CN103063816B - Method for simultaneously detecting nitrogen and phosphorus indexes of water quality - Google Patents
Method for simultaneously detecting nitrogen and phosphorus indexes of water quality Download PDFInfo
- Publication number
- CN103063816B CN103063816B CN201210591017.XA CN201210591017A CN103063816B CN 103063816 B CN103063816 B CN 103063816B CN 201210591017 A CN201210591017 A CN 201210591017A CN 103063816 B CN103063816 B CN 103063816B
- Authority
- CN
- China
- Prior art keywords
- flow
- nitrogen
- mixed solution
- sample
- concentration
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
A method for simultaneously detecting nitrogen and phosphorus indexes of water quality comprises the following steps: (1) through integrating and improving a sample injector and two flow analyzers, enabling a sample to pass through the sample injector and then shunting the sample to the two flow analyzers through a tee-joint, and respectively detecting the nitrogen and phosphorus indexes of the sample; (2) using ammonium nitrogen, nitrate nitrogen, nitrite nitrogen and phosphate as working mother liquors; respectively absorbing the working mother liquors into 6 volumetric flasks; metering the volumes of the volumetric flasks and preparing a mixed standard solution, wherein the concentration of the nitrate nitrogen is the concentration sum of the nitrite nitrogen and the nitrate nitrogen; the total concentration of the nitrogen is the concentration sum of the ammonium nitrogen, the nitrite nitrogen and the nitrate nitrogen; and the total concentration of the phosphorus is equal to the concentration of the phosphate; and (3) detecting an environment water quality sample by using an integrated instrument according to a standard curve method. According to the invention, the defect that the larger error problem is caused by non-simultaneous detection when the nitrogen and phosphorus indexes in the water quality sample are detected by the traditional instrument and technology is overcome; and in particular, simultaneous detection of the nitrogen and phosphorus indexes in the water quality sample with small volume is satisfied.
Description
Technical field
The invention belongs to water quality monitoring technical field, particularly relate to a kind of nitrogen phosphorus that measures and refer to calibration method.
Background technology
Widespread pollution from the overuse of fertilizers and pesticides in rural area brings serious impact to industrial and agricultural production, and a large amount of wait nutritive salt and pollutant emission enter water bodies of rivers and lakes, some areas surface water severe contamination, even directly affect the drinking water source in agricultural irrigation and rural area.Phosphate in farmland fertilization, feces of livestock and poultry and crop material, washing powder, has become the main source of China's Rural Plane Source Pollution, receives much concern to the harm that environment and human health cause.Therefore need to measure water quality nitrogen phosphorus index in time, rapidly and seem very important.
Continuous Flow Analysis instrument is the method according to continuous flow, by the pump line of peristaltic pump compression different tube diameters, reaction reagent and testing sample are injected in proportion an airtight continuous print flowing current-carrying, chromogenic reaction is there is in chemical reaction units, record its signal value in a detector, measure a kind of detecting instrument of the concentration of testing sample according to calibration curve method.Be usually used in water analysis in environmental monitoring field.
When environmental water sample collects lab analysis nitrogen phosphorus index, if single index is tested respectively, after mensuration completes one or several projects, nitrogen, phosphorus element easily there occurs conversion between different shape, makes the nitrogen of certain form, the result of phosphorus element there will be between each form sum and total amount and there is obvious error.Such as: the ammonium nitrogen of environmental water sample, after mensuration completes, ammonia volatilization may occur, now go to measure total nitrogen, total nitrogen result can be less than various nitrogen forms element sum again; After mensuration completes, may there is nitrification in the ammonium nitrogen of environmental water sample, the concentration now measuring nitrate nitrogen has obviously become large, has not been nitrate when measuring ammonium nitrogen, easily misled to scientific research result.In order to avoid such problem, need a kind of analytical approach, can nitrogen phosphorus index in Simultaneously test water sample.
Carrying out in native fish scientific experiment, due in certain hour section, the leaching liquid volume ratio collected is less, but the situation of change of nitrogen in fluid, phosphorus element is drenched in order to investigate different time sections, so need a kind of analytical approach, the Simultaneously test of the nitrogen phosphorus index in the few water sample of volume can be met.
Summary of the invention
The technical matters solved:
The object of this invention is to provide a kind of Simultaneously test water quality nitrogen phosphorus and refer to calibration method, when solving nitrogen phosphorus index in existing instrument and technology mensuration water sample, introduce the defect compared with big error owing to being not Simultaneously test, particularly meet the Simultaneously test of the nitrogen phosphorus index in the few water sample of volume.
