CN103018184A - Method for measuring trace amount of bromate in water - Google Patents
Method for measuring trace amount of bromate in water Download PDFInfo
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- CN103018184A CN103018184A CN2012104846443A CN201210484644A CN103018184A CN 103018184 A CN103018184 A CN 103018184A CN 2012104846443 A CN2012104846443 A CN 2012104846443A CN 201210484644 A CN201210484644 A CN 201210484644A CN 103018184 A CN103018184 A CN 103018184A
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Abstract
The invention relates to a method for measuring trace amount of bromate in water, and particularly relates to a method which utilizes victoria brilliant blue BO (VPBBO) containing an emulsifying agent OP as a color-developing agent and utilizes a spectrophotometric method to measure trace amount of bromate in water. The method comprises the following steps of successively adding 25.0mL of a water sample to be measured, 3.0mL of 0.1mol.L-1 of hydrochloric acid solution and 2.0mL of 0.05 mol.L-1 of solution KI, successively adding 5.0mL of phosphoric acid-sodium dihydrogen phosphate buffer solution with the pH value being 1.9+/-0.1 and 5.0mL of 2.0*10-4mol.L-1 victoria blue BO containing 0.4g.L-1 of emulsifying agent OP after 5min; carrying out constant volume by utilizing distilled water, shaking up, using a color comparison dish being 1cm after 2min, adopting a reagent blank as a reference, and measuring the absorbance of a solution at 580nm wavelength; and calculating the concentration of the bromate ion by using a regression equation according to a standard work curve, namely A=1.40*10-3C (mu g.L-1)-7.11*1.0-4 (r is equal to 0.9995, the linear range is 0-260 mug.L, A is optical density, and C is concentration of bromate ion). The method provided by the invention has the advantages that the sensitivity is high, the result is exact, the operation is simple and convenient, and the cost is low.
Description
Technical field
The present invention relates to a kind of assay method of underwater trace bromate, be particularly related to the Victoria pure blue BO(VPB-BO that a kind of usefulness contains polyoxyethylene nonylphenol ether) (C.I.42595 molecular weight 513.5) as developer, with the method for trace amounts of bromine hydrochlorate in the water by Spectrophotometry.
Background technology
Chlorination is the disinfection of tap water technology that China generally adopts at present, but the method can produce multiple accessory substance, and such as methenyl choloride and poisonous chloracetic acid etc. can consist of potential threat to health.Therefore, people turn on other sterilization methods gradually.Ozone is applied to the beginning of this century as sanitizer, is one of the most effective sanitizer in the present known chemosterilant, and the various microorganisms in the water are had good removal effect.The advantage of ozone disinfection is a lot, and it has avoided the problems such as chlorine residue that chlorination produces and accessory substance, and sterilization speed is fast, Disinfection Effect is good, hidden spore and giardia lamblia killing rate to anti-chlorine are high, and mouthfeel also is better than chlorination water after the sterilization, and therefore present application is more and more wider.But when containing bromide in the water body, ozonization can produce the inorganic byproduct bromate.Bromate is a kind of strong oxidizer, and excessive drinking has carcinogenic risk to the people.Studies show that the bromate concentration in potable water reaches 3.0 μ gL
-1 and 30 μ gL
-1The time, the carcinogenic risk of human body is respectively 0.01 ‰, 0.1 ‰, therefore be decided to be the potential carcinogen of 2B level by international cancer research institution (IARC).For the standard drinking water quality, the content that the natural mineral water standard (GB 8537-2008) of China's revision in 2008 limits bromate in the mineral water is no more than 10 μ gL
-1But random inspection of products quality is the result show, bromate content overproof situation happens occasionally.
