CN103592295A - Testing method of content of peroxymonosulfate in water - Google Patents
Testing method of content of peroxymonosulfate in water Download PDFInfo
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Abstract
The invention relates to a testing method of peroxymonosulfate, in particular to a testing method of the content of peroxymonosulfate in the water, and solves the problems that a conventional testing method is complex in operation step, long in reaction time, large in testing result error, narrow in application range, and high in equipment cost. The testing method comprises the following steps: first, creating a standard curve; second, measuring the absorbance values of azo-dyes at the characteristic peak before/after a to-be-tested water sample is added; third, substituting the difference values of the values measured in the second step into the standard curve in the first step to calculate the content of the peroxymonosulfate in the to-be-tested water sample. The testing method is simple and practicable, the testing result error is small, the testing time is short, the application range is wide, and the cost is low. The testing method is applicable to fields of surface water treatment, industrial wastewater treatment, and surface water and soil remediation.
Description
Technical field
The present invention relates to a kind of assay method of peroxy-monosulfate, relate in particular to a kind of based on utilizing divalence cobalt activation peroxy-monosulfate to produce the method for permonosulphuric acid salt content in the mensuration water of sulfate radical free radical cracking azo dyes.
Background technology
In recent years, the advanced oxidation processes that produces free radical based on activation peroxy-monosulfate be widely used in degrading difficult degradation toxic organic compound and Inactivation in Water endophytic bacteria.The method of common activation peroxy-monosulfate have take metal ion activation method that divalence cobalt and ferrous ion be representative, with CoFe
2o
4and CuFe
2o
4the heterogeneous activation method that is representative Deng spinel magnetic magnetic material, and utilize UV radiation, microwave and ultrasonic cavitation etc. for the external energy activation method of representative.In the activation system of these peroxy-monosulfates, all need to measure wherein remaining peroxy-monosulfate and investigate its utilization factor, operation is responsible for.
At present, in water, the assay method of peroxy-monosulfate mainly comprises fluorimetry, chromatography and titrimetry.Fluorimetry mainly adds and can excite the material that produces fluorescence to measure, although that fluorimetry has advantages of is highly sensitive, detectability is low, but need to purchase expensive fluorophotometric and take into account fluorescer, exist and analyze the high shortcoming of cost of determination, thereby fluorimetry is subject to great restriction in actual applications.Chromatography is mainly high performance liquid chromatography; Chromatography need to configure expensive high performance liquid chromatography and specific separating column, although it is low to measure the detection limit of peroxy-monosulfate, but require strict to all kinds of background impurities in water body, not only analyze cost of determination high, and the complicated finding speed of analytical procedure is slow, measuring a sample often needs more than ten minute, so chromatography is also unsuitable for being widely used in practical measurement.The most frequently used in titrimetry is iodimetric titration, and iodimetric titration is also the main measuring methods of permonosulphuric acid salt content in current water, and iodimetric titration does not need expensive instrument and equipment, measures with low costly, also has advantages of that antijamming capability is strong simultaneously; But iodimetric titration exists that complicated operation is loaded down with trivial details, the assaying reaction time is long in actual applications, titration end-point is wayward, in actual applications the larger shortcoming of measuring error.
Summary of the invention
The object of the invention is in order to solve existing assay method operation steps complexity loaded down with trivial detailsly, the reaction time is long, and measurement result error is large, narrow application range, the problem that equipment cost is high, and the assay method of permonosulphuric acid salt content in a kind of water providing.