Technical scheme: a kind of Simultaneously test water quality nitrogen phosphorus refers to calibration method, is connected with two Flow Analyzers in parallel by an injector, and measure inorganic states concentration and the total amount concentration of nitrogen phosphorus index respectively, concrete steps are: with 200.0mg/L ammonium nitrogen (NH
4cl-N), 100.0mg/L nitrate nitrogen (KNO
3-N), 4.0mg/L nitrite nitrogen (NaNO
2-N), 20.0mg/L phosphate (KH
2pO
4-P) be working stocks, each absorption 0.00,1.00,2.00,3.00,4.00,5.00mL is in 6 100.0mL volumetric flasks respectively, uses pure water constant volume, preparation mixed standard solution; Sample injection time is 50s, and scavenging period is 100s, and sample detection obtains simultaneously:
The typical curve linear equation of ammonium nitrogen 0.32mL/min sample introduction flow is Y=43.5+387.5X;
The typical curve linear equation of nitrite nitrogen 0.42mL/min sample introduction flow is Y=16.8+15664.0X;
The typical curve linear equation of nitrate nitrogen 0.16mL/min sample introduction flow is Y=13.24+306.8X;
The typical curve linear equation of total nitrogen 0.42mL/min sample introduction flow is Y=-71.9+332.3X;
The typical curve linear equation of phosphate 0.80mL/min sample introduction flow is Y=-30309.5+1140024.2X;
The typical curve linear equation of total phosphorus 0.42mL/min sample introduction flow is Y=-17313.4+398251.2X;
Wherein: X is concentration, unit mg/L; Y is Flow Analyzer signal value reading;
Then testing sample sample size is consistent with typical curve, measures its corresponding signal value reading, calculates its concentration according to calibration curve method.
Every nitrogen phosphorus index is calculated by typical curve equation, wherein:
Measuring reaction reagent needed for ammonium nitrogen is: NH
4 +-A is mixed solution, and include sodium potassium tartrate tetrahydrate 33g/L, trisodium citrate 24g/L, pH=5.2, two-way flow is respectively 1mL/min and 0.8mL/min; NH
4 +-B is mixed solution, includes sodium salicylate 80g/L, NaOH 25g/L, and flow is 0.32mL/min; NH
4 +-C is sodium nitroprusside 1g/L, and flow is 0.16mL/min; NH
4 +-D is sodium dichloro cyanurate 2g/L, and flow is 0.32mL/min;
Measuring reaction reagent needed for nitrate nitrogen is: NO
3 --A is mixed solution, includes sodium potassium tartrate tetrahydrate 33g/L, trisodium citrate 24g/L, and flow is 0.8mL/min; NO
3 --B is NaOH 6g/L, and flow is 1mL/min; NO
3 --C is mixed solution, includes hydrazine sulfate 2g/L, copper sulphate 18mg/L, and flow is 0.42mL/min; NO
3 --D is mixed solution, and include N-(1-naphthyl) ethylendiamine dihydrochloride 0.5g/L, sulfanilamide (SN) 10g/L, phosphatase 11 69g/L, flow is 0.42mL/min;
Measuring reaction reagent needed for nitrite nitrogen is: NO
2 --A is pure water, resistivity: 18.3 Μ Ω cm, and flow is 1mL/min; NO
2 --B is mixed solution, include (N-(1-naphthyl) ethylendiamine dihydrochloride 0.5g/L, sulfanilamide (SN) 10g/L, phosphoric acid 253.5g/L, flow is 0.32mL/min;
Measuring reaction reagent needed for total nitrogen is: TN-A is mixed solution, includes potassium persulfate 40g/L, NaOH 12g/L, and flow is 0.42mL/min; TN-B is boric acid 24g/L, and flow is 0.42mL/min; TN-C is ammonium chloride 50g/L, pH=8.2, and two-way flow is respectively 1mL/min and 0.8mL/min; TN-D is mixed solution, and include N-(1-naphthyl) ethylendiamine dihydrochloride 0.5g/L, sulfanilamide (SN) 10g/L, hydrochloric acid 118g/L, flow is 0.23mL/min;
Measuring reaction reagent needed for phosphate is: PO
4 3--A is mixed solution, includes ammonium molybdate 4.8g/L, sulfuric acid 73.6g/L, and flow is 0.42mL/min; PO
4 3--B is mixed solution, includes ascorbic acid 18g/L, potassium antimony tartrate 6mg/L, and flow is 0.42mL/min;
Measuring reaction reagent needed for total phosphorus is: TP-A is mixed solution, includes potassium persulfate 9.9g/L, sulfuric acid 156.4g/L, and flow is 0.23mL/min; TP-B is sulfuric acid 294.4g/L, and flow is 0.32mL/min; TP-C is NaOH 210g/L, and flow is 0.32mL/min; TP-D is mixed solution, includes ammonium molybdate 4.8g/L, sulfuric acid 73.6g/L, and flow is 0.42mL/min; TP-E is mixed solution, includes ascorbic acid 18g/L, potassium antimony tartrate 6mg/L, and flow is 0.42mL/min.