The detection method of bromate in drinking water mainly contains titrimetry, inductively coupled plasma mass spectrometry (ICP-MS), the chromatography of ions and spectrophotometric method etc. at present.Accuracy and the sensitivity of titrimetry are low; The ICP-MS method is subject to bromoacetic acid and disturbs, and it is not high to detect degree of accuracy; The chromatography of ions is owing to need large capacity separating column, and testing cost is higher, and in addition, it also is subject to inorganic chlorine ion interference in the water, and it is not high to detect degree of accuracy yet; The apparent molar absorption coefficient of the used developer of tradition spectrophotometric method is lower, causes detection sensitivity low, can not measure trace amounts of bromine hydrochlorate in the potable water by accurate quantitative analysis, so the application of these methods is subject to certain restrictions all.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, a kind of method of measuring the underwater trace bromate is provided, it is characterized in that, the Victoria pure blue BO that adopts a kind of usefulness to contain polyoxyethylene nonylphenol ether makes trace amounts of bromine hydrochlorate in the water by Spectrophotometry of developer, comprises the steps:
1. the drafting of standard working curve: pipette 500 μ gL
-1Potassium bromate standard solution 0.0mL, 0.2mL, 0.5mL, 1.0mL, 2.0mL, 4.0mL, 6.0mL, 8.0mL inject respectively the brown volumetric flask of 8 50mL, add successively 0.1molL
-1Hydrochloric acid solution 3.0mL, 0.05molL
-1KI solution 2.0mL, add successively the pH value behind the 5min and be 1.9 ± 0.1 damping fluid 5.0mL, contain 2.0 * 10 of polyoxyethylene nonylphenol ether
-4MolL
-1Victoria blue BO 5.0mL, use the distilled water constant volume, shake up, the colour developing 2～15min after, use the 1cm cuvette, make reference with reagent blank, measure the absorbance of solution in 580nm wavelength place, take absorbance as ordinate, take bromate ion concentration as horizontal ordinate, the drawing standard working curve;
2. the foundation of regression equation: the standard working curve according to step (1) obtains regression equation: A=1.40 * 10
-3C (μ gL
-1)-7.11 * 10
-4(r=0.9995, the range of linearity is 0～260 μ gL
-1, A is absorbance, C is the concentration of bromate ion, apparent molar absorption coefficient ε=1.79 * 10
5Lmol
-1Cm
-1);
3. the mensuration of bromate: in the brown volumetric flask of 50mL, add successively water sample 25.0mL to be measured, 0.1molL
-1Hydrochloric acid solution 3.0mL, 0.05molL
-1KI solution 2.0mL, add successively the pH value behind the 5min and be 1.9 ± 0.1 damping fluid 5.0mL, contain 2.0 * 10 of polyoxyethylene nonylphenol ether
-4MolL
-1Victoria blue BO 5.0mL, use the distilled water constant volume, shake up, as the mensuration system, behind colour developing 2～15min, use the 1cm cuvette, make reference with reagent blank, measure the absorbance of solution in 580nm wavelength place, go out the concentration of bromate ion according to the regression equation calculation of step (2) gained.
In addition, the pH value of mensuration system of the present invention is 1.7～2.1; Described damping fluid is monophosphate monophosphate sodium dihydrogen damping fluid; The concentration range of Victoria pure blue BO is 1.0 * 10 in the described mensuration system
-5～3.0 * 10
-5MolL
-1The concentration that contains polyoxyethylene nonylphenol ether in the described developer Victoria pure blue BO aqueous solution is 0.4gL
-1The concentration range of iodide ion is 1.0 * 10 in the described mensuration system
-3～3.0 * 10
-3Mol.
L-1Described developing time is 2min.Further, in the step 3, also comprise, if bromate ion concentration exceeds the range of linearity of regression equation, dilute afterwards first and measure.
Coexisting ion may exert an influence to result of study in the mensuration system.Studies show that, work as BrO
3 -Concentration is 20 μ gL
-1, relative error is less than ± 5% the time, and following ion allowance is (with mg.L
-1Meter): K
+, Na
+, Ca
2+, Sn
2+, Al
3+, Pb
2+, NO
3 -, SO
4 2-, H
2PO
4 -, NH
4 +, Br
-, Ac
-, HC
2O
4 -, H
2BO
3 -, H
4P
3O
10 -, citrate (500), Ni
2+, Cu
2+, Co
2+, Mn
2+, Cr
3+(100), Cl
-(2000), Fe
3+(100), F
-(10), silicic acid hydrogen root (250), Ag
+(0.01), Hg
2+(0.01), Cd
2+(0.01).This shows, except by heavy metal Hg
2+, Cd
2+, Ag
+And F
-The sample of severe contamination, common ion does not produce interference to measuring.
The invention effect
Because the present invention adopts Victoria pure blue BO as developer, newly-established spectrophotometric method apparent molar absorption coefficient has improved the sensitivity of traditional spectrophotometric method greatly up to 105 orders of magnitude.Simultaneously, common ion does not produce interference to the result who measures by this method in the solution, and this experimental result has shown that this method has stronger antijamming capability.In addition, because the used detecting instrument of this method is cheap spectrophotometer, need not the checkout equipment of complexity, costliness, testing process is simple, and detection speed is fast, and testing cost is cheaper, is conducive to popularizing and promoting of method.
