CN108061719A - The quick reagent component and method for measuring permanganate index in water - Google Patents
The quick reagent component and method for measuring permanganate index in water Download PDFInfo
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- CN108061719A CN108061719A CN201711148062.7A CN201711148062A CN108061719A CN 108061719 A CN108061719 A CN 108061719A CN 201711148062 A CN201711148062 A CN 201711148062A CN 108061719 A CN108061719 A CN 108061719A
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- 239000003153 chemical reaction reagent Substances 0.000 title claims abstract description 149
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 110
- 238000000034 method Methods 0.000 title claims abstract description 38
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 90
- 239000011668 ascorbic acid Substances 0.000 claims abstract description 44
- 235000010323 ascorbic acid Nutrition 0.000 claims abstract description 44
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 44
- 238000001514 detection method Methods 0.000 claims abstract description 33
- 239000012286 potassium permanganate Substances 0.000 claims abstract description 24
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- 230000029087 digestion Effects 0.000 claims abstract description 18
- 230000003647 oxidation Effects 0.000 claims abstract description 18
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 18
- 239000002253 acid Substances 0.000 claims abstract description 17
- 230000031700 light absorption Effects 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 8
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 8
- 238000007865 diluting Methods 0.000 claims abstract description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 25
- 239000003638 chemical reducing agent Substances 0.000 claims description 11
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 6
- GDSOZVZXVXTJMI-SNAWJCMRSA-N (e)-1-methylbut-1-ene-1,2,4-tricarboxylic acid Chemical compound OC(=O)C(/C)=C(C(O)=O)\CCC(O)=O GDSOZVZXVXTJMI-SNAWJCMRSA-N 0.000 claims description 5
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 5
- 150000003839 salts Chemical class 0.000 claims description 5
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 claims 1
- 229930003268 Vitamin C Natural products 0.000 claims 1
- 235000019154 vitamin C Nutrition 0.000 claims 1
- 239000011718 vitamin C Substances 0.000 claims 1
- 239000000243 solution Substances 0.000 description 64
- 238000012360 testing method Methods 0.000 description 30
- 238000004458 analytical method Methods 0.000 description 14
- 239000011259 mixed solution Substances 0.000 description 8
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 6
- 238000002835 absorbance Methods 0.000 description 5
- 238000007789 sealing Methods 0.000 description 5
- 238000002798 spectrophotometry method Methods 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 230000035945 sensitivity Effects 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 2
- 108090000913 Nitrate Reductases Proteins 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 230000001419 dependent effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 238000002203 pretreatment Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 230000001988 toxicity Effects 0.000 description 2
- 231100000419 toxicity Toxicity 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- OQVYMXCRDHDTTH-UHFFFAOYSA-N 4-(diethoxyphosphorylmethyl)-2-[4-(diethoxyphosphorylmethyl)pyridin-2-yl]pyridine Chemical compound CCOP(=O)(OCC)CC1=CC=NC(C=2N=CC=C(CP(=O)(OCC)OCC)C=2)=C1 OQVYMXCRDHDTTH-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000005562 fading Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000004401 flow injection analysis Methods 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 150000002697 manganese compounds Chemical class 0.000 description 1
- 239000010841 municipal wastewater Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 238000005375 photometry Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000001568 sexual effect Effects 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 239000002352 surface water Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
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- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (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 Analysing Materials By The Use Of Chemical Reactions (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses the reagent components and method of permanganate index in a kind of quick measure water.The reagent component includes reagent A and reagent B, and reagent A includes quantitative potassium permanganate, and reagent B includes quantitative ascorbic acid.The method of the present invention includes the following steps：The water sample to be measured for diluting n times (n >=1), volume is L is mixed in acid condition with reagent A, heating reaction a period of time postcooling obtains digestion solution, contains excessive potassium permanganate in digestion solution；Reagent B is added in into digestion solution, reducing solution is obtained after reaction, contains excessive ascorbic acid in reducing solution；A characteristic wavelength λ is chosen in the wave-length coverage of 190nm~260nm, by detecting light absorption value of the reducing solution at characteristic wavelength λ, ascorbic acid in reducing solution and its oxidation product are quantitative determined, according to the linear relationship of the synthesis response of ascorbic acid and its oxidation product and permanganate index in detection water sample, the permanganate index of water sample to be measured is obtained.
