CN110632250B - Method for determining concentrations of peroxides in mixed solutions of peroxomonosulfate, peroxodisulfate and hydrogen peroxide based on iodometry - Google Patents

Method for determining concentrations of peroxides in mixed solutions of peroxomonosulfate, peroxodisulfate and hydrogen peroxide based on iodometry Download PDF

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CN110632250B
CN110632250B CN201911109077.1A CN201911109077A CN110632250B CN 110632250 B CN110632250 B CN 110632250B CN 201911109077 A CN201911109077 A CN 201911109077A CN 110632250 B CN110632250 B CN 110632250B
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关英红
张天禹
欧照凡
付强
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Northeast Agricultural University
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Abstract

A method for determining the concentration of each peroxide in a mixed solution of peroxymonosulfate, peroxydisulfate and hydrogen peroxide based on an iodometric method relates to a method for determining the concentration of each peroxide in a mixed solution of peroxymonosulfate, peroxydisulfate and hydrogen peroxide based on an iodometric method. The invention aims to solve the problem that the concentration of each of three oxidants in a mixture of the three oxidants cannot be measured by the existing method, and the method comprises the following steps: and adding sodium bicarbonate and potassium iodide into the solution to be detected, standing, adding glacial acetic acid, titrating, and calculating to obtain the oxidant concentration sum. Adding a sodium monohydrogen phosphate-sodium dihydrogen phosphate buffer solution and a catalase solution into the solution to be detected, adding sodium bicarbonate and potassium iodide, standing, adding glacial acetic acid, and titrating to obtain the concentration sum of PMS and PDS; and adding a sodium monohydrogen phosphate-sodium dihydrogen phosphate buffer solution and catalase into the solution to be detected, adding potassium iodide and an acetic acid-sodium acetate buffer solution, standing, titrating, and calculating to obtain the concentration of PMS. The method is applied to the field of oxidant concentration determination.

Description

Method for determining concentrations of peroxides in mixed solutions of peroxomonosulfate, peroxodisulfate and hydrogen peroxide based on iodometry
Technical Field
The invention relates to a method for determining the concentration of each peroxide in a mixed solution of peroxomonosulfate, peroxodisulfate and hydrogen peroxide on the basis of the iodometric method.
Background
Peroxymonosulfate (PMS), Peroxydisulfate (PDS), and hydrogen peroxide (H)2O2) Is widely used as a strong oxidant in the treatment process of drinking water and waste water. The three oxidants are activated to generate sulfate radicals and/or hydroxyl radicals with strong oxidizability, so that organic pollutants are more effectively oxidized and degraded. When peroxomonosulfates are usedAnd peroxodisulfate technology, two other peroxides may be generated in the system. And in the combined technology of the persulfate (PMS/PDS) and the hydrogen peroxide, the persulfate and the hydrogen peroxide exist at the same time. Therefore, it is very important to establish a method for conveniently and rapidly determining the concentration of each oxidant in the peroxide mixed solution. At present, the existing iodometry based on a spectrophotometer or a titration method can only measure the concentration of the single peroxide, but cannot measure the concentration of various oxidants in a mixture in which three peroxides exist simultaneously.
Disclosure of Invention
The invention aims to solve the problem that the concentration of each of three oxidants in a mixed solution of three peroxides cannot be measured by the conventional method, and provides a method for measuring the concentration of each peroxide in the mixed solution of peroxymonosulfate, peroxydisulfate and hydrogen peroxide based on an iodometric method.
