CN109142249A - A kind of Seawater Nitrate concentration determination method - Google Patents

A kind of Seawater Nitrate concentration determination method Download PDF

Info

Publication number
CN109142249A
CN109142249A CN201811009775.XA CN201811009775A CN109142249A CN 109142249 A CN109142249 A CN 109142249A CN 201811009775 A CN201811009775 A CN 201811009775A CN 109142249 A CN109142249 A CN 109142249A
Authority
CN
China
Prior art keywords
seawater
added
agent
nitrate
quantitative
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.)
Pending
Application number
CN201811009775.XA
Other languages
Chinese (zh)
Inventor
冷俊昭
刘吉堂
王丕波
李在通
谢雷仕
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Qingdao Zhuo Jian Marine Equipment Technology Co Ltd
Original Assignee
Qingdao Zhuo Jian Marine Equipment Technology Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Qingdao Zhuo Jian Marine Equipment Technology Co Ltd filed Critical Qingdao Zhuo Jian Marine Equipment Technology Co Ltd
Priority to CN201811009775.XA priority Critical patent/CN109142249A/en
Publication of CN109142249A publication Critical patent/CN109142249A/en
Pending legal-status Critical Current

Links

Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/3103Atomic absorption analysis
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N21/78Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour

Abstract

The present invention provides a kind of Seawater Nitrate concentration determination method, process and testing process are drawn including working curve, standard working curve can be brought into and calculate total nitrate content, deduct the concentration value of original nitrite in seawater, the nitrate concentration value as in seawater.It is simple and efficient that the beneficial effects of the invention are as follows testing process, and method is stable, favorable reproducibility, and working curve shows good linear relationship, and measurement result accuracy is high, effectively shortens test period, reduces energy consumption, on the other hand can reduce reagent dosage, reduce cost.

