Disclosure of Invention
The invention aims to provide an analysis system and method for automatic total nitrogen monitoring.
The analysis system for automatically monitoring total nitrogen comprises a gas-liquid driving system, a chemical reaction system and an optical detection system, wherein the gas-liquid driving system is connected with the chemical reaction system and used for inputting gas and liquid participating in reaction into the chemical reaction system, the chemical reaction system is connected with the optical detection system and used for respectively mixing the gas and the liquid participating in reaction in sequence to obtain mixed solution and inputting the mixed solution into the optical detection system, and the optical detection system is used for detecting the absorbance of the mixed solution.
The invention relates to an analysis system for automatically monitoring total nitrogen, wherein a gas-liquid driving system comprises a liquid selection device, a peristaltic pump, a liquid inlet pipe, an R1 pump pipe, an R2 pump pipe, an R3 pump pipe, an R4 pump pipe, an R5 pump pipe, a first air pump pipe and a second air pump pipe, the liquid selection device is connected with the liquid inlet pipe, the liquid inlet pipe is connected with a chemical reaction system, the R1 pump pipe, the R2 pump pipe, the R3 pump pipe, the R4 pump pipe and the R5 pump pipe are respectively connected with an R5 container for containing reagent R5, the R5 pump pipe, the first air pump pipe, the second air pump pipe, the R5 pump pipe and the R5 pump pipe, the liquid selection device is used for automatically sucking liquid participating in reaction, and the peristaltic pump is used for inputting gas and the liquid participating in the reaction into the chemical reaction system.
The invention discloses an analysis system for automatically monitoring total nitrogen, wherein a liquid selection device is a multi-way valve or an electric control liquid valve group or an automatic sample injector, and the multi-way valve or the electric control liquid valve group or the automatic sample injector is connected with a peristaltic pump through a liquid inlet pipe.
The invention discloses an analysis system for automatically monitoring total nitrogen, wherein switching valves are respectively arranged on an R1 pump tube, an R2 pump tube, an R3 pump tube, an R4 pump tube and an R5 pump tube.
The invention discloses an analysis system for automatically monitoring total nitrogen, wherein a chemical reaction system comprises a first bubble injection device, a first online mixing coil, a first glass tee joint, a second online mixing coil, an online ultraviolet digestion device and a first online exhaust device, wherein a first inlet of the first bubble injection device is connected with an R1 pump pipe, a second inlet of the first bubble injection device is connected with a liquid inlet pipe, a third inlet of the first bubble injection device is connected with a first air pump pipe, an outlet of the first bubble injection device is connected with the first online mixing coil, the first online mixing coil is connected with a first inlet of the first glass tee joint, a second inlet of the first glass tee joint is connected with an R2 pump pipe, an outlet of the first glass tee joint is connected with the second online mixing coil, the second online mixing coil is connected with an inlet of the online ultraviolet digestion device, an outlet of the online ultraviolet digestion device is connected with an inlet of the first online exhaust device, the first outlet of first online exhaust apparatus connects first pump line, and the second outlet of first online exhaust apparatus connects the second pump line, and chemical reaction system still includes: the other end of a second pump pipe is connected with a first inlet of the second bubble injection device, a second inlet of the second bubble injection device is connected with an R3 pump pipe, a third inlet of the second bubble injection device is connected with a second air pump pipe, an outlet of the second bubble injection device is connected with a first inlet of the second glass tee joint, a second inlet of the second glass tee joint is connected with an R4 pump pipe, an outlet of the second glass tee joint is connected with the third online mixing ring, the third online mixing ring is connected with an inlet of the online low-temperature heating device, an outlet of the online low-temperature heating device is connected with a first inlet of the third glass tee joint, a second inlet of the third glass tee joint is connected with an R5 pump pipe, an outlet of the third glass tee joint is connected with the fourth online mixing ring, the fourth online mixing coil is connected with an inlet of a second online exhaust device, the upper end of the second online exhaust device is connected with a waste liquid bottle, the lower end of the second online exhaust device is connected with an inlet of a flow cell, the outlet end of the flow cell is connected with the waste liquid bottle through a waste liquid pump pipe, the detector is used for detecting the absorbance of liquid in the flow cell, and the waste liquid pump pipe passes through a peristaltic pump.
