CN107144541A - The assay method of total nitrogen content and measure device in a kind of water - Google Patents
The assay method of total nitrogen content and measure device in a kind of water Download PDFInfo
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- CN107144541A CN107144541A CN201710364760.4A CN201710364760A CN107144541A CN 107144541 A CN107144541 A CN 107144541A CN 201710364760 A CN201710364760 A CN 201710364760A CN 107144541 A CN107144541 A CN 107144541A
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- water
- total nitrogen
- nitrogen content
- sampling bottle
- headspace sampling
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 80
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 65
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 40
- 238000003556 assay Methods 0.000 title claims abstract description 25
- 238000005070 sampling Methods 0.000 claims abstract description 38
- 102000012286 Chitinases Human genes 0.000 claims abstract description 23
- 108010022172 Chitinases Proteins 0.000 claims abstract description 23
- 239000000243 solution Substances 0.000 claims abstract description 17
- 238000004401 flow injection analysis Methods 0.000 claims abstract description 11
- 238000007789 sealing Methods 0.000 claims abstract description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 14
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 13
- 235000019394 potassium persulphate Nutrition 0.000 claims description 12
- 230000029087 digestion Effects 0.000 claims description 9
- 238000004659 sterilization and disinfection Methods 0.000 claims description 6
- 238000001953 recrystallisation Methods 0.000 claims description 4
- 230000001954 sterilising effect Effects 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims description 2
- 229910052939 potassium sulfate Inorganic materials 0.000 claims description 2
- 235000011151 potassium sulphates Nutrition 0.000 claims description 2
- 238000012360 testing method Methods 0.000 abstract description 23
- 238000005516 engineering process Methods 0.000 abstract description 4
- 238000000105 evaporative light scattering detection Methods 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 23
- 238000011084 recovery Methods 0.000 description 10
- 238000002798 spectrophotometry method Methods 0.000 description 9
- 239000000126 substance Substances 0.000 description 9
- 238000004458 analytical method Methods 0.000 description 5
- 239000003814 drug Substances 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- -1 nitrite anions Chemical class 0.000 description 5
- 125000001477 organic nitrogen group Chemical group 0.000 description 5
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 4
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 4
- 210000000080 chela (arthropods) Anatomy 0.000 description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 description 4
- 238000003825 pressing Methods 0.000 description 4
- 235000011121 sodium hydroxide Nutrition 0.000 description 4
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- 229910002651 NO3 Inorganic materials 0.000 description 3
- 238000004737 colorimetric analysis Methods 0.000 description 3
- 239000002352 surface water Substances 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 2
- 150000004005 nitrosamines Chemical class 0.000 description 2
- 230000006641 stabilisation Effects 0.000 description 2
- 238000011105 stabilization Methods 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 1
- 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
- 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 description 1
- 238000004847 absorption spectroscopy Methods 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000013505 freshwater Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000003673 groundwater Substances 0.000 description 1
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 description 1
- 230000026030 halogenation Effects 0.000 description 1
- 238000005658 halogenation reaction Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- LYGJENNIWJXYER-BJUDXGSMSA-N nitromethane Chemical class [11CH3][N+]([O-])=O LYGJENNIWJXYER-BJUDXGSMSA-N 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000005789 organism growth Effects 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 238000000746 purification Methods 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
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
-
- 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
Landscapes
- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Measuring Or Testing Involving Enzymes Or Micro-Organisms (AREA)
Abstract
The present invention relates to a kind of assay method of total nitrogen content in water and measure device, belong to water-treatment technology field.The assay method of total nitrogen content in the water of the present invention, including：(1) water sample to be measured and alkaline chitinase solution are placed in headspace sampling bottle, using headspace sampling bottle cap sealing, then cleared up；(2) the headspace sampling bottle after being cleared up in step (1) is put into automatic sampler, and connection flow injection analyzer carries out automatic assay.Assay method can realize mass detection and test result is stable.
Description
Technical field
The present invention relates to a kind of assay method of total nitrogen content in water and measure device, belong to water-treatment technology field.
