CN109142250A - Seawater total nitrogen concentration test method - Google Patents
Seawater total nitrogen concentration test method Download PDFInfo
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- CN109142250A CN109142250A CN201811010298.9A CN201811010298A CN109142250A CN 109142250 A CN109142250 A CN 109142250A CN 201811010298 A CN201811010298 A CN 201811010298A CN 109142250 A CN109142250 A CN 109142250A
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- working curve
- bottle
- seawater
- total nitrogen
- standard
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 239000013535 sea water Substances 0.000 title claims abstract description 23
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 22
- 238000010998 test method Methods 0.000 title claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000000243 solution Substances 0.000 claims description 15
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000002835 absorbance Methods 0.000 claims description 8
- 230000031700 light absorption Effects 0.000 claims description 6
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 5
- 239000011780 sodium chloride Substances 0.000 claims description 5
- MMDJDBSEMBIJBB-UHFFFAOYSA-N [O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[NH6+3] Chemical compound [O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[NH6+3] MMDJDBSEMBIJBB-UHFFFAOYSA-N 0.000 claims description 4
- 238000012417 linear regression Methods 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 239000003638 chemical reducing agent Substances 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 239000013049 sediment Substances 0.000 claims description 3
- 238000010790 dilution Methods 0.000 claims description 2
- 239000012895 dilution Substances 0.000 claims description 2
- 238000005259 measurement Methods 0.000 claims description 2
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims 1
- 238000012360 testing method Methods 0.000 abstract description 14
- 238000000034 method Methods 0.000 abstract description 3
- 239000000523 sample Substances 0.000 description 13
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 2
- 230000029087 digestion Effects 0.000 description 2
- JVMRPSJZNHXORP-UHFFFAOYSA-N ON=O.ON=O.ON=O.N Chemical compound ON=O.ON=O.ON=O.N JVMRPSJZNHXORP-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 1
- 239000013068 control sample Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000012851 eutrophication Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- -1 nitrogenous compound Chemical class 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 125000001477 organic nitrogen group Chemical group 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/3103—Atomic absorption analysis
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems 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
- G01N21/78—Systems 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
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- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Biochemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Analytical Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Plasma & Fusion (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
Abstract
The present invention provides a kind of seawater total nitrogen concentration test method, including working curve drawing program and water determination program.Method of the invention tests seawater total nitrogen, and step is simple, does not need repeatedly to shift sample, it is not easy to cause artificially accidentally；Standard working curve linear relationship is good；Test result precision is high.
Description
Technical field
The present invention relates to seawater quality detection field more particularly to a kind of seawater total nitrogen concentration test methods.
Background technique
Total nitrogen (TN) refers to the total amount of the nitrogen of various forms in water body, exists with variform, including ammoniacal nitrogen, nitrate
Nitrogen, nitrite nitrogen and various organic nitrogens can be mutually converted in water body between the nitrogenous compound of variform.Nitrogen
It closes object to enter in water body by the physical actions such as absorption and part biochemical action, nitrogen is geochemical in participation water body environment
Learn circulation.
According to " national environmental protection " 13 " plans basic ideas ", country will continue to implement national sulfur dioxide, nitrogen
Oxide, COD, ammonia nitrogen prediction emission.It is preliminary to consider to total nitrogen, total phosphorus implementation focus region and key industry
The overall control combined.TN is one of the contaminated degree of reflection water body and important indicator of water eutrophication, and in seawater
Nitrogen existing forms multiplicity, complicated component the content of nutrient in seawater understood by the TN in monitoring analysis seawater, this
There is vital effect to protection marine ecosystems.
National standard method tests seawater total nitrogen, and complex steps need repeatedly to shift sample, be easy to cause human error, cause
Standard working curve linear relationship is poor, and test result precision is low.
