CN104568804A - Method for detecting total nitrogen and total phosphorus of drainage basin - Google Patents
Method for detecting total nitrogen and total phosphorus of drainage basin Download PDFInfo
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- CN104568804A CN104568804A CN201510050021.9A CN201510050021A CN104568804A CN 104568804 A CN104568804 A CN 104568804A CN 201510050021 A CN201510050021 A CN 201510050021A CN 104568804 A CN104568804 A CN 104568804A
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Abstract
The invention provides a method for detecting total nitrogen and total phosphorus of a drainage basin, for improving the total nitrogen and total phosphorus analysis speed. By adopting the method, the content of total nitrogen and total phosphorus can be detected in the same detection process. Moreover, on the one hand, the defect of low total nitrogen and total phosphorus analysis speed under a high temperature and high pressure condition is overcome by using a COD (chemical oxygen demand) digester, and the digestion temperature is not too high; and on the other hand, the problem that other interfering precipitation products may be produced by directly adding alkaline potassium persulfate in the traditional method can be solved by adding alkali and filtering, and observation of a sample in subsequent acid adding is facilitated.
Description
Technical field
The invention belongs to water analysis technical field, more specifically, relate to a kind of basin total nitrogen total phosphorus detection method.
Background technology
Total nitrogen refers to the solubility in water sample and the nitrogen content in suspended particle.In China " water environment quality standard " (GHZB1-1999), the standard value range of total nitrogen is
the laboratory analysis methodologies of total nitrogen is that alkaline chitinase clears up-ultraviolet spectrophotometry.At present, the main Types of total nitrogen on-line automatic analyzer has persulfate to clear up-photometry; Airtight combustion oxidation-chemiluminometry.
Total phosphorus comprises dissolving, particle, organic and Phos.
In relevant water quality standard, China specifies that the environmental standard value scope of total phosphorus is surface water:
; Sewage:
at present, the laboratory analysis methodologies of total phosphorus has potassium persulfate (or nitric acid-perchloric acid) to clear up-ammonium molybdate spectrophotometric method, and this method is also referred to as " molybdenum-antimony anti-spectrophotometric method " or " molybdenum blue method ".At present, the main Types of total phosphorus on-line automatic analyzer has persulfate to clear up-photometry; Ultraviolet radiation-molybdenum catalysis heating and decompose, FIA-photometry.
Many research datas show, the content of total nitrogen, total phosphorus and the Eutrophic Extent correlation in lake.Therefore, want effectively to prevent and treat body eutrophication, measure total nitrogen in the water bottom sediments such as river, lake, river, storehouse, sea, total phosphorus is just very necessary.Total nitrogen is the general name of nitrate nitrogen, nitrite nitrogen, ammonia nitrogen and organic nitrogen, and the total nitrogen total phosphorus content in water is one of important indicator weighing water quality, is the leading indicator of reflection body eutrophication.It measures and contributes to evaluating the contaminated and self-cleaning situation of water body.When in surface water, nitrogen, phosphorus substance exceed standard, microorganism amount reproduction, planktonic organism growth is vigorous, occurs eutrophic state.
In current water quality, the pre-treatment of the assay method of total nitrogen total phosphorus is comparatively loaded down with trivial details, manually consuming time longer, also has certain pollution, make troubles to analytical work to the reagent measured, instrument.
Summary of the invention
In order to improve total nitrogen total phosphorus analysis speed, the invention provides a kind of basin total nitrogen total phosphorus detection method, comprising the steps:
(1) digestion solution utilizing same digestion process to obtain draws total nitrogen typical curve and total phosphorus typical curve simultaneously, and from basin to be detected collecting sample;
(2) sample is divided into two parts, adds the potassium hydroxide solution of variable concentrations respectively;
(3) uniform stirring two increment originally;
(4) sample is filtered;
(5) carry out repeatedly recrystallization to potassium persulfate, then a sample adds this potassium persulfate wherein;
(6) two increments are originally put into COD counteract appearance to heat;
(7) after certain hour, take out two these water-baths of increment and be cooled to room temperature, then respectively HCI is added to the sample wherein adding potassium persulfate solution; Originally ammonium molybdate solution and ascorbic acid solution is added to another increment;
(8) uniform stirring two increment originally;
(9) ultraviolet spectrophotometer is utilized to measure absorbance, and the reference absorbance using result as sample;
(10) compare with reference to absorbance with described, obtain the total nitrogen total phosphorus content of the water body in basin to be detected.
Further, the concentration of described potassium hydroxide solution is respectively 1.02-1.2mol/L and 0.6-0.8mol/L.
Further, the concentration of described potassium hydroxide solution is respectively 1.06mol/L and 0.66mol/L.
