WO2009079903A1 - Procédé et dispositif de détection colorimétrique à injection de flux pour l'azote ammoniacal - Google Patents
Procédé et dispositif de détection colorimétrique à injection de flux pour l'azote ammoniacal Download PDFInfo
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- WO2009079903A1 WO2009079903A1 PCT/CN2008/001334 CN2008001334W WO2009079903A1 WO 2009079903 A1 WO2009079903 A1 WO 2009079903A1 CN 2008001334 W CN2008001334 W CN 2008001334W WO 2009079903 A1 WO2009079903 A1 WO 2009079903A1
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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
- G01N21/75—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
Definitions
- the invention relates to a flow injection ammonia nitrogen colorimetric detection method for detecting ammonia nitrogen content in water or solution or on-line monitoring of ammonia nitrogen content, and belongs to the field of chemical analysis and water environment monitoring and analysis.
- Ammonia is nitrogen in the form of non-ionic ammonia (NH 3 ) or ionic ammonia (NH 4 +). When ammonia is dissolved in water, a part of ammonia reacts with water to form ammonium ions, and part of it forms hydrated ammonia (non-ionic ammonia). Therefore, it is collectively referred to as ammonia nitrogen.
- ammonia is widely present in rivers and lakes and seas, usually as decomposition products of nitrogen-containing organic matter.
- ammonia in water can be converted to nitrite.
- the nitrite present in the water is reduced to ammonia by the action of microorganisms, and even continues to be converted to nitrate.
- the ammonia nitrogen in the aqueous solution is nitrogen in the form of free ammonia (or nonionic ammonia, N) or ionic ammonia (NH 4 + ).
- N nonionic ammonia
- NH 4 + ionic ammonia
- ammonia nitrogen in water is an indicator of the degree of contamination of water bodies by nitrogen-containing organic matter and must be strictly controlled.
- fertilizer production nitric acid, coking, gas, nitrocellulose, rayon, synthetic rubber, calcium carbide, dyes, varnishes, caustic soda, electroplating and petroleum extraction, and petroleum product processing are all major sources of ammonia pollution.
- ammonia nitrogen content in industrial discharges and water bodies such as rivers and lakes is very important to carry out on-line monitoring of ammonia nitrogen content in industrial discharges and water bodies such as rivers and lakes. It can quickly analyze industrial emissions and water bodies such as rivers and lakes, and provide data on the instantaneous content of ammonia nitrogen in water to take corresponding measures to ensure enterprises.
- the ammonia nitrogen content of water bodies such as discharge standards and rivers and lakes is within the safety index.
- methods for measuring ammonia nitrogen mainly include spectrophotometric colorimetric method using acid salicylic acid-hypochlorite or iodine mercury (Nessler's method), acid-base neutralization titration method and ion electrode method.
- Nessler colorimetry is a classic method for the determination of ammonia and is listed as a standard analytical method by many countries.
- An alkaline solution of mercury iodide and potassium iodide reacts with ammonia to form a reddish brown colloidal compound which is strongly absorbed over a wide wavelength.
- the reaction of the Ness reagent with ammonia is actually a precipitation reaction.
- a sample having a turbid or color sample, a metal ion and an organic substance which are precipitated under alkaline conditions may be subjected to pre-treatment by coagulation sedimentation or steam distillation, and then quantified, and there is also a reagent toxicity and method. The sensitivity is not enough.
- the salicylic acid-hypochlorite colorimetric method is the reaction of ammonium with phenol and hypochlorous acid ions to form a blue compound in the presence of sodium nitroferricyanide. This type of reaction is called the Berthelot reaction and has a maximum at a wavelength of 697 nm. absorb.
- sodium hypochlorite is unstable and requires current use, so it is not suitable for unattended online instruments.
- the acid-base titration method requires heating and distillation of the water sample, and the released ammonia is absorbed by the boric acid solution, and the methyl red-methylene blue is used.
- the indicator, the ammonium in the distillate is titrated with an acid standard solution.
- the measurement method is cumbersome and the measurement is time consuming. When the water sample contains a substance which can be distilled under such conditions and can react with the acid at the time of titration, the measurement result will be made high.
- the object of the present invention is to provide a method for detecting ammonia nitrogen by flow injection with simple operation, quick and reliable operation, non-toxic reagent and low running cost, and a flow injection ammonia nitrogen detecting device dedicated to the method, thereby overcoming the traditional Nessler reagent spectrophotometry.
- the ammonia nitrogen detection methods such as salicylic acid-hypochlorite spectrophotometry and ammonia gas sensing electrode method have the disadvantages of cumbersome operation, toxic reagents or long-term preservation of reagents, and automatic on-line detection of NH 3 -N.
