CN109358016A - A portable pressure cooker combined with a colorimetric tube rapid digestion method and device for measuring total nitrogen in water - Google Patents
A portable pressure cooker combined with a colorimetric tube rapid digestion method and device for measuring total nitrogen in water Download PDFInfo
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- CN109358016A CN109358016A CN201810734187.6A CN201810734187A CN109358016A CN 109358016 A CN109358016 A CN 109358016A CN 201810734187 A CN201810734187 A CN 201810734187A CN 109358016 A CN109358016 A CN 109358016A
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- total nitrogen
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- colorimetric cylinder
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 20
- 230000029087 digestion Effects 0.000 title claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims description 22
- 238000005259 measurement Methods 0.000 claims abstract description 19
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims abstract description 7
- 239000000463 material Substances 0.000 claims abstract description 6
- 238000002835 absorbance Methods 0.000 claims description 13
- 238000009423 ventilation Methods 0.000 claims 3
- 235000019394 potassium persulphate Nutrition 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 239000002699 waste material Substances 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 12
- 239000000523 sample Substances 0.000 description 9
- 238000002798 spectrophotometry method Methods 0.000 description 6
- 102000012286 Chitinases Human genes 0.000 description 5
- 108010022172 Chitinases Proteins 0.000 description 5
- 239000012086 standard solution Substances 0.000 description 5
- 239000007788 liquid Substances 0.000 description 4
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 4
- 238000010561 standard procedure Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 238000012937 correction Methods 0.000 description 3
- 238000012851 eutrophication Methods 0.000 description 3
- 230000031700 light absorption Effects 0.000 description 3
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 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 2
- 230000008033 biological extinction Effects 0.000 description 2
- 239000012496 blank sample Substances 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- -1 nitrogenous compound Chemical class 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 235000010333 potassium nitrate Nutrition 0.000 description 2
- 239000004323 potassium nitrate Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Chemical compound [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 description 2
- 241000195493 Cryptophyta Species 0.000 description 1
- 241001411320 Eriogonum inflatum Species 0.000 description 1
- 206010021143 Hypoxia Diseases 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
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 206010044565 Tremor Diseases 0.000 description 1
- YUWBVKYVJWNVLE-UHFFFAOYSA-N [N].[P] Chemical compound [N].[P] YUWBVKYVJWNVLE-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- DNJIEGIFACGWOD-UHFFFAOYSA-N ethanethiol Chemical compound CCS DNJIEGIFACGWOD-UHFFFAOYSA-N 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000007954 hypoxia Effects 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 150000002730 mercury Chemical class 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- LFLZOWIFJOBEPN-UHFFFAOYSA-N nitrate, nitrate Chemical compound O[N+]([O-])=O.O[N+]([O-])=O LFLZOWIFJOBEPN-UHFFFAOYSA-N 0.000 description 1
- NJPPVKZQTLUDBO-UHFFFAOYSA-N novaluron Chemical compound C1=C(Cl)C(OC(F)(F)C(OC(F)(F)F)F)=CC=C1NC(=O)NC(=O)C1=C(F)C=CC=C1F NJPPVKZQTLUDBO-UHFFFAOYSA-N 0.000 description 1
- 125000001477 organic nitrogen group Chemical group 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 description 1
- 150000004968 peroxymonosulfuric acids Chemical class 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- CHKVPAROMQMJNQ-UHFFFAOYSA-M potassium bisulfate Chemical compound [K+].OS([O-])(=O)=O CHKVPAROMQMJNQ-UHFFFAOYSA-M 0.000 description 1
- 229910000343 potassium bisulfate Inorganic materials 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000029058 respiratory gaseous exchange Effects 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002352 surface water Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000004457 water analysis 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
-
- 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
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
- G01N21/03—Cuvette constructions
-
- 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
-
- 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
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
- G01N21/03—Cuvette constructions
- G01N2021/0325—Cells for testing reactions, e.g. containing reagents
-
- 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
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
- G01N21/03—Cuvette constructions
- G01N2021/0367—Supports of cells, e.g. pivotable
-
- 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
- G01N2021/752—Devices comprising reaction zones
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- Chemical & Material Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- 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)
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Abstract
The invention belongs to environmental technology fields, are related to a kind of portable Civil High Pressure pot combination colorimetric cylinder of use and quick and precisely clear up total nitrogen and method for measuring and device.The method and device can make colorimetric cylinder be uniformly distributed vertically in portable high steam pot, contact sample and high-temperature steam complete, the abundant resolution for realizing potassium peroxydisulfate, to solve the problems, such as that the blank absorbency as caused by alkaline potassium per-sulfate digestion is incomplete is excessively high.The application method and apparatus are also capable of fixing colorimetric cylinder pipe close, prevent the measurement error as caused by colorimetric cylinder pipe close loosening in high temperature and high pressure environment or ejection.The devices such as pressure cooker and colorimetric cylinder that the invention makes full use of total nitrogen surveying laboratory there is now, the idle and waste of resource is not will cause, it can prevent to the greatest extent due to the excessively high problem of blank absorbency caused by clearing up not exclusively, to save a large amount of manpower, material resources and financial resources of operator's heuristic process, it is of great significance in total nitrogen measurement.
