CN107727593A - A kind of system and method for total nitrogen in measure water quality - Google Patents
A kind of system and method for total nitrogen in measure water quality Download PDFInfo
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- CN107727593A CN107727593A CN201710942879.5A CN201710942879A CN107727593A CN 107727593 A CN107727593 A CN 107727593A CN 201710942879 A CN201710942879 A CN 201710942879A CN 107727593 A CN107727593 A CN 107727593A
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- total nitrogen
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- 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
- G01N21/314—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry with comparison of measurements at specific and non-specific wavelengths
Abstract
The invention belongs to environmental monitoring technology field, a kind of system and method for determining the total nitrogen in water quality is disclosed, water sample first mixes with alkaline chitinase solution, and by ultraviolet digestion, High-temperature Digestion, the total nitrogen in water is changed into nitrate；NaOH interference is eliminated after being mixed with HCl solution, respectively by two flowing detectors, to determine the response signal of water sample；It is directly proportional to correction signal by formula correction signal, total nitrogen content；Including：Peristaltic pump, hybrid reaction circle, ultraviolet digestion device, heating bath, air bubble eliminating device, dialyzer, the first flowing detection cell, the second flowing detection cell.Present invention decreases the artificial error brought using colorimetric cylinder, pipette, the accuracy and repeatability of testing result are substantially increased；The security of experimentation is improved, has saved the cost of instrument operation；Because the reagent used is less, while the out of order probability of instrument is decreased, add the stability of instrument.
Description
Technical field
The invention belongs to environmental monitoring technology field, more particularly to a kind of system and method for determining the total nitrogen in water quality.
Background technology
At present, the method on the total nitrogen in measure water quality that country puts into effect mainly has five kinds, and prevailing for the time being in force mainly has
①《The measure gas-phase molecular absorption spectrometry method of water quality total nitrogen》(HJ/T 199-2005)；②《The measure alkalescence over cure of water quality total nitrogen
Sour potassium clears up ultraviolet spectrophotometry》(HJ 636-2012)；③《The measure of water quality total nitrogen continuously flows-hydrochloride naphthodiamide point
Light photometry》(HJ 667-2013)；④《Measure flow injection-hydrochloride naphthodiamide AAS of water quality total nitrogen》(HJ
668-2013) four kinds.Wherein《The measure alkaline chitinase resolution ultraviolet spectrophotometry of water quality total nitrogen》(GB 11894-89)
Substituted by (HJ 636-2012) from 1 day June in 2012.《The measure gas-phase molecular absorption spectrometry method of water quality total nitrogen》(HJ/T
199-2005) to be cleared up using high-pressure sterilizing pot, analysis time is longer, the pre-treatment trouble for unknown big concentration water sample,
Pre-treatment is complex for operation step, is readily incorporated error, so as to reduce repeatability and the degree of accuracy, gradually by continuous flowing/stream
Dynamic injection substitution.《The measure alkaline chitinase resolution ultraviolet spectrophotometry of water quality total nitrogen》(HJ 636-2012) is used
High-pressure sterilizing pot is cleared up, and every batch of Specimen eliminating needs 1h or so time, time-consuming, and required reagent toxicity is small, experimental procedure
Simply, but digestion process existence and stability is poor, temperature is whard to control, operating process uneasy congruent factor, repeatability and accuracy
It is poor, calculate trouble.《The measure of water quality total nitrogen continuously flows-hydrochloride naphthodiamide AAS》(HJ 667-2013) and
《Measure flow injection-hydrochloride naphthodiamide AAS of water quality total nitrogen》(HJ 668-2013) can be classified as a kind of research, this
Class method is required to use cadmium post reagent, and toxicity is big, so as to also increase pipe resistance, increase instrument loss.Phosphoric acid, sulphur need to be used
The reagents such as acid, sodium hydroxide, potassium peroxydisulfate, sodium tetraborate, ammonium chloride, hydrochloride naphthodiamide, sulfanilamide (SN), Brij, required reagent kind
Class is more, prepares complicated and time consumption, also increases instrument operating cost.
In summary, the problem of prior art is present be：The method of current Determination TN in water exist analysis time compared with
Long, the pre-treatment trouble for unknown big concentration water sample, pre-treatment is complex for operation step, is readily incorporated error, reduces repetition
Property and the degree of accuracy；Digestion process existence and stability is poor, temperature is whard to control, operating process uneasy congruent factor, repeatability and standard
True property is poor, calculates trouble；Using cadmium post reagent, toxicity is big, increases pipe resistance, increase instrument loss, reagent type is more, matches somebody with somebody
Complicated and time consumption processed, adds operating cost.