Description
Technical field
The present invention relates to a kind of reagent components of permanganate index in Water quality detection more particularly to quick measure water
And method.
Background technology
Permanganate index refers under certain condition, with potassium permanganate (KMnO4) it is oxidant, disappeared when handling water sample
The amount of the oxidant of consumption, can reducing substances (mainly organic matter) pollution level in concentrated expression water body.Therefore, the index quilt
It is widely used in surface water quality analysis.
At present, the test method of permanganate index mainly has volumetric method, electrochemical process, gas molecule in space absorption process, flowing
Injection and spectrophotometry.
Volumetric method is to measure the classical analysis method of permanganate index, has accuracy height, favorable reproducibility, agents useful for same
It is easily obtained with instrument and equipment, is a kind of more satisfactory analysis method.But the method exists, and time-consuming, analysis personnel labor intensity
The shortcomings of big.Li Li etc. (discussion [J] the Hebei Agricultures science and technology of permanganate index (acid process) assay method, 2009,13
(8):165-166,170) it is adjusted by reaction acidity, reduce the reaction time, but for actual sample, change resolution condition
Large error can be generated.
Electrochemical process largely improves analysis efficiency, but the linear relationship of electric current and permanganate index compared with
Difference, and for actual sample, proportionate relationship might have larger difference.
Gas molecule in space absorption process and Flow Injection Analysis realize the automatic continuous analysis of permanganate index, and and volumetric method
With higher comparativity, but equipment is costly, is unfavorable for method popularization.
Spectrophotometry preferably compensate for more than deficiency, have that equipment investment is low, high sensitivity, precision are good, reagent
With amount of samples it is few, quick time saving the features such as.Mainly there are two major classes at present：Direct measuring method and Indirect Determination.Directly measure
Method is analyzed using the color fading reaction of permanganate, but since potassium permanganate can generate particle during heated oxide,
And particulate generation is unstable, is affected to test result；Indirect Determination using nitrite or ferrous salt as reducing agent,
Excessive permanganate after reduction resolution, by testing extra reduction agent content come indirectly testing permanganate index.But
During analysis complexity water sample, easily disturbed by factors such as colourity, turbidity, and analytical reagent has certain toxicity.
The content of the invention
For overcome the deficiencies in the prior art, one of the objects of the present invention is to provide permanganic acid in a kind of quick measure water
The reagent component of salt index.
The second object of the present invention is in a kind of method of the permanganate index in quick measure water is provided.
An object of the present invention adopts the following technical scheme that realization：
The reagent component of permanganate index in a kind of quick measure water, including reagent A and reagent B, the reagent A bag
Quantitative potassium permanganate is included, the reagent A is suitable for mixing with water sample to be measured under sour environment, to aoxidize reproducibility object therein
Matter；The reagent B includes quantitative reducing agent, is suitable for adding in the solution after clearing up, for reducing excessive potassium permanganate,
And the reagent B is excessive, which is characterized in that the reducing agent in the reagent B is ascorbic acid.
Further, the reagent A is liquor potassic permanganate, and concentration is 0.01~0.1mol/L；The reagent B is anti-
Bad hematic acid solution, concentration are 1~5g/L.
Further, phosphoric acid is further included in the reagent B, is used to improve the stability of ascorbic acid, the reagent B is put
In the container with shade function.
Further, the reagent component further includes reagent C, and the reagent C is calibrated solution for permanganate index, is used for
Prepare standard water sample known to permanganate index.