Description

A kind of Seawater Nitrate concentration determination method
Technical field
The present invention relates to seawater quality detection field more particularly to a kind of Seawater Nitrate concentration determination methods.
Background technique
Nutritive salt is as ingredient necessary to marine phytoplankton growth and breeding and primary productivity of marine ecosystem and food chain Basis.And nutritive salt content in the seawater, distribution are significantly influenced by marine organisms are movable, therefore nutrients in sea water The always important research content of chemical oceanography, nutritive salt analytical technology also just become the base of marine biogeochemistry research One of plinth.
Nitrogen is that phytoplankton progress Primary Production must not as one of most basic nutriment of marine organisms vital movement Can nutrient less, the primary productivity in ocean is significantly limited by obtainable nitrogen source when phytoplankton assimilation. In recent years, environment and resource problem become increasingly conspicuous, and people is promoted to deepen research to marine ecosystems and to sea The development and utilization of foreign resource.
It is defeated to be mainly derived from rainwash input, atmospheric sedimentation and colcanism, immediate offshore area, rainwash for nitrogen in ocean Enter to account for total 70% or more input, and exchange of seawater of the nitrogen mainly from itself and immediate offshore area in exposed waters.Rivers mouth seawater and What immediate offshore area was artificially inputted is affected, and nitrogen content is generally higher, nitrogen excess phenomenon even occur in some regions, causes Environment Management of Eutrophication induces the harm of the oceans such as red tide.Exposed waters are opposite smaller by man's activity, substantially also keep it Reset condition, some regions make certain biotic populations since nitrogen is poor, or even as the restriction factor of marine phytoplankton growth Biomass reduce, primary productivity of marine ecosystem is had an impact.
Dissolved Inorganic Nitrogen is mainly with nitrate (NO in seawater3 ), nitrite (NO2 ) and ammonia salt (NH4 +) (i.e. three nitrogen) Form exist.Nutritive salt necessary to growing as marine phytoplankton, dissolved Inorganic Nitrogen are followed in marine biogeochemistry It plays an important role in ring.In euphotic layer, NO3 After being absorbed by phytoplankton, the dissolution in bottom water body and deposit is organic Nitrogen can by nitrification by bacterial oxidation at NO3 Reenter euphotic layer.Nitrate (NO3 ) final oxygen as inorganic nitrogen Change product, NO in general seawater3 Content is higher, accounts for 65% of dissolved nitrogen or more.
Seawater Nitrate tests national standard method, according to " the 4th part of marine monitoring specification: sea water analysis " (GB17378.4- 2007) measuring method of seawater nitric acid is Zn-Cd reduction, Method And Principle: with the zinc metal sheet of cadmium plating by the nitrate in water sample Quantitative reduction is nitrite, and total nitrite in water sample uses diazonium-azo method measurement again, then to original nitrite It is corrected, calculates nitrate content.
The measurement of Zn-Cd reduction nitrate nitrogen suitable for ocean and coastal seawater, estuarine water, measurement range 0.05 μm ol/L~16.0 μm ol/L.
Zn-Cd reduction operating process is complicated, and the waste liquid containing heavy metal generated in test needs to be recycled, and holds Secondary pollution is easily caused, marine environmental protection is unfavorable for.Therefore domestic and foreign scholars have carried out the largely survey about Seawater Nitrate The research of method for testing, to develop more convenient, clean and environmental protection Seawater Nitrate test method.Measure nitric acid in water body The method of salt mainly has fluorescence method, high performance liquid chromatography, chemoluminescence method, liquid core waveguide spectrophotometry, UV absorption light Spectrometry etc..
Fluorescence method: with the high sensitivity of nitrate in fluorescence detection measurement water body.When test, nitrate is as reactant It is acted on reaction reagent, their effect product can generate fluorescence or enhance the intensity of fluorescence signal.Pass through reaction front and back Fluorescence signal intensity variation relation converts to obtain nitrate concentration, and nitrate is dense in the Strength Changes of fluorescence signal and water sample It spends directly proportional.However, fluorescence method is easy the interference by metal ion in water sample and organic substance, lead to the accurate of test data Spend low, detection limit is slightly higher, for the detection of low concentration nitrate in seawater and few.
High performance liquid chromatography: high performance liquid chromatography can detecte the NO3-N and NO2-N of low concentration in seawater. Make the nitrite in seawater and the derivatization reagent of configuration that derivative reaction occur, a kind of stable nitrine chemical combination can be generated Then object is measured the compound with chromatography at wavelength 307nm.When measuring nitrate, it can be first reduced to nitrous Hydrochlorate, then detected.This method advantage is that detection limit is low, and can inhibit nitrogen oxides and inorganic N forms conversion pair in air It is polluted caused by water sample, the interference of other ions and organic matter can be effectively reduced.But works as and contain phosphate radical and sulfuric acid in water sample When radical ion, derivative reaction can be fairly slow, influences test speed.
Chemoluminescence method: mainly including luminol chemiluminescence method and ozone chemistry luminescence method.Luminol chemiluminescence method It is to be irradiated after alkali is added into seawater sample with ultraviolet light, or add hydrogenperoxide steam generator, the nitric acid in water after acid is added Salt will be converted into peroxynitrite, then react with luminol luminous agent and generate chemiluminescence, and wherein luminous intensity becomes Change directly proportional to the concentration of nitrate.The disadvantages of the method are as follows being easy to be influenced by other interfering ions in water body, for example, water Many metal ions can react with hydrogen peroxide in body, and dithizone can also be catalyzed luminol luminous agent, interfering ion Too much, most metal ion is also removed before testing, and big with this method detection Seawater Nitrate error, accuracy is low.
