CN108168995A - The formulating method of total phosphorus and total nitrogen examination criteria in a kind of water quality - Google Patents
The formulating method of total phosphorus and total nitrogen examination criteria in a kind of water quality Download PDFInfo
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- CN108168995A CN108168995A CN201711420805.1A CN201711420805A CN108168995A CN 108168995 A CN108168995 A CN 108168995A CN 201711420805 A CN201711420805 A CN 201711420805A CN 108168995 A CN108168995 A CN 108168995A
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 202
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 114
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 101
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 101
- 229910052698 phosphorus Inorganic materials 0.000 title claims abstract description 99
- 239000011574 phosphorus Substances 0.000 title claims abstract description 99
- 238000000034 method Methods 0.000 title claims abstract description 26
- 239000000243 solution Substances 0.000 claims abstract description 33
- 239000012224 working solution Substances 0.000 claims abstract description 32
- 102000012286 Chitinases Human genes 0.000 claims abstract description 14
- 108010022172 Chitinases Proteins 0.000 claims abstract description 14
- 238000012360 testing method Methods 0.000 claims abstract description 14
- 238000005259 measurement Methods 0.000 claims description 12
- 238000010561 standard procedure Methods 0.000 claims description 12
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 11
- 239000012085 test solution Substances 0.000 claims description 11
- 238000011084 recovery Methods 0.000 claims description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 7
- 235000019394 potassium persulphate Nutrition 0.000 claims description 7
- 239000012153 distilled water Substances 0.000 claims description 6
- 230000003647 oxidation Effects 0.000 claims description 6
- 238000007254 oxidation reaction Methods 0.000 claims description 6
- -1 polyethylene Polymers 0.000 claims description 5
- 239000006228 supernatant Substances 0.000 claims description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- 239000004698 Polyethylene Substances 0.000 claims description 3
- 239000000908 ammonium hydroxide Substances 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 239000012895 dilution Substances 0.000 claims description 3
- 238000010790 dilution Methods 0.000 claims description 3
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 claims description 3
- 238000007689 inspection Methods 0.000 claims description 3
- 229920000573 polyethylene Polymers 0.000 claims description 3
- 239000010453 quartz Substances 0.000 claims description 3
- 238000005070 sampling Methods 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 238000004064 recycling Methods 0.000 claims 1
- 238000001514 detection method Methods 0.000 abstract description 13
- 238000002798 spectrophotometry method Methods 0.000 description 5
- 229910019142 PO4 Inorganic materials 0.000 description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 4
- 239000010452 phosphate Substances 0.000 description 4
- 238000002835 absorbance Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 238000003556 assay Methods 0.000 description 2
- 239000003599 detergent Substances 0.000 description 2
- XPPKVPWEQAFLFU-UHFFFAOYSA-J diphosphate(4-) Chemical compound [O-]P([O-])(=O)OP([O-])([O-])=O XPPKVPWEQAFLFU-UHFFFAOYSA-J 0.000 description 2
- 235000011180 diphosphates Nutrition 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 125000001477 organic nitrogen group Chemical group 0.000 description 2
- 235000011121 sodium hydroxide Nutrition 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- IVAOQJNBYYIDSI-UHFFFAOYSA-N [O].[Na] Chemical compound [O].[Na] IVAOQJNBYYIDSI-UHFFFAOYSA-N 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 1
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 description 1
- 235000018660 ammonium molybdate Nutrition 0.000 description 1
- 239000011609 ammonium molybdate Substances 0.000 description 1
- 229940010552 ammonium molybdate Drugs 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000012851 eutrophication Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 125000005341 metaphosphate group Chemical group 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 239000003987 organophosphate pesticide Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 150000004968 peroxymonosulfuric acids Chemical class 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
-
- 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)
- 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)
- Spectroscopy & Molecular Physics (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
Abstract
The invention discloses the formulating methods of total phosphorus and total nitrogen examination criteria in a kind of water quality, include the following steps：S1：Nitrogen standard working solution and phosphorus standard working solution are prepared, and the nitrogen standard working solution of different volumes and phosphorus standard working solution is taken to add water constant volume respectively；S2：The alkaline chitinase solution for preparing different ratio ratio clears up water sample, determines the best resolution condition of water sample；S3：The content of total nitrogen test total nitrogen in solution and total phosphorus test the content of solution total phosphorus in determination step S1 under the conditions of the best resolution obtained in step S2, and draw total nitrogen content standard curve and total phosphorus content standard curve respectively.Preferably total nitrogen in water quality and total phosphorus content can be detected in conclusion the present invention has, testing result accuracy is high, expends that the time is short, and detection efficiency is high, the advantages of can preferably reducing human cost and operation cost of enterprises.