Further, the reagent component further includes reagent D, and the reagent D is sulfuric acid solution, the reagent D be suitable for
The reagent A is mixed to form the acid permanganate soln needed for resolution.
The second object of the present invention adopts the following technical scheme that realization：
The water sample to be measured for diluting n times (n >=1), volume is L is mixed in acid condition with reagent A, one section of heating reaction
Time postcooling obtains digestion solution, contains excessive potassium permanganate in the digestion solution；
Reagent B is added in into the digestion solution, reducing solution is obtained after reaction, contains excess in the reducing solution
Ascorbic acid；
A characteristic wavelength λ is chosen in the wave-length coverage of 190nm~260nm, by detecting the reducing solution described
Light absorption value at characteristic wavelength λ quantitative determines the ascorbic acid in the reducing solution and its oxidation product, according to anti-
The linear relationship of the synthesis response of bad hematic acid and its oxidation product and permanganate index in detection water sample, obtains water sample to be measured
Permanganate index.
Further, the synthesis response of ascorbic acid and its oxidation product and height in detection water sample in the reducing solution
The linear relationship of mangaic acid salt index is calculated using standard water sample known to permanganate index.
Further, the synthesis response of ascorbic acid and its oxidation product and height in detection water sample in the reducing solution
The linear equation of mangaic acid salt index is obtained by following steps：
(1) standard water sample known to pure water and permanganate index is provided, the permanganate index of standard water sample is remembered
For x；
(2) volume is mixed for the pure water of L or the standard water sample with reagent A, it is cold after heating reaction a period of time
But, the first solution is obtained, reads light absorption value A1 of first solution at the characteristic wavelength λ；
(3) reagent B is added in into first solution, the second solution is obtained after reaction, reads second solution in institute
State the light absorption value A2 at characteristic wavelength λ；
(4) when in the step (2) being pure water, permanganate index zero, A2-A1=c at this time；When the step
(2) when being standard water sample in, x and (A2-A1-c) are in a linear relationship, i.e. (A2-A1-c)=ax+b, utilize the A2's and A1 measured
Numerical value carries out fitting a straight line, obtains the value of a, b.
Further, read light absorption value A1 at the characteristic wavelength λ of the digestion solution and the reducing solution,
A2 brings the value of A1 and A2 in formula (A2-A1-c)=ax+b into, and the permanganate index for obtaining water sample to be measured is nx.
Further, the water sample to be measured is by the water sample of pretreatment, and pre-treatment step is：It is added in into water sample appropriate
Sulfuric acid solution, the pH value for making sample are 1~2.
Compared with prior art, the beneficial effects of the present invention are：
(1) using during permanganate index, detection efficiency is high, surveys in reagent component or detection method the detection water of the present invention
10 samples are tried, can be completed within 40 minutes or so, and in the prior art, 10 samples are detected, then need or so 2 hours；
(2) reagent that reagent component of the invention provides is environmentally friendly, safe；
(3) the ultraviolet light wave band of detection method of the invention in 190nm~260nm has good linear dependence, no
Co-wavelength lower linear related coefficient is 0.99~0.9999, and linearly dependent coefficient reaches more than 0.999 and accounts for 60%, and user can
To select different wavelength, to reduce the influence of interfering material (the nitrogen characteristic absorption peak for such as avoiding 220nm wave bands), this hair
Bright detection method high sensitivity is adapted to the test needs of various concentration water sample；
(4) detection method of the invention has extremely low detection limit and higher sensitivity, and detection range is wide, can quantify
Analyze the permanganate index (calculating upper limit of detection with 10 times of extension rates) of 0.05~80.0mg/L concentration；
(5) detection method of the invention is analyzed in ultraviolet band, avoids the influence of colourity；
(6) since low manganese compound is dissolved in ascorbic acid solution, avoid potassium permanganate and be reduced the turbidity shadow brought
It rings；
(7) detection method of the invention adds the background test of sample to be tested, avoids in water and do before reducing agent is added
Disturb the influence of substance；
(8) detection method of the invention avoids ferro element presence pair in water compared with ferrous salt does the method for reducing agent
The influence of test.
