CN108982388A - The test method of seawater total nitrogen content - Google Patents
The test method of seawater total nitrogen content Download PDFInfo
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- CN108982388A CN108982388A CN201811010913.6A CN201811010913A CN108982388A CN 108982388 A CN108982388 A CN 108982388A CN 201811010913 A CN201811010913 A CN 201811010913A CN 108982388 A CN108982388 A CN 108982388A
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 124
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 62
- 239000013535 sea water Substances 0.000 title claims abstract description 38
- 238000010998 test method Methods 0.000 title claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 38
- 238000012360 testing method Methods 0.000 claims abstract description 27
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 30
- 239000012530 fluid Substances 0.000 claims description 28
- 239000000243 solution Substances 0.000 claims description 22
- 230000003287 optical effect Effects 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 13
- 238000012545 processing Methods 0.000 claims description 13
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 238000002835 absorbance Methods 0.000 claims description 11
- 239000003795 chemical substances by application Substances 0.000 claims description 11
- 238000001816 cooling Methods 0.000 claims description 10
- 230000029087 digestion Effects 0.000 claims description 8
- 239000012086 standard solution Substances 0.000 claims description 8
- 230000005540 biological transmission Effects 0.000 claims description 7
- 239000000284 extract Substances 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- 229910002651 NO3 Inorganic materials 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- 239000002699 waste material Substances 0.000 claims description 3
- 238000004804 winding Methods 0.000 claims description 2
- 230000008033 biological extinction Effects 0.000 claims 1
- 239000003651 drinking water Substances 0.000 abstract description 3
- 235000020188 drinking water Nutrition 0.000 abstract description 3
- 239000002352 surface water Substances 0.000 abstract description 3
- 239000010841 municipal wastewater Substances 0.000 abstract description 2
- 239000000523 sample Substances 0.000 description 20
- 238000000034 method Methods 0.000 description 9
- 238000012544 monitoring process Methods 0.000 description 9
- 238000004458 analytical method Methods 0.000 description 4
- 238000003860 storage Methods 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- IOVCWXUNBOPUCH-UHFFFAOYSA-M nitrite group Chemical group N(=O)[O-] IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 description 2
- 125000001477 organic nitrogen group Chemical group 0.000 description 2
- 238000002798 spectrophotometry method Methods 0.000 description 2
- 230000006641 stabilisation Effects 0.000 description 2
- 238000011105 stabilization Methods 0.000 description 2
- 239000004471 Glycine Substances 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000006855 networking Effects 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
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
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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
-
- 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)
- General Health & Medical Sciences (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Spectroscopy & Molecular Physics (AREA)
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- Engineering & Computer Science (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
The present invention provides a kind of test method of seawater total nitrogen content, including draws total nitrogen absorbance-concentration relationship curve program and seawater total nitrogen test program.The present invention can be used for automatically continuously measuring seawater, drinking water, surface water, underground water, municipal wastewater, the total nitrogen concentration in trade effluent, cannot be used for the test of seawater total nitrogen or the problems such as test accuracy is low, poor repeatability to solve equipment in the market.
Description
Technical field
The present invention relates to seawater quality detection field more particularly to a kind of seawater total nitrogen content test methods.
Background technique
Important component of the total nitrogen as marine environmental monitoring, based on artificial sample and lab analysis, in recent years,
With the multi-platform sensing technology of intelligent Marine Environmental Elements, real-time communication of data technology, standardization data sharing and information
The development of service technology, urgent need establish marine environmental monitoring system, and then realize the synthesis, continuous, in real time, precisely of marine environment
Observation.The measurement of seawater total nitrogen is to the monitoring direction development based on automatic monitoring and intelligent and networking.
The existing much research about total nitrogen water quality online analyzer both at home and abroad, total nitrogen water quality online analyzer use master
Analysis method is wanted to have: (1) alkaline potassium per-sulfate digestion-spectrophotometry；(2) closed combustion oxidation-chemiluminometry.From principle
On say, persulfate resolution-spectrophotometry is the main choosing method of online total nitrogen total phosphorus analysis and the official method of various countries.
