CN210269598U - Chemical analysis system for total nitrogen - Google Patents
Chemical analysis system for total nitrogen Download PDFInfo
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- CN210269598U CN210269598U CN201920808829.2U CN201920808829U CN210269598U CN 210269598 U CN210269598 U CN 210269598U CN 201920808829 U CN201920808829 U CN 201920808829U CN 210269598 U CN210269598 U CN 210269598U
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Abstract
The utility model relates to a chemical analysis system for total nitrogen, which comprises an automatic sample feeding device, a sampling needle, a peristaltic pump, a first reaction flow path, a second reaction flow path and a third reaction flow path; the automatic sample introduction device is connected with a peristaltic pump through a sampling needle, the first reaction flow path, the second reaction flow path and the third reaction flow path are sequentially connected to form a sample reaction flow path, and the peristaltic pump is connected with the first reaction flow path, the second reaction flow path and the third reaction flow path; the first reaction flow path, the second reaction flow path and the third reaction flow path are respectively provided with a first bubble injection device, a second bubble injection device and a third bubble injection device; the first bubble injection device, the second bubble injection device and the third bubble respectively introduce air, reagent and sample through pump tubes on the peristaltic pump, so that the introduced air enters the liquid pipeline to form bubbles, and the sample and the reagent are separated through the bubbles. The utility model discloses can detect sample in batches, analysis speed is fast, the degree of accuracy is high, good reproducibility, detection limit is low, and reagent and sample consumption are few.
Description
Technical Field
The utility model relates to a total nitrogen survey technical field in the water especially relates to a chemical analysis system for total nitrogen.
Background
The total nitrogen is the total amount of various forms of inorganic and organic nitrogen in the water body, and comprises inorganic nitrogen such as nitrite nitrogen and nitrate nitrogen, and organic nitrogen such as protein, amino acid and organic amine, and is calculated by the nitrogen mg in each liter of water. The total nitrogen content is usually used to indicate the degree of the water body polluted by nutrients, and the total nitrogen content in the water body is one of the important indexes for measuring the water quality. The measurement of the method is helpful for evaluating the polluted and self-purification conditions of the water body. When the nitrogen substances in the surface water exceed the standard, the microorganisms propagate in a large quantity, plankton grows vigorously, and a eutrophication state appears; the method has the advantages of mastering the content of total nitrogen in the water body, monitoring the distribution condition and the main source of the total nitrogen, and having very important significance for controlling the eutrophication of the water body and improving the water quality.
At present, four methods of manual operation, program controller, flow injection analysis and continuous flow analysis are mainly used for measuring the total nitrogen.
The manual operation and the program controller adopt a national standard method GB11894-89, namely a steam sterilizer or a household pressure cooker is used for heating for half an hour at 120-124 ℃, so that nitrogen-containing compounds in various forms in a sample are converted into nitrate, and finally, an ultraviolet spectrophotometry is adopted for determination. The method has the problems of complicated operation process, low analysis speed, long working time, large consumption of samples and reagents, large harm to human bodies caused by frequent operation of the reagents and the like.
The measurement of the instrument method includes two types of flow injection method and continuous flow method, which are instrument analysis methods with high automation degree, the instrument adopting the flow injection technology in the prior art is used for detecting in a non-equilibrium state, and due to the limitation of the technical principle, the reaction pipeline is thin and easy to block, the instrument is only used for measuring the total nitrogen in a clean water body, the application range is narrow, the instrument design is more complex, the requirement on the reaction condition in the test is strict, the reagent used for the test needs degassing treatment, and the workload is greatly increased.
SUMMERY OF THE UTILITY MODEL
The utility model aims at providing a chemical analysis system for total nitrogen to solve the problem that current chemical analysis method operation process is loaded down with trivial details, analysis speed is slow, operating time is long, sample and reagent consumption are big, simultaneously, overcome the thin easy stifled of flow injection technical analysis mode pipeline, require stringently, reagent need filter and drawback such as degasification to reaction condition.
