CN101592670A - Automatic analysis quantitatively measure method and automatic analysis quantitatively measure apparatus - Google Patents
Automatic analysis quantitatively measure method and automatic analysis quantitatively measure apparatus Download PDFInfo
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- G—PHYSICS
- G01—MEASURING; TESTING
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- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/18—Water
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- 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
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- G—PHYSICS
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- 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
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Abstract
The present invention relates to total nitrogen content and total phosphorus total content automatic analysis quantitatively measure apparatus and automatic analysis quantitatively measure method, this method adopts the Continuous Flow Analysis method, comprise: utilize air (A) that the sample (S) of sampling is separated, then with the sample and the reagent (B that separate, C) be injected into continuously together and carry out in the pipe (10) quantitatively and mix, after in reaction concetrated pipe (4), the mixed liquor that obtains being decomposed, use detecting device (5) to analyze by usual way, this method is sampled to sample (S) at interval with certain hour, supply to pipe (10), in reaction concetrated pipe (4), described mixed liquor was stopped 10～30 minutes, carry out UV irradiation time described mixed liquor of heating and decomposition under 80～90 ℃ temperature, successively the described 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 total content.
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 is, in pipe, import sample continuously with certain flow, and gases such as injection air or inert gas in pipe regularly, liquid is carried out bubble to be separated, 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) by the detecting instruments such as spectrophotometer that flow cell (Flow Cell) is housed.
The special permission of [patent documentation 1] Japan discloses flat 8-285835 number
Open 2006-234601 number of [patent documentation 2] Japan special permission
Open 2006-208344 number of [patent documentation 3] Japan special permission
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 do not need, can in long-time span, carry out water quality measurement at interval automatically with certain hour by staff.
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 by 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 for, utilize gas that the sample of sampling is separated, then the sample of separating is injected into continuously with reagent and carries out in the pipe quantitatively and mixing, after in the reaction concetrated pipe, the mixed liquor that obtains being decomposed, use detecting device to analyze by usual way, this method is sampled to sample at interval with certain hour, supply to pipe, in the reaction concetrated pipe, described mixed liquor was stopped 10～30 minutes, under 80～90 ℃ temperature, carry out the described mixed liquor of heating and decomposition in ultraviolet ray (UV) irradiation, successively the described 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, be a kind ofly to utilize gas to separate sample by automatic sampler sampling by volume pump, and the sample separated is injected into continuously with reagent 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, described mixed liquor stopped 10～30 minutes, heated mixed liquor when carrying out the UV irradiation under 80～90 ℃ temperature; Automatic sampler was sampled to sample repeatedly with the time interval of heat time heating time of surpassing above-mentioned reaction concetrated pipe; In time beyond injecting sample, in pipe, supply with water.
As mentioned above, 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 be 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, be a kind ofly to utilize air A to separate sample S by automatic sampler 2 sampling by volume pump 3, in being injected into pipe 10 continuously, reagent B, C carry out quantitative, mixing, after in reaction concetrated pipe 4, above-mentioned mixed liquor being decomposed, the measuring equipment that adopts usual ways to analyze by 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 was sampled to sample S repeatedly with the time interval that surpasses 4 heat time heating times of above-mentioned reaction concetrated pipe; In time beyond injecting sample, in pipe 10, supply with pure water W.
Automatic sampler 2 absorbs sample from the sample collecting portion of overflowing under unlatching of absorption of sample pump and while sample electrovalve opened state.Sampling operation approximately continues 5～10 minutes, and after this, electrovalve cuts out, and begins to absorb 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 bubble to the mixed liquor that supplies to sample S in the pipe 10 and reagent B, C and separate.The mixed liquor of sample S and reagent B, C mixes by the overcurrent effect of each separating element of being separated by air A.In addition, pipe 10 can be wound in spiral form, the conduction immixture when utilizing mixed liquor by helical inside makes its mixing.
Importing to the sample S that manages in 10 by 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 mixed liquor that contains acid potassium persulphate.In addition, also can use inert gas as separating gas A.
The structure of reaction concetrated pipe 4 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 as shown in Figure 2.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, there is no 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 by the mixed liquor in the UV irradiation light 42 irradiation quartz ampoules 41 except making mixed liquor.Therefore, after heating 10～30 minutes under 80～90 ℃ the lower temperature, the mixed liquor in the quartz ampoule 41 will become the back and analyze required decomposed solution.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, by 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 less than 1mm, when sample S or reagent B, C flow through quartz ampoule 41, latch up phenomenon occurs easily, if but internal diameter surpasses 5mm, with increasing the consumption of reagent B, C, cause 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 by 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 by 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 by gas A, and inject ascorbic acid reagent G and decomposed solution R2 therein, and the cyan pigment of the molybdenum green grass or young crops of color development imported the flow cell 52 of spectrophotometer 50, near the spectrophotometric with 880nm carries out colorimetric measurement.
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.
By 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 automatically measure repeatedly in long-time span later on.The continuous coverage cycle can reach more than 1 week, sustainable running 1 year.