Total nitrogen in-line analyzer based on closed combustion oxidation-chemiluminometry is limited primarily to Japan, is Japanese Industrial Specifications association
The method that meeting (JIS) is approved.
With the extensive use of total nitrogen on-line automatic monitoring instrument, the equipment of various brands, properties refer on domestic market
Mark, to operate with increasingly specification simple, but still need further understanding there are many problem in terms of application is with development and improve,
Preferably to meet the requirement of Chinese water quality on-line automatic analyzer.
When testing total nitrogen according to national standards, tested with untreated water sample in situ.The online instrument of total nitrogen at present
For device in order to avoid turbid water body blocking pipeline, big city is equipped with sample pretreatment device, the TNP-4110 sampling of such as Japanese Shimadzu
When can remove biggish solid impurity by the strainer of 50 mesh, recycle high-speed stirred knife to crush the suspended particulate of sample, pass through
After homogenizer processing, test of drawing water is carried out, cleans strainer and sample processing part with ejected wash water after sampling, waits draw water next time.
Since the numerous water bodys of Chinese water system are complicated, water sample certainly will will cause the loss of a part of nitrogen by front processor, influence result and sentence
It is fixed.
By the test analysis discovery to seawater total nitrogen on-line instrument, each instrument is doing performance indicator with inorganic standard solution
When the organic nitrogen titer that can be met the requirements substantially when verifying, but glycine is used to prepare is tested, relative error high level can reach
30~50%.To find out its cause, being on the one hand in continuous mode, seawater sample is not required according to national standard method, and digestion condition reaches
120 DEG C are reacted 30 minutes, cause organic nitrogen that cannot clear up completely；It on the other hand is the total nitrogen in water sample through aoxidizing resolution as nitre
It is nitrite test by nitrate reduction, due to by uviol lamp intensity, irradiation using the method for ultraviolet reduction after hydrochlorate
The influence of the factors such as time, sample and light source distance, nitrate cannot be completely reduced as nitrite.Therefore, resolution rate and
The low accuracy for causing seawater total nitrogen on-line instrument of reduction rate and repeatability cannot meet testing requirement.
The equipment for being currently used for the monitoring of seawater total nitrogen, based on cabinet type machine or desktop computer, volume is big, is not suitable for floating online
Mark, monitoring ship.
Total nitrogen on-line monitoring equipment foreign brand name is expensive, and procurement cycle is long, and operation expense is high.Home brands produce
Product are although cheap, and maintenance cost is low, but measuring stability is poor, and failure rate is higher.
Total nitrogen water quality online analyzer on domestic market there are aiming at the problem that, the purpose of the present invention is to provide one
The device for detecting the total nitrogen content in seawater is planted, mainly by sampling system, water sample processing system, detection system and data
It is useless to can be used for automatically continuously measuring seawater, drinking water, surface water, underground water, municipal administration for the compositions such as acquisition, processing and Transmission system
Total nitrogen concentration in water, trade effluent, the test or test that cannot be used for seawater total nitrogen with the equipment of solution in the market are accurately
The problems such as spending low, poor repeatability.
