CN201716269U - Device for determining chemiluminescence characteristics of solid particles oxidized by ozone - Google Patents

Abstract

The utility model proposes an instrument for measuring the law of chemiluminescence produced by ozone-oxidized solid particles, which can quickly detect the content of sediment or soil organic matter and related data on the spot, in real time, and solve the problem of long detection period, high cost, and reagent consumption of existing instruments. Yamato has problems such as pollution. The technical scheme of the utility model is that it includes a power supply unit, a control circuit, external equipment, a serial bus and a reaction chamber, the reaction chamber is provided with a photomultiplier tube and a sample box, and an ozone generator is also provided, and the ozone generator and the reaction chamber Through the pipeline connection, an electromagnetic valve is arranged on the pipeline between the ozone generator and the reaction chamber. The instrument of the utility model can be used as a laboratory research means to obtain the kinetic characteristics of the ozone oxidation of the substance to be studied, so as to deeply understand and study the substance to be tested.

Description

An instrument for measuring the law of chemiluminescence produced by ozone oxidation of solid particles

technical field

The utility model relates to the technical field of chemical oxidation luminescence and analysis, in particular to an instrument for measuring the law of luminescence produced by ozone oxidation of solid particles.

Background technique

At present, the method of domestic detection of sediment, also known as substrate, or soil organic matter content is mainly carried out in the laboratory, using the national standard GB9834-88 "Determination of Soil Organic Matter" and the Ministry of Agriculture standard NY/T85-1988 "Determination of Soil Organic Matter 》The recommended analytical method of potassium dichromate volumetric method, the method and the instruments used take a long time, the analysis process is complicated, the requirements for operators are high, the environmental conditions are harsh, the consumption of reagents is large, and secondary pollution occurs. For occasions that require on-site analysis, such as: in areas polluted by organic matter, different locations have different levels of pollution, and the difference is relatively large. When timely and large-scale monitoring is required, this method is greatly limited in terms of personnel, time, and cost. and constraints. Some simple alternative methods have principle problems and systematic errors, and there are unstable factors, and the accuracy and representativeness of the results cannot be guaranteed. For the characteristics of sediment and soil organic matter, it refers to the content and proportion of active organic matter, organic carbon, and organic pollutants. The detection methods are even more lacking and inaccurate. Simple distinctions and judgments are made by physical, chemical, and biological methods. Unified standards and scientific quantitative basis.

In recent years, with the development of electronic technology, new materials, new processes, and new optical devices, especially the rapid development of computer technology, automatic analysis instruments based on potassium dichromate volumetric method and analyzers based on automatic titration systems are used to measure Sediment and soil organic matter methods appeared accordingly, but because there was no support for new principles, although the instruments using these methods got rid of some shortcomings of laboratory analysis, there was still a distance from the field work mode, such as large consumption of reagents , High requirements for operation and maintenance personnel, poor stability, low sensitivity and resolution, environmental interference and other insurmountable defects, there is no real-time real-time continuous working mode on site.

Contents of the invention

The utility model proposes an instrument for measuring the law of chemiluminescence produced by ozone-oxidized solid particles, which can quickly detect the content of sediment or soil organic matter and related data on the spot, in real time, and solve the problem of long detection period, high cost, and reagent consumption of existing instruments. Yamato has problems such as pollution. It can detect the process of solid particles being oxidized by ozone to produce luminescence, record and analyze the luminescence law, and correspond to the components and contents of the detected substances.

The utility model is an instrument for measuring the law of luminescence produced by ozone oxidation of solid particles, which relates to chemical oxidation luminescence and analysis technology. Specifically, solid particles are used as the measured object, which makes ozone react with it to produce luminescence, and uses photosensitive devices to measure the size and magnitude of luminescence intensity. Change law, through the data processing system to simulate the regular curve equation, and compare and analyze the different equations obtained by different measured objects, corresponding to the content of different elements in the measured object.

In order to achieve the purpose of solving the above-mentioned technical problems, the technical solution of the present utility model is an instrument for measuring the chemiluminescent law of solid particles oxidized by ozone, including a power supply device, a control circuit, external equipment, a serial bus and a reaction chamber. The reaction chamber is provided with a photomultiplier tube and a sample box, and is characterized in that: an ozone generator is also provided, and the ozone generator is connected to the reaction chamber through a pipeline, and between the ozone generator and the reaction chamber There is a solenoid valve on the pipeline between them.

A vacuum pump and a dry filter are arranged on the pipeline at the inlet of the ozone generator.

An ozone decomposing device is also provided, and the ozone decomposing device communicates with the outlet of the reaction chamber and the solenoid valve respectively through pipelines.