The assay method of permonosulphuric acid salt content in a kind of water of the present invention, it is to carry out according to the following steps:
Step 1: production standard curve: bivalent Co solution and azo dyes solution are added in ultrapure water, obtain potpourri A, then the pH value of potpourri A is adjusted to 4-8, the azo dyes in mensuration potpourri A, at the absorbance at characteristic peak place, is designated as a; In the potpourri A of gained, add peroxy-monosulfate standard sample, make peroxy-monosulfate form concentration gradient; Then potpourri A is carried out after decoloring reaction 0.5-5min, measure the rear azo dyes of decolouring at the absorbance at characteristic peak place, be designated as b; The difference of a and b of take is horizontal ordinate, and the peroxy-monosulfate standard sample concentration of take is ordinate, Criterion curve; Wherein, bivalent Co solution concentration is 10-150mmol/L, and azo dyes solution concentration is 0.25-5mmol/L; The volume ratio of bivalent Co solution, azo dyes solution and ultrapure water is (0.01-0.1): (0.01-0.15): 1; It is wherein said that to add peroxy-monosulfate to form concentration gradient be to instigate the final concentration of peroxy-monosulfate to reach 0,10,20,40,80,150,200,300,400,500,600,700,800 and 1000 μ mol/L;
Step 2: bivalent Co solution and azo dyes solution are added in ultrapure water, obtain mixture C, then the pH value of mixture C is adjusted to 4-8, the azo dyes in mensuration mixture C, at the absorbance at characteristic peak place, is designated as c; Wherein, bivalent Co solution concentration is 10-150mmol/L, and azo dyes solution concentration is 0.5-5mmol/L; The volume ratio of bivalent Co solution, azo dyes solution and ultrapure water is (0.01-0.1): (0.01-0.15): 1;
Step 3: add peroxy-monosulfate water sample to be measured to carry out decoloring reaction to the azo dyes in mixture C in the mixture C of gained in step 2, after reaction 0.5-5min, measure azo dyes after decolouring and, at the absorbance at characteristic peak place, be designated as d; Wherein, the volume ratio of peroxy-monosulfate water sample and mixture C is (0.001-0.15): 1;
Step 4: step 2 and the c of step 3 gained and the difference of d are brought in the typical curve formula of gained in step 1, calculate the content of peroxy-monosulfate in water sample to be measured.
The present invention comprises following beneficial effect:
The present invention compared with prior art, utilize divalence cobalt activation peroxy-monosulfate to produce sulfate radical free radical cracking azo dyes, when divalence cobalt and peroxy-monosulfate are added in the reactant liquor that contains azo dyes, divalence cobalt and peroxy-monosulfate first vigorous reaction generate sulfate radical free radical, then azo dyes and the free radical rapid reaction of generation sulfate radical decolouring.The sulfate radical free-radical oxidation reduction potential that divalence cobalt and permonosulphuric acid reactant salt produce is very high, up to 2.5～3.1V, therefore oxidisability is strong, can quantitatively decoloring reaction occur fast with the azo dyes of suboxides reduction potential, reaches the object of measuring the permonosulphuric acid salt content adding.In the reaction system of divalence cobalt, peroxy-monosulfate and azo dyes, by following 1～9 reaction equation, react:
The inventive method is simple, do not need additionally to carry out again aeration, ultraviolet irradiation, microwave irradiation, ultrasonic cavitation, additional electromagnetic field and heating steps, compare with traditional iodimetric titration, measurement result error has reduced 48%-83%, minute is shortened to and is only needed 1min by 30min, being applicable to pH value determination is that in 4-8, water sample, permonosulphuric acid salinity is in the scope of 0-500 μ mol/L, applied widely, and do not need expensive instrument and equipment and reagent, only need the spectrophotometer that a Daepori is logical, reduced cost.Assay method is widely used in the mensuration of peroxy-monosulfate in the repair process of the processing of surface water, the processing of industrial waste water and underground water and soil.
Accompanying drawing explanation
Fig. 1 is the typical curve making in embodiment 1;
Fig. 2 is the typical curve making in embodiment 2.