Summary of the invention
The purpose of the present invention is to provide a kind of test method of seawater total nitrogen content, including drafting total nitrogen absorbance-are dense
Relation curve program and seawater total nitrogen test program are spent, the drafting total nitrogen absorbance-concentration relationship curve program includes following
Step:
Step 1: after extracting pure water rinse pipeline, signal processing system receives the light cast out for passing through counteracting tank, and remembers
It records current collected light intensity, close the step of pure water pipeline, the step for the rinse liquid being discharged in counteracting tank；
Step 2: extracting the nitrate standard solution of known concentration to counteracting tank, then extract the digestion solution of certain volume to resolution
Tank blasts a certain amount of air, is uniformly mixed, then controls fluid temperature in counteracting tank in the first preset temperature range through first
After preset time, then the step of fluid temperature in counteracting tank is down to the second preset temperature；
Step 3: extracting the reducing solution of certain volume to counteracting tank, blast a certain amount of air, be uniformly mixed, later control resolution
The second preset temperature of fluid temperature in tank keeps the second preset time, then the fluid temperature in counteracting tank is down to room temperature, then
A certain amount of color developing agent agent is extracted to counteracting tank and blasts a certain amount of air, is uniformly mixed, then stands colour developing and is preset through third
The step of time；
Step 4: opening light source, acquisition of transmission luminous intensity I1, the mixed solution being then exhausted from counteracting tank, closing light source, calculating suction
The step of shading value；
Step 5: selecting a series of nitrate standard solution of various concentrations, repeat above-mentioned steps 1-4, further according to different dense
The column nitrate of degree and the corresponding relationship of absorbance draw total nitrogen absorbance-concentration relationship curve；
The seawater total nitrogen test program includes following steps:
Step 6: extracting that pure water rinse pipeline, signal processing system is waiting receives the stable light cast out by counteracting tank
After the signal of line conversion, current collected light intensity is recorded, incident intensity I is denoted as2, close pure water pipeline and light source, row
The step of rinse liquid in counteracting tank out；
Step 7: extracting the seawater sample of certain volume to counteracting tank, then the digestion solution for extracting certain volume is blasted to counteracting tank
A certain amount of air is uniformly mixed, then controls fluid temperature in counteracting tank when the first preset temperature range is default through first
Between after, the step of fluid temperature in counteracting tank is down to the second preset temperature；
Step 8: extracting the reducing solution of certain volume to counteracting tank, blast a certain amount of air, after mixing, control counteracting tank
Interior the second preset temperature of fluid temperature keeps the second preset time, then the fluid temperature in counteracting tank is down to room temperature, extracts
A certain amount of color developing agent agent blasts a certain amount of air to counteracting tank again, after mixing, stands colour developing third preset time
The step of；
Step 9: acquisition of transmission luminous intensity I3Afterwards, the mixed solution in counteracting tank is discharged, closes light source, calculates absorbance value, and
According to total nitrogen concentration-absorbance relation curve, the step of calculating the total nitrogen content in sample；
Further, first preset temperature is 120~124 DEG C, and first preset time is 30 minutes, and described second is default
Temperature is 60 DEG C, and second preset time is 20 minutes, and the third preset time is 15 minutes.
Further, the counteracting tank is quartz glass tank, and the raised mode of fluid temperature controlled in quartz glass tank is
Pulsed controls the mode of heater strip, and the device of the reduction fluid temperature in the quartz glass tank is air cooling equipment
The present invention also provides a kind of seawater total nitrogen content on-line measuring devices, include the injection of sample intake passage and stock layout channel
Pump, the stock layout channel are connected with central passage, and the central passage is also connected with multiple channels, which is characterized in that described
One of channel in multiple channels is connected with the reaction solution device for being connected with test device, the reaction solution device packet
The counteracting tank for the winding heater strip including upper cover and lower cover being connected with air cooling equipment is included, the counteracting tank is also connected with gas
Pump, the test device includes light source and optical receiver, and the optical entrance of the light source face counteracting tank, the optical receiver is just
To the optical emission exit of counteracting tank, the optical receiver is connected with signal processing system.
Further, the top and bottom of the test device are connected with the air pump respectively.
Further, the lower end of the test device is connected with drain triple valve, and normally closed channel connects waste discharge liquid pipe, normally opened
Channel is connected by check valve with the air pump.
Further, the upper end of the test device is connected with exhaust three-way valve, and the normally closed channel of the exhaust three-way valve connects
Connect air pump, normally opened channel connection exhaust pipe.