Ozone chemistry luminescence method: this method is nitrate in water body to be reduced to nitric oxide through reducing agent, and be blown into load Gas makes exogenous nitric oxide generate nitrogen dioxide with ozone reaction in Chemiluminescence Apparatus, detects titanium dioxide by photomultiplier tube The optical signal that nitrogen issues measures nitrate concentration, and can to measure low concentration nitrate the advantages of this method in seawater be not have The interference effect of suspended particulate substance and coloring matter in water sample, high sensitivity, but nitrate needs to be converted to an oxidation in water sample Nitrogen cannot be tested directly.
Liquid core waveguide spectrophotometry: measuring Seawater Nitrate concentration with this method, be first with optimun techniques by nitre Hydrochlorate is reduced to nitrite, after adding color developing agent pretreatment, is pumped into waveguide.It is micron amount that this method, which is with diameter, Grade, length to several meters waveguide serve as sample cell, the material properties of the waveguide is stablized, and does not react with water, and roll over The rate of penetrating is less than water sample refractive index, so the light emission that wavelength is 540nm can be on the interface of water sample and waveguide after entering waveguide It is totally reflected, and constantly penetrates water sample always along waveguide onwards transmission, in its measurement of output end absorbance through multiple reflections Value.Therefore, only a small amount of water sample to be measured is needed to be achieved with very long effective light path, the optical signal that can significantly improve output is strong Degree.The advantages of this method is error caused by when being avoided that environmental change and sampling, and can carry out follow-on test.But it develops the color Reaction is influenced vulnerable to temperature change, influences test result accuracy, to reduce temperature influence, it is necessary to be extended developing time, be tested Relatively slow, the too long blank also resulted between test of waveguide optical path is big, influences measurement result.
Ultraviolet absorption spectroscopy: since the nitrate in water body not only has absorption to ultraviolet light, and in certain concentration range Inside meet Lambert-Beer's law, so, the linear pass of nitrate concentration and absorbance can be established by Partial Least Squares It is model, obtains prediction nitrate concentration.Great advantage with ultraviolet absorption spectroscopy detection Nitrate In Sea Water is simple fast Speed, complex reaction cannot occur for substance in test process, and the water sample processing step of no complexity can directly test water sample and obtain nitre Hydrochlorate concentration.The advantages of method be can real-time measurement, measurement process needs chemical reagent to participate in, without secondary pollution, can be used for Long-term early warning and monitoring, but measuring accuracy is low, detects limit for height, is influenced by water turbidity.
The test of Seawater Nitrate follows two kinds of thinkings: one is the direct method of measurement, another kind is the indirect method of measurement.
The direct method of measurement is the nitrate content directly measured in seawater, including fluorescence method and ultraviolet absorption spectroscopy, is surveyed It is low to try precision, detects limit for height.
The indirect method of measurement is first handled seawater sample, is nitrite or an oxidation by the nitrate transformation in seawater Nitrogen passes through the nitrate content in test nitrite or nitric oxide production content indirectly testing water body.Since Ge Lisi is anti- It should be used as the prefered method of test nitrite, testing process is simple and efficient, and method is stable, favorable reproducibility, so surveying indirectly Amount method is paid the utmost attention to when testing nitrate by the nitrate transformation in seawater be nitrite.
The key of influence indirect method of measurement test nitrate accuracy is the efficiency that nitrate is reduced to nitrite.It can To pass through dedicated nitrate reducing for nitrate reduction as nitrite, or using the metal with reproducibility, cadmium is just It is the most commonly used one kind.In order to reduce sample volume demand and increase the reduction efficiency of sample, there are many cadmium reduction methods Improved method research, but there are still following deficiencies for cadmium reduction method: time-consuming, need cadmium column persistently keep activity and Cadmium toxicity is high, and sample and hazardous waste need to handle.
Summary of the invention
The object of the present invention is to provide a kind of Seawater Nitrate concentration determination method, a kind of Seawater Nitrate concentration determination side Method, including working curve draw process and testing process, the working curve draw process successively the following steps are included:
In six colorimetric cylinders, nitrate-nitrogen concentration is moved into respectively and is followed successively by 0,0.05,0.15,0.25,0.35,0.50mg/L Series standard solution;
It is addedIt is quantitativeIt mixes and places after color developing agent 1Predetermined time
It is addedIt is quantitativeIt mixes and places after color developing agent 2Predetermined time
It is addedIt is quantitativeReducing agent, cover tightly glass stopper, gently shake up, 60 DEG C of water-bath predetermined times, are cooled in temperature control sink Room temperature;
With 2.0cm colorimetric pool, reference is made with artificial seawater, tests light absorption value, blank absorbency Ab at 543nm wavelength;With button Except the light absorption value An after Blank absorbance values Ab is ordinate, nitrate-nitrogen concentration is that abscissa draws standard working curve;