Embodiment
Embodiment one: the assay method of permonosulphuric acid salt content in a kind of water of present embodiment, it is to carry out according to the following steps:
Step 1: production standard curve: bivalent Co solution and azo dyes solution are added in ultrapure water, obtain potpourri A, then the pH value of potpourri A is adjusted to 4-8, the azo dyes in mensuration potpourri A, at the absorbance at characteristic peak place, is designated as a; In the potpourri A of gained, add peroxy-monosulfate standard sample, make peroxy-monosulfate form concentration gradient; Then potpourri A is carried out after decoloring reaction 0.5-5min, measure the rear azo dyes of decolouring at the absorbance at characteristic peak place, be designated as b; The difference of a and b of take is horizontal ordinate, and the peroxy-monosulfate standard sample concentration of take is ordinate, Criterion curve; Wherein, bivalent Co solution concentration is 10-150mmol/L, and azo dyes solution concentration is 0.25-5mmol/L; The volume ratio of bivalent Co solution, azo dyes solution and ultrapure water is (0.01-0.1): (0.01-0.15): 1; It is wherein said that to add peroxy-monosulfate to form concentration gradient be to instigate the final concentration of peroxy-monosulfate to reach 0,10,20,40,80,150,200,300,400,500,600,700,800 and 1000 μ mol/L;
Step 2: bivalent Co solution and azo dyes solution are added in ultrapure water, obtain mixture C, then the pH value of mixture C is adjusted to 4-8, the azo dyes in mensuration mixture C, at the absorbance at characteristic peak place, is designated as c; Wherein, bivalent Co solution concentration is 10-150mmol/L, and azo dyes solution concentration is 0.5-5mmol/L; The volume ratio of bivalent Co solution, azo dyes solution and ultrapure water is (0.01-0.1): (0.01-0.15): 1;
Step 3: add peroxy-monosulfate water sample to be measured to carry out decoloring reaction to the azo dyes in mixture C in the mixture C of gained in step 2, after reaction 0.5-5min, measure azo dyes after decolouring and, at the absorbance at characteristic peak place, be designated as d; Wherein, the volume ratio of peroxy-monosulfate water sample and mixture C is (0.001-0.15): 1;
Step 4: step 2 and the c of step 3 gained and the difference of d are brought in the typical curve formula of gained in step 1, calculate the content of peroxy-monosulfate in water sample to be measured.
Embodiment two: present embodiment is different from embodiment one, the bivalent Co described in step 1 and step 2 is a kind of in cobaltous sulphate, cobalt nitrate or cobalt chloride or several potpourris that are mixed by any ratio wherein.Other is identical with embodiment one.
Embodiment three: present embodiment is different from embodiment one or two, the described azo dyes described in step 1 and step 2 is methyl orange, methylene blue, rhodamine B, acid orange 2 or methyl violet.Other is identical with embodiment one or two.
Embodiment four: present embodiment is different from one of embodiment one to three, and the bivalent Co solution concentration described in step 1 and step 2 is 20-50mmol/L, and azo dyes solution concentration is 1-2mmol/L; The volume ratio of bivalent Co solution, azo dye solution and ultrapure water is (0.02-0.05): (0.05-0.1): 1.Other is identical with one of embodiment one to three.
Embodiment five: what present embodiment was different from one of embodiment one to four is, bivalent Co solution concentration described in step 1 and step 2 is 50mmol/L, and azo dyes solution concentration is 0.35mmol/L, 0.45mmol/L, 1.13mmol/L, 1.43mmol/L or 2.12mmol/L; The volume ratio of bivalent Co solution, azo dye solution and ultrapure water is 0.02:0.08:1.Other is identical with one of embodiment one to four.
Embodiment six: present embodiment is different from one of embodiment one to five, the peroxy-monosulfate standard sample described in step 1 is permonosulphuric acid potassium, permonosulphuric acid ammonium, permonosulphuric acid sodium or permonosulphuric acid calcium.Other is identical with one of embodiment one to five.
Embodiment seven: present embodiment is different from one of embodiment one to six, and the volume ratio of the peroxy-monosulfate water sample described in step 2 and potpourri is (0.002-0.1): 1.Other is identical with one of embodiment one to six.