Background technology
Total nitrogen includes inorganic nitrogen and protein, amino acid and the organic amines such as nitrate nitrogen, nitrite nitrogen, ammonia nitrogen in water body
Deng organic nitrogen.On the one hand, when total nitrogen, total phosphorus substance are exceeded in surface water, microorganism amount reproduction, planktonic organism growth is vigorous,
There is eutrophic state.Total nitrogen content in water is to weigh one of important indicator of water quality, and it, which is determined, helps to evaluate water body
Contaminated and self-cleaning situation.On the other hand, during organic nitrogen is through cholorination in water, nitrogenous disinfection byproducts are easily formed,
The respectively nitrosamines of halogenated nitromethane (HNMs), halogenation acetonitrile (HANs), Haloacetamide (HAcAms) and non-halogenated
(Nitrosamines), this carcinogenic concentration of four classes DBPs is relatively low.Organic nitrogen subtracts inorganic nitrogen equal to total nitrogen, organic nitrogen it is dense
Degree level has close correlation with nitrogenous disinfection byproducts generation.Therefore, the accurate measure of total nitrogen concentration level is in water body
Tool is of great significance.
Mainly there be the assay method of total nitrogen in water：(1) alkaline chitinase clears up-ultraviolet spectrophotometry (HJ636-
2012)；(2) gas-phase molecular absorption spectrometry method.(3) measured respectively using ammonia nitrogen, nitrate anion, nitrite anions, then will knot
Fruit accumulated value as total nitrogen measurement result, but this method be only applicable to organic nitrogen concentration level it is negligible in the case of.Mesh
Before, China is in environment surface water, water quality monitoring field, and alkaline chitinase clears up-ultraviolet spectrophotometry (HJ636-2012)
And optimization method is the main method for determining total nitrogen.But, alkaline chitinase clears up-Water by Ultraviolet Spectrophotometry in
Total nitrogen, it determines accuracy is influenceed by several factors, such as：Washed without ammoniacal liquor, reagent purity, glassware, clear up condition
The restriction of the factors such as control.
Application publication number discloses a kind of measure side of fresh water water quality total nitrogen content for CN104076007A patent of invention
Method, first clears up bottle with sealed polytetrafluoroethylene (PTFE) and carries out HTHP and clear up, then carry out ultraviolet spectrophotometry and be measured, and
Specifically disclose and clear up bottle using polytetrafluoroethylene (PTFE) and replace colorimetric cylinder, the process cleared up more is sealed, more fully.But the technology
Quick mass detection can not be carried out, and ensures the stability of test, i.e., it is directed to same testing sample, enters in different time
During row measurement, data difference is larger, there is the defect in practical application.
The content of the invention
It is an object of the invention to provide a kind of assay method of total nitrogen content in water, the assay method can be realized large quantities of
Amount detection and test result stabilization.
It is another object of the present invention to provide a kind of measure device of total nitrogen content in above-mentioned water.
To achieve these goals, assay method of the invention, including：
(1) water sample to be measured and alkaline chitinase solution are placed in headspace sampling bottle, using headspace sampling bottle cap sealing,
Then cleared up；
(2) the headspace sampling bottle after being cleared up in step (1) connects flow injection analyzer by automatic sampler and carried out
Automatic assay.
Above-mentioned automatic assay is measured using colorimetric method.
It is above-mentioned that water sample to be measured and alkaline chitinase solution are placed in headspace sampling bottle, headspace sampling bottle cap is put, is used
Cap pressing pincers are sealed.
It is above-mentioned to clear up for digestion time 30min under the conditions of autoclave sterilization；The autoclave sterilization condition is in temperature
Spend for 120~124 DEG C, pressure is 1.1~1.4kg/cm2Vapor in.
Above-mentioned alkaline chitinase solution is by sodium hydroxide, potassium peroxydisulfate, water composition；The sodium hydroxide, potassium peroxydisulfate,
The mass ratio of water is：3:8:200.
The volume ratio of water sample to be measured and alkaline chitinase solution in above-mentioned steps (1) is 2：1.
The volume of above-mentioned water sample to be measured is 10mL, and the volume of alkaline chitinase solution is 5mL, the volume of headspace sampling bottle
For 20mL.
Potassium peroxydisulfate described in above-mentioned steps (1) is purified by the recrystallization of more than 3 times.
The measure device of total nitrogen content in a kind of water, determining device includes headspace sampling bottle, automatic sampler and flowing
Injection Analysis instrument；It is tightly connected successively between the headspace sampling bottle, automatic sampler and flow injection analyzer.
