CN211086070U - Sulfide analysis system - Google Patents
Sulfide analysis system Download PDFInfo
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- CN211086070U CN211086070U CN201921651686.5U CN201921651686U CN211086070U CN 211086070 U CN211086070 U CN 211086070U CN 201921651686 U CN201921651686 U CN 201921651686U CN 211086070 U CN211086070 U CN 211086070U
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Abstract
The utility model relates to a sulfide analysis system, which comprises a gas-liquid driving system and a chemical reaction system; the gas-liquid driving system comprises an automatic sample introduction device, a sampling needle, a peristaltic pump and a pump pipe; the chemical reaction system comprises a first reaction flow path and a second reaction flow path; the automatic sample introduction device is connected with the peristaltic pump through the sampling needle, and the peristaltic pump is connected with the first reaction flow path and the second reaction flow path; the first reaction flow path comprises a first bubble injection device, a first online mixing ring, a three-way joint, an online heating device, an online distillation device and a first online exhaust device which are connected in sequence; the second reaction flow path comprises a second bubble injection device, a second on-line mixing coil, a third on-line mixing coil and a second on-line exhaust device which are connected in sequence. 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 sulphide survey technical field in the water especially relates to a sulphide analytic system.
Background
The content of sulfide is often used to indicate the degree of pollution of water, and the content of sulfide in water is one of the important indicators for measuring water quality. The measurement of which is helpful for evaluating the contamination condition of the water body. Sulfides in water include soluble H2S、HS-、S2-And soluble sulfides, acid soluble metal sulfides, and unionized inorganic and organic sulfides present in the suspension.
8 mu g/m in air3H of (A) to (B)2S can make human sense of smell sensitive, H in water2S has a threshold of 0.035. mu.g/L the sulfide-containing water is mostly black and has an irritating odor, mainly due to H2S gas is continuously released from the water. Sulfides in water are easily hydrolyzed to H2The S form is released into the air, is nausea and vomiting immediately after being absorbed by people in large quantity, and even has the symptoms of dyspnea, asphyxia and the like, so that strong toxic feeling is generated. If the air content reaches 15-30 mg/m3It can cause inflammation of the eye membrane and damage to the optic nerve. H dissipated in air2S is inhaled by human body for a long time, and can be combined with human body cytochrome, oxidase and human bodyThe disulfide bond (-S-S-) in the body protein and amino acid affects the oxidation process of cells, causes oxygen deficiency of cells and endangers the life of people. Prolonged consumption of water with higher sulfide content can result in poor taste, loss of appetite, weight loss, poor hair growth, and in severe cases, failure and death. The sulfide source mainly comprises mine wastewater, mineral processing wastewater, coking wastewater and the like in the metallurgical industry, the content of sulfide in the water body is mastered, the distribution condition and the main source of the sulfide are monitored, and the method has very important significance for controlling water body pollution and improving water quality
At present, four methods of manual operation, program controller, flow injection analysis and continuous flow analysis are mainly used for measuring the sulfide nitrogen.
The manual operation and the program controller adopt a national standard method GB16489-1996 method. And (3) determining a clean water sample which is colorless, transparent and free of suspended matters by adopting a precipitation separation method. A water sample containing suspended matters and high in turbidity, and colored and opaque is measured by an acidification-blowing-absorption method, wherein a zinc acetate-sodium acetate solution is required to be injected, an antioxidant solution is added, an acid-adding nitrogen-filling pipe is installed, nitrogen is communicated, the nitrogen is continuously communicated after a phosphoric acid solution is added midway, then the absorption color development pipe is taken down and washed, a reagent is added, the vibration and the standing are carried out, and finally, the spectrophotometry is adopted for measurement. 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 market at present detects the reaction 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 sulfide in the 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 in the test needs degassing treatment, and the workload is greatly increased.
SUMMERY OF THE UTILITY MODEL
The utility model aims at providing a sulphide analytic system to solve the problem that current chemical analysis method operation process is loaded down with trivial details, the analysis speed is slow, operating time is long, sample and reagent consumption are big, simultaneously, overcome that the technical analysis of flow analysis way pipeline is thin easily stifled, strict, the reagent of requirement of reaction condition needs drawbacks such as filtration and degasification.