The advantages and positive effects of the present invention are:
Methods and apparatus of the present invention, can be used for automatically continuously measuring seawater, drinking water, surface water, underground water, municipal wastewater,
Total nitrogen concentration in trade effluent, solves the problems, such as to cannot be used for the test of seawater total nitrogen, and test accuracy is high, reproducible
The problems such as.
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 the schematic diagram of seawater total nitrogen content on-line measuring device of the present invention；
Fig. 2 is total nitrogen absorbance of the present invention-concentration working curve test flow chart；
Fig. 3 is the total nitrogen content test flow chart in seawater sample of the present invention；
In figure, syringe pump 1, pure water solenoid valve 2, liquid storage ring 3, Multi-channel switching valve 4, air pump 8, upper cover 51 winds heater strip
Quartz glass tank 52, lower cover 53, air cooling equipment 54, light source 61, optical receiver 62, exhaust three-way valve 71, drain triple valve 72 are single
To valve 73.
Specific embodiment
To keep the purpose of the present invention, technical em- bodiments and advantage clearer, hereinafter with reference in the embodiment of the present invention
Attached drawing clearly and completely describes technical em- bodiments of the invention by embodiment, it is clear that described embodiment is this hair
Bright a part of the embodiment, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not having
Every other embodiment obtained under the premise of creative work is made, shall fall within the protection scope of the present invention.
Embodiment 1, as shown in Figure 1, a kind of seawater total nitrogen on-line measuring device, including syringe pump 1, pure water solenoid valve 2, storage
Pendular ring 3, Multi-channel switching valve 4, reaction solution device, test device, exhaust three-way valve 71, drain triple valve 72, check valve 73
With air pump 8.
The sample intake passage and pure water solenoid valve 2 of the syringe pump 1 connect, for extracting pure water.The stock layout of the syringe pump 1
Channel and pure water liquid storage ring 3 connect, for extracting pure water.
The liquid storage ring 3 is connect with the central passage of Multi-channel switching valve 4, for extracting reagent and sample.
One channel of the Multi-channel switching valve 4 is connect with reaction solution device, for sample and reagent to be added, remaining
Channel is separately connected different reaction reagents.
Reaction solution device upper end is connect with exhaust three-way valve 71.The reaction solution device includes upper cover 51, twines
Around the quartz glass tank 52, lower cover 53 and air cooling equipment 54 of heater strip.
The test device includes light source 61 and optical receiver 62.The light of 61 face quartz glass tank 52 of light source is incident
Mouthful, the liquid in transmitting light irradiation quartz digestion tank.The optical emission exit of 62 face quartz glass tank 52 of optical receiver, connects
The light projected by optical emission exit is received, and is converted into electric signal, output to signal processing system.
The exhaust three-way valve 71, normally closed channel connect air pump 8, normally opened channel connection exhaust pipe, the connection of another channel
Counteracting tank upper end 51.
The drain triple valve 72, normally closed channel connect waste discharge liquid pipe, and normally opened channel connects check valve 73, another channel
Connect quartz glass tank lower end 53.
The check valve 73 connects air pump 8 and triple valve 72.
The air pump 8 is used to pass through the air-blowing into reaction solution device of triple valve 71 and triple valve 72.
Embodiment 2
As shown in Figure 2,3, it is described in detail by monitoring method of the present apparatus to the total nitrogen content in sample solution.
Total nitrogen absorbance-concentration relationship curve is drawn out using the nitrate standard solution of various concentration, testing process is such as
Shown in Fig. 2, include the following steps.