Embodiment eight: present embodiment is different from one of embodiment one to seven, and the volume ratio of the peroxy-monosulfate water sample described in step 3 and potpourri is 0.02:1.Other is identical with one of embodiment one to seven.
Embodiment nine: present embodiment is different from one of embodiment one to eight, and the reaction time described in step 1 and step 3 is 1min.Other is identical with one of embodiment one to eight.
Embodiment 1:
The assay method of permonosulphuric acid salt content in a kind of water of the present embodiment, it is to measure in the steps below:
Step 1: production standard curve: cobalt sulfate solution and methyl orange solution are joined in ultrapure water, obtain potpourri A, then the pH value of potpourri A is adjusted to 5, the methyl orange in mensuration potpourri A, at the absorbance of 464nm, is designated as a; In the potpourri A solution of gained, add respectively permonosulphuric acid potassium standard sample, reaction cumulative volume is 10mL, makes permonosulphuric acid potassium form concentration gradient; Then potpourri A is carried out after decoloring reaction 1min, measure the rear methyl orange of decolouring at the absorbance of 464nm, be designated as b; The difference of a and b of take is horizontal ordinate, and the peroxy-monosulfate standard sample concentration of take is ordinate, Criterion curve; Wherein, cobalt sulfate solution concentration is 50mmol/L, and methyl orange solution concentration is 1.43mmol/L; The volume ratio of cobalt sulfate solution, methyl orange solution and ultrapure water is 0.02:0.08:1; It is wherein said that to add peroxy-monosulfate to form concentration gradient be to instigate the final concentration of permonosulphuric acid potassium to reach respectively 0,10,20,40,80,150,200,300,400,500,600,700,800 and 1000 μ mol/L;
Step 2: cobalt sulfate solution and 0.7mL methyl orange solution to adding 0.2mL in the ultrapure water body of 9mL, obtain mixture C, then the pH value of mixture C is adjusted to 5, measure methyl orange in potpourri A at the absorbance of 464nm, be designated as c; Wherein, cobalt sulfate solution concentration is 50mmol/L, and methyl orange solution concentration is 1.43mmol/L;
Step 3: add 0.1mL peroxy-monosulfate water sample to be measured to carry out decoloring reaction to the methyl orange in mixture C in the mixture C of gained in step 2, after reaction 1min, measure methyl orange after decolouring and, at the absorbance of 464nm, be designated as d;
Step 4: step 2 and the c of step 3 gained and the difference of d are brought in the typical curve formula of gained in step 1, calculate the content of peroxy-monosulfate in water sample to be measured.
As shown in Figure 1, gained formula is as follows for the typical curve of the present embodiment gained:
[permonosulphuric acid potassium]=62.495 △ A
464-1.487
△ A wherein
464difference for c and d.
The c that the present embodiment records is that 2.54, d is 1.23, brings in above-mentioned formula and calculates and finally show that in water sample, permonosulphuric acid salt content is 8.23mmol/L.
The present embodiment utilizes divalence cobalt activation peroxy-monosulfate to produce sulfate radical free radical cracking azo dyes, method is simple, measurement result error is little, do not need additionally to carry out again aeration, ultraviolet irradiation, microwave irradiation, ultrasonic cavitation, additional electromagnetic field and heating steps, minute is short, being applicable to pH value determination is that in 4-8, water sample, permonosulphuric acid salinity is in the scope of 0-500 μ mol/L, applied widely, and do not need expensive instrument and equipment and reagent, only need the spectrophotometer that a Daepori is logical, cost of determination is low.Assay method is widely used in the mensuration of peroxy-monosulfate in the repair process of the processing of surface water, the processing of industrial waste water and underground water and soil.