Above-mentioned automatic sampler includes being provided with two or more on rotating disk, the rotating disk for putting the recessed of headspace sampling bottle
Groove.
Beneficial effects of the present invention：
In the prior art alkaline chitinase clear up-ultraviolet spectrophotometry (HJ636-2012) determine total nitrogen principle it is main
It is：At 120~124 DEG C, alkaline chitinase solution makes the nitrogen of nitrogen-containing compound in sample be converted into nitrate, using ultraviolet
AAS determines absorbance A 220 and A275 respectively at wavelength 220nm and 275nm.But during determination of total nitrogen content, but
In practical measurement process, because the pure potassium peroxydisulfate medicine purity of domestic analysis can not enough cause two aspect influences：On the one hand, water
Sample is not thorough in digestion process, and the nitrogen of part nitrogen-containing compound is also not converted into nitrate in sample；On the other hand, domestic point
Analyse in pure potassium peroxydisulfate medicine other materials interference it is ultraviolet under the conditions of spectrophotometry result.And will be used domestic point
Analyse pure potassium peroxydisulfate medicine and recrystallize purification by more than 3 times (including 3 times), above-mentioned situation can be avoided to occur.Test in addition
In method：" 10ml samples and 5ml alkaline chitinase solution are put into 25ml color-comparison tubes, tied with gauze and cotton rope
Promptly, to prevent ejection." the step, it is on the one hand very cumbersome, take time and effort；On the other hand under the conditions of high-temperature alkaline, in water
Part ammonia nitrogen is converted to gas ammonia and escaped, so as to influence total nitrogen concentration precision.By water sample to be measured and alkaline mistake in the present invention
Potassium sulfate solution is put into headspace sampling bottle, is put headspace sampling bottle cap, is sealed with cap pressing pincers.So not only operate letter
It is single, easy, it is important to which that good sealing ensures that ammonia nitrogen is all converted to nitrate in water, improves measure in headspace sampling bottle
Precision.Finally, alkaline chitinase clear up-ultraviolet spectrophotometry (HJ636-2012) method in：" rear sample will be cleared up to use
Spectrophotometry instrument determines absorbance A 220 and A275 " the step, one respectively at wavelength 220nm and 275nm
Aspect is very cumbersome, is taken time and effort especially for batch samples；On the other hand in manual continuous mode, human factor also may be used
Total nitrogen concentration precision can be influenceed.Operating automation degree in the present invention is high, reduces interference from human factor, it is important to for large quantities of
When measuring water determination, the precision of measure can be greatly improved.
The inventive method from by sample and alkaline chitinase solution according to 2:1 (volume ratio) is added to headspace sampling bottle and entered
After row is cleared up, headspace sampling bottle is put into automatic sampler, follow-up test is all in sealing, auto state also without opening
Under be measured, without artificial disturbance, as a result accurately, measure can be carried out in high volume.
By using headspace sampling bottle in the present invention, water sample only not to be measured provides stabilization, good cleared up
Environment, while constituting the sealed environment of an entirety with automatic sampler and flow injection analyzer, it is to avoid extraneous factor
Interference to test, on the basis of the large quantities of measurements of automation are realized, considerably increases the degree of accuracy and the stability of test.It is right
Than with traditional method of testing, for example：Alkaline potassium per-sulfate digestion-ultraviolet spectrophotometry (HJ636-2012), test of the invention
Method can cause same water sample to be measured to be approached in the test result of different time, greatly strengthen the convincingness of test result,
Also reliable analysis foundation is provided for interpretation of result.The method of testing of the present invention simplifies traditional means of testing, enhances
Application value on practical significance.
Brief description of the drawings
Fig. 1 is headspace sampling bottle overall structure diagram in embodiment 1, wherein 1 headspace sampling bottle, 2 headspace samplings bottle is close
Capping, 3 water sample and alkaline chitinase mixed solutions to be measured；
Fig. 2 is measure total nitrogen schematic device in embodiment 1, wherein the headspace sampling bottle after 4 sealings, 5 automatic samplers,
6 flow injection analyzers.
Embodiment
With reference to specific embodiment, the invention will be further described.
Flow injection analyzer in embodiment, which is determined, to be measured using colorimetric method.