The utility model provides a chemical analysis system for total nitrogen, which comprises an automatic sample feeding device, a sampling needle, a peristaltic pump, a first reaction flow path, a second reaction flow path and a third reaction flow path;
the automatic sample introduction device is connected with the peristaltic pump through the sampling needle, the first reaction flow path, the second reaction flow path and the third reaction flow path are sequentially connected to form a sample reaction flow path, and the peristaltic pump is connected with the first reaction flow path, the second reaction flow path and the third reaction flow path and is used for pumping a sample and a reagent to the first reaction flow path and pumping the reagent and a reacted sample to the second reaction flow path and the third reaction flow path;
the first reaction flow path, the second reaction flow path and the third reaction flow path are respectively provided with a first bubble injection device, a second bubble injection device and a third bubble injection device; the first bubble injection device, the second bubble injection device and the third bubble respectively introduce air, reagent and sample through a pump pipe on the peristaltic pump, so that the introduced air enters a liquid pipeline to form bubbles, and the sample and the reagent are separated through the bubbles.
Further, the first reaction flow path comprises the first bubble injection device, a first tee joint, a first on-line mixing coil, an on-line ultraviolet digestion device and a first on-line exhaust device which are connected in sequence; the first bubble injection device respectively introduces air and potassium persulfate solution through a pump pipe on the peristaltic pump, and introduces sodium tetraborate solution through the first three-way joint and the pump pipe on the peristaltic pump; one end of the first online exhaust device is connected with the waste liquid bottle through a pump pipe on the peristaltic pump.
Further, the second reaction flow path comprises the second bubble injection device, a second on-line mixing coil and an on-line dialysis device which are connected in sequence; the second bubble injection device respectively introduces air and sodium hydroxide solution through a pump pipe on the peristaltic pump and is connected with the other end of the first online exhaust device through the pump pipe on the peristaltic pump; the online dialysis device is composed of an upper pressing block and a lower pressing block, and the outlet end of the upper pressing block is connected with a waste liquid bottle.
Further, the third reaction flow path comprises a second three-way joint, a third online mixing coil, an online heating device, a third three-way joint, a fourth reaction mixing coil, a second online exhaust device, a flow cell and a detector which are connected in sequence; the third bubble injection device respectively introduces air and sodium hydroxide solution through a pump pipe on the peristaltic pump and is connected with the inlet end of the lower pressing block of the online dialysis device through a pipeline; the outlet end of the lower pressure block of the online dialysis device is connected with the second three-way joint; the online dialysis device introduces hydrazine copper solution and a color reagent through the second three-way joint and the second three-way joint respectively; the inlet end of the flow cell is connected with a waste liquid bottle through the second online exhaust device, and the outlet end of the flow cell is connected with the waste liquid bottle through a pump pipe on the peristaltic pump.
Furthermore, U-shaped grooves are formed in the upper pressing block and the lower pressing block, and a dialysis membrane is arranged between the upper pressing block and the lower pressing block to form a U-shaped flow path.
Furthermore, the inner diameters of the first online mixing coil, the second online mixing coil, the third online mixing coil and the fourth online mixing coil are 1.8-2.0 mm.
Furthermore, the first on-line mixing coil, the second on-line mixing coil, the third on-line mixing coil and the fourth on-line mixing coil are made of glass materials.
By means of the scheme, the chemical analysis system for total nitrogen adopts a continuous flow analysis technology, can detect samples in batches, has high analysis speed, high accuracy, good repeatability, low detection limit and low reagent and sample consumption, and can completely replace the traditional chemical analysis method.
The above description is only an overview of the technical solution of the present invention, and in order to make the technical means of the present invention more clearly understood and can be implemented according to the content of the description, the following detailed description is made with reference to the preferred embodiments of the present invention and accompanying drawings.
Drawings
FIG. 1 is a block diagram of a chemical analysis system for total nitrogen in accordance with the present invention;
fig. 2 is a schematic diagram of a chemical analysis system for total nitrogen according to the present invention.