The invention discloses an analysis system for automatically monitoring total nitrogen, which further comprises a data processing system, a circuit control system and a software workstation, wherein the data processing system is connected with a detector, the circuit control system is connected with the data processing system, the detector, a peristaltic pump and a liquid selection device, and the software workstation is connected with the circuit control system.
The invention discloses an analysis method for automatic total nitrogen monitoring, which comprises the following steps: mixing a sample to be measured with an alkaline potassium persulfate solution, adding 20-60 g/L sodium tetraborate solution into the mixed solution, carrying out ultraviolet digestion reaction on the mixed solution, mixing the solution after the ultraviolet digestion reaction with 5-15 g/L sodium hydroxide solution for reaction, mixing the reacted solution with a hydrazine copper solution at 30-50 ℃, mixing the mixed solution with a color developing agent solution for reaction, and carrying out spectrum direct-reading measurement on the reacted solution at 500-700 nm.
The invention relates to an analysis method for automatically monitoring total nitrogen, wherein an alkaline potassium persulfate solution is a mixed solution of 30-70 g/L potassium persulfate and 5-15 g/L sodium hydroxide, a hydrazine copper solution is a mixed solution of 1-5 g/L hydrazine sulfate and 10-20 g/L copper sulfate, and a color developing agent solution is a mixed solution of 10-20 g/L sulfanilamide, 0.1-0.5 g/L (1-naphthyl) ethylenediamine hydrochloride, 0.05-0.1 g/L polyoxyethylene lauryl ether and 10-20% hydrochloric acid in percentage by volume.
The analysis system and method for automatically monitoring total nitrogen have the following advantages: by adopting the bubble injection technology, the mutual interference of different samples can be avoided, so that the samples are completely reacted, and the maximum sensitivity is achieved; the method adopts the full-steady-state detection, and has high accuracy and strong reliability; the adopted components are small and light in size, the whole reaction system is compact in structure and reasonable in layout, and daily maintenance and observation are facilitated; the reagent dosage is saved, and the secondary pollution is reduced.
Detailed Description
As shown in fig. 1 and 2, the analysis system for automatically monitoring total nitrogen of the present invention includes a gas-liquid driving system, a chemical reaction system, and an optical detection system, wherein the gas-liquid driving system is connected to the chemical reaction system, and is configured to input gas and liquid participating in a reaction into the chemical reaction system, the chemical reaction system is connected to the optical detection system, and is configured to sequentially mix the gas and the liquid participating in the reaction to obtain a mixed solution, and input the mixed solution into the optical detection system, and the optical detection system is configured to detect absorbance of the mixed solution.
The invention relates to an analysis system for automatically monitoring total nitrogen, wherein a gas-liquid driving system comprises a liquid selection device, a peristaltic pump, a liquid inlet pipe, an R1 pump pipe, an R2 pump pipe, an R3 pump pipe, an R4 pump pipe, an R5 pump pipe, a first air pump pipe and a second air pump pipe, the liquid selection device is connected with the liquid inlet pipe, the liquid inlet pipe is connected with a chemical reaction system, the R1 pump pipe, the R2 pump pipe, the R3 pump pipe, the R4 pump pipe and the R5 pump pipe are respectively connected with an R5 container for containing reagent R5, the R5 pump pipe, the first air pump pipe, the second air pump pipe, the R5 pump pipe and the R5 pump pipe, the liquid selection device is used for automatically sucking liquid participating in reaction, and the peristaltic pump is used for inputting gas and the liquid participating in the reaction into the chemical reaction system.