The present invention by the integration of an injector and two Flow Analyzers and improvement, make sample by after injector through distributing T-pipe to two Flow Analyzers, measure inorganic states concentration and the total amount concentration of nitrogen phosphorus index respectively.With ammonium nitrogen (NH
4cl), nitrate nitrogen (KNO
3), nitrite nitrogen (NaNO
2), phosphate (KH
2pO
4) be mother liquor blended standard curve (mixed mark).In mixed mark, the concentration of nitrate nitrogen is the concentration sum of nitrite nitrogen and nitrate nitrogen; The concentration of total nitrogen is the concentration sum of ammonium nitrogen, nitrite nitrogen and nitrate nitrogen; The concentration of total phosphorus equals phosphatic concentration.And to the repacking of the project of mensuration pipeline and the adjustment of experiment condition, to guarantee Simultaneously test water quality ammonium nitrogen NH
4 +-N, nitrate nitrogen (NO
3 -+ NO
2 -)-N, nitrite nitrogen NO
2 --N, total nitrogen TN-N, phosphate PO
4 3--P, total phosphorus TP-P six projects.
Beneficial effect:
Integrated by instrument and use the improvement of mixed standard solution can reach the nitrogen phosphorus index simultaneously analyzed in water quality.So both made to analyze required sample size to reduce, (as: native fish is tested, the situation of change of nitrogen in fluid, phosphorus element is drenched in order to investigate different time sections, the volume of the leaching liquor collected is considerably less, only has 3mL leaching liquor), ensure again all items Simultaneously test (if not Simultaneously test, in this time period, nitrogen and phosphorus element easily there occurs conversion between different shape, thus result there will be between each form sum and total amount there is obvious error).Reach object that is timely, quick, accurate analysis water quality nitrogen phosphorus index.Measure eco material science all within guarantee value, recovery of standard addition is between 96.3% ~ 107.6%, and relative standard deviation is between 0.54% ~ 2.85%.The method can be widely used in environmental monitoring field, the nitrogen phosphorus index of a large amount of express-analysis water sample, is particularly useful for the Simultaneously test of the nitrogen phosphorus index in the few water sample of volume.
Accompanying drawing explanation
Fig. 1 is that the present invention measures pipeline connection diagram;
Fig. 2 is module coupling schematic diagram of the present invention.
Embodiment
Following embodiment does not limit technical scheme of the present invention in any form, and the technical scheme that the mode that every employing is equal to replacement or equivalent transformation obtains all drops on protection scope of the present invention.
Embodiment 1
Shown in Fig. 1, by the integration of an injector and two Flow Analyzers and improvement, make sample by after injector through distributing T-pipe to two Flow Analyzers, measure inorganic states concentration and the total amount concentration of nitrogen phosphorus index respectively.With ammonium nitrogen (NH
4cl), nitrate nitrogen (KNO
3), nitrite nitrogen (NaNO
2), phosphate (KH
2pO
4) be mother liquor blended standard curve (mixed mark).In mixed mark, the concentration of nitrate nitrogen is the concentration sum of nitrite nitrogen and nitrate nitrogen; The concentration of total nitrogen is the concentration sum of ammonium nitrogen, nitrite nitrogen and nitrate nitrogen; The concentration of total phosphorus equals phosphatic concentration.And to the repacking of the project of mensuration pipeline and the adjustment of experiment condition, to guarantee Simultaneously test water quality ammonium nitrogen NH
4 +-N, nitrate nitrogen (NO
3 -+ NO
2 -)-N, nitrite nitrogen NO
2 --N, total nitrogen TN-N, phosphate PO
4 3--P, total phosphorus TP-P six projects.