Description
Technical field:
The invention mainly relates to environmental technology fields, and in particular to clears up ultraviolet spectrophotometry using alkaline chitinase
It is a kind of to realize the householder method quick and precisely measured and device when professional standard measures total nitrogen.
Background technique:
With the development of society, the aggravation of mankind's activity, increasing to the disturbance of nature, environmental pollution is at everybody
Problem of interest.In all kinds of problem of environmental pollutions, water eutrophication involves range extensively due to it and influences greatly on living,
It is increasingly becoming one of the object that numerous researchers pay close attention to.Its origin cause of formation is a large amount of sanitary sewages, industrial wastewater and agricultural water
It brings a large amount of nitrogen P elements while being discharged into water body into, so that water body nitrogen phosphorus is exceeded, destroys aquatic ecological balance, wherein nitrogen content is
The principal measure factor.Specially organic nitrogen and all kinds of inorganic nitrogens such as ammonia nitrogen, nitrate nitrogen, nitrite nitrogen, leads to the biologies such as Measures of Algae in Water Body
With microorganism mass propagation, oxygen in water is largely consumed, so as to cause water hypoxia deterioration, stench, nigrescence etc. occur is table
Existing water eutrophication phenomenon.It can be seen that the nitrogen of either which kind of form can destroy water ecology, therefore water body total nitrogen
Content is to measure one of the important indicator of water quality.
Rapidly and accurately detecting nitrogen content in surface water facilitates the generation of science control eutrophication.For this purpose, country is first
The national standard of several measurement total nitrogens has been promulgated afterwards, wherein the total nitrogen measurement standard being most widely used at present is " HJ 636-
The measurement alkaline chitinase of 2012 water quality total nitrogens clears up ultraviolet spectrophotometry ".This method is easy to operate, and accuracy is high, more
It is important that being compared with other methods has without adding the substance that strong acid, highly basic and mercury salt etc. have serious harm to environment
Very high environmental-friendly advantage.
Alkaline chitinase-ultraviolet spectrophotometry generallys use alkaline chitinase high-temperature oxydation sample, so that water body
In various forms of nitrogen be converted into nitrate nitrogen, then be measured with ultraviolet spectrophotometry.Its principle are as follows: water-soluble at 60 DEG C or more
In liquid, potassium peroxydisulfate, which can decompose, generates potassium acid sulfate and atomic oxygen, environment of the atomic oxygen decomposited at 120-140 DEG C
Under, nitrogenous compound in water sample can be made to be converted into nitrate, nitrate all has absorption peak at 220nm and 275nm, and measurement disappears
The absorbance of wavelength at solution two after solution can then calculate the content of total nitrogen by standard curve.Its concentration limit is
0.05mg/L, 4 mg/L of determination of the upper limit.
The national standard method step is simple, and required reagent is few, and instrument requirements are easy to get, but the disadvantage is that in actual operation, is surveying
When determining water sample total nitrogen, it is found that the problem of it is excessively high this national standard method produces sample often and will appear blank value, and then influences measured value.
Relative literature also indicates that, is commonly encountered problems in many water analysis worker real works.
It finds after study, during alkaline chitinase-determined by ultraviolet spectrophotometry, influences total nitrogen blank value extinction
The reason of spending mainly has: 1, when temperature and digestion time do not reach, the potassium peroxydisulfate for having certain content is remained in the sample,
Since potassium peroxydisulfate has the appearance of extinction peak value at 220nm wavelength, cause the absorbance of blank sample excessive, to influence
The accuracy of measurement.2, when high temperature and pressure is cleared up, the pipe close of conventional colorimetric cylinder, which may loosen, to be collapsed out, contaminated samples or reduction
Sample concentration.
Although having there is literature survey to study in response to the above problems and having proposed solution, such as is close using polytetrafluoroethylene (PTFE)
Envelope counteracting tank is cleared up to prevent liquid from leaking out, or extends digestion time and digestion condition to ensure complete resolution.