The utility model provides a sulfide analysis system, which comprises a gas-liquid driving system and a chemical reaction system; the gas-liquid driving system comprises an automatic sampling device, a sampling needle, a peristaltic pump and a pump pipe; the chemical reaction system comprises a first reaction flow path and a second reaction flow path;
the automatic sample introduction device is connected with the peristaltic pump through the sampling needle, and the peristaltic pump is connected with the first reaction flow path and the second reaction flow path;
the first reaction flow path comprises a first bubble injection device, a first online mixing ring, a three-way joint, an online heating device, an online distillation device and a first online exhaust device which are connected in sequence; the first bubble injection device respectively introduces air and a distillation reagent through a pump pipe on the peristaltic pump, so that the introduced air enters a liquid pipeline to form bubbles for separating a sample and the reagent; carrier gas air is introduced into one end of the three-way joint; the online distillation device introduces a sodium hydroxide solution reagent through a pump pipe on the peristaltic pump, and the outlet end of the online distillation device is connected with a waste liquid bottle through a circulating water device and the pump pipe on the peristaltic pump; the first online exhaust device is connected with a waste liquid bottle through a pump pipe on the peristaltic pump;
the second reaction flow path comprises a second bubble injection device, a second on-line mixing coil, a third on-line mixing coil and a second on-line exhaust device which are connected in sequence; the second bubble injection device respectively introduces air and a color reagent through a pump tube on the peristaltic pump, so that the introduced air enters a liquid pipeline to form bubbles for separating a sample and the reagent; the third online mixing loop introduces a ferric chloride solution reagent through a pump pipe on the peristaltic pump; and an outlet at the upper end of the second online exhaust device is connected with a waste liquid bottle.
Further, the analysis system further comprises an optical detection system; the optical detection system comprises a flow cell, two ends of the flow cell are respectively connected with a light source and a detector, the inlet end of the flow cell is connected with the second online exhaust device, and the outlet end of the flow cell is connected with a waste liquid bottle through a pump pipe.
Further, the analysis system further comprises:
a data processing system for processing data of the detector;
and the circuit control system is used for controlling the circuit of the sulfide analysis system.
Furthermore, the inner diameters of the first online mixing coil, the second online mixing coil and the third online mixing coil are 1.8-2.0 mm.
Furthermore, the first online mixing coil, the second online mixing coil and the third online mixing coil are made of glass materials.
By means of the scheme, the sulfide analysis system can detect samples in batches, is high in analysis speed, high in accuracy, good in repeatability, low in detection limit and low in reagent and sample consumption, and can completely replace a conventional 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 sulfide analysis system according to the present invention;
fig. 2 is a schematic diagram of a sulfide analysis system of 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 sulfide analysis system 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 a pump tube (401-411);
the chemical reaction system comprises: the device comprises a first bubble injection device 5, a first online mixing coil 6, a three-way joint 7, an online heating device 8, an online distillation device 9, a circulating water device 10, a first online exhaust device 11, a second bubble injection device 12, a second online mixing coil 13, a third online mixing coil 14 and a second online exhaust device 15.
W1, W2, W3 and W4 are waste liquids, and the waste liquids flow into a waste liquid bottle at last. 19. 20, 21 and 22 are reagent bottles which are respectively filled with reagents R1-R4, wherein R1 is a distilled reagent, R2 is a sodium hydroxide solution, R3 is a color reagent, and R4 is an iron chloride solution.
The optical detection system includes: a flow cell 16 through which a sample to be tested passes, a light source 17, and a detector 18 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 has two main reaction flow paths.