Further, the concentration of described NaOH is 2%, and the concentration added after the potassium persulfate in step (5) is 5%.
Further, in step (6), the temperature of heating is 50 degrees Celsius-60 degrees Celsius.
Further, in step (6), the temperature of heating is 55 degrees Celsius.
Further, being pressurised in step (5): make sample enter closed container and be pressurised into 2 standard atmospheric pressures.
Further, described step (9) comprising: to make reference without ammoniacal liquor, measures absorbance respectively with 10mm quartz colorimetric utensil at 255nm wavelength place and 850nm wavelength place, and respectively as the reference absorbance of total nitrogen and the reference absorbance of total phosphorus.
Further, the described digestion solution utilizing same digestion process to obtain draws total nitrogen typical curve and total phosphorus typical curve comprises simultaneously:
(A) the standard mixed liquor that 4ml contains 3.00 microgram phosphorus and 12 microgram nitrogen is prepared;
(B) ammonium molybdate standard solution, stannous chloride standard solution is prepared, and 1+9 hydrochloric acid standard solution;
(C) potassium persulfate solution of 500ml, 8% concentration is prepared;
(D) sodium hydroxide solution of 500ml, 3% concentration is prepared;
(E) 500ml alkaline chitinase solution is prepared, wherein potassium persulfate 30g, NaOH 12g;
(F) the l alkaline chitinase solution that standard mixed liquor step (A) obtained, 10ml step (E) are prepared adds color comparison tube and uses without ammoniacal liquor constant volume to 30ml;
(G) spin the sealing of color comparison tube lid, put into heater bore, be warming up to 125 DEG C and keep 30min;
(H) after digestion tube cooling, 50ml is diluted to without ammoniacal liquor, and divide equally for two parts, wherein a part adds 1+9 hydrochloric acid standard solution 2ml that step (B) prepares and utilize ultraviolet spectrophotometer to measure typical curve that absorbance obtains total nitrogen; Another part adds the ammonium molybdate standard solution and 0.5ml stannous chloride standard solution that 4ml above-mentioned steps (B) prepares, static rear utilize ultraviolet spectrophotometer to measure typical curve that absorbance obtains total phosphorus.
Beneficial effect of the present invention is: the present invention can record the content of total nitrogen and total phosphorus in same testing process, and on the one hand, the defect utilizing COD counteract appearance to avoid high-temperature and high-pressure conditions to cause total nitrogen total phosphorus analysis speed slow, the Conditions Temperature cleared up need not be too high; On the other hand, through first adding the step of alkali and filtration, can make directly to add in classic method the problem that alkaline chitinase may produce other interference precipitated products and being avoided, be conducive to observation during the follow-up acid adding of sample.
Accompanying drawing explanation
Fig. 1 shows the process flow diagram of the preferred embodiment according to basin of the present invention total nitrogen total phosphorus detection method.
Embodiment
Basin total nitrogen total phosphorus detection method as shown in Figure 1, comprising:
(1) digestion solution utilizing same digestion process to obtain draws total nitrogen typical curve and total phosphorus typical curve simultaneously, and from basin collecting sample 20ml to be detected;
The described digestion solution utilizing same digestion process to obtain draws total nitrogen typical curve simultaneously and total phosphorus typical curve comprises:
(A) the standard mixed liquor that 4ml contains 3.00 microgram phosphorus and 12 microgram nitrogen is prepared;
(B) ammonium molybdate standard solution, stannous chloride standard solution is prepared, and 1+9 hydrochloric acid standard solution;
(C) potassium persulfate solution of 500ml, 8% concentration is prepared;
(D) sodium hydroxide solution of 500ml, 3% concentration is prepared;
(E) 500ml alkaline chitinase solution is prepared, wherein potassium persulfate 30g, NaOH 12g;
(F) the l alkaline chitinase solution that standard mixed liquor step (A) obtained, 10ml step (E) are prepared adds color comparison tube and uses without ammoniacal liquor constant volume to 30ml;
(G) spin the sealing of color comparison tube lid, put into heater bore, be warming up to 125 DEG C and keep 30min;
(H) after digestion tube cooling, 50ml is diluted to without ammoniacal liquor, and divide equally for two parts, wherein a part adds 1+9 hydrochloric acid standard solution 2ml that step (B) prepares and utilize ultraviolet spectrophotometer to measure typical curve that absorbance obtains total nitrogen; Another part adds the ammonium molybdate standard solution and 0.5ml stannous chloride standard solution that 4ml above-mentioned steps (B) prepares, static rear utilize ultraviolet spectrophotometer to measure typical curve that absorbance obtains total phosphorus.