The desiccant in the dry filter is silica gel.

A seal is provided between the reaction chamber and the sample box.

The photomultiplier tube transmits the collected detection signal to the control circuit, the control circuit converts the detection signal, and transmits the generated analysis result to the external device through the serial bus.

The external device is a computer or a microprocessor.

The serial bus is an RS485 or RS232 interface.

Ozone is a strong oxidizing agent, and the technique of analyzing the changes produced by the oxidizing reaction by using the ozone oxidation reaction is a relatively new and hot technique in this field. In particular, the research on the luminescence law of ozone oxidation by oxides is being widely concerned and developed as a new research direction and means.

An instrument that uses ozone oxidation and luminescence to detect the chemiluminescence law of solid particles, fully oxidizes ozone and analyte, detects the oxidation luminescence process, records and analyzes the luminescence law, and the steps of the method for using the instrument of the utility model are as follows:

(1). Use the ozone generator to generate ozone, control the accumulation time so that the concentration and flow of ozone meet the requirements of the reaction conditions, and then send it into the reaction chamber;

(2). The fast loading and unloading mechanism is adopted to conveniently load the tested object into the reaction chamber;

(3). Ozone and the measured substance undergo oxidation reaction in the reaction chamber to ensure the contact area between the ozone and the sample, and optically seal the reaction chamber, and detect the luminous signal from the detection window;

(4). The light intensity signal sent by the reaction is collected, and converted into an electrical signal and sent to the data processing instrument for processing;

(5). Simulate the changing law of the collected signals to obtain the oxidation kinetics curve, and calculate and analyze the obtained simulation curve to find out the corresponding characteristics.

(6). Control the status of pumps and valves, blow out the residual ozone gas in the reaction chamber and pipelines, and ensure the normal operation of the next test.

The utility model can be divided into two parts, one part is composed of high-concentration ozone generator, electromagnetic valve, reaction chamber, etc.; the other part is composed of control circuit, photomultiplier tube and serial bus data processing software.

In the utility model, it also has the following technical features: the sample pool can be loaded and unloaded conveniently and quickly, and is easy to operate and use;

In the utility model, it also has the following technical features: multiple protection measures are taken, and the photoelectric detection part cannot be opened when the sample space is not sealed, so as not to burn out the device;

In the utility model, it also has the following technical features: the ozone concentration accumulation setting is designed, and when the accumulation meets the reaction requirements, the electromagnetic valve is opened and sent into the reaction chamber;

In the utility model, it also has the following technical features: the residual ozone cleaning program is designed to clear the residual ozone in the pipeline and the reaction chamber, so as not to affect the next test.

In the utility model, it also has the following technical features: an ozone decomposing device is used to prevent ozone from entering the air.

In the utility model, it also has the following technical features: a curve fitting program is designed, and the obtained data is fitted into an oxidation luminescence kinetics curve formula;

In the utility model, it also has the following technical features: a curve processing program is designed, and indicators such as integrals, derivatives, slopes, etc. of different stages of the curve are extracted, corresponding to the contents of different elements of the measured object.

In the utility model, it also has the following technical features: the instrument is calibrated. Due to the influence of the external environment, the ozone concentration and luminescence sensitivity of the instrument will change to a certain extent. In order to avoid affecting the output results, a standard sample is sampled to calibrate the instrument. The standard sample is used for testing first, and the obtained value is used as a coefficient , the future data will be corrected with this coefficient to ensure the stability of test results under different time, place and environmental conditions.

The utility model is an instrument for measuring the law of chemiluminescence produced by ozone oxidation of solid particles, which is a new means for studying the oxidation and luminescence characteristics of solid particles. It is based on the principle of ozone oxidation and luminescence, that is, ozone is used as a strong oxidant to react with the sample to be tested, and the light signal generated during the reaction is detected by low-light photoelectric conversion technology, and the kinetics is fitted according to the reaction principle. From the curve, various characteristics of the measured object can be analyzed.

Compared with the prior art, the utility model has the following advantages and positive effects: it is convenient and simple to use, does not need to add reagents, does not produce secondary pollution, avoids the shortcomings of conventional methods requiring high operating conditions, and can accurately and quickly detect the measured object. It can work reliably in ordinary outdoor environment for a long time. It is portable and suitable for use in vehicles, ships, factories and laboratories. The instrument can be used as a laboratory research method to obtain the kinetic characteristics of the ozone oxidation of the substance being studied, so as to deeply understand and study the substance being tested.

Description of drawings

The utility model is described in detail below in conjunction with accompanying drawings and embodiments.