The testing process includes: to take quantitative seawater sample, mixes placement predetermined time step after quantitative chromogenic agent is added, is added After Quantitative reduction agent mixes the step of water-bath, cooling step tests its absorbance value at 543nm wavelength with 2cm colorimetric pool Step.
Further, the colorimetric cylinder that the working curve draws process is 25.0ml, and the addition quantitative chromogenic agent 1 is The concentration of 0.5ml is the P-aminobenzene-sulfonamide solution of 10g/L, the additionIt is quantitativeIt mixes and places after color developing agent 1Predetermined time For5min, the concentration that the addition quantitative chromogenic agent 2 is 0.5ml is 1.0g/L to hydrochloride naphthodiamide solution, the additionIt is quantitativeIt mixes and places after color developing agent 2Predetermined time is15min, the additionIt is quantitativeReducing agent be 2ml vanadium trichloride solution, institute Stating 60 DEG C of water-bath predetermined times is 20min.
Further, the testing process is successively are as follows: takes 25ml seawater sample, 0.5ml color developing agent 1 is added mixes and place 5min is added 0.5ml color developing agent 2 and mixes placement 15min, 2ml reducing agent is added, the step of 60 DEG C of water-bath 20min is kept after mixing Suddenly, it is cooled to room temperature step, with 2cm colorimetric pool, the step of its absorbance value is tested at 543nm wavelength.
Further, the colorimetric cylinder of the working curve drafting process is10.0ml, the addition quantitative chromogenic agent 1 is The concentration of 0.2ml is the P-aminobenzene-sulfonamide solution of 10g/L, the additionIt is quantitativeIt mixes and places after color developing agent 1Predetermined time For5min, the concentration that the addition quantitative chromogenic agent 2 is 0.2ml is 1.0g/L to hydrochloride naphthodiamide solution, the additionIt is quantitativeIt mixes and places after color developing agent 2Predetermined time is10min, the additionIt is quantitativeReducing agent be 0.8ml vanadium trichloride solution, 60 DEG C of water-bath predetermined times are 10min.
Further, the testing process is successively are as follows: takes 10ml seawater sample, 0.2ml color developing agent 1 is added mixes and place 5min is added 0.2ml color developing agent 2 and mixes placement 10min, 0.8ml reducing agent is added, keeps 60 DEG C of water-bath 10min's after mixing Step is cooled to room temperature step, with 2cm colorimetric pool, the step of its absorbance value is tested at 543nm wavelength.
The advantages and positive effects of the present invention are:
Testing process is simple and efficient, and method is stable, favorable reproducibility, and working curve shows good linear relationship, measurement knot Fruit accuracy is high, can effectively shorten test period, reduces energy consumption, and can reduce reagent dosage, reduces cost.
Detailed description of the invention
In order to illustrate the embodiments of the present invention more clearly or technical em- bodiments in the prior art, below will to embodiment or Attached drawing needed to be used in the description of the prior art does one and simply introduces, it should be apparent that, the accompanying drawings in the following description is this Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with It obtains other drawings based on these drawings.
Fig. 1 is a kind of sample test flow chart for Seawater Nitrate concentration determination method that the embodiment of the present invention one provides;
Fig. 2 is the NO that the embodiment of the present invention one provides3The working curve diagram of-N;
Fig. 3 is a kind of sample test flow chart of Seawater Nitrate concentration determination method provided by Embodiment 2 of the present invention;
Fig. 4 is NO provided by Embodiment 2 of the present invention3The working curve diagram of-N;
Fig. 5 is a kind of sample test flow chart for Seawater Nitrate concentration determination method that the embodiment of the present invention three provides;
Fig. 6 is the NO that the embodiment of the present invention three provides3The working curve diagram of-N.
Specific embodiment
To keep the purpose of the present invention, technical em- bodiments and advantage clearer, hereinafter with reference in the embodiment of the present invention Attached drawing clearly and completely describes technical em- bodiments of the invention by embodiment, it is clear that described embodiment is this hair Bright a part of the embodiment, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not having Every other embodiment obtained under the premise of creative work is made, shall fall within the protection scope of the present invention.
Embodiment one:
As shown in Figure 1, 2, testing process includes
(1) working curve is drawn
In six 25.0ml colorimetric cylinders, nitrate standard is moved into respectively and uses solution (0.100 μm of ol/mL) 0,0.50,1.00, 1.50,2.50,4.00ml, graticule is diluted to the artificial seawater that salinity is 35.This standard liquid series nitrate-nitrogen concentration according to It is secondary be 0 μm of ol/L, 2.00 μm of ol/L, 4.00 μm of ol/L, 6.00 μm of ol/L, 10.0 μm of ol/L, 16.0 μm of ol/L.
2.5ml reducing agent is added, covers tightly glass stopper, gently shakes up, 60 DEG C of water-bath 20min, are cooled in temperature control sink 0.5ml color developing agent 1 is added in room temperature, mixes static 5min, and 0.5ml color developing agent 2 is added, and mixes colour developing 15min, is measured with 2.0cm The light absorption value at 543nm wavelength is tested with artificial seawater reference in pond, blank absorbency Ab,
To deduct the light absorption value An after Blank absorbance values Ab as ordinate, nitrate-nitrogen concentration is that abscissa draws standard Working curve, and standard working curve intercept and slope are found out with linear regression method.
(2) sample test
25ml seawater sample is taken, 2.5ml reducing agent is added, is mixed.
Keep 60 DEG C of water-bath 25min.
It is cooled to room temperature.
0.5ml color developing agent 1 is added, mixes static 5min, 0.5ml color developing agent 2 is added, mixes, develop the color 15min.
With 2cm colorimetric pool, its absorbance value is tested at 543nm wavelength.