Description
Technical field
The present invention relates to water quality inspection technique fields, and in particular to the formulation of total phosphorus and total nitrogen examination criteria in a kind of water quality
Method.
Background technology
With concern of the people to water environment safety, to the detection of total nitrogen in water quality and total phosphorus also increasingly by country
Pay attention to.
Total nitrogen refers to the total content of organic nitrogen in water body and inorganic nitride, mainly including nitrate anion, nitrite anions and ammonia
The organic nitrogens such as the inorganic nitrogens such as nitrogen and protein, amino acid and organic amine are to be used to represent the journey that water body is polluted by nutriment
Degree.Total nitrogen content in water is one of important indicator for weighing water quality, and measure contributes to evaluation water body contaminated and self-cleaning shape
Condition.The assay method of total nitrogen is detected after mainly being cleared up with alkaline chitinase with ultraviolet spectrophotometry again in water,
The content of ammonia nitrogen in water, nitrate anion, nitrite anions is measured respectively, and then measurement result adds up the measurement result as total nitrogen.
Total phosphorus refers to various Phos in water, if including element phosphor, orthophosphates, condensed phosphate, pyrophosphate, partially
Phosphate and the phosphoric acid machine of combination etc..Main source is sanitary sewage, chemical fertilizer, organophosphorus pesticide and modern age detergent institute
Phosphate detergent used etc..Excessive phosphorus can cause water body filth smelly so that eutrophication and bay occur for lake
There is red tide phenomenon.When existing water sample detection device is detected total phosphorus, first to water sample under the conditions of alkaline chitinase
Cleared up, be detected again with ultraviolet spectrophotometry after resolution, then by the element phosphor measured respectively, orthophosphates,
The content of condensed phosphate, pyrophosphate, metaphosphate and the phosphoric acid of combination machine etc., then measurement result add up as total
The measurement result of phosphorus.
The standard method that the total nitrogen in water quality and total phosphorus are detected is being distinguished respectively using ultraviolet spectrophotometry
Referring to GB/T 11893-1989《The measure ammonium molybdate spectrophotometric method of water quality total phosphorus》With HJ 636-2012《Water quality total nitrogen
Measure alkaline chitinase resolution ultraviolet spectrophotometry》.
When being detected to the total nitrogen in water quality and total phosphorus, usually the detection of total nitrogen and total phosphorus will separately be carried out,
And need to detect two or more projects when detecting, the consuming time is long, and detection efficiency is low, and human cost is high, enterprise
Operation cost it is high.
Invention content
In view of the above shortcomings of the prior art, the technical problems to be solved by the invention are：How to provide one kind can be more
Good is detected total nitrogen in water quality and total phosphorus content, and testing result accuracy is high, and the consuming time is short, and detection efficiency is high, can
Preferably to reduce the formulating method of total phosphorus and total nitrogen examination criteria in the water quality of human cost and operation cost of enterprises.
In order to solve the above-mentioned technical problem, present invention employs following technical solutions：
The formulating method of total phosphorus and total nitrogen examination criteria in a kind of water quality, includes the following steps：
S1：Nitrogen standard working solution and phosphorus standard working solution are prepared, and takes the nitrogen standard working solution and phosphorus of different volumes respectively
Standard working solution adds the total nitrogen of water isochoric formation different ratio ratio to test solution and total phosphorus test solution；
S2：The alkaline chitinase solution for preparing different ratio ratio clears up water sample, determines that the best of water sample disappears
Solution condition；
S3：Under the conditions of the best resolution obtained in step S2 in determination step S1 the content of total nitrogen test total nitrogen in solution and
Total phosphorus tests the content of solution total phosphorus, and draws total nitrogen content standard curve and total phosphorus content standard curve respectively；
Further, step S4 is further included：Carry out precision and accurate respectively to the step S2 best resolution conditions obtained
Degree is examined.