Instrument and reagent:
Flow Analyzer (Dutch Sakar San
++system) two; Automatic sampler (Auto sampler1075) one; Ultrapure water machine (Chongqing Ai Kepu AJY-6000-U).
It is pure that sodium potassium tartrate tetrahydrate, trisodium citrate, sodium nitroprusside, sodium dichloro cyanurate, hydrazine sulfate, copper sulphate, N-(1-naphthyl) ethylendiamine dihydrochloride, sulfanilamide (SN), ammonium chloride, ammonium molybdate, ascorbic acid, potassium antimony tartrate are analysis, purchased from Chemical Reagent Co., Ltd., Sinopharm Group; Sodium salicylate, NaOH, boric acid, phosphoric acid, hydrochloric acid, sulfuric acid are pure purchased from Nanjing Chemistry Reagent Co., Ltd. for analyzing; Potassium persulfate is pure for analyzing, purchased from Fluka reagent company limited; Experimental water is ultrapure water (resistivity: 18.23 Μ Ω cm).
The integration of instrument and optimum configurations thereof:
By to the integration of an injector and two Flow Analyzers and improvement, make sample by after injector through distributing T-pipe to two Flow Analyzers, measure inorganic states concentration and the total amount concentration of nitrogen phosphorus index respectively.Organic form concentration is that total amount deducts inorganic forms part.Instrument is integrated and is measured schematic flow sheet, sees Fig. 1.While instrument is integrated, also carried out reequiping (comprising: adjustment member semi-permeable diaphragm filter bed, change reagent flow, change the means such as the concentration of reagent) to mensuration project pipeline, the pipeline after repacking, reagent and flow thereof all provide in the diagram.The repacking of instrument adjusts and selects suitable reagent conditions, takes into account the range of linearity of ambient water quality sample tests and the object of sensitivity to reach.Other Main Analysis parameters of instrument are in table 1.
Table 1: the analytical parameters of Flow Analyzer
Note :-represent that this does not need to arrange
Reaction reagent solution concentration used:
Measuring reaction reagent needed for ammonium nitrogen is: NH
4 +-A is mixed solution, and include sodium potassium tartrate tetrahydrate 33g/L, trisodium citrate 24g/L, pH=5.2, two-way flow is respectively 1mL/min and 0.8mL/min; NH
4 +-B is mixed solution, includes sodium salicylate 80g/L, NaOH 25g/L, and flow is 0.32mL/min; NH
4 +-C is sodium nitroprusside 1g/L, and flow is 0.16mL/min; NH
4 +-D is sodium dichloro cyanurate 2g/L, and flow is 0.32mL/min;
Measuring reaction reagent needed for nitrate nitrogen is: NO
3 --A is mixed solution, includes sodium potassium tartrate tetrahydrate 33g/L, trisodium citrate 24g/L, and flow is 0.8mL/min; NO
3 --B is NaOH 6g/L, and flow is 1mL/min; NO
3 --C is mixed solution, includes hydrazine sulfate 2g/L, copper sulphate 18mg/L, and flow is 0.42mL/min; NO
3 --D is mixed solution, and include N-(1-naphthyl) ethylendiamine dihydrochloride 0.5g/L, sulfanilamide (SN) 10g/L, phosphatase 11 69g/L, flow is 0.42mL/min;
Measuring reaction reagent needed for nitrite nitrogen is: NO
2 --A is pure water, resistivity: 18.3 Μ Ω cm, and flow is 1mL/min; NO
2 --B is mixed solution, include (N-(1-naphthyl) ethylendiamine dihydrochloride 0.5g/L, sulfanilamide (SN) 10g/L, phosphoric acid 253.5g/L, flow is 0.32mL/min;
Measuring reaction reagent needed for total nitrogen is: TN-A is mixed solution, includes potassium persulfate 40g/L, NaOH 12g/L, and flow is 0.42mL/min; TN-B is boric acid 24g/L, and flow is 0.42mL/min; TN-C is ammonium chloride 50g/L, pH=8.2, and two-way flow is respectively 1mL/min and 0.8mL/min; TN-D is mixed solution, and include N-(1-naphthyl) ethylendiamine dihydrochloride 0.5g/L, sulfanilamide (SN) 10g/L, hydrochloric acid 118g/L, flow is 0.23mL/min;
Measuring reaction reagent needed for phosphate is: PO
4 3--A is mixed solution, includes ammonium molybdate 4.8g/L, sulfuric acid 73.6g/L, and flow is 0.42mL/min; PO
4 3--B is mixed solution, includes ascorbic acid 18g/L, potassium antimony tartrate 6mg/L, and flow is 0.42mL/min;
Measuring reaction reagent needed for total phosphorus is: TP-A is mixed solution, includes potassium persulfate 9.9g/L, sulfuric acid 156.4g/L, and flow is 0.23mL/min; TP-B is sulfuric acid 294.4g/L, and flow is 0.32mL/min; TP-C is NaOH 210g/L, and flow is 0.32mL/min; TP-D is mixed solution, includes ammonium molybdate 4.8g/L, sulfuric acid 73.6g/L, and flow is 0.42mL/min; TP-E is mixed solution, includes ascorbic acid 18g/L, potassium antimony tartrate 6mg/L, and flow is 0.42mL/min.