The invention relates to a method for measuring the concentration of each peroxide in a mixed solution of peroxymonosulfate, peroxydisulfate and hydrogen peroxide based on an iodometric method, which comprises the following steps:
taking x mL of solution to be detected, adding sodium bicarbonate and potassium iodide, shaking, standing for 15-20min, adding glacial acetic acid, shaking, and using concentration c0Titrating a mol/L sodium thiosulfate solution, taking starch as an indicator, titrating the solution until the solution is colorless, and recording the dosage h of the sodium thiosulfate1 mL；
Adding sodium monohydrogen phosphate-sodium dihydrogen phosphate buffer solution and catalase solution into the to-be-detected solution x mL, shaking, standing for 5-10min, adding sodium bicarbonate and potassium iodide, shaking, standing for 15-20min, adding glacial acetic acid, and adding the solution with concentration of c0Titrating a mol/L sodium thiosulfate solution, taking starch as an indicator, titrating the solution until the solution is colorless, and recording the dosage h of the sodium thiosulfate2 mL；
Thirdly, taking x mL of the solution to be detected, adding sodium monohydrogen phosphate-sodium dihydrogen phosphate buffer solution and catalase solution, shaking up, standing for 5-10min, sequentially adding potassium iodide and acetic acid-sodium acetate buffer solution with the pH value of 3, shaking up, standing for 2-5min, and then using the solution with the concentration of c0mol/L sodium thiosulfateTitrating the solution, taking starch as an indicator, titrating the solution to be colorless, and recording the using amount h of the sodium thiosulfate3 mL；
Wherein the concentration c of peroxymonosulfate in the solution to be tested1＝(h3*c0) 2 x; peroxodisulfate concentration c2＝[(h2-h3)*c0]2 x; hydrogen peroxide concentration c3＝[(h1-h2)*c0]2 x; wherein h is1、h2、h3The unit is mL; c. C0、c1、c2、c3The unit is mol/L.
The invention has the beneficial effects that:
iodometry is a method of analyzing iodine by utilizing the oxidizing property of iodine and the reducing property of iodide ions. Under certain conditions, the iodide ions can reduce corresponding oxidants to generate equivalent iodine, and then sodium thiosulfate standard solution is used for titrating the iodine. Obtaining PMS, PDS and H2O2The three oxidant concentrations are combined. The reaction formula is as follows: i is2+2S2O3 2-＝2I-+S4O6 2-+2I-。
In the invention, the catalase can remove the hydrogen peroxide in the mixed solution and does not influence the reaction of iodide ions and other two oxidants; meanwhile, under the condition of pH 3 acetic acid-sodium acetate buffer solution, PDS hardly reacts with iodide ions, so that the concentration of PMS in the solution to be detected can be determined; and further determining the corresponding concentrations of the three oxidants according to the concentration summation relationship of the three oxidants. The lowest concentration of each oxidant in the liquid to be detected can be detected to be 0.003mmol/L by the detection method.
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FIG. 1 shows the measurement of PMS, PDS, H alone in example 12O2Comparing the theoretical concentration and the actual measured concentration of the solution; wherein a is the theoretical concentration; b is the actual measured concentration;
FIG. 2 shows the measurement of PMS, PDS, H in example 22O2A comparison graph of the theoretical concentration of the oxidant and the actual measured concentration of the mixed solution; wherein a is the theoretical concentration; b is the actual measured concentration;
FIG. 3 is a graph comparing the concentrations of the oxidant, PMS and PDS, and the theoretical values measured before and after catalase is added to the three peroxide mixtures of example 2; wherein b is a measured value before adding catalase, c is a measured value after adding catalase, and d is the concentration and theoretical value of PDS and PMS in the mixed solution;
FIG. 4 is a graph comparing the concentration of oxidant measured in example 3 with the theoretical concentration of PMS; wherein a is the actually measured oxidant concentration in the mixed solution; b is a PMS concentration theoretical value.