Detailed Description
The following detailed description of the embodiments of the present invention is provided with reference to the accompanying drawings and examples. The following examples are intended to illustrate the invention, but are not intended to limit the scope of the invention.
Referring to fig. 1, the chemical analysis system for total nitrogen is composed of a gas-liquid driving system, a chemical reaction system, an optical detection system, a data processing system and a circuit control system, referring to fig. 2, wherein:
the gas-liquid drive system includes: the device comprises an automatic sample introduction device 1, a sampling needle 2, a peristaltic pump 3 and pump tubes (401-413);
the chemical reaction system comprises: the online ultraviolet digestion device comprises a first bubble injection device 5, a first three-way joint 6, a first online mixing coil 7, an online ultraviolet digestion device 8, a first online exhaust device 9, a second bubble injection device 10, a second online mixing coil 11, an online dialysis device 12, a third bubble injection device 13, a second three-way joint 14, a third online mixing coil 15, an online heating device 16, a third three-way joint 17, a fourth reaction mixing coil 18 and a second online exhaust device 28.
W1, W2, W3 and W4 are waste liquids, and all the waste liquids finally flow into the waste liquid bottle 25. The reagent bottles 22, 23, 24, 26 and 27 are respectively filled with potassium persulfate solution, sodium tetraborate solution, sodium hydroxide solution, hydrazine copper solution and color developing reagent.
The optical detection system includes: a flow cell 19 through which a sample to be tested passes, a light source 20, and a detector 21 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.
The system can be divided into three reaction flow paths according to the reaction sequence.
First reaction flow path:
a sampling needle 2 of the automatic sample introduction device 1 is sequentially connected in series with a pump tube 401, a first bubble injection device 5, a first three-way joint 6, a first online mixing coil 7, an online ultraviolet digestion device 8 and a first online exhaust device 9 on a peristaltic pump 3 through pipelines; pump tubes 402 and 403 on the peristaltic pump 3 are both connected with a first bubble injection device 5, air and an oxidizing reagent potassium persulfate solution are respectively introduced, the other end of the pump tube 402 is suspended in air G, and the other end of the pump tube 403 is connected with a potassium persulfate solution reagent bottle 22 through a pipeline; the other two ends of the first online exhaust device 9 are respectively connected with the pump pipes 408 and 405, and the other end of the pump pipe 408 is connected with the waste liquid bottle 25 through a pipeline; the sodium tetraborate solution reagent bottle 23 is connected in series with the pump pipe 404 and the first bubble injecting device 5 in sequence through a pipeline.
A second reaction flow path:
the other end of the pump tube 405 is sequentially connected in series with a second bubble injection device 10, a second on-line mixing coil 11 and an on-line dialysis device 12 through pipelines; the pump pipes 406 and 407 are both connected with the second bubble injection device 10, the other end of the pump pipe 406 is suspended in the air G, and the other end of the pump pipe 407 is connected with the sodium hydroxide solution reagent bottle 24 through a pipeline; the on-line dialysis device 12 is composed of an upper pressing block and a lower pressing block, wherein the upper pressing block and the lower pressing block are both provided with U-shaped grooves, and a dialysis membrane is arranged between the pressing blocks to form a U-shaped flow path. The outlet end of the upper pressing block of the online dialysis device 12 is connected with a waste liquid bottle 25 through a pipeline. The inlet end of the lower pressing block of the online dialysis device 12 is connected with a third bubble injection device 13, the other two ends of the third bubble injection device 13 are respectively introduced with air and sodium hydroxide solution through pump pipes 409 and 410, the other end of the pump pipe 409 is suspended in air G, and the other end of the pump pipe 410 is connected with a sodium hydroxide solution reagent bottle 24 through a pipeline.
