CN101592670B - Automatic analysis quantitative measurement method and automatic analysis quantitative measuring apparatus - Google Patents
Automatic analysis quantitative measurement method and automatic analysis quantitative measuring apparatus Download PDFInfo
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- 238000004458 analytical method Methods 0.000 title claims abstract description 29
- 238000000691 measurement method Methods 0.000 title 1
- 238000006243 chemical reaction Methods 0.000 claims abstract description 37
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 27
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 15
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 14
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 14
- 239000011574 phosphorus Substances 0.000 claims abstract description 14
- 238000005070 sampling Methods 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 13
- 239000007789 gas Substances 0.000 claims description 9
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 claims description 9
- 238000000354 decomposition reaction Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 abstract description 5
- 230000001678 irradiating effect Effects 0.000 abstract 1
- 239000010453 quartz Substances 0.000 description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 10
- 239000003708 ampul Substances 0.000 description 9
- 238000005259 measurement Methods 0.000 description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 7
- 238000010586 diagram Methods 0.000 description 4
- 238000005206 flow analysis Methods 0.000 description 4
- 239000004159 Potassium persulphate Substances 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000008676 import Effects 0.000 description 3
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 3
- 235000019394 potassium persulphate Nutrition 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 239000013535 sea water Substances 0.000 description 3
- 235000019832 sodium triphosphate Nutrition 0.000 description 3
- UNXRWKVEANCORM-UHFFFAOYSA-I triphosphate(5-) Chemical compound [O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O UNXRWKVEANCORM-UHFFFAOYSA-I 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- ZKHQWZAMYRWXGA-KQYNXXCUSA-N Adenosine triphosphate Chemical compound C1=NC=2C(N)=NC=NC=2N1[C@@H]1O[C@H](COP(O)(=O)OP(O)(=O)OP(O)(O)=O)[C@@H](O)[C@H]1O ZKHQWZAMYRWXGA-KQYNXXCUSA-N 0.000 description 2
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-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
- 238000010521 absorption reaction Methods 0.000 description 2
- PLZFHNWCKKPCMI-UHFFFAOYSA-N cadmium copper Chemical compound [Cu].[Cd] PLZFHNWCKKPCMI-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000002572 peristaltic effect Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 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
- 238000012952 Resampling Methods 0.000 description 1
- 229960005070 ascorbic acid Drugs 0.000 description 1
- 235000010323 ascorbic acid Nutrition 0.000 description 1
- 239000011668 ascorbic acid Substances 0.000 description 1
- 230000008033 biological extinction Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- XPPKVPWEQAFLFU-UHFFFAOYSA-N diphosphoric acid Chemical compound OP(O)(=O)OP(O)(O)=O XPPKVPWEQAFLFU-UHFFFAOYSA-N 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002460 imidazoles Chemical class 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 238000005375 photometry Methods 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 238000009428 plumbing Methods 0.000 description 1
- 230000010349 pulsation Effects 0.000 description 1
- 229940005657 pyrophosphoric acid Drugs 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000001054 red pigment Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/18—Water
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/22—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using chemical indicators
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
- G01N35/10—Devices for transferring samples or any liquids to, in, or from, the analysis apparatus, e.g. suction devices, injection devices
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
- G01N2035/00346—Heating or cooling arrangements
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- General Health & Medical Sciences (AREA)
- Immunology (AREA)
- Pathology (AREA)
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- Food Science & Technology (AREA)
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Abstract
The invention relates to a total nitrogen content and a total phosphorus total content automatic analysis quantitatively measure apparatus and an automatic analysis quantitatively measure method, wherein the method adopts continuous streaming analytical method, which comprises the following procedures: separate a sample (S) by using air (A); inject the separated sample and a reagent (B,C) into a tube (10) together continuously for quantity determination and mixture; after analysis of the obtained mixed liquor in a reaction collecting tube (4), analyze in usual way by a detector (5), and sample the sample (S) at a certain time interval to supply to the tube (10); in the reaction collecting tube (4), the mixed liquor is remained for 10-30 min, heat and decompose the mixed liquor under the temperature from 80 to 90 DEG while irradiating UV; analyze the mixed liquor that generated repeatedly at a certain time interval so as to quantitatively measure total nitrogen content and total phosphorus total content of a sampling position.