Detailed Description
The first embodiment is as follows: the method for measuring the concentration of each peroxide in the mixed solution of peroxymonosulfate, peroxydisulfate and hydrogen peroxide based on an iodometric method is carried out according to the following steps:
taking x mL of solution to be detected, adding sodium bicarbonate and potassium iodide, shaking, standing for 15-20min, adding glacial acetic acid, shaking, and using concentration c0Titrating a mol/L sodium thiosulfate solution, taking starch as an indicator, titrating the solution until the solution is colorless, and recording the dosage h of the sodium thiosulfate1 mL；
Adding sodium monohydrogen phosphate-sodium dihydrogen phosphate buffer solution and catalase solution into the to-be-detected solution x mL, shaking, standing for 5-10min, adding sodium bicarbonate and potassium iodide, shaking, standing for 15-20min, adding glacial acetic acid, and adding the solution with concentration of c0Titrating a mol/L sodium thiosulfate solution, taking starch as an indicator, titrating the solution until the solution is colorless, and recording the dosage h of the sodium thiosulfate2 mL；
Thirdly, taking x mL of the solution to be detected, adding sodium monohydrogen phosphate-sodium dihydrogen phosphate buffer solution and catalase solution, shaking up, standing for 5-10min, sequentially adding potassium iodide and acetic acid-sodium acetate buffer solution with the pH value of 3, shaking up, standing for 2-5min, and then using the solution with the concentration of c0Titrating the solution of sodium thiosulfate in mol/L, titrating the solution to be colorless by taking starch as an indicator, and recording the using amount h of the sodium thiosulfate3 mL；
Wherein the concentration c of peroxymonosulfate in the solution to be tested1＝(h3*c0) 2 x; peroxodisulfate concentration c2＝[(h2-h3)*c0]2 x; hydrogen peroxide concentration c3＝[(h1-h2)*c0]2 x; wherein h is1、h2、h3The unit is mL; c. C0、c1、c2、c3The unit is mol/L.
The concentration sum of peroxymonosulfate, peroxydisulfate and hydrogen peroxide is calculated in the first step; step two, calculating to obtain the sum of the concentrations of peroxymonosulfate and peroxydisulfate; and step three, calculating the concentration of the peroxymonosulfate.
In the embodiment, the catalase can remove the hydrogen peroxide in the mixed solution and does not influence the reaction of the iodide ions and the other two oxidants; meanwhile, under the condition of adding a pH (3) acetic acid-sodium acetate buffer solution, PDS hardly reacts with iodide ions, so that the concentration of PMS in the solution to be detected can be determined; and the corresponding concentrations of the three oxidants can be determined through the concentration summation relation of the three oxidants, and the lowest concentration of the oxidant in the liquid to be measured, which can be measured by the measuring method of the embodiment, can reach 0.003 mmol/L.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: the concentration of potassium iodide in the solution to be detected in the first step and the second step is more than or equal to 1.81mol/L, and the concentration of sodium bicarbonate is 0.79 mmol/L. The rest is the same as the first embodiment.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: the volume ratio of the glacial acetic acid to the liquid to be detected in the first step and the second step is 3.3 (100-. The others are the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment mode and one of the first to third embodiment modes is: in the second step and the third step, the volume ratio of the sodium monohydrogen phosphate-sodium dihydrogen phosphate buffer solution to the liquid to be detected is 1:100, and the volume ratio of the catalase solution to the liquid to be detected is 1: 500. The rest is the same as one of the first to third embodiments.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: in the third step, the volume ratio of the acetic acid-sodium acetate buffer solution to the solution to be detected is 1: 20. The rest is the same as one of the first to fourth embodiments.
The sixth specific implementation mode: the difference between this embodiment and one of the first to fifth embodiments is: and step three, the concentration of potassium iodide in the solution to be detected is more than or equal to 0.06 mol/L. The rest is the same as one of the first to fifth embodiments.
The seventh embodiment: the difference between this embodiment and one of the first to sixth embodiments is: in the sodium monohydrogen phosphate-sodium dihydrogen phosphate buffer solution, the concentration of the sodium monohydrogen phosphate is 0.039 mol/L; the concentration of sodium dihydrogen phosphate is 0.070 mol/L. The rest is the same as one of the first to sixth embodiments.
The specific implementation mode is eight: the present embodiment differs from one of the first to seventh embodiments in that: the concentration of the catalase solution is more than or equal to 5g/L, and the catalase activity is 2000-5000 units/mg. The rest is the same as one of the first to seventh embodiments.
The specific implementation method nine: the present embodiment differs from the first to eighth embodiments in that: the starch indicator was made from 0.5g of soluble starch and 100mL of distilled water. The rest is the same as the first to eighth embodiments.