Specific embodiment
In the following, with reference to specific embodiment, the present invention is described further, it is necessary to which explanation is, what is do not collided
Under the premise of, new embodiment can be formed between various embodiments described below or between each technical characteristic in any combination.
The present invention provides a kind of reagent component of permanganate index in quick measure water, including reagent A and reagent B；
The reagent A includes quantitative potassium permanganate, and the reagent A is suitable for mixing with water sample to be measured under sour environment, to aoxidize it
In reducing substances；The reagent B includes quantitative ascorbic acid, be suitable in the solution after addition resolution (namely it is to be measured
In solution after water sample and reagent A reaction), excessive potassium permanganate is reduced, wherein ascorbic acid is excessive.
Reagent component provided by the invention and the main distinguishing feature of the prior art are to have used ascorbic acid as reduction
Agent.In the prior art, in permanganate index in measuring water, usually using ferrous salt or nitrite as reducing agent, but
It is using after ferrous salt or the potassium permanganate of nitrate reductase excess, it is also necessary to add in other reagents and excessive ferrous salt
Or nitrite reaction, and then excessive ferrous salt or nitrite are measured, this allows for detection method complexity, less efficient.
Inventor has found that in the range of wavelength is 190nm~260nm, " ascorbic acid and ascorbic acid are by oxygen in solution
The content of product (hereinafter referred to as ascorbic acid and its oxidation product) after change " and the linear positive correlation of absorbance, therefore can
To measure the ascorbic acid and its oxidation product in solution using ultraviolet spectrophotometry direct quantitative.On the other hand, in solution
Ascorbic acid and its oxidation product content and water sample to be measured in permanganate index be linear relationship.Therefore, in wavelength
In the range of 190nm~260nm, the light absorption value of ascorbic acid and its oxidation product and the permanganate index in water sample to be measured
For linear relationship, and the linear relationship can utilize the standard solution the Fitting Calculation of known permanganate index, utilize the line
Sexual intercourse, and according to the light absorption value of solution after ultraviolet spectrophotometry detection reaction, it is possible to obtain permanganate index.
The present invention use ascorbic acid as reducing agent measure permanganate index method compared with prior art, be not required to
The excessive reducing agent of detection is quantified using additional reagent, detection method is simple, at low cost.It is in addition, provided by the invention
Reagent component can be completed to test, avoids interference of traditional spectrophotometry there are colourity and turbidity in ultraviolet band.
In addition, the quantitative reaction of ascorbic acid and potassium permanganate is very fast, it can complete in 1~2min, contract significantly
The time of short analysis, provide efficiency.
In addition, ascorbic acid reduces secondary pollution of the analytic process to environment, also improves analysis and survey without overt toxicity
The security of examination.
The reagent A of the present invention and reagent B can be solution form or solid form.
When reagent A and reagent B are solid forms, can place it in respectively in the graduated test tube of mark.When in use,
Quantitative pure water is added in into test tube, and then certain density liquor potassic permanganate and ascorbic acid solution is prepared.
In order to ensure the accuracy of Accuracy of Permanganate Index Determination, it is preferable to provide the reagent A of solution form and reagent B.It is excellent
Selection of land, the concentration of potassium permanganate is 0.01~0.1mol/L in reagent A, and the concentration of ascorbic acid is 1~5g/L in reagent B.
Phosphoric acid is further included in the reagent B, is used to improve the stability of ascorbic acid.It is meanwhile anti-to further improve
The stability of bad hematic acid, the reagent B are placed in the container with shade function.
The reagent component further includes reagent C, and the reagent C calibrates solution for permanganate index, for preparing Gao Meng
Standard water sample known to hydrochlorate index.