- the method for detecting ammonia nitrogen by flow injection is as follows - a concentration of 0.01 to 0.03 mol of NaOH solution is used as a release liquid, and the release liquid is injected into a capillary system connected with a gas-liquid separator, the gas-liquid separator containing samples and ventilation a deep groove in contact with the membrane; a quantitative water sample is injected into the capillary path of the release liquid to form a sample strip; and the sample strip is circulated by the pump in the capillary-gas-liquid separator flow path system by pumping, and in the flow After passing through the deep groove of the gas-liquid separator, ammonia gas is released and rises to the notch, and then passes through the gas permeable membrane, and the accepting liquid containing the acid-base indicator in the capillary groove on the other side of the film is absorbed into ammonium ions, so that the acid-base indicator Discoloration, the sample strip is continuously circulated to release ammonia, and the accepting solution that absorbs ammonia is transported to the flow
- the quantitative water sample can be injected into the circulating carrier liquid through the injection valve at intervals, and a plurality of sample strips are arranged in the circulation capillary-gas-liquid separator flow path to make the quantitative water sample be separated in the release liquid. Mix and accelerate the release and enrichment of ammonia.
- the acid-base indicator of the accepting liquid indicated by the acid-base indicates a slightly acidic acidic bromo-perphenol blue solution.
- the NaOH diluted solution is used as the ammonia releasing liquid of the sample to be tested and the carrier liquid is carried, and the ammonium ion in the sample reacts with the hydroxide to form ammonia gas, ⁇ + ⁇ 3 + ⁇ 2 0 .
- the water sample circulates with the carrier fluid and releases ammonia gas when passing through the gas-liquid separator, and passes through the gas permeable membrane into the receiving liquid and is absorbed into the ammonium ion by the acid-base indicator solution (hereinafter referred to as the receiving liquid), and the receiving liquid follows
- the ammonium ion increases and the alkalinity increases.
- the acid-base indicator bromene blue changes from yellow-green to blue, and the blue color becomes darker as the ammonium ion concentration increases, and is linear. Therefore, it can be irradiated with 560 nm wavelength light, and photoelectric conversion
- the measured value of the light-transmitting light voltage of the receiving liquid is obtained, and a response curve having a corresponding peak height is obtained, and the ammonia nitrogen concentration in the water sample is calculated by comparing with the measured value of the known standard.
- the present invention designs a dedicated flow injection ammonia nitrogen detecting device.
- the flow injection ammonia nitrogen detecting device comprises a gas-liquid separator, a photoelectric detection flow cell, a release liquid transfer pump P2, a water sample transfer pump Pl, a receiving liquid injection pump P3, a six-way injection valve VI and a seven-way reversing valve V2 through a capillary tube.
- the gas-liquid separator is provided with a deep-slot ammonia release tank, and the upper mouth of the ammonia release tank is sequentially provided with a gas permeable membrane and a liquid tank plate; the inner bottom surface of the deep tank of the ammonia release tank is provided with a capillary of a discharge liquid a guiding groove, the two ends of the groove are respectively provided with inlet and outlet nozzles; the lower surface of the groove plate is provided with a receiving liquid capillary groove with an opening downward and two ends at the inlet and outlet, wherein the outlet is connected Connected to the photoelectric colorimetric flow cell; a sampling loop S is connected between the interfaces 2 and 5 of the six-way injection valve VI, and the interface 4 is connected to the inlet nozzle of the ammonia release liquid capillary groove, and the interface 1 is water sample waste.
- the interface 6 is a water sample inlet
- the interface 3 is connected to the interface 5 of the seven-way valve V2
- the interface 1 of the seven-way valve V2 is connected to the receiving liquid inlet of the slot plate
- the interface 2 is connected with the injection pump P3
- the interface 3 is the receiving liquid inlet
- the interface 4 is the release liquid inlet
- the interface 6 is connected to the outlet connection of the carrier liquid capillary groove of the ammonia release tank by the release liquid transfer pump P2
- the interface 7 is the release liquid Waste liquid outlet.
- a support plate is disposed between the upper mouth of the ammonia release tank and the gas permeable membrane, and the support plate is provided with a through hole which matches the capillary sulcus of the receiving plate of the groove plate; Supports the gas permeable membrane and allows the ascending ammonia to pass.