Description
Technical field
The present invention relates to utilize Continuous Flow Analysis method (Continuous Flow Analysis, be called for short CFA) in long-time span to detected object in the automatic analysis quantitatively measure apparatus measured automatically of the concentration of ultramicron concentration composition.
Background technology
In the past,, adopt the analytical equipment of having utilized Continuous Flow Analysis method principle in order to measure nitrogen, the phosphorus total concentration that contains in the detected objects such as seawater or waste water always.
The measuring method that above-mentioned analytical equipment adopts does; In pipe, import sample continuously with certain flow, and in pipe, inject gases such as air or inert gas regularly, liquid is carried out bubble separate; Inject sample and required reagent then successively; Utilize hybrid coil or reactor coil to react, the reactant of generation is measured (for example, with reference to patent documentation 1～3) through the detecting instruments such as spectrophotometer that flow cell (Flow Cell) is housed.
[patent documentation 1] japanese openly flat 8-285835 number
Open 2006-234601 number of [patent documentation 2] japanese
Open 2006-208344 number of [patent documentation 3] japanese
Above-mentioned analytical equipment is mainly used in the water quality management of seawater or waste water etc.Consider from the angle of water quality management, preferably need not pass through staff, can in long-time span, carry out water quality measurement at interval automatically with certain hour.
But therefore above-mentioned analytical equipment in the past need, in order to make provision against emergencies, must have the staff to monitor with high temperature, hyperbaric environment heater coil when using reactor coil to react, and is difficult to realize operatorless automatic measurement.
For this reason, can consider to use long loop, and can realize under unmanned heating of measuring automatically, the pressurized conditions still, realizing that the required loop length of said circumstances does not correspond to reality through reacting for a long time.
Summary of the invention
The present invention proposes for addressing the above problem, its objective is provide need not through staff can be in long-time span be the cycle with the certain hour, safety, carry out the automatic analysis quantitatively measure apparatus of water quality measurement automatically exactly.
For achieving the above object, the automatic analysis quantitatively measure method that the present invention relates to adopts the Continuous Flow Analysis method, specify into; Utilize gas that the sample of sampling is separated, then the sample of separating is injected into reagent continuously and carries out in the pipe quantitatively and mix, after in the reaction concetrated pipe, the mixed liquor that obtains being decomposed; Use detecting device to analyze through usual way; This method is sampled to sample with certain hour at interval, supplies to pipe, in the reaction concetrated pipe; Said mixed liquor was stopped 10～30 minutes; Under 80～90 ℃ temperature, carry out the said mixed liquor of heating and decomposition in ultraviolet ray (UV) irradiation, successively the said mixed liquor that generates repeatedly at interval with certain hour is analyzed, thus the total nitrogen content of quantitative measurment sampling position and total phosphorus content.
In addition; The automatic analysis quantitatively measure apparatus that the present invention relates to is a kind ofly to utilize gas to separate the sample by automatic sampler sampling through volume pump, and the sample of separating is injected into reagent continuously carries out in the pipe quantitatively and mix; In the reaction concetrated pipe to after obtaining mixed liquor and decomposing; The measuring equipment that uses detecting device to adopt usual way to analyze, wherein, in the reaction concetrated pipe; Said mixed liquor stopped 10～30 minutes, under 80～90 ℃ temperature, heated mixed liquor when carrying out the UV irradiation; Automatic sampler is sampled to sample with the time interval of heat time heating time of surpassing above-mentioned reaction concetrated pipe repeatedly; In time beyond injecting sample, in pipe, supply with water.