The reagent component further includes reagent D, and the reagent D is sulfuric acid solution, and the reagent D is suitable for and the reagent A
It is mixed to form the acid permanganate soln needed for resolution.Why liquor potassic permanganate and sulfuric acid solution are provided separately, it is main
If in view of potassium permanganate with sulfuric acid incorporation time is long to react, decompose potassium permanganate, influence final detection
As a result.Certainly, reagent component of the invention can not also provide reagent D, when actually detected, be provided for oneself by user.
It is noted that the quality or volume or concentration of each reagent can be adjusted as needed, as long as ensureing high
The amount that potassium manganate and ascorbic acid add in is understood and potassium permanganate is excessive during resolution, reduction when ascorbic acid excess, until
It is how many in concrete content, will be readily apparent for those skilled in the art, therefore the present invention is not to containing specifically
Amount is defined, and different content reagent each falls within protection scope of the present invention.
Further, the reagent A and reagent D are placed in high-boron-silicon glass test tube, the high-boron-silicon glass test tube choosing
With screw-cap test tube, reagent is not easy to reveal.
Further, the reagent B is placed in the container with shade function, is such as stored in brown bottle or in Reagent Tube
Outer setting black light-shielding sheet.
Further, the reagent component further includes test tube and stands frame, convenient for users to placing each reagent.
Further, the reagent component further includes environment-protective sealing bag, for collecting waste liquid and test tube after testing.Institute
It states environment-protective sealing bag and uses 8 or more PE materials.
The present invention provides a kind of method for quickly measuring permanganate index in water using reagent component described above, including
The water sample to be measured for diluting n times (n >=1), volume is L is mixed in acid condition with reagent A, one section of heating reaction
Time postcooling obtains digestion solution, contains excessive potassium permanganate in the digestion solution；
Reagent B is added in into the digestion solution, reducing solution is obtained after reaction, contains excess in the reducing solution
Ascorbic acid；
A characteristic wavelength λ is chosen in the wave-length coverage of 190nm~260nm, by detecting the reducing solution described
Light absorption value at characteristic wavelength λ quantitative determines the ascorbic acid in the reducing solution and its oxidation product, according to anti-
The linear relationship of the synthesis response of bad hematic acid and its oxidation product and permanganate index in detection water sample, obtains water sample to be measured
Permanganate index.
The synthesis response of ascorbic acid and its oxidation product refers to permanganate in detection water sample in the reducing solution
Several linear relationships is calculated using standard water sample known to permanganate index.
The synthesis response of ascorbic acid and its oxidation product refers to permanganate in detection water sample in the reducing solution
Several linear equations are obtained by following steps：
(1) standard water sample known to pure water and permanganate index is provided, the permanganate index of standard water sample is remembered
For x；
(2) volume is mixed for the pure water of L or the standard water sample with reagent A, it is cold after heating reaction a period of time
But, the first solution is obtained, reads light absorption value A1 of first solution at the characteristic wavelength λ；
(3) reagent B is added in into first solution, the second solution is obtained after reaction, reads second solution in institute
State the light absorption value A2 at characteristic wavelength λ；
(4) when in the step (2) being pure water, permanganate index zero, A2-A1=c at this time；When the step
(2) when being standard water sample in, x and (A2-A1-c) are in a linear relationship, i.e. (A2-A1-c)=ax+b, utilize the A2's and A1 measured
Numerical value carries out fitting a straight line, obtains the value of a, b.
It is noted that in order to improve the accuracy of linear equation, more parts of permanganate indexs should be selected as far as possible not
Same standard water sample, the A2 and the value of A1 measured according to every group of standard water sample obtain linear equation with least square fitting.
Further, read light absorption value A1 at the characteristic wavelength λ of the digestion solution and the reducing solution,
A2 brings the value of A1 and A2 in formula (A2-A1-c)=ax+b into, and the permanganate index for obtaining water sample to be measured is nx.