The content of the invention
The problem of existing for prior art, the invention provides a kind of system and method for determining the total nitrogen in water quality.
The present invention is achieved in that a kind of method for determining the total nitrogen in water quality, the total nitrogen in the measure water quality
Method comprises the following steps：
(1) water sample first mixes with alkaline chitinase solution, by ultraviolet digestion, 107 DEG C~110 DEG C High-temperature Digestions, water
In total nitrogen be changed into nitrate；
(2) NaOH interference is eliminated after being mixed with HCl solution, respectively by two flowing detectors, is existed with determining water sample
Response signal A under 220nm and 275nm220And A275；
(3) formula A=A is pressed220-2A275Correction signal A, total nitrogen content are directly proportional to correction signal A.
Another object of the present invention is in the measure water quality for the method for providing the total nitrogen in a kind of measure water quality
The system of total nitrogen, the system for determining the total nitrogen in water quality are provided with：
The peristaltic pump passes on left pump line connection reagent, automatic sampler；Connected and mixed by pump line on the right side of peristaltic pump
Reacting ring；Hybrid reaction circle right-hand member connects ultraviolet digestion device by pump line；Ultraviolet digestion device right-hand member is added by pump line connection
Hot device；Heater right-hand member connects hybrid reaction circle by pump line；Hybrid reaction circle right-hand member is connected by pump line (passing through peristaltic pump)
Air bubble eliminating device；Air bubble eliminating device right-hand member connects dialyzer by pump line (passing through peristaltic pump)；Dialyzer right-hand member is connected by pump line
Connect air bubble eliminating device；Air bubble eliminating device right-hand member passes through pump line connecting detection unit.
Further, the optical filter of the first flowing detection cell is 220nm, light path 30mm.
Further, the optical filter of the second flowing detection cell is 275nm, light path 30mm.
Advantages of the present invention and good effect are：
(1) compared with manual method, sample, clear up, colorimetric is automatically brought into operation by instrument completely, due to instrument measure it is more accurate
Really, the artificial error brought using colorimetric cylinder, pipette is reduced, substantially increases the accuracy and repeatability of testing result；
Analysis process reduces the influence that reagent volatilizees to operator's health, improves experimentation in the closed progress of instrument internal
Security；
(2) manual method needs to generally require resolution today, is analyzed within second day after cooling down a whole night, otherwise just needs to work overtime,
And instrumental method can be analyzed and finished on the same day, it is not necessary to which operating personnel work overtime, and sample analysis speed is faster；The present invention is doing sample process
In, as a result it is shown on collection of illustrative plates, if result is bad, reason can be gone out according to atlas analysis at once, reformed in time, and manual method is only
Have after result is calculated, the place malfunctioned in experimentation could be derived from result, increase time and the cost of error correction.
(3) present invention compared with instrumental method, it is not necessary to use poisonous cadmium post, mainly using potassium peroxydisulfate, sodium hydroxide,
Three big reagent of hydrochloric acid, the reagent type used is few, saves the time with reagent, has saved the cost of instrument operation；Due to making
Reagent is less, while decreases the out of order probability of instrument, adds the stability of instrument.
Brief description of the drawings
Fig. 1 is the system structure diagram of the total nitrogen in measure water quality provided in an embodiment of the present invention；
In figure：1st, peristaltic pump；2nd, hybrid reaction circle；3rd, ultraviolet digestion device；4th, heating bath；5th, air bubble eliminating device；6th, thoroughly
Parser；7th, the first flowing detection cell；8th, the second flowing detection cell；R1：Alkaline chitinase solution 0.80mL/min；R2：Hydrochloric acid
Solution 0.32mL/min；R3：Brij solution 0.80mL/min；S：Sample 1.00mL/min；ReS：Sub-sampling 1.6mL/min；
G：Air；W：Waste liquid.