As stated, the present invention rests in the reaction concetrated pipe mixed liquor, with the heating of 80～90 ℃ temperature, carries out the UV irradiation, need not high temperature, high pressure can decompose.Therefore, even for the composition of denier in the sample, also can be with good precision measure total nitrogen content and total phosphorus content.In addition, owing to be not under high temperature, hyperbaric environment, mixed liquor to be analyzed, can carry out unattendedly, successively the above-mentioned mixed liquor that generates at interval with certain hour analyzed, safely the total nitrogen content of measuring samples sampling position and total phosphorus content.
In addition, the automatic analysis quantitatively measure apparatus that the present invention relates to, except make decomposed solution rest on the reaction concetrated pipe in 10～30 minutes; Outside with 80～90 ℃ temperature decomposed solution being heated; Also carry out the UV irradiation simultaneously, therefore, have good mixed liquor decomposability.
Description of drawings
Fig. 1 is the integrally-built circuit diagram of automatic analysis quantitatively measure apparatus that explanation the present invention relates to;
Fig. 2 is the enlarged diagram of reaction concetrated pipe among Fig. 1.
Reference numeral
1: automatic analysis quantitatively measure apparatus 10: pipe
2: automatic sampler 3: volume pump
4: reaction concetrated pipe 5: detecting device
S: sample A: air (gas)
B: reagent C: reagent
D: reagent E: reagent
F: reagent G: reagent
Embodiment
Below in conjunction with accompanying drawing the embodiment of the invention is elaborated.
Fig. 1 is the one-piece construction synoptic diagram of automatic analysis quantitatively measure apparatus 1, and Fig. 2 is reaction concetrated pipe 4 synoptic diagram of automatic analysis quantitatively measure apparatus 1.
Promptly; Above-mentioned automatic analysis quantitatively measure apparatus 1 is a kind ofly to utilize air A to separate the sample S by automatic sampler 2 sampling through volume pump 3, in reagent B, C are injected into pipe 10 continuously, carries out quantitatively, mixes; After in reaction concetrated pipe 4, above-mentioned mixed liquor being decomposed; The measuring equipment that adopts usual ways to analyze through detecting device 5, wherein, in reaction concetrated pipe 4; Mixed liquor was stopped 10～30 minutes, under 80～90 ℃ temperature, carry out heating mixed liquor in the UV irradiation; Automatic sampler 2 is sampled to sample S with the time interval that surpasses 4 heat time heating times of above-mentioned reaction concetrated pipe repeatedly; In time beyond injecting sample, in pipe 10, supply with pure water W.
Volume pump 3 has used the peristaltic pump (peristaltic pump) that the fixed displacement pump suction pipe can be installed, and can supply with sample S or reagent B, the C of sampling with certain flow continuously to pipe 10.Volume pump 3 is provided with the injecting gas controlling plumbing fixtures 11 that keeps injecting synchronously, regularly air A with the pulsation of pump, can carry out the bubble separation to sample S and the mixed liquor of reagent B, C that supplies in the pipe 10.The mixed liquor of sample S and reagent B, C is through being mixed by the overcurrent effect of each separating element of air A separation.In addition, can pipe 10 be wound in spiral form, the conduction immixture when utilizing mixed liquor through helical inside makes its mixing.
Importing to the sample S in the pipe 10 through volume pump 3, at first separated regularly, all be injected into reagent B in each separating element that is separated by air S---alkaline potassium persulphate becomes the mixed liquor that alkalescence is decomposed usefulness.In addition, another kind of reagent C---sulfuric acid is injected in the centre position of reaction concetrated pipe 4, becomes the acidity decomposition that contains acid potassium persulphate and uses mixed liquor.In addition, also can use inert gas as separating gas A.