Summary of the invention
The purpose of the present invention is to provide a kind of seawater total nitrogen concentration test methods, including working curve drawing program and water
Sample mensuration program, which is characterized in that the working curve drawing program includes the following steps:
Working curve drawing program
Step 1: in two groups of each six 25ml volumetric flasks, moving into the nitrate standard that concentration is 10.0 μm of ol/ml respectively and use
Solution 0,1.00,2.00,4.00,6.00,8.00ml, are diluted to 25ml graticule with the sodium chloride solution of ρ=35.0g/L, mix；
Step 2: full dose is transferred to disappear and boils in bottle the standard liquid series that the dilution is mixed respectively, each that 4.0ml resolution is added
Liquid mixes, screws bottle cap；
Step 3: disappear described in and boil bottle and be placed in basket, be put into the high steam heating in boiler that disappears and disappear and boil, to pressure rise to 1.1kPa,
When temperature is 122 DEG C, control pressure keeps 30min in 120~124 DEG C of 1.1~1.4kPa, temperature, stops naturally cold after heating
When being but " 0 " to pressure, pot cover is opened, taking-up, which disappears, boils bottle,
Step 4: adding 2.5ml neutralizer, shaking dissolves sediment；
Step 5: adding 2ml reducing agent, keep 60 DEG C of heating 20min, be cooled to room temperature after stopping heating；
Step 6: 1ml color developing agent is added, mixes, places 15min；
Step 7: after colour stable, on spectrophotometer, with 2cm colorimetric pool, reference is made with water, at 543nm wavelength, measurement
Its light absorption value, blank absorbency Ab；
Step 8: to deduct the light absorption value An after Blank absorbance values Ab as ordinate, nitrate-nitrogen concentration is drawn for abscissa
Standard working curve processed, and standard working curve intercept a and slope b are found out with linear regression method；
Water determination program
Step 9: measuring 25.0ml seawater sample and boiled in bottle (double samples) in disappearing, 10ml sodium chloride solution, then plus 4.0ml over cure is added
Sour potassium solution screws bottle cap after mixing；
Step 10: measuring water sample absorbance value after being repeated in abovementioned steps 3 to step 8 step.
Further, the nitrate standard is followed successively by 0 μm of ol/L, 4.00 μm of ol/L, 8.00 μm of ol/ using the concentration of solution
L, 16.00 μm of ol/L, 24.00 μm of ol/L, 32.00 μm of ol/L.
The advantages and positive effects of the present invention are:
Method of the invention tests seawater total nitrogen, and step is simple, does not need repeatedly to shift sample, it is not easy to cause artificially accidentally；Mark
Quasi- working curve linear relationship is good；Test result precision is high.
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 seawater total nitrogen sample test flow chart of the present invention；
Fig. 2 is the working curve of seawater total nitrogen of the present invention.
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.
As shown in Fig. 1 seawater total nitrogen sample test flow chart, step of the invention is respectively as follows:
(1) in two groups of each six 25ml volumetric flasks, the nitrate standard that concentration is 10.0 μm of ol/ml is moved into respectively and uses solution
0,1.00,2.00,4.00,6.00,8.00ml, are diluted to 25ml graticule with sodium chloride solution (ρ=35.0g/L), mix.This mark
The concentration of quasi- solution series is followed successively by 0 μm of ol/L, 4.00 μm of ol/L, 8.00 μm of ol/L, 16.00 μm of ol/L, 24.00 μm of ol/L,
32.00μmol/L。
(2) by above-mentioned standard solution series, full dose is transferred to disappear and boils in bottle respectively.It is each that 4.0ml digestion solution is added, it mixes, rotation
Tight bottle cap.
(3) above-mentioned disappear is boiled bottle and be placed in stainless steel basket, be put into the high steam heating in boiler that disappears and disappear and boil, risen to pressure
When 1.1kPa (temperature is 122 DEG C), control pressure keeps 30min in 1.1~1.4kPa (120~124 DEG C of temperature).Then, stop
It only heats, when to naturally cool to pressure be " 0 ", pot cover can be opened, taking-up, which disappears, boils bottle.
(4) after sample is cooling, 2.5ml neutralizer is added, shaking dissolves sediment.
(5) 2ml reducing agent is added, 60 DEG C, heats 20min, is cooled to room temperature.
(6) 1ml color developing agent is added, mixes, places 15min.
(7) after colour stable, on spectrophotometer, with 2cm colorimetric pool, reference is made with water, at 543nm wavelength, is surveyed
Its fixed light absorption value, blank absorbency Ab.
(8) to deduct the light absorption value An after Blank absorbance values Ab as ordinate, nitrate-nitrogen concentration is drawn for abscissa
Standard working curve processed, and standard working curve intercept a and slope b are found out with linear regression method.
4.1.2 sample test
It measures 25.0ml seawater sample and boils in bottle (double samples) in disappearing, add 4.0ml digestion solution, mix, screw bottle cap.Below according to
(3)~(8) step measures water sample absorbance value, the average value Aw for taking two Duplicate Samples to measure.
(1) result calculates
C (TN-N): the concentration of total nitrogen in seawater sample, μm ol/L
Aw: the mean absorbance values of total nitrogen in seawater sample
Ab: blank absorbency
A: standard working curve intercept b: standard working curve slope
4.1 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=
0.0236x-0.0175, related coefficient 0.9944.
The working curve of 1 seawater total nitrogen of table tests tables of original record
Internal control sample is 20 μm of ol/L, and test absorbance value is 0.519, and substituting into working curve and calculating test concentrations value is 21.67 μ
Mol/L, relative deviation 8.37%.