Further, in step S1, the nitrogen standard working solution and phosphorus standard working solution are 10mg/L, are drawn respectively
The nitrogen standard working solution of 0mL, 2.0mL, 4.0mL, 6.0mL, 8.0mL, 10.0mL and 12.0mL add water in 50mL volumetric flasks
The total nitrogen test solution that 25mL forms various concentration in 50mL colorimetric cylinders is drawn after constant volume respectively；0mL, 1.0 are drawn respectively
ML, 2.0mL, 3.0mL, 4.0mL, 5.0mL and 6.0mL phosphorus standard working solution are inhaled respectively in 50mL volumetric flasks after adding water constant volume
25mL is taken to form the total phosphorus test solution of various concentration in 50mL colorimetric cylinders.
Further, in step S2, in the best resolution condition for determining water sample, first to water sample progress total nitrogen content and always
Then the simultaneous determination of phosphorus content is respectively measured the total nitrogen content in water sample and total phosphorus content with standard method, will join
It closes the result that the result measured is measured with standard method to be compared, obtains total nitrogen and the best persulfuric acid of total phosphorus resolution in water sample
The best resolution condition of potassium ratio, as water sample.
Further, in step S2,6 parts of 20g potassium peroxydisulfates is weighed, are separately added into 2g, 3g, 4g, 5g, 7g and 10g hydrogen-oxygen
Change sodium, and be diluted to 1000mL after being dissolved in no ammonium hydroxide, by the solution storage after dilution in obtained in polyethylene bottle A, B, C, D,
The alkaline chitinase solution of E and six kinds of the F different ratio ratios；Then water sampling 25mL, be separately added into 25mLA, B, C,
D, it is placed in autoclave after E and the alkaline chitinase solution of six kinds of the F different ratio ratios, it is same with standard series
When 30min is aoxidized under the conditions of 120 DEG C, taking-up is cooled to room temperature, and then carries out simultaneous determination.
Wherein, the simultaneous determination includes water sample total nitrogen content measure and water sample total phosphorus content measures, the water sample total nitrogen
Take the water sample supernatant after oxidation in wavelength to use the quartz colorimetric utensil of 1cm at 210nm in uv-spectrophotometric during assay
It is measured on meter；The water sample total phosphorus content takes the water sample supernatant 10mL after oxidation to be pressed in 25mL colorimetric cylinders when measuring
The colour developing of total phosphorus, and the colorimetric estimation at 700nm wavelength are carried out according to GB/T 11893-1989 methods.
Wherein, the standard series is distilled water or the aqueous solution with distilled water comparable purity.
Further, in step S4, the precision takes identical water sample repeatedly to be measured when detecting, and measurement result is taken to put down
The measurement result that mean value is obtained with standard method is compared and calculates relative standard deviation.
Wherein, the measure number is 8 times.
Further, in step S4, the accuracy takes 10.00mL water samples and adds in the nitrogen of different ratio ratio when detecting
Standard working solution and phosphorus standard working solution carry out the measure of total nitrogen content and the survey of total phosphorus content according to step S2 and step S3
It is fixed, and measure total nitrogen recovery and total phosphorous recovery.
Beneficial effects of the present invention are：The present invention provides the formulation sides of total phosphorus and total nitrogen examination criteria in a kind of water quality
Method finds best resolution condition using water sample, in detection total nitrogen test solution and total phosphorus test solution under the conditions of best resolution
Then the content of total nitrogen and the content of total phosphorus draw total nitrogen content standard curve and total phosphorus content standard curve, formed in drawing
The examination criteria of total phosphorus and total nitrogen.When being detected to water quality, the total phosphorus content in water quality and total nitrogen content are detected,
Then it is compared with total nitrogen content standard curve and total phosphorus content standard curve, when total phosphorus content in water quality or total nitrogen content
Be above standard value, then proves that water quality is unqualified.