Further, the water sample to be measured is by the water sample of pretreatment, and pre-treatment step is：It is added in into water sample appropriate
Sulfuric acid solution, the pH value for making sample are 1~2.Sulfuric acid solution is added in into water sample also for avoiding before measuring, in water sample
Reducing substances aoxidized.
It is noted that obtained ascorbic acid surplus and the linear equation of permanganate index, can be stored in instrument
In device, subsequently when detecting the permanganate index of water sample, the surplus of the ascorbic acid directly obtained according to uv-spectrophotometric
The permanganate index of water sample can be provided.
[embodiment 1]
A kind of reagent component of permanganate index in quick measure water is provided, including reagent A, reagent B, reagent C and
Reagent D.Each reagent is contained in the screw-cap test tube of the 10ml of outer diameter 16mm, and gasket is equipped at sealed piece, prevents leakage.Examination
Pipe is preferably high-boron-silicon glass test tube.Each reagent component includes multiple reagent As, reagent B, reagent D.
The reagent component further includes stands frame for the test tube of holding test tubes, and test tube stands frame and tried for 40 holes in 16mm apertures
Pipe support.Test tube is stood frame and can be formed using three layers or more corrugated paper perforates.
The reagent component further includes environment-protective sealing bag, and for recycling the waste product after testing, environment-protective sealing bag uses 8 or more
PE materials.The size of environment-protective sealing bag is 14*20cm.
Reagent A is the liquor potassic permanganate that 0.5ml concentration is 0.01mol/L.Concentration is that the potassium permanganate of 0.01mol/L is molten
The preparation method of liquid is：It is soluble in water to weigh 3.2g potassium permanganate, is settled to 1000ml, pipetting 10ml after shaking up is settled to
100ml。
Reagent B is the ascorbic acid solution of 0.5ml.The preparation method of ascorbic acid solution is：Weigh 0.1g ascorbic acid
It is dissolved in (1+5) phosphoric acid, is then settled in 100ml water.Wherein (1+5) phosphoric acid solution is that volume ratio is 1:5 water and dense phosphorus
The mixed solution of acid.The test tube of reagent B is externally provided with black light-shielding sheet.
Reagent C calibrates solution for permanganate index, and its preparation method is：It is soluble in water to weigh 0.63g potassium permanganate, it is fixed
Hold to 500ml, therefrom pipette 2.5ml and be settled in 100ml water.
Reagent D is (1+3) sulfuric acid solution of 0.25ml.(1+3) sulfuric acid solution is that volume ratio is 1:3 water and the concentrated sulfuric acid
Mixed solution specifically prepares normative reference《The measure of GB 11892-1989 water quality permanganate indexs》.
Using embodiment 1 reagent Assembly calculation ascorbic acid surplus with detection water sample in permanganate index it is linear
Equation comprises the following steps：
(1) reagent A with reagent D is mixed, obtains acid permanganate soln；
(2) reagent C of the pure water of middle addition a ml and (5-a) ml into the acid permanganate soln of step (1), obtains
Mixed solution；
(3) heating digestion device is opened, set temperature is 100 DEG C, after temperature reaches 100 DEG C, the mixing of step (2) is molten
Liquid is placed in heating digestion device, is taken out after stopped pipe resolution 30min, is cooled to room temperature to obtain the first solution, read the first solution and exist
Wavelength is the light absorption value A1 under 250nm light sources；
(4) reagent B is added in into the first solution, after mixing, 2min is stood, obtains the second solution, then read the
Absorbance A 2 of two solution in the case where wavelength is 250nm light source.
According to above-mentioned steps (1)~(4), a is chosen respectively and is carried out for 5,4.75,4.5,4.25,4,3.75,3.5,3.25,3
Experiment, obtains the data of nine groups of A1 and A2, is shown in Table 1.