The effect of the invention is demonstrated by the following examples:
example 1: this example demonstrates that Peroxymonosulfate (PMS), Peroxydisulfate (PDS) and hydrogen peroxide (H) can be measured separately at a potassium iodide concentration of 1.81mol/L and a sodium bicarbonate concentration of 0.79mmol/L2O2) The concentration comprises the following specific steps:
firstly, respectively configuring PMS, PDS and H2O2Mother liquor, the concentration of three prepared oxidants is cPMS＝0.1248mol/L，cPDS＝0.1mol/L，cH2O2＝0.1239mol/L。
And secondly, adding 0.5mL of corresponding oxidant mother liquor into 100mL of ultrapure water, shaking up, sequentially adding 30g of potassium iodide and 0.66g of sodium bicarbonate, standing for 15min, adding 3.3mL of acetic acid, titrating with 0.01287mol/L sodium thiosulfate solution, adding 1 mL0.5% starch as an indicator, titrating the solution until the solution is colorless, and recording the dosage h of the sodium thiosulfate.
The corresponding oxidant mother liquor concentration c which is separately measured under the conditions that the potassium iodide concentration is 1.81mol/L and the sodium bicarbonate concentration is 0.79mmol/L can be obtained;
c＝h*0.01287；
wherein: h is mL, c is mol/L;
the concentration of potassium iodide was 1.81mol/L and the concentration of sodium bicarbonate was 0.79mmol/L, and PMS, PDS and H were measured separately2O2The resulting ratio of the theoretical concentration to the actual concentration of the mother liquor is shown in FIG. 1. It can be considered from fig. 1 that this condition allows the above three oxidizer concentrations to be measured separately.
Example two: this example demonstrates that catalase can effectively remove H from mixed solution2O2While not aiming at PDS, H2O2The reaction with iodide ion has the following specific implementation steps:
firstly, respectively configuring PMS, PDS and H2O2Mother liquor, the concentration of three prepared oxidants is cPMS＝0.1248mol/L，cPDS＝0.1mol/L，cH2O2＝0.1239mol/L。
Secondly, sequentially taking 0.17mLPMS, 0.17mLPDS and 0.17mLPDS 0.17mLH from the prepared mother liquor2O2Adding into 100mL of ultrapure water, shaking uniformly, sequentially adding 30g of potassium iodide and 0.66g of sodium bicarbonate, standing for 15min, adding 3.3mL of glacial acetic acid, titrating with 0.01287mol/L sodium thiosulfate solution, adding 1mL of 0.5% starch as an indicator, titrating the solution until the solution is colorless, and recording the dosage of sodium thiosulfate h1。
Then PMS, PDS and H can be measured under the conditions that the concentration of potassium iodide is 1.81mol/L and the concentration of sodium bicarbonate is 0.79mmol/L2O2Three oxidant concentrations in the mixed solution and c1；
c1＝h1*0.01287/200；
Wherein: h is1Units are mL, c1The unit is mol/L;
the concentration of potassium iodide is 1.81mol/L, and the concentration of sodium bicarbonate is 0.79mmol/L2O2The concentration and theoretical value of the three oxidants in the mixed solution are shown in the graph of fig. 2 together with the actual measured value. It can be considered from FIG. 2 that under this condition, the sum of the three oxide concentrations can be determined.
Thirdly, sequentially taking 0.17mLPMS, 0.17mLPDS and 0.17mLPDS 0.17mLH from the prepared mother liquor2O2After adding to 100mL of ultrapure water and shaking, 1mL of sodium monohydrogen phosphate-sodium dihydrogen phosphate buffer solution and 0.2mL of catalase solution were added in this order and shaken. After standing for 5min, sodium bicarbonate and potassium iodide were added so that the potassium iodide concentration in the solution was 1.81mol/L and the sodium bicarbonate concentration was 0.79 mmol/L. Shaking up. Standing for 15min, adding 3.3mL of glacial acetic acid, titrating with 0.01287mol/L sodium thiosulfate solution, adding 1 mL0.5% starch as indicator, titrating the solution to colorless, and recording the dosage h of sodium thiosulfate2。
Then PMS, PDS and H can be obtained under the conditions that the concentration of potassium iodide is 1.81mol/L, the concentration of sodium bicarbonate is 0.79mmol/L and catalase exists2O2Concentration of oxidant in mixed solution and measured value c2；
c2＝h2*0.01287/200；
Wherein: h is2Units are mL, c2The unit is mol/L;
FIG. 3 is a graph showing the comparison between the measured oxidant concentration in the mixed solution and the concentrations of PMS and PDS and the theoretical values, measured before and after addition of catalase under the measurement conditions of potassium iodide concentration of 1.81mol/L and sodium bicarbonate concentration of 0.79 mmol/L. According to the third figure, catalase can be considered to be capable of effectively removing H in the mixed solution2O2Meanwhile, the reaction of PDS, PMS and iodide ions is not affected.