It brings standard working curve into and calculates total nitrate content, deduct the concentration value of original nitrite in seawater, Nitrate concentration value as in seawater.
(3) test result
Working curve test original record is as shown in table 1, and the standard working curve of drafting is shown in Fig. 2, equation of linear regression y= 0.0286x-0.0119, related coefficient 0.9961 illustrate to test nitrate according to embodiment one, as nitrate concentration changes Show good linear relationship.
1 embodiment of table, one NO3The working curve of-N tests tables of original record
Embodiment two
As shown in Fig. 3,4,5, Seawater Nitrate is tested according to embodiment one, working curve shows good linear relationship, but It is that absorbance value is integrally lower than Zn-Cd reduction, reduction efficiency may be relatively low, therefore designs embodiment two
(1) working curve is drawn
In six 25.0ml colorimetric cylinders, move into respectively this standard liquid series nitrate-nitrogen concentration be followed successively by 0,0.05, 0.15, the standard solution of 0.25,0.35,0.50mg/L.
0.5ml color developing agent 1 is added, mixes static 5min, 0.5ml color developing agent 2 is added, mixes, develop the color 15min.
The reducing agent of 2ml is added, covers tightly glass stopper, gently shakes up, 60 DEG C of water-bath 20min, are cooled in temperature control sink Room temperature.
With 2.0cm cell, with artificial seawater reference, the light absorption value at 543nm wavelength is tested, blank absorbency Ab, with Light absorption value An after deducting Blank absorbance values Ab is ordinate, and nitrate-nitrogen concentration is that abscissa drafting standard work is bent Line, and standard working curve intercept and slope are found out with linear regression method.
(2) sample test
25ml seawater sample is taken, 1ml color developing agent is added, is mixed.
0.5ml color developing agent 1 is added, mixes static 5min, 0.5ml color developing agent 2 is added, mixes, develop the color 15min.
2ml reducing agent is added, covers tightly glass stopper, gently shakes up, 60 DEG C of water-bath 20min, are cooled to room in temperature control sink Temperature.
With 2cm colorimetric pool, its absorbance value is tested at 543nm wavelength.
It brings standard working curve into and calculates total nitrate content, deduct the concentration value of original nitrite in seawater, Nitrate concentration value as in seawater.
(3) test result
Working curve test original record is as shown in table 2, and the standard working curve of drafting is shown in Fig. 4, equation of linear regression y= 2.575x+0.0056, related coefficient 0.9998 illustrate to test nitrate according to embodiment two, as nitrate concentration changes Show good linear relationship.
2 embodiment of table, two NO3The working curve of-N tests tables of original record
The NO for being 0.2mg/L and 0.4mg/L with concentration value3- N standard sample is that internal control sample is tested, and substitutes into working strategy y =2.575x+0.0056 calculates its test concentrations value and is followed successively by 0.204mg/L and 0.398mg/L, and test relative deviation≤± 3%.
Embodiment three
Embodiment one and two amount of samples of embodiment are 25ml, are researched and developed based on the considerations of online equipment, it is desirable to reduce sample volume, one Aspect can shorten test period, reduce energy consumption, on the other hand can reduce reagent dosage, reduce cost.
(1) working curve is drawn
In six 10.0ml colorimetric cylinders, move into respectively this standard liquid series nitrate-nitrogen concentration be followed successively by 0,0.05, 0.15, the standard solution of 0.25,0.35,0.50mg/L.
0.2ml color developing agent 1 is added, mixes static 5min, 0.2ml color developing agent 2 is added, mixes, develop the color 10min.
The reducing agent of 0.8ml is added, covers tightly glass stopper, gently shakes up, 60 DEG C of water-bath 10min in temperature control sink are cooling To room temperature.
With 2.0cm cell, with artificial seawater reference, the light absorption value at 543nm wavelength is tested, blank absorbency Ab, with Light absorption value An after deducting Blank absorbance values Ab is ordinate, and nitrate-nitrogen concentration is that abscissa drafting standard work is bent Line, and standard working curve intercept and slope are found out with linear regression method.
(2) sample test
10ml seawater sample is taken, 0.4ml color developing agent is added, is mixed.
0.2ml color developing agent 1 is added, mixes static 5min, 0.2ml color developing agent 2 is added, mixes, develop the color 10min.
0.8ml reducing agent is added, mixes.
Keep 60 DEG C of water-bath 10min.
It is cooled to room temperature.
With 2cm colorimetric pool, its absorbance value is tested at 543nm wavelength.
It brings standard working curve into and calculates total nitrate content, deduct the concentration value of original nitrite in seawater, Nitrate concentration value as in seawater.
(3) test result
The standard working curve of drafting is shown in Fig. 6, equation of linear regression y=2.3483x-0.0041, related coefficient 0.9993, Illustrate to test nitrate according to embodiment three, as nitrate concentration variation shows good linear relationship.
The NO for being 0.2mg/L and 0.4mg/L with concentration value3- N standard sample is that internal control sample is tested, and substitutes into work Equation y=2.3483x-0.0041 calculates its test concentrations value and is followed successively by 0.206mg/L and 0.400mg/L, tests relative deviation ≤ ± 3%.
Note that the above is only a better embodiment of the present invention and the applied technical principle.It will be appreciated by those skilled in the art that The invention is not limited to the specific embodiments described herein, be able to carry out for a person skilled in the art it is various it is apparent variation, It readjusts and substitutes without departing from protection scope of the present invention.Therefore, although being carried out by above embodiments to the present invention It is described in further detail, but the present invention is not limited to the above embodiments only, without departing from the inventive concept, also It may include more other equivalent embodiments, and the scope of the invention is determined by the scope of the appended claims.