- the device can first send the water sample into the quantitative sampling ring S of the sample valve VI through the water sample pump P1; the receiving liquid is injected into the receiving liquid groove and the flow cell of the gas-liquid separator slot plate by the injection pump P3; Conveying, sending the release liquid into the capillary channel of the release liquid and the capillary groove of the ammonia release tank; switching the valve VI to connect the sampling ring into the flow path of the release liquid; switching the valve V2 to form a loop of the release liquid capillary path
- the discharge liquid circulates under the action of the pump P2; thus, under the action of the pump P2, the water sample in the sampling ring forms a sample strip which circulates with the release liquid and continuously diffuses to the release liquid, and flows through the gas and liquid.
- the ammonia in the sample is released and rises due to the sudden expansion of the deep groove type airlift tank above the groove, and is absorbed by the receiving liquid in the groove of the groove plate through the gas permeable membrane, and the acid-base indicator is discolored.
- the syringe pump is pushed, and the discolored liquid is sent to the flow cell to measure the ammonia content in the sample.
- the outlet end of the receiving capillary channel extends through the through hole to the upper surface of the slot plate to form an open upward capillary groove, and the groove end is expanded into a wide groove.
- a gas permeable membrane and a cover plate are arranged on the upper side of the trough plate, and a lower surface of the cover plate is provided with a gas collecting groove which is opposite to the wide groove notch on the surface of the groove plate, and the gas collecting groove is provided with a row which is open to the atmosphere. Stomata.
- the fine bubbles When the fine bubbles are present in the receiving liquid, the fine bubbles rise from the lower surface groove of the groove plate to the groove on the upper surface, and the bubbles rise at the wide groove, and rise to the gas permeable membrane above the groove plate to rise to The gas collecting groove of the cover plate is discharged into the atmosphere from the vent hole, so that the phenomenon that the detection accuracy is affected by the bubble entering the photoelectric flow cell can be blocked.
- the device is provided with 1 ⁇ 3 solenoid valves for the conversion of the water sample and the standard sample in the connecting line of the injection valve VI interface 6 and the water raft.
- the release tank in the gas-liquid separator is a deep tank type, and ammonia gas released from the tank bottom groove is diffused upward through the deep groove, and then enters the receiving liquid system through the gas permeable membrane. Since the gas permeable membrane can only be ventilated and cannot be permeable to water, further ensure the separation of the ammonia gas and the liquid; the deep groove keeps the gas permeable membrane away from the sample in the groove, and prevents the particulate impurities in the sample from blocking the pores of the gas permeable membrane.
- the detecting device can realize the automatic online ammonia nitrogen detection by automatically controlling each valve according to a predetermined program through an automatic control system.
- the present invention adopts a flow injection analysis technology (FIA) and a dedicated detection device, using sodium hydroxide as a release liquid, and a slightly acidic acid-base indicator distilled water as a receiving liquid to realize automatic N3 ⁇ 4-N On-line measurement, the detection process is simple and fast, the detection data is accurate and reliable, and the water sample used for one injection is only 50 ⁇ 1 ⁇ 1 ⁇ 1, the amount of reagents consumed is very small, the operation cost is low, the reagent is non-toxic, and there is no emission pollution.
- FFA flow injection analysis technology
- Figure 1 (1) and Figure 1 (2) are the flow charts of the injection state and cycle enrichment state of the flow injection ammonia nitrogen colorimetric detection system, respectively.
- FIG. 2 is a schematic perspective view of a gas-liquid separator.
- Figure 3 is a schematic cross-sectional view of a gas-liquid separator.
- Figure 4 is a cross-sectional view of A-A.
- Figure 5 is a cross-sectional view taken along line B-B.
- Figure 6 is a schematic diagram showing the flow structure of a flow injection ammonia nitrogen colorimetric detection device system.
- Figure 6 (1) and Figure 6 (2) show the switching states of valves VI and V2 in Figure 6, respectively.
- Figure 7 is a schematic flow chart showing the flow of a flow injection ammonia nitrogen colorimetric detection device comprising a standard system.
- P1 water sample transfer pump
- P2 release liquid transfer pump
- P3 receiving liquid injection pump.
- Figure 1 (1) and Figure 2 (2) both show that the upper part is the color-receiving liquid capillary system and the lower part is the release liquid hair.
- the thin piping system is connected by a gas-liquid separator.
- Figure 1 (1) shows that the system is in the injection state, the receiving liquid is injected into the capillary by the syringe pump and passes through the capillary groove (above the gas permeable membrane) in the upper part of the gas-liquid separator, and flows into the flow cell, and flows out from the flow cell to accept
- the liquid fills the upper capillary system and the syringe pump stops.
- the peristaltic pump pumps the release liquid (diluted NaOH) through the switching valve into the lower piping system and flows in the direction of the arrow to the end.