Embodiment 1
Headspace sampling bottle structure in the present embodiment is as shown in figure 1, determine total nitrogen schematic device such as Fig. 2 in the present embodiment
It is shown.
The assay method of total nitrogen content in the water of the present embodiment, including：
(1) potassium peroxydisulfate medicine is purified by 3 recrystallizations, 40g potassium peroxydisulfates and 15g sodium hydroxides is added
Alkaline chitinase solution is configured in 1000g water；
(2) take 10ml water samples to be measured and 5ml alkaline chitinase solution to be put into headspace sampling bottle, put headspace sampling bottle
Lid, is sealed with cap pressing pincers, is subsequently placed in autoclave sterilizer, is 120 DEG C in temperature, pressure is 1.1kg/cm2's
Under the conditions of clear up 30min；
(3) it is placed on carrying out clearing up the straight room temperature of rear headspace sampling bottle cooling in autoclave sterilizer, liquid is reverse to mix 3
Secondary, in the slotted eye for being put into automatic sampler rotating disk, automatic sampler and headspace sampling bottle are tightly connected, then automatic sampler with
Flow injection analyzer is tightly connected, and is then measured.
Test example 1
According to the method in embodiment 1, according to above-mentioned method, the water sample to be measured in this test example is taken respectively from underground
Water, reservoir water and certain river water.During measure, setting 3 is parallel, and determines recovery of standard addition, and test data is listed in table 1.This examination
Test that 3 set in example are parallel to be referred to, 3 parts of the water sample that same place takes point is with once determining.
Test example 2
According to the method in embodiment 1, according to above-mentioned method, increase the concentration of mark-on amount, determine recovery of standard addition, survey
Examination data are listed in table 2.
Test example 3
According to the method in embodiment 1, two kinds of standard substances are carried out with the experimental test of 6 groups of different digestion times, is cleared up
Time is respectively set to 4 minutes, 8 minutes, 12 minutes, 18 minutes, 24 minutes, 30 minutes, except digestion time in every group of experiment
Difference, other are identical, and the contrast test data measured are listed in table 3.
Table 1
As can be seen from Table 1, assay method of the invention determines total nitrogen concentration suitable for different water environments, from underground water
To surface water, concentration range is from 0.214mg/L to 1.559mg/L, and change in concentration amplitude is larger.But recovery of standard addition is preferably, water
Level equal recovery of standard addition in storehouse is 96.5%, and certain equal recovery of standard addition of river water is 98.4%, and underground water recovery of standard addition is
98.5%, all reach quantitative recovery.This illustrates that the concentration range that assay method of the present invention is not only applicable is wide, and measurement accuracy
Also it is high, the automaticity of determination of total nitrogen content is also improved, greatly reduces labor workload.
Table 2
When table 1,2 can be seen that the assay method mark-on amount of the present invention from 1mg/L to 3mg/L, but recovery of standard addition is preferable
Stably, the average recovery of standard addition of reservoir water is 97.3%, and the equal recovery of standard addition of Groundwater is 98.4%, all reaches quantitative return
Receive.
Table 3
Table 3 is as can be seen that determine 2 kinds of standard substances, and it is respectively 4 minutes, 8 minutes, 12 minutes, 18 points to set digestion time
Clock, 24 minutes and 30 minutes, different digestion time the inventive method are all more accurate to the measure of standard substance.Illustrate the present invention
Method good airproof performance, clears up fully, digestion time is short, it is only necessary to 4 minutes.
Embodiment 2
The assay method of total nitrogen content in the water of the present embodiment, including：
(1) potassium peroxydisulfate medicine is purified by 3 recrystallizations, 40g potassium peroxydisulfates and 15g sodium hydroxides is added
Alkaline chitinase solution is configured in 1000g water；
(2) take 10ml water samples to be measured and 5ml alkaline chitinase solution to be put into headspace sampling bottle, put headspace sampling bottle
Lid, is sealed with cap pressing pincers, is subsequently placed in autoclave sterilizer, is 124 DEG C in temperature, pressure is 1.4kg/cm2's
Under the conditions of clear up 30min；
(3) it is placed on carrying out clearing up the straight room temperature of rear headspace sampling bottle cooling in autoclave sterilizer, liquid is reverse to mix 3
Secondary, in the slotted eye for being put into automatic sampler rotating disk, automatic sampler and headspace sampling bottle are tightly connected, then automatic sampler with
Flow injection analyzer is tightly connected, and is then measured.