Example three, this example demonstrates that the concentration of the oxidant measured by adding catalase to three peroxide mixed solutions and 5mL of a buffer solution of acetic acid-sodium acetate with pH 3 is the actual concentration of PMS, and the specific implementation steps are as follows:
firstly, respectively configuring PMS, PDS and H2O2Mother liquor, the concentration of three prepared oxidants is cPMS＝0.1248mol/L，cPDS＝0.1mol/L，cH2O2＝0.1239mol/L。
Secondly, sequentially taking 0.17mLPMS, 0.17mLPDS and 0.17mLPDS 0.17mLH from the prepared mother liquor2O2After adding to 100mL of ultrapure water and shaking, 1mL of sodium monohydrogen phosphate-sodium dihydrogen phosphate buffer solution and 0.2mL of catalase solution were added in this order and shaken. Standing for 5min, adding 1g of potassium iodide and 5ml of acetic acid-sodium acetate buffer solution with pH value of 3, standing for 2min, titrating with 0.01287mol/L sodium thiosulfate solution, adding 1ml of 0.5% starch as an indicator, titrating the solution until the solution is colorless, and recording the dosage h of the sodium thiosulfate3.
Then the concentration c of the oxidant is measured by adding catalase and 5ml pH 3 acetic acid-sodium acetate buffer solution to obtain three peroxide mixed solutions3；
c3＝h3*0.01287/200；
Wherein: h is3The unit is mL; c. C3The unit is mol/L;
thirdly, taking 0.17mL LPMS and 0.17mL LPDS from the mother liquor, adding the mother liquor into 100mL of ultrapure water, shaking the mother liquor evenly, adding 1g of potassium iodide and 5mL of acetic acid-sodium acetate buffer solution with pH being 3, standing the mother liquor for 2min, titrating the mother liquor by using 0.01287mol/L sodium thiosulfate solution, adding 1mL of 0.5% starch as an indicator, titrating the solution until the solution is colorless, and recording the dosage h of the sodium thiosulfate4；
c4＝h4*0.01287/200；
Wherein: h is4Units are mL, c4The unit is mol/L;
the ratio of the concentration of the oxidizing agent measured under the condition of adding catalase to 5mL of acetic acid-sodium acetate buffer solution with pH 3, the measured concentration of the mixed solution of PMS and PDS under the condition of pH 3, and the theoretical concentration of PMS is shown in fig. 4. The oxidant concentration measured under the condition of adding catalase to the three peroxide mixed solutions and 5mL of acetic acid-sodium acetate buffer solution with pH being 3 is considered as the actual concentration of PMS, which indicates that the measurement of PMS concentration is not interfered by PDS under the method. In conclusion, the catalase can remove the hydrogen peroxide in the mixed solution and does not influence the reaction of the iodide ions and the other two oxidants; meanwhile, under the condition of adding a pH (3) acetic acid-sodium acetate buffer solution, PDS hardly reacts with iodide ions, so that the concentration of PMS in the solution to be detected can be determined; and further determining the corresponding concentrations of the three oxidants according to the concentration summation relationship of the three oxidants. The lowest concentration of the oxidant in the liquid to be detected, which can be detected by the detection method, can reach 0.003 mmol/L.