1 permanganate index standard curve of table
According to the data of table 1, and with least square fitting linear equation, when permanganate index is 0~8mg/L, y
=0.212x+0.016 (wherein x is permanganate index), linearly dependent coefficient r=0.9992.When concentration be more than 8.0mg/L,
When reaching 9.0mg/L, absorbance has apparent falling, and to increase the accuracy of result, test value preferably falls in 0~8.0mg/L models
In enclosing.
The method that permanganate index in water is quickly measured using mentioned reagent component is comprised the following steps
Water sample pre-processes：Appropriate (1+3) sulfuric acid solution is added in into water sample to be measured, it is 1~2 to make its pH value；
Clear up step：5ml pretreatment water samples is taken to add in the mixed solution of reagent A and reagent D (when the concentration of sample is higher
When, it is necessary to first dilute, diluted multiple is denoted as n), and mixed solution is placed in 100 DEG C of heating digestion device, stopped pipe resolution
30min postcoolings read absorbance A 1 of the mixed solution in the case where wavelength is 250nm light source at this time to room temperature；
Reduction step：Reagent B is added in the mixed solution obtained to resolution step, stands 2min after mixing, then
Read absorbance A2 of the mixed solution in the case where wavelength is 250nm light source；
Permanganate index calculates：Permanganate index (mg/L)=[(A2-A1-1.143) -0.016)/0.212] n.
Permanganate index standard sample is tested using the reagent component of embodiment 1, to verify the examination of the present invention
The accuracy of agent component and test method.
Three permanganate index standard samples are provided first：
Permanganate index standard sample 1 (GSB50025-94 203149,5.11mg/L ± 0.46)
Permanganate index standard sample 2 (GSB50025-94 203151,4.73mg/L ± 0.38)
Permanganate index standard sample 3 (GSB50025-94 203152,2.91mg/L ± 0.26)
Then, referred to using the permanganate of reagent component provided by the invention and method testing standard sample 1-3 respectively
Number, and 6 tests are carried out per a sample, test result is shown in Table 2.
2 permanganate index standard sample analysis result (unit of table：mg/L)
From table 2 it can be seen that the test value of three standard samples is in the range of standard specimen limitation, and relative deviation is only
1.3%~2.4%, illustrate that permanganate index detection reagent component provided by the invention and detection method accuracy are high.
Using the permanganate index of the sample of the reagent component detection separate sources of embodiment 1, while National Standard Method is examined
The permanganate index measured is as true value, to analyze detection error.In addition, when also providing a comparison of using different reducing agents, point
The test error of the permanganate index of light photometry detection sample.Test result is shown in Table 3.
3 distinct methods of table compare (concentration unit to actual sample analysis result：mg/L)
As seen from the above table, for this kind of low concentration sample of reservoir, the relative error of this reagent component is minimum, this main and side
The detection limit of method is related with sensitivity.For black smelly river, wawter bloom river and municipal wastewater treatment plant Pai Kou downstreams sample, this reagent set
Part method and the analysis result of ferrous reduction method can be received, and the analysis deviation of nitrate reductase method is slightly higher, this is mainly
Since the nitrogen in water body has this method certain influence.And factory Pai Kou downstreams sample is surface-treated to Mr. Yu, ferrous iron reduction
The analytical error of method substantially increases, this may be since there are ferro element interference in the sample.
In conclusion the scope of application of this reagent assembly method is wider, anti-interference is stronger, can be suitably used under different situations
The analysis of river water sample.
The above embodiment is only the preferred embodiment of the present invention, it is impossible to the scope of protection of the invention is limited with this,
The variation and replacement for any unsubstantiality that those skilled in the art is done on the basis of the present invention belong to institute of the present invention
Claimed scope.
Claims (10)
1. the reagent component of permanganate index, includes including reagent A and reagent B, the reagent A in a kind of quick measure water
Quantitative potassium permanganate, the reagent A is suitable for mixing with water sample to be measured under sour environment, to aoxidize reproducibility object therein
Matter；The reagent B includes quantitative reducing agent, is suitable for adding in the solution after clearing up, for reducing excessive potassium permanganate,
And the reagent B is excessive, which is characterized in that the reducing agent in the reagent B is ascorbic acid.