Embodiment 2:
The assay method of permonosulphuric acid salt content in a kind of water of the present embodiment, it is to measure in the steps below:
Step 1: production standard curve: cobalt sulfate solution and acid orange 2 solution are joined in ultrapure water, obtain potpourri A, then the pH value of potpourri A is adjusted to 5, the acid orange 2 in mensuration potpourri A, at the absorbance of 485nm, is designated as a; In the potpourri A solution of gained, add respectively permonosulphuric acid potassium standard sample, reaction cumulative volume is 10mL, makes permonosulphuric acid potassium form concentration gradient; Then potpourri A is carried out after decoloring reaction 1min, measure the rear acid orange 2 of decolouring at the absorbance of 485nm, be designated as b; The difference of a and b of take is horizontal ordinate, and the peroxy-monosulfate standard sample concentration of take is ordinate, Criterion curve; Wherein, cobalt sulfate solution concentration is 50mmol/L, and acid orange 2 solution concentrations are 2.12mmol/L; The volume ratio of cobalt sulfate solution, acid orange 2 solution and ultrapure water is 0.02:0.08:1; It is wherein said that to add peroxy-monosulfate to form concentration gradient be to instigate the final concentration of permonosulphuric acid potassium to reach respectively 0,10,20,40,80,150,200,300,400,500,600,700,800 and 1000 μ mol/L;
Step 2: cobalt sulfate solution and 0.7mL acid orange 2 solution to adding 0.2mL in the ultrapure water body of 9mL, obtain mixture C, then the pH value of mixture C is adjusted to 5, measure acid orange 2 in potpourri A at the absorbance of 485nm, be designated as c; Wherein, cobalt sulfate solution concentration is 50mmol/L, and acid orange 2 solution concentrations are 2.12mmol/L;
Step 3: add 0.1mL peroxy-monosulfate water sample to be measured to carry out decoloring reaction to the acid orange 2 in mixture C in the mixture C of gained in step 2, after reaction 1min, measure acid orange 2 after decolouring and, at the absorbance of 485nm, be designated as d;
Step 4: step 2 and the c of step 3 gained and the difference of d are brought in the typical curve formula of gained in step 1, calculate the content of peroxy-monosulfate in water sample to be measured.
As shown in Figure 2, gained formula is as follows for the typical curve of the present embodiment gained:
[permonosulphuric acid potassium]=86.518 △ A
485-0.4528.
△ A wherein
485difference for c and d.
The c that the present embodiment records is that 2.77, d is 1.81, brings in above-mentioned formula and calculates and finally show that in water sample, permonosulphuric acid salt content is 8.26mmol/L.
The present embodiment utilizes divalence cobalt activation peroxy-monosulfate to produce sulfate radical free radical cracking azo dyes, method is simple, measurement result error is little, do not need additionally to carry out again aeration, ultraviolet irradiation, microwave irradiation, ultrasonic cavitation, additional electromagnetic field and heating steps, minute is short, being applicable to pH value determination is that in 4-8, water sample, permonosulphuric acid salinity is in the scope of 0-500 μ mol/L, applied widely, and do not need expensive instrument and equipment and reagent, only need the spectrophotometer that a Daepori is logical, cost of determination is low.Assay method is widely used in the mensuration of peroxy-monosulfate in the repair process of the processing of surface water, the processing of industrial waste water and underground water and soil.