Fig. 2 is total nitrogen calibration curve peak shape figure provided in an embodiment of the present invention；
Fig. 3 is total nitrogen calibration graph provided in an embodiment of the present invention.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
It is of the invention compared with environmentally friendly ministerial standard HJ 636-2012, HJ 667-2013, the results showed that the present invention both had
There is the advantages of sample treatment of traditional-handwork method is simple, reagent dosage is few, there is Dutch Skalar analytical instrument company San++ again
Continuous Flow Analysis instrument accurately and efficiently advantage.
The application principle of the present invention is explained in detail below in conjunction with the accompanying drawings.
As shown in figure 1, the system of the total nitrogen in measure water quality provided in an embodiment of the present invention includes：Peristaltic pump 1, mixing are anti-
2, ultraviolet digestion device 3, heating bath 4, air bubble eliminating device 5, dialyzer 6, first should be enclosed and flow detection cell 7, the second flow detection
Pond 8.
Peristaltic pump 1 passes on left pump line connection air bubble eliminating device 5；The right side of peristaltic pump 1 connects dialyzer 6 by pump line；Thoroughly
The right side of parser 6 top connects air bubble eliminating device 5 by pump line；The right side of air bubble eliminating device 5 connects the first flow detection by pump line
Pond 7；The first flowing right-hand member of detection cell 7 passes through pump line connection the second flowing detection cell 8；The right side of peristaltic pump 1 is connected mixed by pump line
Close reacting ring 2；The right-hand member of hybrid reaction circle 2 connects ultraviolet digestion device 3 by pump line；The right-hand member of ultraviolet digestion device 3 passes through pump line
Connect heating bath 4；The right-hand member of heating bath 4 connects hybrid reaction circle 2 by pump line.
The optical filter of first flowing detection cell 7 is 220nm, light path 30mm；Second flowing detection cell 8 optical filter be
275nm, light path 30mm.
The method of total nitrogen in measure water quality provided in an embodiment of the present invention comprises the following steps：
(1) water sample first mixes with alkaline chitinase solution, then by ultraviolet digestion, then by 107 DEG C~110 DEG C high temperature
Clear up, the total nitrogen in water is changed into nitrate；
(2) NaOH interference is eliminated after being mixed with HCl solution, respectively by two flowing detectors, is existed with determining water sample
Response signal A under 220nm and 275nm220And A275；
(3) formula A=A is pressed220-2A275Correction signal A, total nitrogen (in terms of N) content are directly proportional to correction signal A.
The application effect of the present invention is explained in detail with reference to experiment.
1st, standard curve
The standard substance that mass concentration is 100mg/L is diluted step by step with water, prepares the standard series of 5 concentration points, always
Nitrogen concentration is respectively 1.00mg/L, 2.00mg/L, 3.00mg/L, 4.00mg/L, 5.00mg/L.Peak shape figure is shown in Table 1, calibration
Curve map is shown in Table 2.
Fig. 2 total nitrogen calibration curve peak shape figures, Fig. 3 total nitrogen calibration graphs, wherein a=0.0006, b=0.0052, r=
0.9994；Calibration curve peak shape figure coefficient correlation is 0.9998>0.995, meet measure and require.
2nd, method detection limit
Detection limit (Limit of detection or minimum detectability) be certain particular analysis method to
The Cmin or minimum of test substance can be detected in fixed confidence level from sample.So-called " detection " refers to qualitative detection,
Judge there is the test substance that concentration is higher than blank in sample.
Prescriptive procedure detection limit in U.S. EPA SW -846：
MDL=3.143 δ；
In formula：MDL-method detection limit；
δ-blank parallel determination (in batch) standard deviation；
This experiment is determined to 12 parts of samples of zero-dose, and test result see the table below
The zero-dose solution testing result of table 1
Method detection is limited in this experiment：DL=3.143*0.0033=0.010mg/L.
《The measure of water quality total nitrogen continuously flows-hydrochloride naphthodiamide AAS》The detection of (HJ 667-2013)
0.004mg/L is limited to, from the point of view of detection limit, the present invention and National Standard Method are without significant difference, even better than National Standard Method.
3rd, method precision
This experiment has carried out parallel determination to 12 parts of samples that total nitrogen concentration is 3.00mg/L, and test result see the table below.Its
Average value x=2.979, average deviation S0=0.0555, relative average debiation d=2%.