(2) sample is divided into two parts, every part of 10ml, adds the potassium hydroxide of variable concentrations 1.06mol/L and 0.66mol/L respectively; In other examples, the concentration of described potassium hydroxide solution is respectively 1.02-1.2mol/L and 0.6-0.8mol/L.
(3) uniform stirring two increment originally;
(4) sample is filtered, the impurity such as the blade of grass in filtering sample;
(5) carry out repeatedly recrystallization to potassium persulfate, then a sample adds the potassium persulfate solution of 5% concentration prepared through this potassium persulfate wherein;
Above-mentioned recrystallization process is: in the beaker of 1L, add about 800ml ultrapure water, heat in 2 standard atmospheric pressures, the water-bath of 50 DEG C, then add potassium persulfate gradually, limit edged stirs, until potassium persulfate no longer dissolves, then filter out impurity with clean glass sand hourglass, filtrate is placed in after wide-necked bottle is cooled to room temperature, put into the refrigerator recrystallization of 4 DEG C, should notice that wide-necked bottle should be added a cover avoids impurity to enter, while recrystallization, and ice one bottle of ultrapure water in refrigerator.Recrystallization is after 12 hours, and potassium persulfate can form a certain amount of loose crystals at the bottom of wide-necked bottle, now outwells supernatant, crystal is done loose with glass rod, clean 3 times with the ultrapure water that prior ice is good again, outwell upper liquid after cleaning, the baking oven flood then crystal being put into 50 DEG C is dry.For ensureing crystallization effect, best recrystallization is (such as, twice) repeatedly; After crystallization, originally add each 2ml of this potassium persulfate respectively equally to two increments;
(6) two increments are originally put into COD counteract appearance and heat 20min under 55 degrees Celsius; In other examples, the thermal creep stress of heating is at 50 degrees Celsius-60 degrees Celsius.
(7) take out two these water-baths of increment and be cooled to room temperature, such as, 25 degrees Celsius, then add hydrochloric acid respectively to the sample wherein adding potassium persulfate solution, the mode that titration crossed by the graduated cylinder of hydrochloric acid is determined, is as the criterion finally to reach neutrality; Because the present invention preferably adopts the mode of titration to add hydrochloric acid, therefore, the color of observing solution in the process of titration is needed.Based on this, applicant devises the step through first adding alkali and filtration, can make directly to add in classic method the problem that alkaline chitinase may produce other interference precipitated products and be avoided, and is conducive to observation during the follow-up acid adding of sample.
(8) uniform stirring two increment originally;
(9) utilize ultraviolet spectrophotometer, to make reference without ammoniacal liquor, utilize 1cm quartz colorimetric utensil to measure absorbance at 255nm and 850nm place respectively, and respectively as the reference absorbance of total nitrogen and the reference absorbance of total phosphorus;
(10) compare with reference to absorbance with described, obtain the total nitrogen total phosphorus content of the water body in basin to be detected.
It is illustrate and explain that the above-mentioned disclosure of the present invention describes, and being used for various modifications embodiment disclosed herein and changing is obvious for a person skilled in the art.Be intended that within all these improve and variation all drops on application claims rights protection spirit and scope.
Claims (9)
1. a basin total nitrogen total phosphorus detection method, comprises the steps:
(1) digestion solution utilizing same digestion process to obtain draws total nitrogen typical curve and total phosphorus typical curve simultaneously, and from basin to be detected collecting sample;
(2) sample is divided into two parts, adds the potassium hydroxide solution of variable concentrations respectively;
(3) uniform stirring two increment originally;
(4) sample is filtered;
(5) carry out repeatedly recrystallization to potassium persulfate, then a sample adds this potassium persulfate wherein;
(6) two increments are originally put into COD counteract appearance to heat;
(7) after certain hour, take out two these water-baths of increment and be cooled to room temperature, then respectively HCI is added to the sample wherein adding potassium persulfate solution; Originally ammonium molybdate solution and ascorbic acid solution is added to another increment;
(8) uniform stirring two increment originally;
(9) ultraviolet spectrophotometer is utilized to measure absorbance, and the reference absorbance using result as sample;
(10) compare with reference to absorbance with described, obtain the total nitrogen total phosphorus content of the water body in basin to be detected.
2. basin according to claim 1 total nitrogen total phosphorus detection method, it is characterized in that, the concentration of described potassium hydroxide solution is respectively 1.02-1.2mol/L and 0.6-0.8mol/L.
3. basin according to claim 2 total nitrogen total phosphorus detection method, it is characterized in that, the concentration of described potassium hydroxide solution is respectively 1.06mol/L and 0.66mol/L.