Test example 4
Two groups of standard substances are determined with traditional colorimetric cylinder digestion procedure according to the method in embodiment 2 and contrasted,
Determination data is listed in table 4.
Test example 5
According to the method in embodiment 2 will clear up the sample after 30 minutes place different time 1 hour, 2 hours, 4 hours,
Two groups of standard substances are measured after 8 hours, 12 hours, 24 hours, determination data is listed in table 5.
Table 4
Table 4 is as can be seen that determine 2 kinds of standard substances, compared with traditional colorimetric method, assay method of the invention all compares
Accurately, it is a kind of reliable method of testing.
Table 5
Table 5 is cleared up after 30 minutes as can be seen that determine 2 kinds of standard substances, sample place different time 1 hour, 2 hours,
Determine and contrasted after 4 hours, 8 hours, 12 hours, 24 hours, the inventive method is all more accurate to the measure of standard substance.
Illustrate that the inventive method places different intervals section, survey the test data of same water sample, it was demonstrated that it is same that different time sections are determined
The sample determination data of sample is more or less the same, and measure is stablized.
Claims (8)
1. the assay method of total nitrogen content in a kind of water, it is characterised in that including：
(1) water sample to be measured and alkaline chitinase solution are placed in headspace sampling bottle, using headspace sampling bottle cap sealing, then
Cleared up；
(2) the headspace sampling bottle after being cleared up in step (1) connects flow injection analyzer by automatic sampler and carried out automatically
Change and determine.
2. the assay method of total nitrogen content in water as described in claim 1, it is characterised in that step is cleared up described in (1)
For digestion time 30min under the conditions of autoclave sterilization；The autoclave sterilization condition be temperature be 120~124 DEG C, pressure
Power is 1.1~1.4kg/cm2Vapor in.
3. the assay method of total nitrogen content in water as described in claim 1, it is characterised in that the alkaline chitinase is molten
Liquid is by sodium hydroxide, potassium peroxydisulfate, water composition；The sodium hydroxide, potassium peroxydisulfate, the mass ratio of water is 3:8:200.
4. the assay method of total nitrogen content in water as described in claim 1, it is characterised in that the water to be measured in step (1)
The volume ratio of sample and alkaline chitinase solution is 2：1.
5. the assay method of total nitrogen content in water as described in claim 4, it is characterised in that the volume of the water sample to be measured
For 10mL, the volume of alkaline chitinase solution is 5mL, and the volume of headspace sampling bottle is 20mL.
6. the assay method of total nitrogen content in water as described in claim 1, it is characterised in that the mistake described in step (1)
Potassium sulfate is purified by the recrystallization of more than 3 times.
7. the measure device of total nitrogen content in a kind of water, it is characterised in that the measure device includes headspace sampling bottle, entered automatically
Sample device and flow injection analyzer；It is close successively between the headspace sampling bottle, automatic sampler and flow injection analyzer
Envelope connection.
8. the measure device of total nitrogen content in water as claimed in claim 7, it is characterised in that the automatic sampler includes turning
The groove that two or more is used to put headspace sampling bottle is provided with disk, the rotating disk.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108168995A (en) * | 2017-12-25 | 2018-06-15 | 重庆市宇驰检测技术有限公司 | The formulating method of total phosphorus and total nitrogen examination criteria in a kind of water quality |
| CN115344598A (en) * | 2022-08-11 | 2022-11-15 | 生态环境部南京环境科学研究所 | Mobile monitoring system for operating condition of leachate equipment |
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| CN103196987A (en) * | 2013-02-22 | 2013-07-10 | 福建中烟工业有限责任公司 | Determination method for phosphine residues in tobacco |
| CN104076007A (en) * | 2014-07-10 | 2014-10-01 | 江苏省水产技术推广站 | Method for measuring total content of nitrogen of fresh water quality |
| CN206096050U (en) * | 2016-10-12 | 2017-04-12 | 北京中仪宇盛科技有限公司 | Full -automatic head space sampling device |
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- 2017-05-22 CN CN201710364760.4A patent/CN107144541A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
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