Claims (5)

1. a kind of Seawater Nitrate concentration determination method, including working curve draw process and testing process, which is characterized in that institute State working curve draw process successively the following steps are included:
In six colorimetric cylinders, nitrate-nitrogen concentration is moved into respectively and is followed successively by 0,0.05,0.15,0.25,0.35,0.50mg/L Series standard solution;
The placement predetermined time is mixed after quantitative chromogenic agent 1 is added;
The placement predetermined time is mixed after quantitative chromogenic agent 2 is added;
Quantitative reducing agent is added, covers tightly glass stopper, gently shakes up, 60 DEG C of water-bath predetermined times, are cooled in temperature control sink Room temperature;
With 2.0cm colorimetric pool, reference is made with artificial seawater, tests light absorption value, blank absorbency Ab at 543nm wavelength;With button Except the light absorption value An after Blank absorbance values Ab is ordinate, nitrate-nitrogen concentration is that abscissa draws standard working curve;
The step of testing process includes: to take quantitative seawater sample, is mixed after addition quantitative chromogenic agent stands the pre- timing of colour developing Between the step of, Quantitative reduction agent is added, after mixing the step of water-bath, cooling step is surveyed at 543nm wavelength with 2cm colorimetric pool The step of trying its absorbance value.
2. Seawater Nitrate concentration determination method according to claim 1, which is characterized in that the working curve draws stream The colorimetric cylinder of journey is 25.0ml, the sulfanilyl that the concentration that the addition quantitative chromogenic agent 1 is 0.5ml is 10g/L Amine aqueous solution mixes after the addition quantitative chromogenic agent 1 and places the predetermined time as 5min, and the addition quantitative chromogenic agent 2 is 0.5ml Concentration to be 1.0g/L mix to hydrochloride naphthodiamide solution, after the additions quantitative chromogenic agent 2 that the placement predetermined time is 15min, described that quantitative reducing agent is added as 2ml vanadium trichloride solution, 60 DEG C of water-bath predetermined times are 20min.
3. Seawater Nitrate concentration determination method according to claim 2, which is characterized in that the testing process is successively Are as follows: 25ml seawater sample is taken, 0.5 ml color developing agent 1 is added and mixes placement 5min, the mixing of 0.5 ml color developing agent 2 is added and places The step of 2ml reducing agent is added in 15min, and 60 DEG C of water-bath 20min are kept after mixing, is cooled to room temperature step, with 2cm colorimetric pool, The step of its absorbance value is tested at 543nm wavelength.
4. Seawater Nitrate concentration determination method according to claim 1, which is characterized in that the working curve draws stream The colorimetric cylinder of journey is 10.0ml, the sulfanilyl that the concentration that the addition quantitative chromogenic agent 1 is 0.2ml is 10g/L Amine aqueous solution mixes after the addition quantitative chromogenic agent 1 and places the predetermined time as 5min, and the addition quantitative chromogenic agent 2 is 0.2ml Concentration to be 1.0g/L mix to hydrochloride naphthodiamide solution, after the additions quantitative chromogenic agent 2 that the placement predetermined time is 10min, described that quantitative reducing agent is added as 0.8ml vanadium trichloride solution, 60 DEG C of water-bath predetermined times are 10min.
5. according to right want 1 described in Seawater Nitrate concentration determination method, which is characterized in that the testing process is successively are as follows: 10ml seawater sample is taken, 0.2 ml color developing agent 1 is added and mixes placement 5min, the mixing of 0.2 ml color developing agent 2 is added and places 10min, The step of 0.8ml reducing agent is added, 60 DEG C of water-bath 10min are kept after mixing, is cooled to room temperature step, with 2cm colorimetric pool, The step of its absorbance value is tested at 543nm wavelength.
CN201811009775.XA 2018-08-31 2018-08-31 A kind of Seawater Nitrate concentration determination method Pending CN109142249A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201811009775.XA CN109142249A (en) 2018-08-31 2018-08-31 A kind of Seawater Nitrate concentration determination method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201811009775.XA CN109142249A (en) 2018-08-31 2018-08-31 A kind of Seawater Nitrate concentration determination method