The preparation of typical curve:
With 200.0mg/L ammonium nitrogen (NH
4cl-N), 100.0mg/L nitrate nitrogen (KNO
3-N), 4.0mg/L nitrite nitrogen (NaNO
2-N), 20.0mg/L phosphate (KH
2pO
4-P) be working stocks, above concentration represents the concentration of N, P element, and employing-N ,-P identify, and each absorption 0.00,1.00,2.00,3.00,4.00,5.00mL is in 6 100.0mL volumetric flasks respectively, uses pure water constant volume, preparation mixed standard solution.In mixed mark, the concentration of nitrate nitrogen is the concentration sum of nitrite nitrogen and nitrate nitrogen; The concentration of total nitrogen is the concentration sum of ammonium nitrogen, nitrite nitrogen and nitrate nitrogen; The concentration of total phosphorus equals phosphatic concentration.Sample injection time is 50s, and scavenging period is 100s.The each concentration of component of mixed solution of the standard solution of 6 indexs, linear equation, linear coefficient and detection limit, in table 2.
Table 2: the linear coefficient of method and detection limit
Note: X is the concentration of sample, unit mg/L; Y is Flow Analyzer signal value reading
Sample tests:
Adopt the inventive method to carry out analysis to eco material science to measure.Eco material science is purchased from eco material science research institute of national environmental protection portion.From testing result, measured value, within guarantee value scope, proves that the method measures the accuracy of nitrogen phosphorus index.The results are shown in Table 3.
Table 3: the accuracy test of method
Embodiment 2
Only Instrument crosslinking, the sensing range that still can not meet each index can the common concentration of overlay environment water sample, needs module and reagent optimization.Now module and reagent optimization are tested with comparing without optimization.In order to the sensing range meeting each index can the common concentration of overlay environment water sample, according to the typical curve compound method of embodiment 1, nitrate is 0.00,1.04,2.08,3.12,4.16,5.20mg/L; The concentration of phosphate and total phosphorus is 0.00,0.20,0.40,0.60,0.80,1.00mg/L, and determination data is in table 4.
The nitrate range of variation of ambient water quality sample is larger, substantially in the scope of 0.5 to 5mg/L.When sample size is 0.42mg/L, the peak of typical curve is close to saturated, and typical curve is bent, and linear coefficient is deteriorated.If its sample size is become 0.16mg/L, typical curve obviously improves, and can meet the requirement that nitrate range of variation is large.
The phosphorus concentration of ambient water quality sample is lower, in order to improve the sensitivity measuring phosphorus, as shown in phosphate in Fig. 1 and total phosphorus module, the worry film of original instrument phosphate and total phosphorus module is removed, whole sample introduction reagent is participated in reaction, improve sensitivity, simultaneously owing to having gone film the concentration of reagent N aOH will be reduced to 210g/L, to ensure the pH of the anti-colour developing of molybdenum antimony.Remove after considering film, the slope of the typical curve of phosphate and total phosphorus obviously becomes large, and sensitivity uprises, and the low concentration meeting phosphorus measures.
In a word, the instrument after coupling, after module and reagent are optimized, more superior than measuring successful without optimization.The sensing range that can meet each index can the common concentration of overlay environment water sample, meets the analysis demand of surroundings water sample.