The invention discloses an analysis system for automatically monitoring total nitrogen, wherein a liquid selection device is a multi-way valve or an electric control liquid valve group or an automatic sample injector, and the multi-way valve or the electric control liquid valve group or the automatic sample injector is connected with a peristaltic pump through a liquid inlet pipe.
The invention discloses an analysis system for automatically monitoring total nitrogen, wherein switching valves are respectively arranged on an R1 pump tube, an R2 pump tube, an R3 pump tube, an R4 pump tube and an R5 pump tube.
The analysis system for automatic total nitrogen monitoring of the present invention, wherein,
the invention discloses an analysis system for automatically monitoring total nitrogen, which further comprises a data processing system, a circuit control system and a software workstation, wherein the data processing system is connected with a detector, the circuit control system is connected with the data processing system, the detector, a peristaltic pump and a liquid selection device, and the software workstation is connected with the circuit control system.
The invention discloses an analysis method for automatic total nitrogen monitoring, which comprises the following steps: mixing a sample to be measured with an alkaline potassium persulfate solution, adding 20-60 g/L sodium tetraborate solution into the mixed solution, carrying out ultraviolet digestion reaction on the mixed solution, mixing the solution after the ultraviolet digestion reaction with 5-15 g/L sodium hydroxide solution for reaction, mixing the reacted solution with a hydrazine copper solution at 30-50 ℃, mixing the mixed solution with a color developing agent solution for reaction, and carrying out spectrum direct-reading measurement on the reacted solution at 500-700 nm.
The invention relates to an analysis method for automatically monitoring total nitrogen, wherein an alkaline potassium persulfate solution is a mixed solution of 30-70 g/L potassium persulfate and 5-15 g/L sodium hydroxide, a hydrazine copper solution is a mixed solution of 1-5 g/L hydrazine sulfate and 10-20 g/L copper sulfate, and a color developing agent solution is a mixed solution of 10-20 g/L sulfanilamide, 0.1-0.5 g/L (1-naphthyl) ethylenediamine hydrochloride, 0.05-0.1 g/L polyoxyethylene lauryl ether and 10-20% hydrochloric acid in percentage by volume.
According to the technical scheme, the reaction is detected in a balanced state, bubbles are injected into the reaction system, so that the reaction is more sufficient, the maximum sensitivity can be achieved, the sample residue can be reduced, the reaction speed is high, the use amounts of the sample and the reagent are small, the generated waste liquid is less, the test accuracy is high, the integration degree is high, the size is small, the test result cannot be influenced by small changes of the reaction environment, and the method is more suitable for automatic monitoring of the total nitrogen in the water sample.
The invention adopts a continuous flow analysis technology and can be used for automatically monitoring the total nitrogen in the water quality of a water sample.
The technical scheme of the invention provides the total nitrogen analysis system and the chemical method which have the advantages of high analysis speed, high accuracy, less consumption of chemical reagents and samples, less generated waste liquid and small volume and are suitable for online monitoring.
The technical scheme of the invention can overcome the defects of complicated chemical reaction process, long analysis time, large consumption of samples and chemical reagents, large discharge amount of waste liquid, easy secondary pollution, complex structure of an analysis system, large volume and the like of the traditional system.
The analysis system for automatic total nitrogen monitoring of the present invention comprises a total of 6 parts:
(1) gas-liquid driving system
(2) Chemical reaction system
(3) Optical detection system
(4) Data processing system
(5) Circuit control system
(6) Software workstation
The gas-liquid driving system is used for inputting gas and liquid participating in reaction into an analysis system, and comprises:
(1) a liquid selection device: the selection of liquid is realized by adopting an electric control multi-way valve or an electric control liquid valve group or an automatic sample injector;
(2) a gas-liquid driving device: a multi-channel peristaltic pump is used as a liquid input leading-in device;
(3) and (4) a pump pipe.
