time, diluting with water, titrating with standard solution of sodium thiosulfate until it is just colorless, adding starch solution, and titrating until blue is just disappeared.
Preferably, accurately transferring 2.5mL of the sample into a 250mL volumetric flask, fixing the volume by deionized water, and shaking uniformly to obtain the sample solution with the fixed volume.
Preferably, 25mL of the constant-volume sample solution is accurately removed in a 250mL conical flask, and a certain amount of molybdate and 6mol.L are added -1 Covering a surface dish, fully mixing, placing in a dark place for a period of time, adding 50mL of deionized water for dilution, titrating with a calibrated standard solution of sodium thiosulfate to be just colorless, adding 5mL of starch solution, continuously titrating until blue just disappears, and within 30 secondsThe end point is the end point without bluing.
Further preferably, the starch solution concentration is 0.5wt%.
Preferably, the preparation process of the sodium thiosulfate standard solution comprises the following steps: 25g of sodium thiosulfate pentahydrate was weighed, dissolved in 1000mL of distilled water freshly boiled and cooled to room temperature, added with 0.1mg of sodium carbonate, shaken well, left for several days, filtered and stored in a brown bottle.
Preferably, the calibration process of the sodium thiosulfate standard solution is as follows: accurately weighing 0.13-0.18g of potassium dichromate in a 250mL conical flask, adding 25mL of deionized water to dissolve completely, cooling to room temperature, and adding 8-10mL and 6mol.L of 20wt% potassium iodide solution -1 And (3) covering 5mL of hydrochloric acid solution with a surface dish, fully mixing, standing in a dark place for 3-5min, adding 50mL of water for dilution, titrating with sodium thiosulfate solution until reddish brown becomes light obviously, adding 5mL of starch solution, continuously titrating until blue just disappears and transparent green is presented, namely, the end point is the end point, and calculating the concentration of the sodium thiosulfate standard solution.
Preferably, the molybdate comprises ammonium molybdate, lithium molybdate, sodium molybdate, potassium molybdate.
Preferably, the molybdate is used as a catalyst in an amount of 1 to 3 drops of a molybdate solution having a concentration of 1 to 30 g/L.
Preferably, after the potassium iodide solution is added, the solution is left in the dark for a period of 5 to 10 minutes.
Preferably, after the potassium iodide solution is added, the solution is left in the dark at 8-20 ℃ for 5-10min.
Preferably, the method for rapidly detecting the hydrogen peroxide content in the industrial hydrogen peroxide specifically comprises the following steps:
(1) Preparing a sodium thiosulfate standard solution: 25g of sodium thiosulfate pentahydrate was weighed, dissolved in 1000mL of distilled water freshly boiled and cooled to room temperature, added with 0.1mg of sodium carbonate, shaken well, left for several days, filtered and stored in a brown bottle.
(2) Calibrating a sodium thiosulfate standard solution: accurately weighing potassium dichromate 0.13-0.18g in a 250mL conical flask, adding 25mL deionized water to dissolve completely (if necessary, heating to aid dissolution), and cooling to obtain a solutionAfter room temperature, adding 8-10mL and 6mol.L of 20wt% potassium iodide solution -1 And (3) covering 5mL of hydrochloric acid solution with a surface dish, fully mixing, standing in a dark place for 3-5min, adding 50mL of water for dilution, titrating with sodium thiosulfate solution until reddish brown becomes light obviously, adding 5mL of starch solution, continuously titrating until blue just disappears and transparent green is presented, namely, the end point is the end point, and calculating the concentration of the sodium thiosulfate solution.
(3) Determination of hydrogen peroxide content in industrial hydrogen peroxide: accurately transferring 2.5mL of the sample into a 250mL volumetric flask, and shaking uniformly by using deionized water to fix the volume. Accurately transferring 25mL of the solution into a 250mL conical flask, adding a certain amount of molybdate and 6mol.L -1 Covering a surface dish for fully mixing, placing in a dark place for a period of time, adding 50mL of deionized water for dilution, titrating with a calibrated sodium thiosulfate standard solution until the solution is just colorless, adding 5mL of starch solution, continuously titrating until the blue just disappears, and not returning to the blue within 30 seconds to obtain the final point. The hydrogen peroxide content was calculated from the concentration of the sodium thiosulfate standard solution, the amount used and the volume of the sample.
Further preferably, the starch solution concentration in step (2) and step (3) is 0.5wt%.