Embodiment
Below in conjunction with embodiment a kind of method of measuring the underwater trace bromate of the present invention is described further:
Measuring principle of the present invention is as described below:
In the acid solution that has the excess iodine ion, treat that the trace bromate ion in the test sample can be oxidized to I with the part iodide ion
2, I
2Iodide ion reaction with excessive finally is converted into I
3 -Negative ion.In pH is phosphoric acid-sodium dihydrogen phosphate buffer of 1.9 ± 0.1, I
3 -Negative ion reacts the ionic associate that generates cobalt blue with the victoria blue BO that contains non-ionic surfactant OP.This associated matter absorption peak is at 580nm wavelength place, and its apparent molar absorption coefficient can be up to 10
5The order of magnitude is so can obtain the concentration of bromate ion in the solution by the absorbance of measuring solution.
It is pure that the selected reagent of the present invention is analysis.
In the present embodiment, in order to improve as far as possible sensitivity, adopt Victoria pure blue BO as developer, and with polyoxyethylene nonylphenol ether as stabilizing agent, thereby make colour developing associated matter apparent molar absorption coefficient up to 10
5The order of magnitude is convenient to the concentration with trace bromate ion in the water by Spectrophotometry.
Implementation process of the present invention is described below:
1. the preparation of reaction reagent: victoria blue BO solution: commercial dye is refining through hot water, and 80 ℃ of oven dry are configured to 2.0 * 10 after the constant weight
-4MolL
-1Solution (containing the 0.4g polyoxyethylene nonylphenol ether in every liter of solution).Phosphoric acid-sodium dihydrogen phosphate buffer: 0.6molL
-1(using pHS-2C type precision acidity meter that its pH value is transferred to 1.9 ± 0.1), liquor kalii iodide: 0.05molL
-1, take by weighing potassium iodide (A.R) 0.83g and be diluted to 100mL after with dissolved in distilled water.
2. the drafting of standard working curve: pipette 500 μ gL
-1Potassium bromate standard solution 0.0mL, 0.2mL, 0.5mL, 1.0mL, 2.0mL, 4.0mL, 6.0mL, 8.0mL inject respectively the brown volumetric flask of 8 50mL, add successively 0.1molL
-1Hydrochloric acid solution 3.0mL, 0.05molL
-1KI solution 2.0mL, add successively the pH value behind the 5min and be 1.9 ± 0.1 phosphoric acid-sodium dihydrogen phosphate buffer 5.0mL, contain 0.4gL
-12.0 * 10 of polyoxyethylene nonylphenol ether
-4MolL
-1Victoria blue BO 5.0mL, use the distilled water constant volume, shake up.Behind the colour developing 2min, use the 1cm cuvette, make reference with reagent blank, measure the absorbance of solution in 580nm wavelength place, take absorbance as ordinate, take bromate ion concentration as horizontal ordinate, the drawing standard working curve.
3. the foundation of regression equation: obtain regression equation: A=1.40 * 10 according to standard working curve
-3C (μ gL
-1)-7.11 * 10
-4(r=0.9995, the range of linearity is 0～260 μ gL
-1, A is absorbance, C is the concentration of bromate solution, apparent molar absorption coefficient ε=1.79 * 10
5Lmol
-1Cm
-1).
4. the mensuration of bromate ions in drinking water: pipette respectively bottled mineral water 1, bottled mineral water 2 and commercially available drummed pure water 25.0mL in the brown volumetric flask of 50mL with transfer pipet, add successively 0.1molL
-1Hydrochloric acid solution 3.0mL, 0.05molL
-1KI solution 2.0mL, add successively the pH value behind the 5min and be 1.9 ± 0.1 phosphoric acid-sodium dihydrogen phosphate buffer 5.0mL, contain 0.4gL
-12.0 * 10 of polyoxyethylene nonylphenol ether
-4MolL
-1Victoria blue BO 5.0mL, use the distilled water constant volume, shake up, behind the colour developing 2min, use the 1cm cuvette, make reference with reagent blank, in the absorbance of 580nm wavelength place mensuration solution.Go out the concentration of bromate ion according to regression equation calculation.Each sample is done parallel recovery test altogether 8 times, and calculate recovery rate and RSD the results are shown in Table 1.
The measurement result of bromate in table 1. sample
As shown in Table 1, the bromate ion concentration determination value of mineral water 1, mineral water 2 is all less than 10.00 μ gL
-1, be lower than national standard, be qualified water sample, and commercially available drummed pure water measured value is 13.90 μ gL
-1, be higher than national standard, be defective water sample.All water samples are all done parallel recovery experiment 8 times, and experimental result shows that this method testing result is accurate, as a result favorable reproducibility.