The units and components of the system are suitable for total nitrogen testing of samples.
The chemical reaction system comprises a first bubble injection device 4, a first online mixing coil 5, a first glass tee joint 6, a second online mixing coil 7, an online ultraviolet digestion device 8, a first online exhaust device 9, a second bubble injection device 10, a second glass tee joint 11, a third online mixing coil 12, an online low-temperature heating device 13, a third glass tee joint 14, a fourth online mixing coil 15, a second online exhaust device 16, a first switching valve 20, a second switching valve 21, a third switching valve 22, a fourth switching valve 23, a fifth switching valve 24, a first air pump pipe 301, an inlet pipe 302, an R1 pump pipe 303, an R2 pump pipe 304, an R3 pump pipe 308, an R4 pump pipe 309, an R5 pump pipe 310, a second air pump pipe 307, a waste liquid pump pipe 311, a first pump pipe 305, and a second pump pipe 306. The pump tubes all pass through a peristaltic pump.
The chemical reaction system further includes: r1 container 25, R2 container 26, R3 container 27, R4 container 28, R5 container 29.
W1, W2 and W3 are waste liquids, and the waste liquids flow into a waste liquid bottle at last.
S, S1, S2, S3, QC and UP are respectively a sample, a standard solution 1, a standard solution 2, a standard solution 3, a quality control sample and pure water. Except that the sample S is a water sample which is directly collected, other solutions are collected from corresponding reagent bottles.
The reagent R1 is an alkaline potassium persulfate solution, namely a mixed solution of 30-70 g/L potassium persulfate and 5-15 g/L sodium hydroxide;
the reagent R2 is 20-60 g/L sodium tetraborate solution;
the reagent R3 is 5-15 g/L sodium hydroxide solution;
the reagent R4 is a hydrazine copper solution, namely a mixed solution of 1-5 g/L hydrazine sulfate and 10-20 g/L copper sulfate;
the reagent R5 is a mixture of 10-20 g/L sulfanilamide, 0.1-0.5 g/L (1-naphthyl) ethylenediamine hydrochloride, 0.05-0.1 g/L polyoxyethylene lauryl ether and 10-20% hydrochloric acid by volume percentage.
The optical detection system includes:
a flow cell 17 through which a sample to be tested passes, a light source 18, and a detector 19 for receiving a signal generated by the sample to be tested after absorbing light.
A data processing system: for processing of the detector data signals.
The circuit control system comprises: for circuit control of the analysis system.
And the software workstation is used for controlling the whole analysis system, transmitting an instruction to the circuit control system through a data line to realize the control of the whole system, transmitting the received data through the data line to process and analyze the data, and listing all results into a monitoring picture.
The working process of the analysis system for automatically monitoring the total nitrogen comprises the following steps:
the system collects a sample S through a pipeline of the liquid selection device 1, the sample S and a reagent R enter a chemical reaction system through a pump pipe under the pushing of a peristaltic pump 2, and continuously flow in a closed pipeline and generate a color reaction.
Wherein: air is introduced into the first air pump pipe 301 and the second air pump pipe 307 on the peristaltic pump 2, and enters the liquid pipeline to form bubbles, so that a reaction flow path is formed, wherein the sample S and the reagent R are regularly separated by the air bubbles at certain intervals.
The multi-way valve or the electric control liquid valve group or the automatic sample injector is sequentially connected in series with a liquid inlet pipe 302, a first bubble injection device 4, a first on-line mixing coil 5, a first glass tee joint 6, a second on-line mixing coil 7, an on-line ultraviolet digestion device 8 and a first on-line exhaust device 9 on the peristaltic pump 2 through pipelines.