2. the quick reagent component for measuring permanganate index in water as described in claim 1, which is characterized in that the reagent
A is liquor potassic permanganate, and concentration is 0.01~0.1mol/L；The reagent B is ascorbic acid solution, and concentration is 1~5g/
L。
3. the quick reagent component for measuring permanganate index in water as claimed in claim 2, which is characterized in that the reagent
Phosphoric acid is further included in B, is used to improve the stability of ascorbic acid, the reagent B is placed in the container with shade function.
4. the quick reagent component for measuring permanganate index in water as described in claim 1, which is characterized in that the reagent
Component further includes reagent C, and the reagent C calibrates solution for permanganate index, for preparing mark known to permanganate index
Quasi- water sample.
5. the quick reagent component for measuring permanganate index in water as described in claim 1, which is characterized in that the reagent
Component further includes reagent D, and the reagent D is sulfuric acid solution, and the reagent D is suitable for being mixed to form needed for resolution with the reagent A
Acid permanganate soln.
6. a kind of method of permanganate index in quick measure water, using the reagent component as described in claim 1-5 is any,
It is characterised in that it includes following steps：
The water sample to be measured for diluting n times (n >=1), volume is L is mixed in acid condition with reagent A, heating reaction a period of time
Postcooling obtains digestion solution, contains excessive potassium permanganate in the digestion solution；
Reagent B is added in into the digestion solution, reducing solution is obtained after reaction, contains the anti-bad of excess in the reducing solution
Hematic acid；
A characteristic wavelength λ is chosen in the wave-length coverage of 190nm~260nm, by detecting the reducing solution in the feature
The light absorption value of af at wavelength lambda quantitative determines the ascorbic acid in the reducing solution and its oxidation product, according to Vitamin C
The linear relationship of the synthesis response of acid and its oxidation product and permanganate index in detection water sample, obtains the height of water sample to be measured
Mangaic acid salt index.
7. method as claimed in claim 6, which is characterized in that ascorbic acid and its oxidation product is comprehensive in the reducing solution
It closes response and with detecting the linear relationship of permanganate index in water sample standard water sample known to permanganate index is utilized to calculate
It obtains.
8. the method for claim 7, which is characterized in that ascorbic acid and its oxidation product is comprehensive in the reducing solution
It closes response and is obtained with detecting the linear equation of permanganate index in water sample by following steps：
(1) pure water and permanganate index are provided known to standard water sample, the permanganate index of standard water sample is denoted as X；
(2) volume is mixed for the pure water of L or the standard water sample with reagent A, heating reaction a period of time postcooling obtains
To the first solution, light absorption value A1 of first solution at the characteristic wavelength λ is read；
(3) reagent B is added in into first solution, the second solution is obtained after reaction, reads second solution in the spy
Levy the light absorption value A2 of af at wavelength lambda；
(4) when in the step (2) being pure water, permanganate index zero, A2-A1=c at this time；When in the step (2)
For standard water sample when, X and (A2-A1-c) are in a linear relationship, i.e. (A2-A1-c)=aX+b, utilize the A2 and the numerical value of A1 measured
Fitting a straight line is carried out, obtains the value of a, b.
9. method as claimed in claim 8, which is characterized in that read the digestion solution with the reducing solution in the spy
Light absorption value A1, A2 of af at wavelength lambda are levied, the value of A1 and A2 is brought into formula (A2-A1-c)=ax+b, obtains the height of water sample to be measured
Mangaic acid salt index is nx.
10. method as claimed in claim 6, which is characterized in that the water sample to be measured is by the water sample of pretreatment, pretreatment
Step is：Moderate amount of sulfuric acid solution is added in into water sample, the pH value for making sample is 1~2.
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