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 (2)
1. seawater total nitrogen concentration test method, including working curve drawing program and water determination program, which is characterized in that described
Working curve drawing program includes the following steps:
Step 1: in two groups of each six 25ml volumetric flasks, moving into the nitrate standard that concentration is 10.0 μm of ol/ml respectively and use
0,1.00,2.00,4.00,6.00,8.00 ml of solution is diluted to 25ml graticule with the sodium chloride solution of the g/L of ρ=35.0, mixes
It is even；
Step 2: full dose is transferred to disappear and boils in bottle the standard liquid series that the dilution is mixed respectively, each that 4.0 ml resolution is added
Liquid mixes, screws bottle cap；
Step 3: disappearing described in and boil bottle and be placed in basket, be put into the high steam heating in boiler that disappears and disappear and boil, rise to 1.1 to pressure
When kPa, temperature are 122 DEG C, control pressure keeps 30 min in 120~124 DEG C of 1.1~1.4 kPa, temperature, after stopping heating
When to naturally cool to pressure be 0, pot cover is opened, taking-up disappears and boils bottle,
Step 4: adding 2.5 ml neutralizers, shaking dissolves sediment；
Step 5: adding 2ml reducing agent, keep 60 DEG C of heating 20min, be cooled to room temperature after stopping heating；
Step 6: 1ml color developing agent is added, mixes, places 15min；
Step 7: after colour stable, on spectrophotometer, with 2cm colorimetric pool, reference is made with water, at 543nm wavelength, measurement
Its light absorption value, blank absorbency Ab；
Step 8: to deduct the light absorption value An after Blank absorbance values Ab as ordinate, nitrate-nitrogen concentration is drawn for abscissa
Standard working curve processed, and standard working curve intercept a and slope b are found out with linear regression method；
Water determination program
Step 9: measuring 25.0 ml seawater samples and boiled in bottle (double samples) in disappearing, 10 ml sodium chloride solutions, then plus 4.0 ml are added
Potassium persulfate solution screws bottle cap after mixing；
Step 10: measuring water sample absorbance value after being repeated in abovementioned steps 3 to step 8 step.
2. seawater total nitrogen concentration test method as described in claim 1, which is characterized in that the nitrate standard uses solution
Concentration be followed successively by 0 μm of ol/L, 4.00 μm of ol/L, 8.00 μm of ol/L, 16.00 μm of ol/L, 24.00 μm of ol/L, 32.00 μm of ol/
L。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811010298.9A CN109142250A (en) | 2018-08-31 | 2018-08-31 | Seawater total nitrogen concentration test method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811010298.9A CN109142250A (en) | 2018-08-31 | 2018-08-31 | Seawater total nitrogen concentration test method |
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| Publication Number | Publication Date |
|---|---|
| CN109142250A true CN109142250A (en) | 2019-01-04 |
Family
ID=64825924
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811010298.9A Pending CN109142250A (en) | 2018-08-31 | 2018-08-31 | Seawater total nitrogen concentration test method |
Country Status (1)
| Country | Link |
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| CN (1) | CN109142250A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113655012A (en) * | 2020-05-12 | 2021-11-16 | 华奇（中国）化工有限公司 | high-COD (chemical oxygen demand) wastewater total nitrogen testing method |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102980865A (en) * | 2012-11-17 | 2013-03-20 | 中国水产科学研究院渔业机械仪器研究所 | Measurement method for seawater total nitrogen content |
| 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 |
| CN106525739A (en) * | 2016-11-08 | 2017-03-22 | 青岛理工大学 | Method for measuring ammonia nitrogen concentration value in water body |
| 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 |
-
2018
- 2018-08-31 CN CN201811010298.9A patent/CN109142250A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102980865A (en) * | 2012-11-17 | 2013-03-20 | 中国水产科学研究院渔业机械仪器研究所 | Measurement method for seawater total nitrogen content |
| 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 |
| CN106525739A (en) * | 2016-11-08 | 2017-03-22 | 青岛理工大学 | Method for measuring ammonia nitrogen concentration value in water body |
| 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 (1)
| Title |
|---|
| 中华人民共和国国家质量监督检验检疫总局中国国家标准化管理委员会发布: "海洋调查规范第4部分：海水化学要素调查" * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113655012A (en) * | 2020-05-12 | 2021-11-16 | 华奇（中国）化工有限公司 | high-COD (chemical oxygen demand) wastewater total nitrogen testing method |
| CN113655012B (en) * | 2020-05-12 | 2024-03-08 | 华奇（中国）化工有限公司 | High COD wastewater total nitrogen testing method |
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Application publication date: 20190104 |