Claims (7)
1. a method of measuring the underwater trace bromate is characterized in that, comprises following determination step:
(1). the drafting of standard working curve:
Pipette 500 μ gL
-1Potassium bromate standard solution 0.0mL, 0.2mL, 0.5mL, 1.0mL, 2.0mL, 4.0mL, 6.0mL, 8.0mL inject respectively the brown volumetric flask of 8 50mL, add successively 0.1molL
-1Hydrochloric acid solution 3.0mL, 0.05molL
-1KI solution 2.0mL, add successively the pH value behind the 5min and be 1.9 ± 0.1 damping fluid 5.0mL, contain 2.0 * 10 of polyoxyethylene nonylphenol ether
-4MolL
-1Victoria blue BO 5.0mL, use the distilled water constant volume, shake up, the colour developing 2～15min after, use the 1cm cuvette, make reference with reagent blank, measure the absorbance of solution in 580nm wavelength place, take absorbance as ordinate, take bromate ion concentration as horizontal ordinate, the drawing standard working curve;
(2). the foundation of regression equation:
Standard working curve according to step (1) obtains regression equation: A=1.40 * 10
-3C (μ gL
-1)-7.11 * 10
-4(r=0.9995, the range of linearity is 0～260 μ gL
-1, A is absorbance, C is the concentration of bromate ion, apparent molar absorption coefficient ε=1.79 * 10
5Lmol
-1Cm
-1);
(3). the mensuration of bromate:
In the brown volumetric flask of 50mL, add successively water sample 25.0mL to be measured, 0.1molL
-1Hydrochloric acid solution 3.0mL, 0.05molL
-1KI solution 2.0mL, add successively the pH value behind the 5min and be 1.9 ± 0.1 damping fluid 5.0mL, contain 2.0 * 10 of polyoxyethylene nonylphenol ether
-4MolL
-1Victoria blue BO 5.0mL, use the distilled water constant volume, shake up, as the mensuration system, behind colour developing 2～15min, use the 1cm cuvette, make reference with reagent blank, measure the absorbance of solution in 580nm wavelength place, go out the concentration of bromate ion according to the regression equation calculation of step (2) gained.
2. as claimed in claim 1, the pH value that it is characterized in that the system of measuring is 1.7～2.1, and damping fluid is phosphoric acid-phosphate sodium dihydrogen buffer solution.
3. the concentration range that as claimed in claim 1, it is characterized in that Victoria pure blue BO in the mensuration system is 1.0 * 10
-5～3.0 * 10
-5MolL
-1
4. the concentration that as claimed in claim 1, it is characterized in that containing in the developer Victoria pure blue BO aqueous solution polyoxyethylene nonylphenol ether is 0.4gL
-1
5. the concentration range that as claimed in claim 1, it is characterized in that iodide ion in the mensuration system is 1.0 * 10
-3～3.0 * 10
-3MolL
-1
6. as claimed in claim 1, it is characterized in that developing time is 2min.
7. as claimed in claim 1, it is characterized in that diluting afterwards first and measuring if bromate ion concentration exceeds the range of linearity of regression equation.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210484644.3A CN103018184B (en) | 2012-11-23 | 2012-11-23 | A kind of method measuring underwater trace bromate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210484644.3A CN103018184B (en) | 2012-11-23 | 2012-11-23 | A kind of method measuring underwater trace bromate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104406950A (en) * | 2014-12-11 | 2015-03-11 | 福州大学 | Fluorescence analysis method for simultaneously measuring bromate and chlorite |
| CN114814070A (en) * | 2022-03-25 | 2022-07-29 | 拱北海关技术中心 | Method for measuring bromate content in drinking water |
-
2012
- 2012-11-23 CN CN201210484644.3A patent/CN103018184B/en not_active Expired - Fee Related
Non-Patent Citations (2)
| Title |
|---|
| 刘贞，崔艳，胡志军: "紫外分光光度法测定水中微量溴酸盐的含量", 《中国无机分析化学》, vol. 2, no. 2, 15 June 2012 (2012-06-15) * |
| 施文健: "用维多利亚蓝BO作显色剂光度法测定微量碘", 《理化检验-化学分册》, vol. 42, no. 2, 18 February 2006 (2006-02-18) * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104406950A (en) * | 2014-12-11 | 2015-03-11 | 福州大学 | Fluorescence analysis method for simultaneously measuring bromate and chlorite |
| CN114814070A (en) * | 2022-03-25 | 2022-07-29 | 拱北海关技术中心 | Method for measuring bromate content in drinking water |
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| Publication number | Publication date |
|---|---|
| CN103018184B (en) | 2015-12-23 |
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