Third reaction flow path:
the outlet end of the lower pressure block of the online dialysis device 12 is connected in series with a second three-way joint 14, a third online mixing coil 15, an online heating device 16, a third three-way joint 17, a fourth reaction mixing coil 18, a second online exhaust device 28, a flow cell 19 and a detector 21 through pipelines. The hydrazine solution is introduced through a pump pipe 411, one end of the pump pipe 411 is connected in series with the hydrazine solution reagent bottle 26, and the other end is connected with the second three-way joint 14 through a pipeline. The color reagent is introduced through the pump tube 412, one end of the pump tube 412 is connected in series with the color reagent bottle 27, and the other end is connected with the second three-way joint 17 through a pipeline. The inlet end of the flow-through cell 19 is connected with a waste liquid bottle 25, and the outlet end is connected with the waste liquid bottle 25 through a pump pipe 413.
The system collects a sample S through a sampling needle 2 of an automatic sampling device 1, the sample S and a reagent (R1-R5, which respectively correspond to a potassium sulfate solution, a sodium tetraborate solution, a sodium hydroxide solution, a hydrazine copper solution and a chromogenic reagent) enter a chemical reaction system through pump pipes (401-413) under the pushing of a peristaltic pump 3, and the sample S and the reagent continuously flow in a closed pipeline and generate chromogenic reaction. Wherein: air is respectively introduced into pump pipes 402, 406 and 409 on the peristaltic pump 3, air entering pipelines form air bubbles in the liquid flow, and the sample S and the reagent (R1-R5) are regularly separated by the air bubbles at certain intervals.
Under the alkaline condition of sodium tetraborate solution R5 introduced by a pump pipe 404, nitrogen-containing compounds in a sample S are converted into nitrate under the action of potassium persulfate solution R1 introduced by a pump pipe 403 and an online ultraviolet digestion device 8, macromolecular, particle impurities and the like in the sample S are discharged out of a reaction system through an online dialysis device 12, the generated nitrate is reduced into nitrite by hydrazine copper solution R4 introduced by a pump pipe 411 under the alkaline condition of sodium hydroxide solution R3 introduced by pump pipes 407 and 410, then the nitrite reacts with sulfanilamide introduced by a pump pipe 412 in a chromogenic reagent R5 to generate diazonium salt under the acidic condition, finally the diazonium salt is coupled with naphthyl ethylenediamine hydrochloride in the chromogenic reagent to generate a mauve dye, the colored compound passes through a flow cell 19 and has maximum absorption at the wavelength of 520nm under the action of a light source 20, and the absorbance of the resultant is measured by a detector 21, and processing the data by a data processing system to obtain the total nitrogen content in the sample.
The system adopts a continuous flow technology, is used for detecting in a reaction balance state, namely, a physical mixing state and a chemical reaction state are complete, bubbles are injected into the chemical reaction system, so that the reaction is more sufficient, the maximum sensitivity can be achieved, the sample concentration also reaches a continuous maximum value, the sample residue can be effectively reduced, the test result cannot be influenced by the tiny change of the reaction environment, the test accuracy is high, the repeatability is good, and the detection limit is low.
The chemical analysis system for total nitrogen can detect samples in batches, has high analysis speed, high accuracy, good repeatability, low detection limit and less reagent and sample consumption, can completely replace the traditional chemical analysis method, and particularly has the following technical effects:
1. the system adopts a bubble injection technology, so that the existence of bubbles can enable a sample to react completely, the reaction precision is improved, and the sample residue in a pipeline can be reduced remarkably;
2. the system adopts full steady state detection (namely complete reaction), and has high accuracy and strong reliability;
3. the method has the advantages that the total nitrogen sample is completely processed on line, the functions are comprehensive, and the functions of on-line sample adding, mixing, ultraviolet digestion, dialysis, heating and the like are included;
4. the efficient long-distance online ultraviolet digestion device can quickly finish the decomposition and conversion of nitrogen-containing compounds, and meets the online detection requirement;
5. the online mixing coil in the system is made of glass with a large pipe diameter, has good trafficability and chemical inertness, the sectional area of the pipeline is 5-10 times of that of the pipeline applied by the flow injection technology, the pipeline is large in sectional area and not easy to block, and the online mixing coil has good trafficability to sewage samples and is easier to maintain in use;