Pure water solenoid valve, light source and syringe pump are opened, pure water rinse pipeline is extracted；
The light cast out for passing through quartz glass tank is received by photodiode, receives stabilization to signal processing system
Signal after, record current collected light intensity, be denoted as incident intensity I1, close pure water solenoid valve and light source；
Drain triple valve is opened, the rinse liquid in quartz glass tank is discharged；
Syringe pump is opened, extracts the nitrate standard solution of known concentration to quartz glass tank；
The digestion solution of certain volume is extracted to quartz glass tank, blasts a certain amount of air, is uniformly mixed；
Pulsed controls the energized state of heater strip, and then the fluid temperature controlled in counteracting tank divides in 120~124 DEG C of ranges 30
Clock；
Air cooling equipment is opened, the fluid temperature in quartz glass tank is down to 60 DEG C；
The reducing solution of certain volume is extracted to quartz glass tank；
A certain amount of air is blasted, is uniformly mixed；
Pulsed controls the energized state of heater strip, and then controls 60 DEG C of fluid temperature in counteracting tank and kept for 20 minutes；
Air cooling equipment is opened, the fluid temperature in quartz glass tank is down to room temperature；
A certain amount of color developing agent agent is extracted to quartz glass tank；
A certain amount of air is blasted, is uniformly mixed；
Stand colour developing 15 minutes；
Open light source, acquisition of transmission luminous intensity I2；
Drain triple valve is opened, the mixed solution in quartz glass tank is discharged, closes light source, calculates absorbance value；
A series of nitrate standard solution for selecting various concentrations, repeats above-mentioned steps；
According to a series of corresponding relationship of nitrate concentrations and absorbance, total nitrogen absorbance-concentration relationship curve is drawn.
Total nitrogen content testing process in seawater sample is as shown in Figure 3, comprising the following steps:
Pure water solenoid valve, light source and syringe pump are opened, pure water rinse pipeline is extracted；
The light cast out for passing through quartz glass tank is received by photodiode, receives stabilization to signal processing system
Signal after, record current collected light intensity, be denoted as incident intensity I3, close pure water solenoid valve and light source；
Drain triple valve is opened, the rinse liquid in quartz glass tank is discharged；
Syringe pump is opened, extracts the seawater sample of certain volume to quartz glass tank；
The digestion solution of certain volume is extracted to quartz glass tank, blasts a certain amount of air, is uniformly mixed；
Pulsed controls the energized state of heater strip, and then the fluid temperature controlled in counteracting tank divides in 120~124 DEG C of ranges 30
Clock；
Air cooling equipment is opened, the fluid temperature in quartz glass tank is down to 60 DEG C；
The reducing solution of certain volume is extracted to quartz glass tank；
A certain amount of air is blasted, is uniformly mixed；
Pulsed controls the energized state of heater strip, and then controls 60 DEG C of fluid temperature in counteracting tank and kept for 20 minutes；
Air cooling equipment is opened, the fluid temperature in quartz glass tank is down to room temperature；
A certain amount of color developing agent agent is extracted to quartz glass tank；
A certain amount of air is blasted, is uniformly mixed；
Stand colour developing 15 minutes；
Open light source, acquisition of transmission luminous intensity I4；
Drain triple valve is opened, the mixed solution in quartz glass tank is discharged, closes light source, calculates absorbance value；
According to total nitrogen concentration-absorbance relation curve, the total nitrogen content in sample is calculated.