The structure of reaction concetrated pipe 4 is as shown in Figure 2, after the center of the quartz ampoule 41 that spiral form twines is provided with UV irradiation light 42, covers well heater 43 at its outside surface and constitutes.The pars intermedia of quartz ampoule 41 also is provided with and is used to inject reagent C---the take-off pipe 44 of sulfuric acid.Above-mentioned reaction concetrated pipe 4 can heat 10～30 minutes quartz ampoule 41 with 80～90 ℃ temperature when carrying out the UV irradiation.In 10～30 minutes of heating, the mixed liquor in the quartz ampoule 41 is slack.If residence time less than 10 minutes can't fully be decomposed mixed liquor.The residence time because mixed liquor fully decomposes, does not have too many practical significance so prolong the residence time when surpassing 30 minutes.In addition, if 80 ℃ of heating-up temperature less thaies then can't fully be decomposed.As for the upper limit of heating-up temperature, high more helping more of temperature decomposes certainly, if too high but temperature is provided with, can bring safety problem, therefore, preferably is limited in below 90 ℃.In addition, stop, outside it is heated, react concetrated pipe 4, play the effect that promotes decomposition also through the mixed liquor in the UV irradiation light 42 irradiation quartz ampoules 41 except making mixed liquor.Therefore, after 10～30 minutes, the mixed liquor in the quartz ampoule 41 will become the back and analyze required decomposed solution in heating under 80～90 ℃ the lower temperature.In addition, the downside of take-off pipe 44 will form and use mixed liquor, upside will form the alkalescence decomposition to use mixed liquor, therefore, through reacting the decomposition of concetrated pipe 4, be the boundary with take-off pipe 44, form acid decomposed solution and alkaline decomposed solution respectively acid the decomposition.
The internal diameter that forms the quartz ampoule 41 of reaction concetrated pipe 4 is generally 1mm～5mm, preferably 2mm～3mm.If internal diameter is less than 1mm, sample S or reagent B, when C flows through quartz ampoule 41, latch up phenomenon appears easily, if but internal diameter surpasses 5mm, and the consumption with increasing reagent B, C causes waste.In addition, the length of quartz ampoule 41 is generally 50cm～10m, preferably 1m～3m.If curtailment 50cm can't form the decomposed solution of analyzing required abundance.If but length surpasses 10m, the decomposed solution of formation will cause waste considerably beyond analyzing required amount.
The decomposed solution that is oxidized to nitrate nitrogen that detecting device 5 at first will decompose in reaction concetrated pipe 4 through divider (Splitter) be oxidized to ortho-phosphoric decomposed solution separated into two parts and carry out resampling, and import total nitrogen content analysis meter 6 and total phosphorus content analysis meter 7 respectively.
Total nitrogen content analysis meter 6 is separated the imidazoles D that is injected in the pipe 10 through air A, and injects decomposed solution R1, makes it pass through cadmium-copper reduction coil 61 then, and nitrate nitrogen is reduced to nitrite nitrogen.Then, inject naphthodiamide E, and the red pigments of color development is imported the flow cell 51 of spectrophotometer 50, use near the spectrophotometric the 550nm to carry out colorimetric measurement.
Though; Above-mentioned total nitrogen content analysis meter 6 has adopted the ethylenediamine absorption photometry of utilizing cadmium-copper coil to analyze, but the present invention is not limited thereto, also can in pipe 10, inject pure water or sulfuric acid solution; Use air A to separate; After injecting decomposed solution R1 therein, import flow cell 51, carry out colorimetric measurement with near the spectrophotometric the 220nm.
Total phosphorus content analysis meter 7 is separated the molybdate luminescence reagent F that is injected in the pipe 10 through gas A; And inject ascorbic acid reagent G and decomposed solution R2 therein; And the flow cell 52 of the cyan pigment importing spectrophotometer 50 that the molybdenum of color development is blue or green, carry out colorimetric measurement with near the spectrophotometric the 880nm.
In addition, above-mentioned detecting device 7 uses spectrophotometer 50 as pick-up unit, but the present invention is not confined to spectrophotometer 50 especially, and the S kind can also adopt ultraviolet extinction photometer, fluorophotometer, flame photometer etc. per sample.