6. the reaction system adopts small and portable elements, has compact structure and reasonable layout and arrangement, and is convenient for daily maintenance and observation.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and it should be noted that, for those skilled in the art, a plurality of modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (7)
1. A chemical analysis system for total nitrogen is characterized by comprising an automatic sample introduction device, a sampling needle, a peristaltic pump, a first reaction flow path, a second reaction flow path and a third reaction flow path;
the automatic sample introduction device is connected with the peristaltic pump through the sampling needle, the first reaction flow path, the second reaction flow path and the third reaction flow path are sequentially connected to form a sample reaction flow path, and the peristaltic pump is connected with the first reaction flow path, the second reaction flow path and the third reaction flow path and is used for pumping a sample and a reagent to the first reaction flow path and pumping the reagent and a reacted sample to the second reaction flow path and the third reaction flow path;
the first reaction flow path, the second reaction flow path and the third reaction flow path are respectively provided with a first bubble injection device, a second bubble injection device and a third bubble injection device; the first bubble injection device, the second bubble injection device and the third bubble respectively introduce air, reagent and sample through a pump pipe on the peristaltic pump, so that the introduced air enters a liquid pipeline to form bubbles, and the sample and the reagent are separated through the bubbles.
2. The chemical analysis system for total nitrogen according to claim 1, wherein the first reaction flow path comprises the first bubble injection device, a first tee joint, a first on-line mixing coil, an on-line ultraviolet digestion device and a first on-line exhaust device which are connected in sequence; the first bubble injection device respectively introduces air and potassium persulfate solution through a pump pipe on the peristaltic pump, and introduces sodium tetraborate solution through the first three-way joint and the pump pipe on the peristaltic pump; one end of the first online exhaust device is connected with the waste liquid bottle through a pump pipe on the peristaltic pump.
3. The chemical analysis system for total nitrogen according to claim 2, wherein the second reaction flow path comprises the second bubble injection means, the second on-line mixing coil and the on-line dialysis means connected in this order; the second bubble injection device respectively introduces air and sodium hydroxide solution through a pump pipe on the peristaltic pump and is connected with the other end of the first online exhaust device through the pump pipe on the peristaltic pump; the online dialysis device is composed of an upper pressing block and a lower pressing block, and the outlet end of the upper pressing block is connected with a waste liquid bottle.
4. The chemical analysis system for total nitrogen according to claim 3, wherein the third reaction flow path comprises a second tee joint, a third on-line mixing coil, an on-line heating device, a third tee joint, a fourth reaction mixing coil, a second on-line exhaust device, a flow cell and a detector which are connected in sequence; the third bubble injection device respectively introduces air and sodium hydroxide solution through a pump pipe on the peristaltic pump and is connected with the inlet end of the lower pressing block of the online dialysis device through a pipeline; the outlet end of the lower pressure block of the online dialysis device is connected with the second three-way joint; the online dialysis device introduces hydrazine copper solution and a color reagent through the second three-way joint and the second three-way joint respectively; the inlet end of the flow cell is connected with a waste liquid bottle through the second online exhaust device, and the outlet end of the flow cell is connected with the waste liquid bottle through a pump pipe on the peristaltic pump.
5. The chemical analysis system for total nitrogen according to claim 3, wherein each of the upper and lower pressure blocks has a U-shaped groove, and a dialysis membrane is provided between the upper and lower pressure blocks to form a U-shaped flow path.
6. The chemical analysis system for total nitrogen according to claim 4, wherein the first, second, third and fourth inline mixing coils have a tube inner diameter of 1.8 to 2.0 mm.
7. The chemical analysis system for total nitrogen of claim 6, wherein the first, second, third and fourth on-line mixing coils are made of glass.
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| CN110220855A (en) * | 2019-05-31 | 2019-09-10 | 北京海光仪器有限公司 | A kind of chemical analysis system for total nitrogen |
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| CN110220855A (en) * | 2019-05-31 | 2019-09-10 | 北京海光仪器有限公司 | A kind of chemical analysis system for total nitrogen |
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