Table 4: whether module and reagent optimize Comparability test
Note: X is the concentration of sample, unit mg/L; Y is Flow Analyzer signal value reading
Embodiment 3
Adopt summary of the invention method to carry out analysis to field water quality sample to measure.Instrument crosslinking and experiment condition are with embodiment 1.Pick up from Yixing City great Pu town rice field (31 ° 16 ' 32 " N, 119 ° 53 ' 32 " E), be the runoff water sample gathered after basal dressing sowing waterflooding, belong to Taihu Lake basin pollution of area source monitoring water sample.Its pH value is 6.70; Chemical oxygen demand cod
cr(Chemical Oxygen Demand) is 68.0mg/L.Its nitrogen phosphorus index of replication, calculates relative standard deviation RSD(Relative Standard Deviation) between 0.54% ~ 2.85% (n=11).Divide five groups to carry out mark-on recovery test to this ambient water quality sample, draw 40.0 respectively, 30.0,25.0, this ambient water quality sample of 20.0,10.0mL, adds the standard solution of respective amount, constant volume, to 50.0mL, measures its concentration, and its recovery is (n=5) between 96.3% ~ 107.6%.Data are in table 5.
Table 5: the precision of ambient water quality sample and recovery of standard addition
Embodiment 4
Adopt the inventive method to carry out analysiss mensuration to native fish liquid, collected by obtain woods liquor capacity be 3mL.Instrument crosslinking and experiment condition are with embodiment 1.Record its ammonium nitrogen, nitrite nitrogen, nitrate nitrogen, total nitrogen, phosphate, total phosphorus concentration 4.02mg/L, 0.015mg/L, 2.07mg/L, 6.80mg/L, 0.212mg/L, 0.245mg/L respectively.Existing equipment and method can not analyze the nitrogen phosphorus index (comprising: ammonium nitrogen, nitrite nitrogen, nitrate nitrogen, total nitrogen, phosphate, total phosphorus) of drenching in fluid, because each index is analyzed separately, the sample volume needed is nowhere near, have no idea to investigate the variation relation of its nitrogen of haveing suffered leaching process, phosphorus element, and the present invention solves this problem of Simultaneously test of the nitrogen phosphorus index in the few water sample of volume just.
Claims (1)
1. Simultaneously test water quality nitrogen phosphorus refers to a calibration method, it is characterized in that by Auto sampler 1075 injector and two Sakar San in parallel
++system Flow Analyzer connects, and removes the phosphate of Flow Analyzer and the filter membrane of total phosphorus module simultaneously, and measure inorganic states concentration and the total amount concentration of nitrogen phosphorus index respectively, concrete steps are: with 200.0 mg/L ammonium nitrogen (NH
4cl-N), 100.0 mg/L nitrate nitrogen (KNO
3-N), 4.0 mg/L nitrite nitrogen (NaNO
2-N), 20.0 mg/L phosphate (KH
2pO
4-P) be working stocks, respectively in each absorption 0.00,1.00,2.00,3.00,4.00,5.00 mL to 6 100.0 mL volumetric flasks, use pure water constant volume, preparation mixed standard solution; Sample injection time is 50 s, and scavenging period is 100 s, and sample detection obtains simultaneously:
The typical curve linear equation of ammonium nitrogen 0.32 mL/min sample introduction flow is Y=43.5+387.5X;
The typical curve linear equation of nitrite nitrogen 0.42 mL/min sample introduction flow is Y=16.8+15664.0X;
The typical curve linear equation of nitrate nitrogen 0.16 mL/min sample introduction flow is Y=13.24+306.8X;
The typical curve linear equation of total nitrogen 0.42 mL/min sample introduction flow is Y=-71.9+332.3X;
The typical curve linear equation of phosphate 0.80 mL/min sample introduction flow is Y=-30309.5+1140024.2X;
The typical curve linear equation of total phosphorus 0.42 mL/min sample introduction flow is Y=-17313.4+398251.2X;
Wherein: X is concentration, unit mg/L; Y is Flow Analyzer signal value reading;
Then testing sample sample size is consistent with typical curve, measures its corresponding signal value reading, calculates its concentration according to calibration curve method;