The 3.00mg/L solution testing results of table 2
| Numbering | 1 time | 2 times | 3 times | 4 times | 5 times | 6 times | 7 times |
| As a result | 2.884 | 2.991 | 2.898 | 3.018 | 3.007 | 3.011 | 3.014 |
| Numbering | 8 times | 9 times | 10 times | 11 times | 12 times | X (average value) | S0(standard deviation) |
| As a result | 2.883 | 3.013 | 3.018 | 3.009 | 3.007 | 2.979 | 0.0555 |
《Water and effluent monitoring analysis method》In regulation on " water quality monitoring Good Laboratory Con trolling index (it is recommended that) ",
As total nitrogen concentration ﹥ 1.0mg/L, precision≤5%.Test result indicates that the ＜ 10% of precision 2% of the invention, this
The precision of invention meets the requirement of environmental monitoring.
4th, the method degree of accuracy
Former state performance number average out to 2.979mg/L, determine 12 times altogether, the results are shown in Table 3, it is total that 1mL is added in 250mL volumetric flasks
Nitrogen concentration is 300mg/L standard liquid, carries out 12 measurements, average value 4.129, the results are shown in Table 3.
Recovery of standard addition=(mark-on Specimen Determination value-Specimen Determination value)/mark-on amount × 100%=(4.129 × 250-
2.979 × 249)/(300 × 1.00) × 100%=97%
The mark-on reclaims solution testing result of table 3
《Water and effluent monitoring analysis method》In regulation on " water quality monitoring Good Laboratory Con trolling index (it is recommended that) ",
As total nitrogen concentration ﹥ 1.0mg/L, 95%≤degree of accuracy≤105%.Test result indicates that the degree of accuracy of the invention is
97%, meet the requirement of environmental monitoring.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement made within refreshing and principle etc., should be included in the scope of the protection.
Claims (4)
1. it is a kind of determine water quality in total nitrogen method, it is characterised in that it is described measure water quality in total nitrogen method include with
Lower step：
(1) water sample first mixes with alkaline chitinase solution, by ultraviolet digestion, 107 DEG C~110 DEG C High-temperature Digestions, in water
Total nitrogen is changed into nitrate；
(2) NaOH interference is eliminated after being mixed with HCl solution, respectively by two flowing detectors, with determine water sample in 220nm and
Response signal A under 275nm220And A275；
(3) formula A=A is pressed220-2A275Correction signal A, total nitrogen content are directly proportional to correction signal A.
2. total nitrogen system in a kind of measure water quality of the method for the total nitrogen in water quality of measure as claimed in claim 1, its feature
It is, the system of the total nitrogen in the measure water quality is provided with：
Peristaltic pump；
The peristaltic pump passes on left pump line connection air bubble eliminating device；Dialyzer is connected by pump line on the right side of the peristaltic pump；
Top connects air bubble eliminating device by pump line on the right side of the dialyzer；Pass through pump line connection the on the right side of the air bubble eliminating device
One flowing detection cell；
The first flowing detection cell right-hand member passes through pump line connection the second flowing detection cell；
Hybrid reaction circle is connected by pump line on the right side of the peristaltic pump side；Hybrid reaction circle right-hand member connects ultraviolet digestion by pump line
Device；
The ultraviolet digestion device right-hand member connects heating bath by pump line；Heating bath right-hand member connects hybrid reaction circle by pump line.
3. the system of the total nitrogen in measure water quality as claimed in claim 2, it is characterised in that the first flowing detection cell
Optical filter be 220nm, light path 30mm.
4. the system of the total nitrogen in measure water quality as claimed in claim 2, it is characterised in that the second flowing detection cell
Optical filter be 275nm, light path 30mm.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110220855A (en) * | 2019-05-31 | 2019-09-10 | 北京海光仪器有限公司 | A kind of chemical analysis system for total nitrogen |
| CN112924405A (en) * | 2021-01-27 | 2021-06-08 | 华能（天津）煤气化发电有限公司 | Concentrated seawater total nitrogen data continuous online monitoring system for seawater cooling power plant |
| CN113155588A (en) * | 2021-05-13 | 2021-07-23 | 武汉新烽光电股份有限公司 | Rapid automatic water quality detection system and method based on micro-fluidic |
| CN116840219A (en) * | 2023-07-31 | 2023-10-03 | 上海博取仪器有限公司 | Method for detecting total nitrogen concentration of water quality |
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| CN116840219B (en) * | 2023-07-31 | 2024-03-19 | 上海博取仪器有限公司 | Method for detecting total nitrogen concentration of water quality |
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