But on the one hand the above settling mode can increase considerably Instrument purchase expense, cause the increase of testing cost, separately
On the one hand, the reaction condition for changing national standard, will cause experiment it is not rigorous, also will affect the result of detection.In view of the above problems, this
Patent application personnel have found after study, in actual operation, under the conditions of national standard total nitrogen clear up incomplete main cause be by
Be not equipped with dedicated digestion instrument in ordinary high pressure resolution pot, and pot internal volume is limited, if having a certain number of samples simultaneously into
Row is cleared up, and the gap between colorimetric cylinder is insufficient, is caused high steam not come into full contact with sample, is caused uneven heating even, thus
Resolution is caused not exclusively to influence the accuracy and precision of measurement.
Summary of the invention:
For in the measurement of practical total nitrogen, blank absorbency is excessive and High-temperature Digestion causes liquid after bottle stopper shakiness to leak out
Problem, a kind of cheap and simple of the application patented invention using ordinary high pressure pot measurement total nitrogen method and apparatus, not only may be used
To be greatly lowered due to the excessively high possibility for causing failure of blank sample absorbance, pipe close caused by hot conditions can also be prevented
Loosening problem, and the adjustable nut used can flexible adaptation in the colorimetric cylinder of different size.In addition, the method can also be abundant
Using devices such as the pressure cookers and colorimetric cylinder having been provided with, the idle and waste of resource not will cause.In short, this method operation letter
It is single, the excessively high problem of blank absorbency can be prevented to the greatest extent, improve determination of total nitrogen content precision and accuracy.Its method particularly includes:
1. a kind of method and apparatus using portable civil pressure cooker and colorimetric cylinder rapid-digestion measurement water body total nitrogen, tool
Body is related to potassium peroxydisulfate capable of being made sufficiently to clear up, and prevents it because resolution not exclusively interferes absorbance, prevents under high temperature and pressure
Pipe lid loose or dislocation, causes measurement error；It is characterized in that, the easy device includes: a conductivity of heat well and makes colorimetric cylinder
The support frame come into full contact with high steam, a pipe lid fixator.
2. support frame according to claim 1, it is preferred that so that colorimetric cylinder is uniformly distributed in pressure cooker, any two
Tube hub aligned gaps are 15mm between pipe.
3. support frame according to claim 1, it is preferred that support frame has upper layer and lower layer, up and down at a distance of 13mm, so as to
There is provided enough support forces is put in colorimetric cylinder in pressure cooker vertically.
4. support frame according to claim 3, it is preferred that upper layer and lower layer are connected by connection sheet, and number is 2, every
Width is 10mm.
5. support frame according to claim 4, it is preferred that pedestal need to have air hole, and hole area of breathing freely is entire bottom
The 60% of seat surface product.
6. support frame according to claim 1, it is preferred that all material is high temperature resistant and the good material of heating conduction
Material.
7. support frame according to claim 1, it is preferred that top has handle to be connected, and takes out after facilitating Specimen eliminating.
8. fixator according to claim 1, it is preferred that there is upper and lower two panels, it is intermediate for fixing colorimetric cylinder pipe lid
It is connected by movable screw.
9. fixator according to claim 8, it is preferred that bottom sheet side have can hand adjustment screw, it is different straight for adapting to
Diameter colorimetric cylinder.
10. fixator according to claim 9, it is preferred that head have can hand adjustment screw, it is high for adapting to different pipe lids
The colorimetric cylinder of degree.
The present invention has the advantages that
Based on alkaline chitinase-uv-spectrophotometric concerned countries standard method measurement, existing set is being made full use of
On the basis of standby, increase economic easy small equipment, the excessively high problem of blank absorbency can be prevented to the greatest extent, significant increase disappears
The success rate of solution.The error as caused by the bottle cap pop-up of digestion process is eliminated simultaneously.Compare original ordinary high pressure pot+ratio
Colour tube combination has a clear superiority.
The innovation of the invention consists in that:
Although existing research proposes, total nitrogen measures the excessively high reason of blank value, mostly makes since resolution is not thorough
At, but it is only limited to theoretical research, and unanimously think that extending digestion time is solution.But for prolonging for digestion time
Long, on the one hand inconsistent with national standard method, still further aspect lacks unified standard for the extended time, and measurement is be easy to cause to grasp
The disunity of work, to influence result of study.The application patent thinks to increase digestion container and the contact area of high steam is
Optimal solution, to innovatively solve above-mentioned two problems, for related national standard practice operation measurement provide it is good
Good resolution environment.