Every nitrogen phosphorus index is calculated by typical curve equation, wherein:
Measuring reaction reagent needed for ammonium nitrogen is: NH
4 +-A is mixed solution, and include sodium potassium tartrate tetrahydrate 33 g/L, trisodium citrate 24 g/L, pH=5.2, two-way flow is respectively 1 mL/min and 0.8 mL/min; NH
4 +-B is mixed solution, and include sodium salicylate 80 g/L, NaOH 25 g/L, flow is 0.32 mL/min; NH
4 +-C is sodium nitroprusside 1 g/L, and flow is 0.16 mL/min; NH
4 +-D is sodium dichloro cyanurate 2 g/L, and flow is 0.32 mL/min;
Measuring reaction reagent needed for nitrate nitrogen is: NO
3 --A is mixed solution, and include sodium potassium tartrate tetrahydrate 33 g/L, trisodium citrate 24 g/L, flow is 0.8 mL/min; NO
3 --B is NaOH 6 g/L, and flow is 1 mL/min; NO
3 --C is mixed solution, and include hydrazine sulfate 2 g/L, copper sulphate 18 mg/L, flow is 0.42 mL/min; NO
3 --D is mixed solution, and include N-(1-naphthyl) ethylendiamine dihydrochloride 0.5 g/L, sulfanilamide (SN) 10 g/L, phosphatase 11 69 g/L, flow is 0.42 mL/min;
Measuring reaction reagent needed for nitrite nitrogen is: NO
2 --A is pure water, resistivity: 18.3 Μ Ω cm, and flow is 1 mL/min; NO
2 --B is mixed solution, include (N-(1-naphthyl) ethylendiamine dihydrochloride 0.5 g/L, sulfanilamide (SN) 10 g/L, phosphoric acid 253.5 g/L, flow is 0.32 mL/min;
Measuring reaction reagent needed for total nitrogen is: TN-A is mixed solution, and include potassium persulfate 40 g/L, NaOH 12 g/L, flow is 0.42 mL/min; TN-B is boric acid 24 g/L, and flow is 0.42 mL/min; TN-C is ammonium chloride 50 g/L, pH=8.2, and two-way flow is respectively 1 mL/min and 0.8 mL/min; TN-D is mixed solution, and include N-(1-naphthyl) ethylendiamine dihydrochloride 0.5 g/L, sulfanilamide (SN) 10 g/L, hydrochloric acid 118 g/L, flow is 0.23 mL/min;
Measuring reaction reagent needed for phosphate is: PO
4 3--A is mixed solution, includes ammonium molybdate 4.8 g/L, sulfuric acid 73.6g/L, and flow is 0.42 mL/min; PO
4 3--B is mixed solution, and include ascorbic acid 18 g/L, potassium antimony tartrate 6 mg/L, flow is 0.42 mL/min;
Measuring reaction reagent needed for total phosphorus is: TP-A is mixed solution, and include potassium persulfate 9.9 g/L, sulfuric acid 156.4 g/L, flow is 0.23 mL/min; TP-B is sulfuric acid 294.4 g/L, and flow is 0.32 mL/min; TP-C is NaOH 210 g/L, and flow is 0.32 mL/min; TP-D is mixed solution, includes ammonium molybdate 4.8 g/L, sulfuric acid 73.6g/L, and flow is 0.42 mL/min; TP-E is mixed solution, and include ascorbic acid 18 g/L, potassium antimony tartrate 6 mg/L, flow is 0.42 mL/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210591017.XA CN103063816B (en) | 2012-12-31 | 2012-12-31 | Method for simultaneously detecting nitrogen and phosphorus indexes of water quality |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210591017.XA CN103063816B (en) | 2012-12-31 | 2012-12-31 | Method for simultaneously detecting nitrogen and phosphorus indexes of water quality |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103063816A CN103063816A (en) | 2013-04-24 |
| CN103063816B true CN103063816B (en) | 2015-06-03 |
Family
ID=48106527
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210591017.XA Active CN103063816B (en) | 2012-12-31 | 2012-12-31 | Method for simultaneously detecting nitrogen and phosphorus indexes of water quality |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103063816B (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106093139A (en) * | 2016-06-29 | 2016-11-09 | 中国科学院长春应用化学研究所 | A kind of detection method of concentration of methanol solution |
| CN109682944A (en) * | 2019-02-21 | 2019-04-26 | 生态环境部南京环境科学研究所 | Rice field nitrogen phosphorus detection system |
| CN114354594A (en) * | 2019-08-23 | 2022-04-15 | 中国科学院沈阳应用生态研究所 | Method for measuring ammonium nitrogen, nitrate nitrogen, nitrite nitrogen and total dissolved nitrogen in sample |
| CN111208075A (en) * | 2020-01-15 | 2020-05-29 | 兖矿水煤浆气化及煤化工国家工程研究中心有限公司 | Phosphorus-containing water treatment agent total phosphorus detection method based on continuous flow analyzer |