Fig. 1 is a schematic diagram of an instrument for measuring the chemiluminescent law of solid particles oxidized by ozone according to the present invention;

In Fig. 1: 1. power supply device; 2. sample inlet; 3. touch control panel; 4. reaction chamber; 5. sample box; 6. photomultiplier tube; 7. solenoid valve; 8. pipeline; 9. Ozone generator; 10. Pipeline; 11. Vacuum pump; 12. Dry filter; 13. Serial bus; 14. Ozone decomposition device; 15. Control circuit;

Fig. 2 is the sectional view of reaction chamber and sample box in the utility model;

In Fig. 2: 3-1, detection window; 4-1, reaction chamber seat; 4-2, ozone inlet; 4-3, sealing ring; 5, sample box; 5-1, sample to be tested.

Fig. 3 is the flow chart that the utility model detects.

Detailed ways

Referring to Fig. 1 and Fig. 2, an instrument for measuring the chemiluminescent law of ozone oxidation of solid particles includes a power supply unit 1, a control circuit 15, external equipment, a serial bus 13 and a reaction chamber 4, and the reaction chamber 4 is provided with Photomultiplier tube 6 and sample box 5, ozone generator 9 is connected with described reaction chamber 4 by pipeline 8, is provided with electromagnetic valve 7 on pipeline 8 between described ozone generator 9 and described reaction chamber 4 . The pipeline 10 at the inlet of the ozone generator 9 is provided with a vacuum pump 11 and a dry filter 12 . The ozonolysis device 14 communicates with the outlet of the reaction chamber 4 and the solenoid valve 7 through pipelines.

The desiccant in the dry filter 12 is silica gel. A seal 4 - 3 is provided between the reaction chamber 4 and the sample box 5 . The photomultiplier tube 6 transmits the collected detection signal to the control circuit 15, the control circuit 15 converts the detection signal, and transmits the generated analysis result to the external device through the serial bus 13, the external device diagram not shown in The external device is a computer or a microprocessor. The serial bus 13 is an RS485 or RS232 interface. In this embodiment, the serial bus 13 is an RS232 interface.

An instrument for measuring the law of chemiluminescence produced by ozone-oxidized solid particles, the flow chart of the detection by the instrument is shown in Figure 3, and see Figures 1 and 2.

After receiving the command to start the test, the air passes through the filter and dry filter 12 and enters the ozone generator 9 to generate ozone gas. The flow is controlled by the vacuum air pump 11 and pressed into the solenoid valve 7. In the initial state, the solenoid valve 7 leads to the ozone decomposition device 14 , after the ozone concentration reaches the requirement, it sends a message that the next step can be started. The sample to be tested is pre-treated according to the sample detection requirements and then loaded into the sample box 5 and sent to the sample reaction chamber 4 . The program prompts to check whether the reaction chamber 4 is sealed, and after confirmation, the solenoid valve 7 and the photomultiplier tube 6 are activated, and the ozone gas enters the reaction chamber 4, and the ozone reacts with the sample to generate chemiluminescence. This luminescence changes from strong to weak over time. The photomultiplier tube 6 detects the whole process of luminescence, and the program of the control circuit 15 performs analysis and processing synchronously to determine whether the end condition is satisfied, and if so, the test ends and the data analysis process is transferred to. Now the ozone generator 9 stops producing ozone, the photomultiplier tube 6 power supply is turned off, and air is pumped to wash away the residual ozone gas in the pipeline 8 and the reaction chamber 4 . The data analysis program simulates the oxidation kinetics curve according to the change data, and obtains the relevant characteristics of the curve as the representative parameters of the tested sample.

See Figure 2, the sample chamber and quick loading and unloading structure diagram of the instrument.

The tested sample 5-1 is installed in the corresponding position of the sample box 5, and is connected to the reaction chamber seat 4-1 by a quick loading and unloading structure to form a reaction chamber space. The ozone inlet 4 is connected to ozone, and a chemiluminescent reaction occurs when it encounters the tested sample 5-1, and the emitted light passes through the detection window 3-1 to the receiving surface of the photomultiplier tube 6, and the reacted gas is discharged from the outlet. The fast loading and unloading structure is to align the sample box 5 into the reaction chamber seat 4-1, and rotate the sample box 5 so that the inclined surface is pressed against the boss at the bottom of the reaction chamber seat 4-1.

The measurement method 1 of the embodiment of the utility model is to measure the properties of soil carbon.

(1).Use an ozone generator to generate ozone. The concentration of ozone is 18mg/L and the flow rate is 0.51/min. The solenoid valve controls the direction of ozone. Before the reaction, the ozone is passed into the digestion device for ozone digestion. into the reaction chamber.