Through computing machine the signal of detecting device 5 is handled automatically, can be calculated the concentration of various sample S.
Measurement of concetration result with 1 couple of sample S of automatic analysis quantitatively measure apparatus stores on the computers in advance, just can in long-time span, automatically measure repeatedly later on.The continuous coverage cycle can reach more than 1 week, sustainable running 1 year.
In addition, to the not special restriction of the sampling time interval of sample S, as long as surpass the residence time (10～300 minutes) in reaction concetrated pipe 4, for example, can be whenever at a distance from 30 minutes, or, also can be set at the longer time whenever at a distance from 1 hour.In reaction concetrated pipe 4, mixed liquor is stopped; Mixed liquor in the equipment path flows and also can stop to flow, therefore, if time interval setting is very short; Just need the adjustment time interval; After the sample S of front being accomplished detect in detecting device 5, the sample S of back is rested in the reaction concetrated pipe 4, or 10 length is managed in adjustment.If the time interval is oversize; The time that water except that sample S flows in the equipment path will increase greatly, causes waste, therefore; In detecting device 5, accomplish to detect the next time interval from the sample S of front, preferably stop liquid flowing in the equipment path.
In addition, according to the cycle that configures in advance, regularly to only measuring the data during as calculation sample S concentration through the pure water W and the titer of reagent modulation.Above-mentioned basic measurement or titer are measured and can when carrying out plant maintenance, be accomplished, and for the situation of in long-time span, carrying out unmanned operation, also programmed is in advance accomplished it automatically when sample S is sampled.
In addition,, carry out resolution process,, make it be filled into reaction concetrated pipe 4 inside so will transmit sample S at least because the sample S of sampling need rest in the reaction concetrated pipe 4.With the capacity of reaction concetrated pipe 4 or according to the capacity of calculating to the length of the pipe 10 that reacts concetrated pipe 4 is benchmark, can adjust the supply mode of sample S through volume pump 3.In addition, W controls through pure water, and except carrying out the sample S of resolution process in the concetrated pipe 4 in reaction, making in the path of above-mentioned automatic analysis quantitatively measure apparatus 1 does not have unnecessary sample S to flow.Through flowing of pure water W, when each the measurement, realize the effect of washing path.
Prepare automatic analysis quantitatively measure apparatus, the quartz ampoule that this equipment has internal diameter 2mm, long 4m is wound in coiled type, connects coil central authorities the UV lamp is set, thereby and twine the reaction concetrated pipe that heating collar can be heated to 40～100 ℃ on every side at quartzy coil.
With 40g potassium persulphate, 4g dissolution of sodium hydroxide in the 1000ml pure water as reagent, with the 100ml sulfuric acid dissolution in the 1000ml pure water as another kind of reagent.
The 0.5g tripolyphosphate is dissolved in the 1000ml pure water, as sample.
As shown in table 1, with the condition that does not heat, is heated to 70 ℃, is heated to 80 ℃ the mixed liquor situation that do not stop, stop 5～30 minutes in the reaction concetrated pipe has been measured the concentration as the tripolyphosphate WS of sample respectively.The result is as shown in table 1.
Table 1
Can find out that from table 1 heating-up temperature is high more, stand-by time is long more, the recovery is good more, particularly, is being heated under 80 ℃ the condition, when stopping more than 10 minutes, has realized surpassing 86% the good recovery.
Prepare all cpds shown in the table 2 as sample, adopt with the foregoing description 1 identical reagent and reaction concetrated pipe and analyze.Under 80 ℃ heating condition, the situation that the reaction concetrated pipe stops 20 minutes is tested.The result is as shown in table 2.
Table 2
| Compound | The present invention (mg/l) | Manual analyzing (mg/l) |
| Tripolyphosphate | 0.95 | 0.99 |
| Pyrophosphoric acid | 1.0 | 1.0 |
| ATP (atriphos) | 1.0 | 1.0 |
Can find out that from table 2 all compounds in the his-and-hers watches have all been realized the good recovery.