The present invention overcomes carry out resolution detection when in the prior art detecting total phosphorus content and total nitrogen content respectively to lack
Point, providing a kind of can carry out two kinds of factors of total nitrogen in water quality and total phosphorus while clear up the method for detection.Present invention selection
To the best potassium peroxydisulfate ratio that total nitrogen and total phosphorus are cleared up, and select to measure water quality total nitrogen using the wavelength of 210nm
Concentration gives up the method that two kinds of wavelength subtractions of 220nm and 275nm finally calculate standard curve and total nitrogen concentration, when reducing experiment
Between, human cost is saved, detection efficiency is improved, can preferably reduce operation cost of enterprises.
Description of the drawings
Fig. 1 is the formulating method of total phosphorus and total nitrogen examination criteria in a kind of water quality described in the specific embodiment of the invention
Flow chart.
Fig. 2 is total nitrogen content standard curve.
Fig. 3 is total phosphorus content standard curve.
Specific embodiment
The present invention is described in further detail below in conjunction with the accompanying drawings.
When it is implemented, as shown in Figure 1, the formulating method of total phosphorus and total nitrogen examination criteria in a kind of water quality, including following
Step：
S1：It prepares nitrogen standard working solution and phosphorus standard working solution, the nitrogen standard working solution and phosphorus standard working solution is
10mg/L draws the nitrogen standard working solution of 0mL, 2.0mL, 4.0mL, 6.0mL, 8.0mL, 10.0mL and 12.0mL in 50mL respectively
In volumetric flask, the total nitrogen test solution that 25mL forms various concentration in 50mL colorimetric cylinders is drawn respectively after adding water constant volume；Respectively
0mL, 1.0mL, 2.0mL, 3.0mL, 4.0mL, 5.0mL and 6.0mL phosphorus standard working solution are drawn in 50mL volumetric flasks, water is added to determine
The total phosphorus test solution that 25mL forms various concentration in 50mL colorimetric cylinders is drawn after appearance respectively；
S2：The alkaline chitinase solution for preparing different ratio ratio clears up water sample, weighs 20g potassium peroxydisulfates 6
Part, 2g, 3g, 4g, 5g, 7g and 10g sodium hydroxide are separately added into, and 1000mL is diluted to after being dissolved in no ammonium hydroxide, after dilution
Solution storage in the alkaline chitinase solution that six kinds of A, B, C, D, E and F different ratio ratios are obtained in polyethylene bottle；
Then water sampling 25mL is separately added into the alkaline chitinase solution of six kinds of 25mLA, B, C, D, E and F different ratio ratios
After be placed in autoclave, with distilled water or with the aqueous solution of the distilled water comparable sodium oxygen under the conditions of 120 DEG C simultaneously
Change 30min, taking-up is cooled to room temperature, and then carries out simultaneous determination, and the simultaneous determination includes water sample total nitrogen content measure and water
Sample total phosphorus content measures, and the water sample total nitrogen content takes the water sample supernatant after oxidation in wavelength to use 1cm at 210nm when measuring
Quartz colorimetric utensil be measured on ultraviolet specrophotometer；The water sample total phosphorus content is taken when measuring on the water sample after oxidation
Clear liquid 10mL carries out the colour developing of total phosphorus according to GB/T 11893-1989 methods, and at 700nm wavelength in 25mL colorimetric cylinders
Colorimetric estimation；Then the total nitrogen content in water sample and total phosphorus content are measured respectively with standard method, by simultaneous determination
As a result the result measured with standard method is compared, and is obtained total nitrogen and the best potassium peroxydisulfate of total phosphorus resolution in water sample and is matched frequently
The best resolution condition of example, as water sample；The result of the simultaneous determination the results are shown in Table 1 with what standard method measured：
Table 1 is that the result table that simultaneous determination is measured with standard method is carried out to water sample：
The best resolution condition of water sample is as can be drawn from Table 1:When water sample is 10.00mL, B potassium persulfate solutions are selected
The measurement result that ratio obtains is approached with the results contrast that standard method measures.Alkaline chitinase solution ratio ratio at this time
Example be：20g potassium peroxydisulfate+3g sodium hydroxides.