- the water sample is cut into the piping through the injection valve to form a sample strip.
- Figure 1 (2) shows that the system is in an enriched state, the switching valve makes the lower pipeline a closed system, and the release liquid circulates.
- the ammonia in the water rises through the deep groove and It is absorbed by the receiving liquid through the gas permeable membrane, and as the sample is continuously circulated, the ammonia is enriched by the retained receiving liquid.
- the enlarged portion of the figure shows that the lower sample strip is diffused in the flowing release liquid, and the release of ammonia (NH 3 ) in the sample rises to the gas permeable membrane and enters the receiving liquid above the membrane.
- the receiving liquid is pushed to the flow cell by a syringe pump for photoelectric detection, and a peak height curve is obtained, and the ammonia content is converted.
- 2 to 5 show the structure of an embodiment of the gas-liquid separator.
- the gas-liquid separator is sequentially connected from the bottom to the top by the ammonia release tank 13, the support plate 15, the gas permeable membrane 16, the groove plate 17, the gas permeable membrane 16', and the cover plate 18, and the ammonia release tank 13 is provided.
- the liquid inlet and outlet nozzles 11, 10 are provided, the tank plate 17 is provided with receiving liquid inlet nozzles 12 and 14, and the cover plate 18 is provided with a venting opening 19.
- the internal structure of the separator can be seen from Figure 3.
- the ammonia release tank 13 is provided with a deep groove 23, and the bottom surface of the tank is provided with a discharge liquid capillary guide groove 24 (see Fig. 5).
- One end of the groove is connected with an inlet nozzle 11, and the other end is connected to the outlet nozzle 10.
- the lower side of the gas permeable membrane 16 is provided with a support plate 15 for supporting the film, and the support plate is provided with a through hole 25.
- the lower surface of the groove plate 17 is provided with a receiving liquid groove 21, and the upper surface is provided with an exhaust groove 22 which communicates with the through hole 26.
- a through hole 25 is formed between the groove plate 17 and the cover plate 18 to provide a gas permeable membrane 16'.
- the separator is connected to the release liquid capillary system through the nozzles 11, 10, and is connected to the receiving liquid capillary system through the nozzles 12, 14.
- the ammonia gas is released upward from the groove 24, rises to the upper port of the deep groove 23, and passes through the through hole 25 of the support plate 15 and penetrates through the gas permeable membrane 16
- the liquid receiving groove 21 of the groove plate 17 is absorbed by the receiving liquid.
- the receiving liquid If the receiving liquid contains microbubbles, the receiving liquid passes through the hole 26, and the microbubbles therein rise to the groove 22, and enter the gas collecting groove 20 through the gas permeable membrane 16' while passing through the gas permeable membrane on the lower side of the gas collecting tank 20. And discharge the system from the vent 19 .
- Fig. 6 shows the system flow structure of the flow injection ammonia nitrogen colorimetric detecting device. The working process of the ammonia nitrogen detecting device of the device is described below with reference to Fig. 6 as follows:
- V2 turn to the B state as shown in Figure 6, the peristaltic pump P2 is pumped, release liquid presses the flow path: release liquid - V2 interface 4 - interface 5 - VI interface 3 - interface 4 - gas-liquid separator - creep Pump P2 - V2 interface 6 - Interface 7 - Waste bottle, wash separator residual H 3 , seconds.
- Syringe pump P3 advance, make the receiving liquid from the syringe pump - V2 interface 2 - interface 1 - gas-liquid separator - flow tank a waste liquid bottle, until the photoelectric voltage returns to the baseline and maintain for 20 seconds, the cleaning is completed.
- V2 is turned to A state as shown in Fig. 6 (2), P2 is stopped, P1 is moved, 60 seconds, water sample is from water sample bottle - VI interface 6 - interface 5 - interface 2 - interface 1 - creep Pump P1 - waste bottle.
- the water sample is filled with a sampling ring S.
- V2 is turned to the A state as shown in Fig. 6 (2), the release liquid forms a closed system, the pump P2 continues to move, and the release liquid pushes the water sample to flow in the following flow path for 3 seconds to make the water sample
- the ammonia in the gas is released and enriched into the receiving liquid:
- V2 interface 5 V2 interface 6—peristaltic pump P2
- V2 stops, after 4 seconds, VI is still in the state, V2 goes to the B state, and the cycle ends.
- the pump P3 is propelled, and according to the injection pump P3—V2 interface 2—interface 1—gas-liquid separator-flow cell-waste bottle, the receiving liquid absorbed by ammonia in the gas-liquid separator is pushed into the photoelectric colorimetric flow cell, and the measurement is performed. Photoelectric light pressure, baseline and peak were measured, and ammonia content was calculated.