Publications (1)

Publication Number Publication Date
CN109142249A true CN109142249A (en) 2019-01-04

Family

ID=64825844

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201811009775.XA Pending CN109142249A (en) 2018-08-31 2018-08-31 A kind of Seawater Nitrate concentration determination method

Country Status (1)

Country Link
CN (1) CN109142249A (en)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110887834A (en) * 2019-11-05 2020-03-17 中国水产科学研究院黄海水产研究所 Water body nitrate content determination method based on fading of indigo disulfonic acid sodium
CN110987846A (en) * 2019-11-27 2020-04-10 中国科学院西安光学精密机械研究所 Nitrate concentration prediction method based on iPLS-PA algorithm
CN111239071A (en) * 2020-02-19 2020-06-05 中国科学院烟台海岸带研究所 Method for detecting concentration of nitrate in seawater by spectrometry
CN113884459A (en) * 2021-09-07 2022-01-04 海南大学 Direct determination method for nitrate content in seawater and application
CN117524339A (en) * 2024-01-04 2024-02-06 攀枝花市东区生态环境监测站 Method and system for measuring residual chlorine

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104730012A (en) * 2015-03-19 2015-06-24 中国科学院南海海洋研究所 Method for rapidly measuring water body nitrate by using small system
CN107356539A (en) * 2017-07-13 2017-11-17 山东科技大学 A kind of method of nitrogen nutrition salinity in quick detection seawater

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104730012A (en) * 2015-03-19 2015-06-24 中国科学院南海海洋研究所 Method for rapidly measuring water body nitrate by using small system
CN107356539A (en) * 2017-07-13 2017-11-17 山东科技大学 A kind of method of nitrogen nutrition salinity in quick detection seawater

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
王燕: "化学发光法测定海水中低浓度硝酸盐和亚硝酸盐含量的方法探究及应用", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 *
闫坤朋等: "重氮偶联法测定水中亚硝酸盐氮的改进", 《中国环境监测》 *