S3：Solution is tested to the content of total nitrogen test total nitrogen in solution and total phosphorus in step S1 using B potassium persulfate solutions
The content of total phosphorus, and total nitrogen content standard curve and total phosphorus content standard curve are drawn respectively；Total nitrogen content standard curve is shown in
Bright book attached drawing Fig. 2, total phosphorus content standard curve are shown in Figure of description Fig. 3：
In Figure of description Fig. 2, horizontal axis x represents total nitrogen concentration, and longitudinal axis y represents absorbance under the concentration, R2Represent related
Coefficient.
In Figure of description Fig. 3, horizontal axis x represents total phosphorus concentration, and longitudinal axis y represents total phosphorus absorbance, R2Represent related coefficient.
S4：Preci-sion and accuracy inspection is carried out to water sample respectively using B potassium persulfate solutions；During the precision detection
It takes identical water determination 8 times, the measurement result that measurement result average value is obtained with standard method is taken to be compared and calculates and is opposite
Standard deviation, the precision testing result are shown in Table 4；It takes 10.00mL water samples during the accuracy detection and adds in different ratio
The nitrogen standard working solution of ratio and phosphorus standard working solution carry out the measure of total nitrogen content according to step S2 and step S3 and total phosphorus contain
The measure of amount, and total nitrogen recovery and total phosphorous recovery are measured, the B accuracy testing result is shown in Table 5；
Table 4 is precision testing result：
As can be drawn from Table 4, the average and standard law pair of joint-detection 8 times is carried out to water sample using B potassium persulfate solutions
The relative standard deviation for the value that water sample is detected is smaller, illustrates that measurement result precision is good.
Table 5 is accuracy testing result：
| Volume (mL) | 10 | 10+0.2 | 10+0.4 | 10+0.6 |
| Absorbance (A) | 0.236 | 0.381 | 0.558 | 0.682 |
| Phosphorus content (mg/L) | 0.620 | 0.996 | 1.454 | 1.770 |
| The rate of recovery (%) | 94.1 | 104.3 | 96.3 | |
| Nitrogen content (mg/L) | 4.17 | 6.10 | 8.28 | 10.20 |
| The rate of recovery (%) | 96.5 | 102.8 | 100.5 |
As can be drawn from Table 5, the rate of recovery of total nitrogen is 96.5%-102.8%, and the rate of recovery of total phosphorus is 94.1%-
104.3%, testing result is relatively satisfactory.
Finally it should be noted that：The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although
The present invention is described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that；It still may be used
Either which part or all technical features are equal with modifying to the technical solution recorded in previous embodiment
It replaces；And these modifications or replacement, the model for technical solution of the embodiment of the present invention that it does not separate the essence of the corresponding technical solution
It encloses, should all cover in the claim of the present invention and the range of specification.
Claims (10)
1. the formulating method of total phosphorus and total nitrogen examination criteria in a kind of water quality, which is characterized in that include the following steps：
S1：Nitrogen standard working solution and phosphorus standard working solution are prepared, and takes the nitrogen standard working solution of different volumes and phosphorus standard respectively
Working solution adds the total nitrogen of water isochoric formation different ratio ratio to test solution and total phosphorus test solution；
S2：The alkaline chitinase solution for preparing different ratio ratio clears up water sample, determines the best resolution item of water sample
Part；
S3：Total nitrogen tests the content and total phosphorus of total nitrogen in solution in determination step S1 under the conditions of the best resolution obtained in step S2
The content of solution total phosphorus is tested, and draws total nitrogen content standard curve and total phosphorus content standard curve respectively.
2. the formulating method of total phosphorus and total nitrogen examination criteria in a kind of water quality according to claim 1, which is characterized in that also
Including step S4：Preci-sion and accuracy inspection is carried out respectively to the step S2 best resolution conditions obtained.