First reaction flow path:
a sampling needle 2 of the automatic sample introduction device 1 is sequentially connected in series with a pump tube 403, a first bubble injection device 5, a first online mixing coil 6, a three-way joint 7, an online heating device 8, an online distillation device 9 and a first online exhaust device 11 on a peristaltic pump 3 through pipelines; pump tubes 401 and 402 on the peristaltic pump 3 are both connected with a first bubble injection device 5, air and a reagent R1 distillation reagent are respectively introduced, the other end of the pump tube 401 is suspended in air G, and the other end of the pump tube 402 is connected with a reagent R1 reagent bottle 19 through a pipeline; the glass tee joint 7 introduces carrier air, and the carrier air is provided by a micro air pump. Reagent R2 sodium hydroxide solution was introduced from reagent R2 reagent bottle 20 through pump tube 405 onto the in-line distillation apparatus 9. The waste liquid W1 generated by the online distillation device 9 is cooled by the circulating water device 10 and then is discharged to a waste liquid bottle through the pump pipe 404. The waste liquid W2 generated by the online distillation device 9 is directly discharged to a waste liquid bottle through a pipeline. The other two ends of the first online exhaust device 11 are respectively connected with pump pipes 406 and 407, and the other end of the pump pipe 406 is connected with a waste liquid bottle through a pipeline.
A second reaction flow path:
the other end of the pump pipe 407 is sequentially connected in series with a second bubble injection device 12, a second on-line mixing coil 13, a third on-line mixing coil 14, a second on-line exhaust device 15, a flow cell 16 and a detector 18 through pipelines; the pump pipes 408 and 409 are both connected with the second bubble injection device 12, the other end of the pump pipe 408 is suspended in the air G, and the other end of the pump pipe 409 is connected with the reagent bottle 21 of the reagent R3 for color development through a pipeline; a reagent R4 ferric chloride solution reagent bottle is connected to the third in-line mixing coil 14 by a pump tube 410. The other end of the second online exhaust device 15 is connected with a waste liquid bottle. The outlet end of the flow cell 16 discharges the waste liquid W5 to a waste liquid bottle through the pump pipe 411.
A light source 17 and a detector 18 are connected to both ends of the flow cell 16, respectively.
The system collects a sample S through a sampling needle 2 of an automatic sampling device 1, the sample S and a reagent (R1-R4) enter a chemical reaction system through pump tubes (401-411) under the pushing of a peristaltic pump 3, and continuously flow in a closed pipeline, and a color reaction is generated. Wherein: air is respectively introduced into pump tubes 401 and 408 of the peristaltic pump 3, and enters the liquid pipeline to form bubbles, so that a reaction flow path is formed, wherein the sample S and the reagents (R1-R4) are regularly separated by the air bubbles at certain intervals.
Under the action of the distilled reagent of the reagent R1 introduced by the pump pipe 402, the sulfur-containing compounds in the sample S flowing through the pump pipe 403 are converted into hydrogen sulfide gas by the on-line heating device 8 and the on-line distillation device 9, and the gas is absorbed by the sodium hydroxide solution of the reagent R2 introduced by the pump pipe 405 to generate a sodium sulfide solution. Under the acidic condition and the action of a reagent R4 ferric chloride solution introduced by a pump tube 410, sulfur ions in an absorption liquid and p-aminodimethylaniline in a reagent R3 chromogenic reagent introduced by a pump tube 409 act to generate a blue compound methylene blue, the colored compound has maximum absorption at a wavelength of 660nm under the action of a light source 17 through a flow cell 16, a detector 18 is adopted to determine the absorbance of the product, and a data processing system is used to process data to obtain the content of sulfide in a sample.
The system adopts a continuous flow analysis technology, the reaction is detected in an equilibrium state, namely, the physical mixing and the chemical reaction are completely carried out, the reaction is more sufficient by injecting bubbles into the reaction system, the maximum sensitivity can be reached, the sample concentration also reaches the continuous maximum value, the sample residue can be reduced, the test result cannot be influenced by the small change of the reaction environment, the test accuracy is high, the repeatability is good, the detection limit is low, the large-pipe-diameter design is adopted, and the application range is wider.