Detailed description of the invention:
Attached drawing is the structural schematic diagram for a kind of device of civil pressure cooker rapid-digestion measurement water body total nitrogen.
Its composition includes:
A, device main view B, device top view C, bottle cap fixator enlarged drawing D, on fixator under section E, fixator
Section
1, handle 2, colorimetric cylinder fixed disk
Specific embodiment:
The present invention is described further below in conjunction with Figure of description and specific implementation.
Foregoing invention device, with reference to concerned countries standard, " alkaline chitinase clears up ultraviolet spectrophotometry HJ 636-
2012 ", 0,0.2,0.5,1.0,2.0,3.0 and 7.0 potassium nitrate standard solution (10.0mg N/L) is measured respectively to have in 25mL
It fills in grournd glass colorimetric cylinder, wherein corresponding total nitrogen (in terms of N) content is respectively 0.0,2.0,5.0,10.0,30.0 Hes
70.0ug.It is diluted with water to 10.0mL, adds 5.0mL alkaline chitinase solution (40g sodium peroxydisulfate and 15g sodium hydroxide
Every liter).Pipe close is stoppered, is fixed with herein described fixator, to prevent pop-up.Colorimetric cylinder is uniformly filled as described in this patent
It sets, 10mm or more is spaced between every pipe, then the device for being loaded with colorimetric cylinder is placed in pressure cooker, be heated to press valve and blow afloat,
Valve is closed, continues to be heated to 120 DEG C of beginning timing, maintains the temperature at 30min between 120~140 DEG C.Valve opening is deflated, natural
It is cooling, outer cover is removed, colorimetric cylinder is taken out and is cooled to room temperature, pin pipe close and be mixed by inversion liquid in colorimetric cylinder 2~3 times.
It is separately added into 10% hydrochloric acid solution of 1.0mL in each colorimetric cylinder, is diluted with water to 25mL graticule, lid plug mixes.Make
Absorbance is measured at 220 and 275nm with 10mm quartz colorimetric utensil, and draws standard curve.
Embodiment 1:
Traditional resolution mode and above-mentioned equipment is respectively adopted and mode is carried out in Civil High Pressure pot at the resolution of total nitrogen
Reason, the light absorption value of each concentration are as follows:
It is handled using traditional digestion procedure, too small due to being spaced between colorimetric cylinder, high steam is unable to fully contact, not
Sufficiently resolution, causes persulfate to remain, impacts to light absorption value, the potassium nitrate light absorption value of various concentration gradient such as following table institute
Show:
Table 1: the total nitrogen mark of tradition resolution processing is bent
Total nitrogen concentration CN=3.6739Ar-0.1293 R2=0.8924
Wherein CNIt is that standard solution corrects absorbance and the correction of zero-dose solution is inhaled for total nitrogen concentration mg/L in colorimetric cylinder, Ar
The difference of luminosity, formula are as follows:
Ab=Ab220-2Ab275
As=As220-2As275
Ar=As-Ab
In formula:
Ab: the correction absorbance of zero-dose solution
Ab220: absorbance of the zero-dose solution at wavelength 220nm
Ab275: absorbance of the zero-dose solution at wavelength 275nm
As: the correction absorbance of standard solution
As220: absorbance of the standard solution at wavelength 220nm
As275: absorbance of the standard solution at wavelength 275nm
Table 2: the total nitrogen mark of the invention patent is bent
Total nitrogen concentration CN=4.6737Ar-0.0582 R2=0.999
Calculation method is same as above
Total nitrogen resolution is carried out using conventional method it can be seen from above two embodiments to not only result in due to persulfuric acid
The excessively high problem of blank absorbency caused by potassium resolution not exclusively, and the bent degree of fitting of mark is greatly lowered, so that sample report
Useless rate greatly promotes.Using the device and method of the application patent, high steam can be made to be contacted with sample completely, so as to over cure
Hydrochlorate is sufficiently cleared up, and convenient rate and accuracy rate in total nitrogen measurement process are greatly promoted.
Claims (10)
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| CN201810734187.6A CN109358016A (en) | 2018-07-06 | 2018-07-06 | A portable pressure cooker combined with a colorimetric tube rapid digestion method and device for measuring total nitrogen in water |
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| CN201810734187.6A CN109358016A (en) | 2018-07-06 | 2018-07-06 | A portable pressure cooker combined with a colorimetric tube rapid digestion method and device for measuring total nitrogen in water |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113720675A (en) * | 2021-08-31 | 2021-11-30 | 辽宁通正检测有限公司 | Digestion device for total nitrogen and total phosphorus analysis pretreatment in environmental monitoring |
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