A first air pump pipe 301 on the peristaltic pump 2 is connected with a first bubble injection device to introduce air G, and the other end of the first air pump pipe 301 is suspended in the air; the R1 container 25 is introduced into the flow path by the pump pipe through the first switching valve 20, the other end of the first switching valve 20 is connected with the pure water barrel, and the other end of the R1 pump pipe 303 is connected with the first bubble injection device 4; the R2 container 26 is introduced into the flow path by the R2 pump pipe 304 through the second switching valve 21, the other end of the second switching valve 21 is connected with the pure water barrel, and the other end of the R2 pump pipe 304 is connected with the first glass tee 6; the upper end of the first online exhaust device 9 is connected with a first pump pipe 305, the other end of the first pump pipe 305 is connected with a waste liquid bottle through a pipeline, and the lower end of the first online exhaust device 9 is connected with a second pump pipe 306.
The other end of the second pump pipe 306 is connected in series with a second bubble injection device 10, a second glass tee joint 11, a third on-line mixing coil 12, an on-line low-temperature heating device 13, a third glass tee joint 14, a fourth on-line mixing coil 15 and a second on-line exhaust device 16 in sequence through pipelines.
A second air pump pipe 307 on the peristaltic pump 2 is connected with the second bubble injection device 10 to introduce air G, and the other end of the second air pump pipe 307 is suspended in the air; the R3 container 27 is introduced into the flow path by the R3 pump tube 308 through the third switching valve 22, the other end of the third switching valve 22 is connected to the pure water tank, and the other end of the R3 pump tube 308 is connected to the second bubble injecting device 10; the R4 container 28 is introduced into the flow path by the R4 pump pipe 309 through the fourth switching valve 23, the other end of the fourth switching valve 23 is connected to the pure water tank, and the other end of the R4 pump pipe 309 is connected to the second glass tee 11; the R5 container 29 is introduced into the flow path by the R5 pump line 310 through the fifth switching valve 24, the other end of the fifth switching valve 24 is connected to the pure water tank, and the other end of the R5 pump line 310 is connected to the third glass tee 14; the upper end of the second online exhaust device 16 is connected with a waste liquid bottle, the lower end is connected with an inlet of the flow cell 17, and the outlet end of the flow cell 17 is connected with the waste liquid bottle through a waste liquid pump pipe 311.
A light source 18 and a detector 19 are connected to both ends of the flow cell 17.
Key components:
the first bubble injection means 4 and the second bubble injection means 10 are each a multi-channel device capable of injecting bubbles uniformly and introducing a sample or a reagent simultaneously.
The length ranges of the glass rings of the first online mixing coil 5 and the second online mixing coil 7 are both 0.5-1.0 m; the length ranges of the glass rings of the third online mixing coil 12 and the fourth online mixing coil 15 are both 1.0-2.0 m; the length range of the glass ring in the on-line low-temperature heating device 13 is 1.5-3.0 m; the length range of the glass ring in the online ultraviolet digestion device is 4.0-6.5 m.
The on-line low-temperature heating device 13 comprises a heating rod, heat insulation cotton sleeved outside the heating rod, a glass tube and a temperature measuring thermal resistor which are wound on the heating rod to form a heated reaction pipeline, and a temperature protection sleeve.
The online ultraviolet digestion device 8 is connected with a power supply by an ultraviolet lamp tube, an ultraviolet lamp holder, a glass ring in a reaction flow path. The ultraviolet lamp tube is arranged on the ultraviolet lamp holder, the glass ring is wound outside the ultraviolet lamp tube, and the ultraviolet lamp tube is connected with the power supply.
The inner diameters of the first air pump pipe 301, the liquid inlet pipe 302, the R1 pump pipe 303, the R2 pump pipe 304, the R3 pump pipe 308, the R4 pump pipe 309, the R5 pump pipe 310, the second air pump pipe 307, the waste liquid pump pipe 311, the first pump pipe 305 and the second pump pipe 306 are 0.51-1.30 mm.