Claims (9)
1. an assay method for permonosulphuric acid salt content in water, is characterized in that it is to carry out according to the following steps:
Step 1: production standard curve: bivalent Co solution and azo dyes solution are added in ultrapure water, obtain potpourri A, then the pH value of potpourri A is adjusted to 4-8, the azo dyes in mensuration potpourri A, at the absorbance at characteristic peak place, is designated as a; In the potpourri A of gained, add peroxy-monosulfate standard sample, make peroxy-monosulfate form concentration gradient; Then potpourri A is carried out after decoloring reaction 0.5-5min, measure the rear azo dyes of decolouring at the absorbance at characteristic peak place, be designated as b; The difference of a and b of take is horizontal ordinate, and the peroxy-monosulfate standard sample concentration of take is ordinate, Criterion curve; Wherein, bivalent Co solution concentration is 10-150mmol/L, and azo dyes solution concentration is 0.25-5mmol/L; The volume ratio of bivalent Co solution, azo dyes solution and ultrapure water is (0.01-0.1): (0.01-0.15): 1; It is wherein said that to add peroxy-monosulfate to form concentration gradient be to instigate the final concentration of peroxy-monosulfate to reach 0,10,20,40,80,150,200,300,400,500,600,700,800 and 1000 μ mol/L;
Step 2: bivalent Co solution and azo dyes solution are added in ultrapure water, obtain mixture C, then the pH value of mixture C is adjusted to 4-8, the azo dyes in mensuration mixture C, at the absorbance at characteristic peak place, is designated as c; Wherein, bivalent Co solution concentration is 10-150mmol/L, and azo dyes solution concentration is 0.5-5mmol/L; The volume ratio of bivalent Co solution, azo dyes solution and ultrapure water is (0.01-0.1): (0.01-0.15): 1;
Step 3: add peroxy-monosulfate water sample to be measured to carry out decoloring reaction to the azo dyes in mixture C in the mixture C of gained in step 2, after reaction 0.5-5min, measure azo dyes after decolouring and, at the absorbance at characteristic peak place, be designated as d; Wherein, the volume ratio of peroxy-monosulfate water sample and mixture C is (0.001-0.15): 1;
Step 4: step 2 and the c of step 3 gained and the difference of d are brought in the typical curve formula of gained in step 1, calculate the content of peroxy-monosulfate in water sample to be measured.
2. the assay method of permonosulphuric acid salt content in a kind of water according to claim 1, is characterized in that the bivalent Co described in step 1 and step 2 is a kind of in cobaltous sulphate, cobalt nitrate or cobalt chloride or several potpourris that are mixed by any ratio wherein.
3. the assay method of permonosulphuric acid salt content in a kind of water according to claim 1, is characterized in that the described azo dyes described in step 1 and step 2 is methyl orange, methylene blue, rhodamine B, acid orange 2 or methyl violet.
4. the assay method of permonosulphuric acid salt content in a kind of water according to claim 1, is characterized in that the bivalent Co solution concentration described in step 1 and step 2 is 20-50mmol/L, and azo dyes solution concentration is 1-2mmol/L; The volume ratio of bivalent Co solution, azo dye solution and ultrapure water is (0.02-0.05): (0.05-0.1): 1.
5. the assay method of permonosulphuric acid salt content in a kind of water according to claim 1, it is characterized in that the bivalent Co solution concentration described in step 1 and step 2 is 50mmol/L, azo dyes solution concentration is 0.35mmol/L, 0.45mmol/L, 1.13mmol/L, 1.43mmol/L or 2.12mmol/L; The volume ratio of bivalent Co solution, azo dye solution and ultrapure water is 0.02:0.08:1.
6. the assay method of permonosulphuric acid salt content in a kind of water according to claim 1, is characterized in that the peroxy-monosulfate standard sample described in step 1 is permonosulphuric acid potassium, permonosulphuric acid ammonium, permonosulphuric acid sodium or permonosulphuric acid calcium.
7. the assay method of permonosulphuric acid salt content in a kind of water according to claim 1, the volume ratio that it is characterized in that the peroxy-monosulfate water sample described in step 2 and potpourri is (0.002-0.1): 1.
8. the assay method of permonosulphuric acid salt content in a kind of water according to claim 1, the volume ratio that it is characterized in that the peroxy-monosulfate water sample described in step 3 and potpourri is 0.02:1.
9. the assay method of permonosulphuric acid salt content in a kind of water according to claim 1, is characterized in that the reaction time described in step 1 and step 3 is 1min.
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| CN103592295B (en) | 2015-09-09 |
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