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110887834A (en) * 2019-11-05 2020-03-17 中国水产科学研究院黄海水产研究所 Water body nitrate content determination method based on fading of indigo disulfonic acid sodium
CN110987846A (en) * 2019-11-27 2020-04-10 中国科学院西安光学精密机械研究所 Nitrate concentration prediction method based on iPLS-PA algorithm
CN111239071A (en) * 2020-02-19 2020-06-05 中国科学院烟台海岸带研究所 Method for detecting concentration of nitrate in seawater by spectrometry
CN111239071B (en) * 2020-02-19 2023-03-31 中国科学院烟台海岸带研究所 Method for detecting concentration of nitrate in seawater by spectrometry
CN113884459A (en) * 2021-09-07 2022-01-04 海南大学 Direct determination method for nitrate content in seawater and application
CN117524339A (en) * 2024-01-04 2024-02-06 攀枝花市东区生态环境监测站 Method and system for measuring residual chlorine
CN117524339B (en) * 2024-01-04 2024-03-19 攀枝花市东区生态环境监测站 Method and system for measuring residual chlorine

Similar Documents

Publication Publication Date Title
CN109142249A (en) A kind of Seawater Nitrate concentration determination method
McCarthy et al. Nitrogenous nutrition of the plankton in the Chesapeake Bay. 1. Nutrient availability and phytoplankton preferences
Zhang Shipboard automated determination of trace concentrations of nitrite and nitrate in oligotrophic water by gas-segmented continuous flow analysis with a liquid waveguide capillary flow cell
Grande et al. Primary production in the North Pacific gyre: a comparison of rates determined by the 14C, O2 concentration and 18O methods
Brzezinski Vertical distribution of ammonium in stratified oligotrophic waters
CN101782508B (en) Method for measuring contents of ferrous, ferric iron and total iron in seawater
Monteiro et al. Simplified version of the sodium salicylate method for analysis of nitrate in drinking waters
Li et al. Continuous colorimetric determination of trace ammonium in seawater with a long-path liquid waveguide capillary cell
Young et al. RAPID AMMONIUM‐AND NITRATE‐INDUCED PERTURBATIONS TO CHL a FLUORESCENCE IN NITROGEN‐STRESSED DUNALIELLA TERTIOLECTA (CHLOROPHYTA) 1
CN107356539A (en) A kind of method of nitrogen nutrition salinity in quick detection seawater
Hernández‐López et al. A microplate technique to quantify nutrients (NO2−, NO3−, NH4+ and PO43−) in seawater
Kodama et al. A highly sensitive and large concentration range colorimetric continuous flow analysis for ammonium concentration
Cartisano et al. Investigating the sources and structure of chromophoric dissolved organic matter (CDOM) in the North Pacific Ocean (NPO) utilizing optical spectroscopy combined with solid phase extraction and borohydride reduction
CN101187637B (en) Automatic analysis method for seawater phenols compounds
CN110887834A (en) Water body nitrate content determination method based on fading of indigo disulfonic acid sodium
Shaw Development and construction of an analyser for the determination of the hydrogen peroxide content of natural water using a chemiluminescent reaction
CN109115756A (en) A kind of method of small system Fast Continuous Determination sea water solubility ammonium salt
US6967104B2 (en) Rapid method for estimation of Chemical Oxygen Demand
US20050191753A1 (en) Rapid method for estimation of chemical oxygen demand
Grantham The Loch Eil project: Chlorophyll a and nutrients in the water column of Loch Eil
Rees et al. Carbon, nitrogen and phosphorus budgets within a mesoscale eddy: comparison of mass balance with in vitro determinations
Smith et al. Colorimetric determination of halogenated nitrophenols added to streams as sea lamprey larvicides
Ishikawa et al. Dissolved organic carbon concentration of a natural water body and its relationship to water color in Central Kalimantan, Indonesia
CN205449813U (en) Dissolved oxygen photoelectric detection probe and dissolved oxygen detection instrument based on LED light source
CN104142307B (en) The method utilizing ozone oxidation luminescence spectral detection wine sulfite salt content

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20190104

WD01 Invention patent application deemed withdrawn after publication