Compared with the prior art, the invention has the following advantages:
1. the method adopts the sodium thiosulfate standard titration solution to replace the potassium permanganate standard solution in GB/T1616-2014 for titrating the hydrogen peroxide content, and the method does not need to use potassium permanganate with high corrosiveness, strong oxidability and low safety coefficient in the whole determination process;
2. the invention adopts molybdate as the catalyst, so that the detection efficiency can be greatly improved, and the detection time can be shortened;
3. compared with other methods, the method does not need expensive instruments and equipment, has simple operation, high efficiency and low energy consumption, and has wide application prospect.
4. The invention provides a method for rapidly, simply and safely measuring the hydrogen peroxide content in industrial hydrogen peroxide.
Detailed Description
The following examples of the present invention are described in detail, and are given by way of illustration of the present invention, but the scope of the present invention is not limited to the following examples.
Example 1
A rapid detection method for hydrogen peroxide content in industrial hydrogen peroxide is carried out at 18 ℃ according to the following steps:
1) Preparing a sodium thiosulfate standard solution: 25g of sodium thiosulfate pentahydrate was weighed, dissolved in 1000mL of distilled water freshly boiled and cooled to room temperature, added with 0.1mg of sodium carbonate, shaken well, left for several days, filtered and stored in a brown bottle.
2) Calibrating a sodium thiosulfate standard solution: accurately weighing 0.13-0.18g of potassium dichromate in a 250mL conical flask, adding 25mL of deionized water to dissolve completely (if necessary, heating to assist dissolution), cooling to room temperature, and adding 8-10mL and 6mol.L of 20wt% potassium iodide solution -1 And (3) covering 5mL of hydrochloric acid solution, fully mixing the solution with a surface dish, standing in a dark place for 3-5min, adding 50mL of deionized water for dilution, titrating with a sodium thiosulfate standard solution until reddish brown is obviously lightened, adding 5mL of 0.5% starch solution, continuously titrating until blue just disappears and transparent green is presented, namely, the end point is the end point, and calculating the concentration of the sodium thiosulfate standard solution.
The concentration of the sodium thiosulfate standard solution was calculated as follows:
wherein: c-concentration of sodium thiosulfate standard solution, mol/L; m-mass of potassium dichromate, g; m-relative molecular mass of potassium dichromate, 294.2g/mol; v-sodium thiosulfate standard solution dosage, mL.
3) Determination of the hydrogen peroxide content: accurately transferring 2.5mL of the sample into a 250mL volumetric flask, and shaking uniformly by using deionized water to fix the volume. Accurately transferring 25mL of the solution into a 250mL conical flask, adding 1mg/mL of ammonium molybdate 2 drops (0.1 mL) and 6 mol.L -1 5mL of a hydrochloric acid solution of (2), 20% potassium iodide solutionAnd (3) 5mL of liquid, covering a surface dish, fully mixing, placing in a dark place for 5min, adding 50mL of deionized water for dilution, titrating with a calibrated sodium thiosulfate standard solution until the standard solution is just colorless, adding 5mL of a 0.5wt% starch solution, continuously titrating until the blue color just disappears, and not returning to the blue within 30s to obtain the final point. The hydrogen peroxide content was calculated from the concentration of the sodium thiosulfate standard solution, the amount used and the volume of the sample.
The calculation formula of the content of hydrogen peroxide is:
wherein: c-concentration of sodium thiosulfate standard solution, mol/L; c 1 Hydrogen peroxide molar concentration, mol/L; v-the dosage of the sodium thiosulfate standard solution, mL; v (V) 1 Hydrogen peroxide volume, mL.
In order to verify the accuracy of the detection method of the present invention, the hydrogen peroxide content in the same sample was measured in parallel for 3 times by using the national standard method and the method of example 1, and the results are shown in table 1:
TABLE 1 Hydrogen peroxide content in samples measured by EXAMPLE 1 and national Standard method
Project | Example 1 | National standard method |
Concentration (mol/L) | 3.545 | 3.538 |
Mean deviation from relative | 0.05% | 0.08% |
As can be seen from Table 1, the results obtained in example 1 of the method are consistent with those obtained in the national standard method, and the relative average deviation is smaller, which indicates that the results obtained in the measurement method of the invention have no significant difference from those obtained in the national standard method.