But through this sulphide analytic system batch detection sample, analysis fast, the degree of accuracy is high, good reproducibility, detection limit are low, reagent and sample consumption are few, can replace the sulphide analytic system of traditional chemical analysis method completely, specifically include following technological effect:
1. the system adopts a bubble injection technology, the existence of bubbles can enable the sample to react completely, the sample residue in the pipeline can be reduced remarkably, and the mutual interference of different samples can be avoided;
2. the system adopts the method of detecting in a fully steady state (namely complete reaction), and has high accuracy and strong reliability;
3. the online stripping distillation technology is adopted, the efficiency is high, the service life is long, and the online stripping distillation technology is particularly suitable for sewage detection with complex matrixes;
4. the sulfide sample treatment is completely on-line, the functions are comprehensive, and the functions of on-line sample adding, mixing, heating, distilling and the like are covered;
5. the reaction mixing ring in the system is made of glass with large pipe diameter (the inner diameter is 1.8-2.0 mm), so that the reaction mixing ring has good trafficability and chemical inertness, the sectional area of a pipeline is 3-5 times of that of an application pipeline of a flow injection technology, the pipeline is large in sectional area and not easy to block, a sewage sample is good trafficability, and the reaction mixing ring 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 (5)
1. A sulfide analysis system is characterized by comprising a gas-liquid driving system and a chemical reaction system; the gas-liquid driving system comprises an automatic sampling device, a sampling needle, a peristaltic pump and a pump pipe; the chemical reaction system comprises a first reaction flow path and a second reaction flow path;
the automatic sample introduction device is connected with the peristaltic pump through the sampling needle, and the peristaltic pump is connected with the first reaction flow path and the second reaction flow path;
the first reaction flow path comprises a first bubble injection device, a first online mixing ring, a three-way joint, an online heating device, an online distillation device and a first online exhaust device which are connected in sequence; the first bubble injection device respectively introduces air and a distillation reagent through a pump pipe on the peristaltic pump, so that the introduced air enters a liquid pipeline to form bubbles for separating a sample and the reagent; carrier gas air is introduced into one end of the three-way joint; the online distillation device introduces a sodium hydroxide solution reagent through a pump pipe on the peristaltic pump, and the outlet end of the online distillation device is connected with a waste liquid bottle through a circulating water device and the pump pipe on the peristaltic pump; the first online exhaust device is connected with a waste liquid bottle through a pump pipe on the peristaltic pump;
the second reaction flow path comprises a second bubble injection device, a second on-line mixing coil, a third on-line mixing coil and a second on-line exhaust device which are connected in sequence; the second bubble injection device respectively introduces air and a color reagent through a pump tube on the peristaltic pump, so that the introduced air enters a liquid pipeline to form bubbles for separating a sample and the reagent; the third online mixing loop introduces a ferric chloride solution reagent through a pump pipe on the peristaltic pump; and an outlet at the upper end of the second online exhaust device is connected with a waste liquid bottle.
2. The sulfide analysis system according to claim 1, further comprising an optical detection system, wherein the optical detection system comprises a flow cell, two ends of the flow cell are respectively connected with a light source and a detector, an inlet end of the flow cell is connected with the second online exhaust device, and an outlet end of the flow cell is connected with a waste liquid bottle through a pump tube.
3. The sulfide analysis system of claim 2, further comprising:
a data processing system for processing data of the detector;
and the circuit control system is used for controlling the circuit of the sulfide analysis system.
4. The sulfide analysis system of claim 1, wherein the first, second, and third in-line mixing coils have a tube inner diameter of 1.8-2.0 mm.
5. The sulfide analysis system of claim 4, wherein the first, second, and third in-line mixing coils are glass.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201921651686.5U CN211086070U (en) | 2019-09-29 | 2019-09-29 | Sulfide analysis system |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201921651686.5U CN211086070U (en) | 2019-09-29 | 2019-09-29 | Sulfide analysis system |
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| CN211086070U true CN211086070U (en) | 2020-07-24 |
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| CN201921651686.5U Active CN211086070U (en) | 2019-09-29 | 2019-09-29 | Sulfide analysis system |
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