(2). After the pre-treatment of the measured soil is carried out in the standard, it is loaded into the sample pool, and the sample pool containing the tested soil is loaded into the reaction chamber with a quick locking mechanism;

(3). Ozone and soil samples are mixed and reacted in the reaction chamber to ensure sufficient contact between ozone and soil samples, and the reaction chamber is optically sealed to detect luminescence signals from the detection window;

(4).Use the photomultiplier tube to collect the light intensity signal sent by the reaction, and convert it into an electrical signal and send it to the data processing part for processing, and judge whether it is completed according to the conditions;

(5). Ozone remains in the flushing pipelines of the pumps and valves of the control instrument;

(6). Start the data analysis program, carry out curve fitting to the collected data, obtain the area of the fitting curve formula, multiply it by the coefficient 0.715 and get the carbon content of the measured soil sample.

The measurement method 2 of the embodiment of the present utility model is to measure the oxidative luminescence characteristics of different particulate matter samples.

(1). Use an ozone generator to generate ozone. The concentration of ozone is 18 mg/L and the flow rate is 0.5 l/min. The solenoid valve controls the direction of ozone. Before the reaction, the ozone is passed into the decomposition device for ozone decomposition. into the reaction chamber.

(2). After the pre-treatment of the measured particulate matter is carried out in the standard, it is loaded into the sample pool, and the sample pool containing the measured particulate matter is loaded into the reaction chamber with a quick locking mechanism;

(3). Ozone and particulate matter samples are mixed and reacted in the reaction chamber to ensure sufficient contact between ozone and particulate matter samples, and the reaction chamber is optically sealed to detect luminescent signals from the detection window;

(4).Use the photomultiplier tube to collect the light intensity signal sent by the reaction, and convert it into an electrical signal and send it to the data processing part for processing, and judge whether it is completed according to the conditions;

(5). Ozone remains in the flushing pipelines of the pumps and valves of the control instrument;

(6). Start the data analysis program, perform curve fitting on the collected data, and obtain the coefficient, maximum value, area, and time corresponding to the maximum value of the fitting curve formula;

(7). The obtained data is drawn into a radar chart as the oxidative luminescence characteristic of the measured particulate matter sample;

(8). Comparing the luminescence characteristics of different particulate matter samples, it is possible to distinguish the changes in the type, source, and pollution status of the sample.

The above is only a preferred embodiment of the utility model, and is not intended to limit the utility model in other forms. Any skilled person who is familiar with this profession may use the technical content disclosed above to change or remodel it into an equivalent change. Equivalent embodiment. However, any simple modifications, equivalent changes and modifications made to the above embodiments according to the technical essence of the present utility model without departing from the content of the technical solution of the utility model still belong to the protection scope of the technical solution of the utility model.

Claims (8)

1. instrument of measuring ozone oxidation solid particle deposits yields chemiluminescence rule, comprise supply unit, control circuit, external unit, universal serial bus and reaction chamber, described reaction chamber is provided with photomultiplier and sample box, it is characterized in that: also be provided with ozone generator, described ozone generator is connected by pipeline with described reaction chamber, is provided with solenoid valve on the pipeline between described ozone generator and the described reaction chamber.

2. a kind of instrument of measuring ozone oxidation solid particle deposits yields chemiluminescence rule according to claim 1, it is characterized in that: the pipeline of described ozone generator import is provided with vacuum pump and device for drying and filtering.

3. a kind of instrument of measuring ozone oxidation solid particle deposits yields chemiluminescence rule according to claim 2, it is characterized in that: also be provided with ozonolysis equipment, described ozonolysis equipment is communicated with the outlet and the described solenoid valve of described reaction chamber respectively by pipeline.

4. a kind of instrument of measuring ozone oxidation solid particle deposits yields chemiluminescence rule according to claim 3, it is characterized in that: the drying agent in the described device for drying and filtering is a silica gel.

5. a kind of instrument of measuring ozone oxidation solid particle deposits yields chemiluminescence rule according to claim 1 is characterized in that: be provided with seal between described reaction chamber and the described sample box.

6. according to claim 2 or 3 described a kind of instruments of measuring ozone oxidation solid particle deposits yields chemiluminescence rule, it is characterized in that: described photomultiplier transfers to control circuit with the detectable signal that collects, control circuit carries out conversion process to detectable signal, and to generate analysis result transfer to described external unit by universal serial bus.

7. a kind of instrument of measuring ozone oxidation solid particle deposits yields chemiluminescence rule according to claim 6, it is characterized in that: described external unit is computing machine or microprocessor.

8. a kind of instrument of measuring ozone oxidation solid particle deposits yields chemiluminescence rule according to claim 7, it is characterized in that: described universal serial bus is RS485 or RS232 interface.

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