3. the formulating method of total phosphorus and total nitrogen examination criteria in a kind of water quality according to claim 1, which is characterized in that step
In rapid S1, the nitrogen standard working solution and phosphorus standard working solution are 10mg/L, draw respectively 0mL, 2.0mL, 4.0mL,
The nitrogen standard working solution of 6.0mL, 8.0mL, 10.0mL and 12.0mL draw 25mL respectively in 50mL volumetric flasks after adding water constant volume
The total nitrogen test solution of various concentration is formed in 50mL colorimetric cylinders；Respectively draw 0mL, 1.0mL, 2.0mL, 3.0mL, 4.0mL,
5.0mL and 6.0mL phosphorus standard working solution draws 25mL shapes in 50mL colorimetric cylinders respectively in 50mL volumetric flasks after adding water constant volume
Total phosphorus into various concentration tests solution.
4. the formulating method of total phosphorus and total nitrogen examination criteria in a kind of water quality according to claim 1, which is characterized in that step
In rapid S2, in the best resolution condition for determining water sample, the simultaneous determination of total nitrogen content and total phosphorus content is first carried out to water sample, so
The total nitrogen content in water sample and total phosphorus content are measured respectively with standard method afterwards, by the result of simultaneous determination and standard side
The result that method measures is compared, and obtains total nitrogen and the best potassium peroxydisulfate ratio of total phosphorus resolution, as water sample in water sample
Best resolution condition.
5. the formulating method of total phosphorus and total nitrogen examination criteria in a kind of water quality according to claim 1, which is characterized in that step
In rapid S2,6 parts of 20g potassium peroxydisulfates are weighed, are separately added into 2g, 3g, 4g, 5g, 7g and 10g sodium hydroxide, and are dissolved in no ammonium hydroxide
After be diluted to 1000mL, by the solution storage after dilution in obtaining six kinds of different ratios of A, B, C, D, E and F in polyethylene bottle
The alkaline chitinase solution of ratio；Then water sampling 25mL is separately added into six kinds of differences of 25mLA, B, C, D, E and F and matches
Than being placed in autoclave after the alkaline chitinase solution of ratio, aoxidized under the conditions of 120 DEG C simultaneously with standard series
30min, taking-up are cooled to room temperature, and then carry out simultaneous determination.
6. the formulating method of total phosphorus and total nitrogen examination criteria in a kind of water quality according to claim 5, which is characterized in that institute
It states simultaneous determination and includes water sample total nitrogen content measure and water sample total phosphorus content measure, the water sample total nitrogen content takes oxidation when measuring
Water sample supernatant afterwards is in wavelength to be measured on ultraviolet specrophotometer with the quartz colorimetric utensil of 1cm at 210nm；It is described
Water sample total phosphorus content takes the water sample supernatant 10mL after oxidation in 25mL colorimetric cylinders when measuring, according to GB/T 11893-1989
Method carries out the colour developing of total phosphorus, and the colorimetric estimation at 700nm wavelength.
7. the formulating method of total phosphorus and total nitrogen examination criteria in a kind of water quality according to claim 5, which is characterized in that institute
Standard series is stated as distilled water or the aqueous solution with distilled water comparable purity.
8. the formulating method of total phosphorus and total nitrogen examination criteria in a kind of water quality according to claim 2, which is characterized in that step
In rapid S4, the precision takes identical water sample repeatedly to be measured when detecting, and measurement result average value is taken to be obtained with standard method
Measurement result be compared and calculate relative standard deviation.
9. the formulating method of total phosphorus and total nitrogen examination criteria in a kind of water quality according to claim 8, which is characterized in that institute
It is 8 times to state and measure number.
10. the formulating method of total phosphorus and total nitrogen examination criteria in a kind of water quality according to claim 2, which is characterized in that
In step S4, the accuracy takes 10.00mL water samples and adds in the nitrogen standard working solution of different ratio ratio and phosphorus mark when detecting
Quasi- working solution carries out the measure of total nitrogen content and the measure of total phosphorus content according to step S2 and step S3, and calculates total nitrogen recycling
Rate and total phosphorous recovery.
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