Comparative example 1
All experimental procedures were as in example 1, except that no ammonium molybdate was added. At this time, in the step of measuring the hydrogen peroxide content, 5mL of a starch solution with the weight percent is added, and after the solution is titrated continuously with a sodium thiosulfate standard solution until the blue color just disappears, the solution is blued for 30 seconds, after half drops of the sodium thiosulfate standard solution are added, the blue color is disappeared, 30 seconds is not reached, the solution is blued again, the process is repeated for 20 times, and the excessive consumption is about 7 minutes; the relative average deviation of the experimental results was 0.29%. Comparative example 1 illustrates that when no ammonium molybdate is added, not only is the experiment time-consuming, but also the experiment repeatability is poor, and the requirement of titration analysis is not met.
The above embodiment is only used for further explaining a method for rapidly determining the hydrogen peroxide content in industrial hydrogen peroxide, but the invention is not limited to the embodiment, and any simple modification, equivalent variation and modification of the above embodiment according to the technical substance of the invention falls within the scope of the technical solution of the invention.
Claims (10)
1. A rapid detection method for hydrogen peroxide content in industrial hydrogen peroxide is characterized in that a sample solution with fixed volume is removed in a container, molybdate, hydrochloric acid solution and potassium iodide solution are added, the mixture is fully mixed, the mixture is placed in a dark place for a period of time, water is added for dilution, the calibrated sodium thiosulfate standard solution is used for titration until the solution is just colorless, starch solution is added, and the titration is continued until blue just disappears, so that the hydrogen peroxide content is calculated according to the concentration of the sodium thiosulfate standard solution, the dosage of the sodium thiosulfate standard solution and the volume of the sample.
2. The method for rapidly detecting the hydrogen peroxide content in the industrial hydrogen peroxide according to claim 1, wherein 2.5mL of the sample is accurately removed in a 250mL volumetric flask, the volume is fixed by deionized water, and the sample solution after the volume fixing is obtained by shaking.
3. The method for rapidly detecting hydrogen peroxide content in industrial hydrogen peroxide according to claim 1, wherein 25mL of the constant-volume sample solution is accurately removed in a 250mL conical flask, and a certain amount of molybdate and 6mol.L are added -1 Covering a surface dish for fully mixing, placing in a dark place for a period of time, adding 50mL of deionized water for dilution, titrating with a calibrated sodium thiosulfate standard solution until the solution is just colorless, adding 5mL of starch solution, continuously titrating until the blue just disappears, and not returning to the blue within 30 seconds to obtain the final point.
4. The method for rapid detection of hydrogen peroxide content in industrial hydrogen peroxide according to claim 3, wherein the concentration of the starch solution is 0.5wt%.
5. The rapid detection method for hydrogen peroxide content in industrial hydrogen peroxide according to claim 1, wherein the preparation process of the sodium thiosulfate standard solution is as follows: 25g of sodium thiosulfate pentahydrate was weighed, dissolved in 1000mL of distilled water freshly boiled and cooled to room temperature, added with 0.1mg of sodium carbonate, shaken well, left for several days, filtered and stored in a brown bottle.
6. The rapid detection method for hydrogen peroxide content in industrial hydrogen peroxide according to claim 1, wherein the calibration process of the sodium thiosulfate standard solution is as follows: accurately weighing 0.13-0.18g of potassium dichromate in a 250mL conical flask, adding 25mL of deionized water to dissolve completely, cooling to room temperature, and adding 8-10mL and 6mol.L of 20wt% potassium iodide solution -1 5mL of hydrochloric acid solution, covering a surface dish, fully mixing, standing in the dark for 3-5min, and adding 50mL of water for dilutionAnd (3) releasing, namely titrating the sodium thiosulfate solution until the reddish brown color becomes obviously lighter, adding 5mL of starch solution, continuously titrating until the blue color just disappears and the transparent green color is presented as an end point, and calculating the concentration of the sodium thiosulfate standard solution.
7. The method for rapidly detecting the hydrogen peroxide content in industrial hydrogen peroxide according to claim 1, wherein the molybdate comprises ammonium molybdate, lithium molybdate, sodium molybdate and potassium molybdate.
8. The method for rapidly detecting the hydrogen peroxide content in industrial hydrogen peroxide according to claim 1, wherein the molybdate is used as a catalyst in an amount of 1-3 drops of 1-30g/L molybdate solution.
9. The method for rapidly detecting hydrogen peroxide content in industrial hydrogen peroxide according to claim 1, wherein the time for placing in the dark after adding the potassium iodide solution is 5-10min.
10. The method for rapidly detecting the hydrogen peroxide content in industrial hydrogen peroxide according to claim 1, wherein the potassium iodide solution is added and then left in the dark at 8-20 ℃ for 5-10min.
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