4. basin according to claim 1 total nitrogen total phosphorus detection method, is characterized in that, the concentration of described NaOH is 2%, and the concentration added after the potassium persulfate in step (5) is 5%.
5. basin according to claim 1 total nitrogen total phosphorus detection method, is characterized in that, in step (6), the temperature of heating is 50 degrees Celsius-60 degrees Celsius.
6. basin according to claim 1 total nitrogen total phosphorus detection method, is characterized in that, in step (6), the temperature of heating is 55 degrees Celsius.
7. basin according to claim 1 total nitrogen total phosphorus detection method, is characterized in that, being pressurised in step (5): make sample enter closed container and be pressurised into 2 standard atmospheric pressures.
8. basin according to claim 1 total nitrogen total phosphorus detection method, it is characterized in that, described step (9) comprising: to make reference without ammoniacal liquor, absorbance is measured at 255nm wavelength place and 850nm wavelength place respectively with 10mm quartz colorimetric utensil, and respectively as the reference absorbance of total nitrogen and the reference absorbance of total phosphorus.
9. basin according to claim 1 total nitrogen total phosphorus detection method, is characterized in that, the described digestion solution utilizing same digestion process to obtain draws total nitrogen typical curve simultaneously and total phosphorus typical curve comprises:
(A) the standard mixed liquor that 4ml contains 3.00 microgram phosphorus and 12 microgram nitrogen is prepared;
(B) ammonium molybdate standard solution, stannous chloride standard solution is prepared, and 1+9 hydrochloric acid standard solution;
(C) potassium persulfate solution of 500ml, 8% concentration is prepared;
(D) sodium hydroxide solution of 500ml, 3% concentration is prepared;
(E) 500ml alkaline chitinase solution is prepared, wherein potassium persulfate 30g, NaOH 12g;
(F) the l alkaline chitinase solution that standard mixed liquor step (A) obtained, 10ml step (E) are prepared adds color comparison tube and uses without ammoniacal liquor constant volume to 30ml;
(G) spin the sealing of color comparison tube lid, put into heater bore, be warming up to 125 DEG C and keep 30min;
(H) after digestion tube cooling, 50ml is diluted to without ammoniacal liquor, and divide equally for two parts, wherein a part adds 1+9 hydrochloric acid standard solution 2ml that step (B) prepares and utilize ultraviolet spectrophotometer to measure typical curve that absorbance obtains total nitrogen; Another part adds the ammonium molybdate standard solution and 0.5ml stannous chloride standard solution that 4ml above-mentioned steps (B) prepares, static rear utilize ultraviolet spectrophotometer to measure typical curve that absorbance obtains total phosphorus.
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Cited By (5)
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| CN106865503A (en) * | 2017-03-15 | 2017-06-20 | 华南理工大学 | A kind of method of micro total nitrogen and ammonia nitrogen in removal potassium peroxydisulfate |
| CN109655419A (en) * | 2018-12-15 | 2019-04-19 | 南京鸿恺环保科技有限公司 | A kind of improvement test method of total phosphorus and total nitrogen |
| CN110133226A (en) * | 2019-05-28 | 2019-08-16 | 河海大学 | A kind of the phosphorus pollution level judgment method and experimental provision of middle and small river beach |
| CN111562226A (en) * | 2020-04-10 | 2020-08-21 | 中国科学院西安光学精密机械研究所 | Method and system for analyzing total nitrogen and total phosphorus in seawater based on characteristic peak area of absorption spectrum |
| CN113029993A (en) * | 2021-03-24 | 2021-06-25 | 中南大学 | Ultraviolet spectrum rapid total nitrogen online detection method based on attention mechanism |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106865503A (en) * | 2017-03-15 | 2017-06-20 | 华南理工大学 | A kind of method of micro total nitrogen and ammonia nitrogen in removal potassium peroxydisulfate |
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| CN110133226A (en) * | 2019-05-28 | 2019-08-16 | 河海大学 | A kind of the phosphorus pollution level judgment method and experimental provision of middle and small river beach |
| CN111562226A (en) * | 2020-04-10 | 2020-08-21 | 中国科学院西安光学精密机械研究所 | Method and system for analyzing total nitrogen and total phosphorus in seawater based on characteristic peak area of absorption spectrum |
| CN111562226B (en) * | 2020-04-10 | 2021-10-15 | 中国科学院西安光学精密机械研究所 | Method and system for analyzing total nitrogen and total phosphorus in seawater based on characteristic peak area of absorption spectrum |
| CN113029993A (en) * | 2021-03-24 | 2021-06-25 | 中南大学 | Ultraviolet spectrum rapid total nitrogen online detection method based on attention mechanism |
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