Industrialization prospect
The present invention can be used for the water quality management in upper and lower water course, seawater, rivers and creeks, lake, pond etc.
Claims (2)
1. total nitrogen content and total phosphorus total content automatic analysis quantitatively measure method; This method comprises: utilize gas that the sample of sampling is separated; Then the sample of separating is injected into reagent continuously and carries out in the pipe quantitatively and mix, after in the reaction concetrated pipe, the mixed liquor that obtains being decomposed, in detecting device, be divided into two parts through divider; Then total nitrogen content and total phosphorus content are carried out parallel parsing, it is characterized in that:
The time interval with heat time heating time of surpassing said reaction concetrated pipe samples to sample, supplies to pipe;
In the reaction concetrated pipe, said mixed liquor was stopped 10～30 minutes, when carrying out the UV irradiation under 80～90 ℃ temperature the said mixed liquor of heating and decomposition;
Successively the said mixed liquor that generates repeatedly at interval with certain hour is analyzed, thus the total nitrogen content of quantitative measurment sampling position and total phosphorus content.
2. total nitrogen content and total phosphorus content automatic analysis quantitatively measure apparatus; This equipment is a kind ofly to utilize gas to separate the sample by automatic sampler sampling through volume pump; And the sample of separating is injected into reagent continuously carries out in the pipe quantitatively and mix; After in the reaction concetrated pipe, the mixed liquor that obtains being decomposed; In detecting device, be divided into two parts, total nitrogen content and total phosphorus content carried out the total nitrogen content and the total phosphorus content automatic analysis quantitatively measure apparatus of parallel parsing, it is characterized in that through divider:
In the reaction concetrated pipe, said mixed liquor was stopped 10～30 minutes, under 80～90 ℃ temperature, heat said mixed liquor when carrying out the UV irradiation;
Said automatic sampler is sampled to sample with the time interval of heat time heating time of surpassing said reaction concetrated pipe repeatedly;
In time beyond injecting sample, in pipe, supply with water.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1020080050164 | 2008-05-29 | ||
| KR10-2008-0050164 | 2008-05-29 | ||
| KR1020080050164A KR100875629B1 (en) | 2008-05-29 | 2008-05-29 | Automatic analysis quantitative measurement method and automatic analysis quantitative measurement device |
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| Publication Number | Publication Date |
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| CN101592670A CN101592670A (en) | 2009-12-02 |
| CN101592670B true CN101592670B (en) | 2012-09-19 |
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| JP (1) | JP2009288228A (en) |
| KR (1) | KR100875629B1 (en) |
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Families Citing this family (22)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101655501B (en) * | 2009-09-30 | 2012-02-01 | 河北科技大学 | On-line automatic monitoring system and monitoring method of total nitrogen and total phosphorus in seawater |
| CN102253232B (en) * | 2010-05-21 | 2013-06-05 | 北京吉天仪器有限公司 | Automatic analyzer and analysis method for water soluble total phosphorus |
| CN102636446B (en) * | 2012-05-09 | 2013-11-20 | 江南大学 | On-line detection device for detecting total nitrogen and total phosphorus through ozone ultraviolet collaborative oxidative digestion |
| CN103217394B (en) * | 2013-04-10 | 2014-11-26 | 中国科学院合肥物质科学研究院 | Online detection device of water dissolved-out nitrogen nutrients of chemical fertilizer |
| CN104914064A (en) * | 2014-03-14 | 2015-09-16 | 株式会社岛津制作所 | Analytical device |
| CN104142323A (en) * | 2014-07-04 | 2014-11-12 | 中国热带农业科学院橡胶研究所 | A method for simultaneous determination of plant nitrogen and phosphorus |
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| CN101592670A (en) | 2009-12-02 |
| KR100875629B1 (en) | 2008-12-26 |
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