In addition, the sampling time interval of sample S is not particularly limited, as long as surpass residence time (10～300 minutes) in reaction concetrated pipe 4, for example, can be every 30 minutes, or, also can be set at the longer time every 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 it is very short that the time interval is provided with, just need to adjust the time interval, after making the sample S of front in detecting device 5, finish detection, the sample S of back is rested in the reaction concetrated pipe 4, or adjust the length of pipe 10.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, finish 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 by the pure water W and the titer of reagent modulation.Above-mentioned basic measurement or titer are measured and can be finished when carrying out plant maintenance, and for the situation of carrying out unmanned operation in long-time span, also programmed is in advance finished 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 by volume pump 3.In addition, W controls by 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.By flowing of pure water W, when each the measurement, realize the effect of washing path.
Embodiment 1
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 concentration as the tripolyphosphate aqueous solution of sample respectively.The result is as shown in table 1.
Table 1
As can be seen from Table 1, heating-up temperature is high more, stand-by time is long more, and 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.
Embodiment 2
Prepare all cpds shown in the table 2 as sample, adopt the reagent identical and react concetrated pipe and analyze with the foregoing description 1.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 |
As can be seen 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, a kind of 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 continuously with reagent and carries out in the pipe quantitatively and mixing, after in the reaction concetrated pipe, the mixed liquor that obtains being decomposed, in detecting device, be divided into two parts by divider, then total nitrogen content and total phosphorus content are carried out parallel parsing, it is characterized in that:
At interval sample is sampled with certain hour, supply to pipe;
In the reaction concetrated pipe, described mixed liquor was stopped 10～30 minutes, when carrying out the UV irradiation under 80～90 ℃ temperature the described mixed liquor of heating and decomposition;
Successively the described 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, a kind of total nitrogen content and total phosphorus content automatic analysis quantitatively measure apparatus, this equipment is a kind ofly to utilize gas to separate sample by automatic sampler sampling by volume pump, and the sample separated is injected into continuously with reagent 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 by divider, total nitrogen content and total phosphorus content are carried out the total nitrogen content and the total phosphorus content automatic analysis quantitatively measure apparatus of parallel parsing, it is characterized in that:
In the reaction concetrated pipe, described mixed liquor was stopped 10～30 minutes, under 80～90 ℃ temperature, heat described mixed liquor when carrying out the UV irradiation;
Described automatic sampler was sampled to sample repeatedly with the time interval of heat time heating time of surpassing described reaction concetrated pipe;
In time beyond injecting sample, in pipe, supply with water.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR10-2008-0050164 | 2008-05-29 | ||
| KR1020080050164A KR100875629B1 (en) | 2008-05-29 | 2008-05-29 | Automatic analysis quantitative monitoring method and automatic analysis quantitative monitoring device |
| KR1020080050164 | 2008-05-29 |
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| Publication Number | Publication Date |
|---|---|
| CN101592670A true CN101592670A (en) | 2009-12-02 |
| CN101592670B CN101592670B (en) | 2012-09-19 |
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| CN2009101300568A Expired - Fee Related CN101592670B (en) | 2008-05-29 | 2009-04-03 | Automatic analysis quantitative measurement method and automatic analysis quantitative measuring apparatus |
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|---|---|
| JP (1) | JP2009288228A (en) |
| KR (1) | KR100875629B1 (en) |
| CN (1) | CN101592670B (en) |
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| CN102253232A (en) * | 2010-05-21 | 2011-11-23 | 北京吉天仪器有限公司 | Automatic analyzer and analysis method for water soluble total phosphorus |
| CN102636446A (en) * | 2012-05-09 | 2012-08-15 | 江南大学 | On-line detection device for detecting total nitrogen and total phosphorus through ozone ultraviolet collaborative oxidative digestion |
| CN104142323A (en) * | 2014-07-04 | 2014-11-12 | 中国热带农业科学院橡胶研究所 | Method for simultaneously measuring content of nitrogen and phosphorus of plant |
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| JP3496779B2 (en) * | 1995-04-17 | 2004-02-16 | ブラン・ルーベ株式会社 | Method and apparatus for automatic analysis of total nitrogen and total phosphorus |
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| CN1632525A (en) * | 2004-12-19 | 2005-06-29 | 中国海洋大学 | On-line photocatalysis total phosphorus and total nitrogen counteraction analyzer |
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- 2008-05-29 KR KR1020080050164A patent/KR100875629B1/en active IP Right Grant
- 2008-06-03 JP JP2008145560A patent/JP2009288228A/en active Pending
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- 2009-04-03 CN CN2009101300568A patent/CN101592670B/en not_active Expired - Fee Related
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| CN102636446A (en) * | 2012-05-09 | 2012-08-15 | 江南大学 | On-line detection device for detecting total nitrogen and total phosphorus through ozone ultraviolet collaborative oxidative digestion |
| 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 |
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| CN110646561A (en) * | 2019-10-10 | 2020-01-03 | 杭州浅海科技有限责任公司 | Flow injection method for injecting reagent at fixed time |
| CN110646561B (en) * | 2019-10-10 | 2022-03-08 | 杭州浅海科技有限责任公司 | Flow injection method for injecting reagent at fixed time |
| CN114981664A (en) * | 2020-01-27 | 2022-08-30 | 必艾路泰克株式会社 | Flow analysis method and flow analysis device |
| CN114981664B (en) * | 2020-01-27 | 2023-02-03 | 必艾路泰克株式会社 | Flow analysis method and flow analysis device |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101592670B (en) | 2012-09-19 |
| JP2009288228A (en) | 2009-12-10 |
| KR100875629B1 (en) | 2008-12-26 |
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