Claims (8)

1. A method for determining the concentration of each peroxide in a mixed solution of peroxomonosulfate, peroxodisulfate and hydrogen peroxide on the basis of iodometry, characterized in that the method is carried out as follows:
taking x mL of solution to be detected, adding sodium bicarbonate and potassium iodide, shaking, standing for 15-20min, adding glacial acetic acid, shaking, and using concentration c0Titrating a mol/L sodium thiosulfate solution, taking starch as an indicator, titrating the solution until the solution is colorless, and recording the dosage h of the sodium thiosulfate1 mL；
Adding sodium monohydrogen phosphate-sodium dihydrogen phosphate buffer solution and catalase solution into the to-be-detected solution x mL, shaking, standing for 5-10min, adding sodium bicarbonate and potassium iodide, shaking, standing for 15-20min, adding glacial acetic acid, and adding the solution with concentration of c0Titrating a mol/L sodium thiosulfate solution, taking starch as an indicator, titrating the solution until the solution is colorless, and recording the dosage h of the sodium thiosulfate2 mL；
Thirdly, taking x mL of the solution to be detected, adding sodium monohydrogen phosphate-sodium dihydrogen phosphate buffer solution and catalase solution, shaking up, standing for 5-10min, sequentially adding potassium iodide and acetic acid-sodium acetate buffer solution with the pH value of 3, shaking up, standing for 2-5min, and then using the solution with the concentration of c0Titrating the solution of sodium thiosulfate in mol/L, titrating the solution to be colorless by taking starch as an indicator, and recording the using amount h of the sodium thiosulfate3 mL；
Wherein the concentration c of peroxymonosulfate in the solution to be tested1 =（h3*c0) 2 x; peroxodisulfate concentration c2=[（h2-h3）*c0]2 x; hydrogen peroxide concentration c3=[（h1-h2）*c0]2 x; wherein h is1、h2、h3The unit is mL;c0、c1、c2、c3the unit is mol/L; the molar concentration ratio of the sum of the molar concentrations of peroxymonosulfate, peroxydisulfate and hydrogen peroxide to KI in the solutions to be detected in the first step and the second step is less than or equal to 0.59279:1810, and the concentration of sodium bicarbonate is 0.79 mmol/L; in the third step, the molar concentration ratio of the sum of the molar concentrations of peroxymonosulfate, peroxydisulfate and hydrogen peroxide to the molar concentration of KI in the solution to be detected is less than or equal to 0.59279: 60.
2. The method for iodometry-based determination of the concentration of each peroxide in a mixed solution of peroxomonosulfate, peroxodisulfate and hydrogen peroxide as claimed in claim 1, wherein the ratio by volume of glacial acetic acid to the test solution in the first and second steps is 3.3 (100- "101").
3. The iodometry-based method for determining the concentration of each peroxide in a mixed solution of peroxymonosulfate, peroxydisulfate, and hydrogen peroxide as claimed in claim 1, wherein the volume ratio of the sodium monohydrogen phosphate-sodium dihydrogen phosphate buffer to the test solution in the second step and the third step is 1:100, and the volume ratio of the catalase solution to the test solution is 1: 500.
4. The iodometry-based method for determining the concentration of each peroxide in a mixed solution of peroxymonosulfate, peroxydisulfate and hydrogen peroxide as claimed in claim 1, wherein the volume ratio of the acetic acid-sodium acetate buffer to the test solution in step three is 1: 20.
5. The method for iodometry-based determination of the concentrations of peroxides in a mixed solution of peroxymonosulfate, peroxydisulfate and hydrogen peroxide as claimed in claim 1, wherein the concentration of potassium iodide in the test solution of step three is 0.06mol/L or more.
6. The method for iodometry-based determination of the concentrations of peroxides in a mixed solution of peroxymonosulfate, peroxydisulfate, and hydrogen peroxide as claimed in claim 1, wherein the concentration of sodium monohydrogen phosphate in the sodium monohydrogen phosphate-sodium dihydrogen phosphate buffer described in step two and step three is 0.039 mol/L; the concentration of sodium dihydrogen phosphate is 0.070 mol/L.
7. The method for iodometry-based determination of the concentrations of peroxides in a mixed solution of peroxymonosulfate, peroxydisulfate and hydrogen peroxide as claimed in claim 1, wherein the concentration of the catalase solution in step two and step three is 5g/L or more and the catalase activity is 2000-5000 units/mg.
8. The iodometry-based method for determining the concentration of each peroxide in a mixed solution of peroxymonosulfate, peroxydisulfate, and hydrogen peroxide as recited in claim 1, wherein the starch indicator in step one, step two, and step three is made from 0.5g of soluble starch and 100mL of distilled water.
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