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 (7)
1. the test method of seawater total nitrogen content, including draw total nitrogen absorbance-concentration relationship curve program and the survey of seawater total nitrogen
Try program, the drafting total nitrogen absorbance-concentration relationship curve program the following steps are included:
Step 1: after extracting pure water rinse pipeline, signal processing system receives the light cast out for passing through counteracting tank, and remembers
It records current collected light intensity, close the step of pure water pipeline, the rinse liquid being discharged in counteracting tank；
Step 2: extracting the nitrate standard solution of known concentration to counteracting tank, then extract the digestion solution of certain volume to resolution
Tank blasts a certain amount of air, is uniformly mixed, then controls fluid temperature in counteracting tank in the first preset temperature range through first
After preset time, then the step of fluid temperature in counteracting tank is down to the second preset temperature；
Step 3: extracting the reducing solution of certain volume to counteracting tank, blast a certain amount of air, be uniformly mixed, later control resolution
Fluid temperature to the second preset temperature in tank keeps the second preset time, then the fluid temperature in counteracting tank is down to room temperature,
A certain amount of color developing agent is extracted again to counteracting tank and blasts a certain amount of air, is uniformly mixed, then is stood colour developing and preset through third
The step of time；
Step 4: opening light source, acquisition of transmission luminous intensity, the mixed solution being then exhausted from counteracting tank closes light source, calculates extinction
The step of angle value；
Step 5: selecting a series of nitrate standard solution of various concentrations, repeat above-mentioned steps 1-4, further according to different dense
The column nitrate of degree and the corresponding relationship of absorbance draw total nitrogen absorbance-concentration relationship curve；
The seawater total nitrogen test program includes following steps:
Step 6: extracting pure water rinse pipeline, signal processing system is waiting to receive the stable light cast out by counteracting tank
After the signal of line conversion, current collected light intensity is recorded, incident intensity is denoted as, closes pure water pipeline and light source, discharge
The step of rinse liquid in counteracting tank；
Step 7: extracting the seawater sample of certain volume to counteracting tank, then the digestion solution for extracting certain volume is blasted to counteracting tank
A certain amount of air is uniformly mixed, then controls fluid temperature in counteracting tank when the first preset temperature range is default through first
Between after, the step of fluid temperature in counteracting tank is down to the second preset temperature；
Step 8: extracting the reducing solution of certain volume to counteracting tank, blast a certain amount of air, after mixing, control counteracting tank
Interior the second preset temperature of fluid temperature keeps the second preset time, then the fluid temperature in counteracting tank is down to room temperature, extracts
A certain amount of color developing agent agent blasts a certain amount of air to counteracting tank again, after mixing, stands colour developing third preset time
The step of；
Step 9: after acquisition of transmission luminous intensity, the mixed solution in counteracting tank is discharged, closes light source, calculates absorbance value, and root
According to total nitrogen concentration-absorbance relation curve, the step of calculating the total nitrogen content in sample.
2. the test method of seawater total nitrogen content as described in claim 1, which is characterized in that first preset temperature is
120~124 DEG C, first preset time is 30 minutes, and second preset temperature is 60 DEG C, and second preset time is
20 minutes, the third preset time was 15 minutes.
3. the test method of seawater total nitrogen content as described in claim 1, which is characterized in that the counteracting tank is quartz glass
Tank, the raised mode of fluid temperature in quartz glass tank that controls are the mode that pulsed controls heater strip, the quartz glass
The device of reduction fluid temperature in tank is air cooling equipment.
4. seawater total nitrogen content on-line measuring device includes the syringe pump of sample intake passage and stock layout channel, the stock layout channel
It is connected with central passage, the central passage is also connected with multiple channels, which is characterized in that wherein the one of the multiple channel
A channel is connected with the reaction solution device for being connected with test device, and the reaction solution device includes being connected with air cooling equipment
What is connect includes the counteracting tank of the winding heater strip of upper cover and lower cover, and the counteracting tank is also connected with air pump, the test device packet
Include light source and optical receiver, the optical entrance of the light source face counteracting tank, the light outgoing of the optical receiver face counteracting tank
Mouthful, the optical receiver is connected with signal processing system.
5. seawater total nitrogen content on-line measuring device as claimed in claim 4, which is characterized in that the upper end of the test device
It is connected respectively with the air pump with lower end.
6. seawater total nitrogen content on-line measuring device as claimed in claim 4, which is characterized in that the lower end of the test device
It is connected with drain triple valve, normally closed channel connects waste discharge liquid pipe, and normally opened channel is connected by check valve with the air pump.
7. seawater total nitrogen content on-line measuring device as claimed in claim 4, which is characterized in that the upper end of the test device
It is connected with exhaust three-way valve, the normally closed channel connection air pump of the exhaust three-way valve, normally opened channel connect exhaust pipe.
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