The analysis method comprises the following steps:
the analysis method for automatically monitoring the total nitrogen is suitable for testing the total nitrogen:
mixing a sample to be measured with an alkaline potassium persulfate solution, adding 20-60 g/L sodium tetraborate solution into the mixed solution, carrying out ultraviolet digestion reaction on the mixed solution, mixing the solution after the ultraviolet digestion reaction with 5-15 g/L sodium hydroxide solution for reaction, mixing the reacted solution with a hydrazine copper solution at 30-50 ℃, mixing the mixed solution with a color developing agent solution for reaction, and carrying out spectrum direct-reading measurement on the reacted solution at 500-700 nm.
The alkaline potassium persulfate solution is a mixed solution of 30-70 g/L potassium persulfate and 5-15 g/L sodium hydroxide.
The hydrazine copper solution is a mixed solution of 1-5 g/L hydrazine sulfate and 10-20 g/L copper sulfate.
The color developing agent solution is a mixed solution of 10-20 g/L sulfanilamide, 0.1-0.5 g/L (1-naphthyl) ethylenediamine hydrochloride, 0.05-0.1 g/L polyoxyethylene lauryl ether and hydrochloric acid with the volume percentage content of 10% -20%.
The analysis system and method for automatically monitoring total nitrogen have the following advantages:
1. by adopting the bubble injection technology, the mutual interference of different samples can be avoided, so that the samples are completely reacted, and the maximum sensitivity is achieved;
2. the adopted full steady state detection technology has high accuracy and strong reliability;
3. the reaction ring in the system is made of glass with a large pipe diameter, has good trafficability and chemical inertia, is not easy to block, and has good trafficability to water samples with complex conditions;
4. the reaction system has the advantages that the adopted components are small and exquisite in size and light, the whole reaction system is compact in structure and reasonable in layout, and daily maintenance and observation are facilitated;
5. the system adopts a multi-way valve or an electric control liquid valve group or an automatic sample injector to realize the sequential introduction of standard series solution, quality control solution, sample and pure water (cleaning water), and the switching is convenient;
6. and the switching valve is adopted to freely switch the reagent and the pure water, so that the reagent dosage is saved, and the secondary pollution is reduced.
The technical scheme of the invention provides the automatic total nitrogen monitoring and analyzing system and the method which have the advantages of high analyzing speed, high accuracy, low reagent and sample consumption, less generated waste liquid and small volume and can completely replace the traditional method.
The analysis system of the invention collects the standard solution S1, the standard solution S2, the standard solution S3, the quality control sample QC and the sample S (water sample) in turn through the pipeline of the liquid selection device 1, and switches to the pure water UP to carry out the pipeline solution transportation and cleaning after the collection is finished each time. The standard solution S1, the standard solution S2, the standard solution S3, the quality control sample QC and the sample S respectively enter a chemical reaction system together with a reagent R1, a reagent R2, a reagent R3, a reagent R4 and a reagent R5 through a pump tube under the pushing of a peristaltic pump 2, continuously flow in a closed pipeline and completely react, wherein: air is introduced into the first air pump pipe and the second air pump pipe on the peristaltic pump 2, the air enters the liquid pipeline to form bubbles, and the standard series solution, the quality control, the sample and the reagent are regularly separated by the air bubbles at certain intervals.
The standard solution S1, the standard solution S2, the standard solution S3, the quality control sample QC and the sample S respectively react with a reagent R1, a reagent R2, a reagent R3, a reagent R4 and a reagent R5 which are introduced by a pump tube, the reaction is completed through a first online mixing coil, a second online mixing coil, an online ultraviolet digestion device, a third online mixing coil, an online low-temperature heating device and a fourth online mixing coil, a reaction product passes through the flow cell 17 and has maximum absorption at the wavelength of 500-700 nm under the action of a light source 18, the absorbance of the product is measured by using the detector 19, data is processed by the data processing system, and the total nitrogen content of a water sample can be calculated reversely according to a working curve formed by a standard series.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.