- Fig. 7 is a flow chart of an ammonia nitrogen flow injection detecting device including a standard measuring system, which is a three-way solenoid valve V3, V4, V5 added to the system of Fig. 6.
- Preparation of the release solution Weigh 0.8g of analytically pure sodium hydroxide, dissolve it in 100ml of water, add water to 1000ml capacity and shake the line. Made of 0.02M NaOH solution
- Preparation of the receiving solution Weigh 50mg of bromothymol blue, placed in a small beaker; add 8mL of absolute ethanol to dissolve, transfer to a 1000ml volumetric flask; add water to nearly 1000ml, add 0.02M NaOH to brownish yellow (pH-6.7) , dilute to 1000ml with water.
- Ammonia detection is carried out according to the above washing, injection, sample cutting, cycle enrichment, and measurement operation procedures.
- the standard and sample 1 were measured (set enrichment time: 100 seconds, rest time: 5 seconds, number of cleanings: 12 times), and the data is as follows:
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Abstract
La présente invention concerne un procédé de détection colorimétrique par injection de flux pour l'azote ammoniacal. Le liquide de dégagement est une solution de NaOH dans une plage de concentration de 0,01-0,03 mol injectée dans un système capillaire relié à un séparateur gaz-liquide comportant une rainure profonde. Un échantillon de liquide de quantification injecté dans le liquide de dégagement à l'intérieur du système capillaire vient former une bande échantillon. Celle-ci s'écoule de façon circulaire, accompagnée du liquide de dégagement pompé dans le système capillaire. Elle dégage du NH3 pendant l'écoulement au niveau de la rainure profonde du séparateur gaz-liquide. Le NH3 se diffuse jusqu'à la sortie de la rainure et subit une perméation au travers d'une membrane osmotique puis modifie la couleur de l'indicateur d'acidité-alcalinité dans une fente capillaire. L'écoulement en cercles de la bande échantillon se prolonge en continu jusqu'à la fin du dégagement de NH3. Le NH3 absorbé dans liquide accepteur est pompé par une pompe d'injection dans une cuve à circulation d'un colorimètre puis soumis à un rayonnement lumineux d'une longueur d'ondes de 560 nm. La concentration de l'azote ammoniacal dans le liquide échantillon est détectée par conversion photoélectrique.
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JP2010539993A JP5000766B2 (ja) | 2007-12-25 | 2008-07-17 | フローインジェクションによるアンモニア態窒素の比色検出方法及びその装置 |
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CN2007101923358A CN101226153B (zh) | 2007-12-25 | 2007-12-25 | 流动注射氨氮比色检测装置 |
CN200710192335.8 | 2007-12-25 |
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WO2009079903A1 true WO2009079903A1 (fr) | 2009-07-02 |
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PCT/CN2008/001334 WO2009079903A1 (fr) | 2007-12-25 | 2008-07-17 | Procédé et dispositif de détection colorimétrique à injection de flux pour l'azote ammoniacal |
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WO (1) | WO2009079903A1 (fr) |
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2007
- 2007-12-25 CN CN2007101923358A patent/CN101226153B/zh not_active Expired - Fee Related
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2008
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CN101788493B (zh) * | 2010-01-19 | 2011-07-27 | 成都海兰天澄科技有限公司 | 一种水质中氨氮测试方法 |
CN103076320A (zh) * | 2012-12-28 | 2013-05-01 | 重庆川仪分析仪器有限公司 | 氨氮检测器及检测方法 |
CN103076320B (zh) * | 2012-12-28 | 2015-07-15 | 重庆川仪分析仪器有限公司 | 氨氮检测器及检测方法 |
CN105352948A (zh) * | 2015-10-20 | 2016-02-24 | 深圳市清时捷科技有限公司 | 一种水质在线检测仪液路装置及检测方法 |
CN106745629A (zh) * | 2016-12-22 | 2017-05-31 | 重庆淼森环保工程有限公司 | 一种废水中的氨氮处理装置 |
CN110441539A (zh) * | 2019-08-21 | 2019-11-12 | 东软威特曼生物科技(沈阳)有限公司 | 用于固体直热式或空气浴式反应盘的反应杯架及全自动生化分析仪 |
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JP5000766B2 (ja) | 2012-08-15 |
CN101226153A (zh) | 2008-07-23 |
CN101226153B (zh) | 2010-09-08 |
JP2011508227A (ja) | 2011-03-10 |
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