| CN111721757A (en) * | 2020-03-06 | 2020-09-29 | 中国农业科学院农业资源与农业区划研究所 | Water body phosphate continuous flow analyzer and detection method |
| CN114441519B (en) * | 2022-01-24 | 2024-04-02 | 四川为众检测科技有限公司 | Reagent for semi-quantitatively and rapidly determining iodine content in iodized salt, preparation method and application |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101105440A (en) * | 2007-08-01 | 2008-01-16 | 山东省科学院海洋仪器仪表研究所 | Method for measuring water body total nitrogen and total phosphorous by digestion spectrophotometry of ultraviolet cooperating with ozone |
| CN102226770A (en) * | 2011-03-30 | 2011-10-26 | 江苏德林环保技术有限公司 | Flow injection analysis device for nitrite or nitrate in water |
-
2012
- 2012-12-31 CN CN201210591017.XA patent/CN103063816B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101105440A (en) * | 2007-08-01 | 2008-01-16 | 山东省科学院海洋仪器仪表研究所 | Method for measuring water body total nitrogen and total phosphorous by digestion spectrophotometry of ultraviolet cooperating with ozone |
| CN102226770A (en) * | 2011-03-30 | 2011-10-26 | 江苏德林环保技术有限公司 | Flow injection analysis device for nitrite or nitrate in water |
Non-Patent Citations (2)
| Title |
|---|
| AA3自动分析仪测定地表水中的NO2-N、NO3-N+NO2-N、NH3-N、PO43-;袁斌伟等;《污染防治技术》;20050831;第18卷(第4期);第56-58页 * |
| 王云芳等.连续流动分析仪检定规程JJG(烟草)11-1998.《国家烟草专卖局部门计量检定规程》.1998, * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103063816A (en) | 2013-04-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103063816B (en) | Method for simultaneously detecting nitrogen and phosphorus indexes of water quality | |
| CN103335955B (en) | A kind of on-line water quality monitoring method and device | |
| CN102375068B (en) | Full-automatic nutrient salt analyzer and analysis method thereof | |
| Zimmer et al. | High resolution determination of nanomolar concentrations of dissolved reactive phosphate in ocean surface waters using long path liquid waveguide capillary cells (LWCC) and spectrometric detection | |
| CN103217394B (en) | Online detection device of water dissolved-out nitrogen nutrients of chemical fertilizer | |
| CN101793902A (en) | Device for fluidly injecting and rapidly analyzing residual chlorine of water quality and analysis method thereof | |
| Li et al. | High-frequency underway analysis of ammonium in coastal waters using an integrated syringe-pump-based environmental-water analyzer (iSEA) | |
| Kim et al. | PVC membrane-based portable ion analyzer for hydroponic and water monitoring | |
| Copetti et al. | Direct measurement of nutrient concentrations in freshwaters with a miniaturized analytical probe: evaluation and validation | |
| CN101603969A (en) | Flow-injection quick analysis system for hexavalent chromium water quality | |
| CN112685522A (en) | River health management method and system | |
| CN102980858A (en) | Small-size sequential injection nitride analysis system | |
| CN101101264B (en) | Automatic analysis method for seawater sulfide | |
| CN105158018A (en) | Semi-permeable membrane continuous sampling device for passive sampling of water body | |
| CN101776580A (en) | Portable dichromatic wave spectrum spectrometer used for detecting nutrient content in crops | |
| CN202903673U (en) | Full-automatic quick water quality measuring system with hexavalent chromium | |
| Henríquez et al. | Conductometric determination of ammonium by a multisyringe flow injection system applying gas diffusion | |
| CN108572000A (en) | One kind being used for river water sample collection and field assay device | |
| CN203101272U (en) | Ammonia nitrogen detector | |
| CN102375073A (en) | Fully automatic fluorine analyzer and analytical method thereof | |
| CN103913421A (en) | Method for determining water-soluble Fe content of eutrophic lake | |
| CN201765236U (en) | Full-automatic nutritive salt analyzer | |
| CN102590535A (en) | Automatic analysis method of nitrite in water sample | |
| CN109709197A (en) | BOD Quick testing instrument and accurately compensate measuring method | |
| CN109060692A (en) | Active phosphorus automatic analyzer and its measuring method based on syringe pump |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |