Automatic quality inspection system for gas standard substance

Abstract

The utility model relates to the technical field of preparation inspection and verification of gas standard substances, and discloses an automatic quality inspection system for gas standard substances, which comprises an upper computer data processing terminal, a spectrum direct reading instrument, a gas chromatographic analyzer, a diluting device and an automatic sampling device, the upper computer data processing terminal processes the real-time working states read from the automatic sampling device and the diluting device and issues a valve command; the automatic sample introduction device is connected with multiple bottles of gas to multiple spectrum direct reading instruments or dilution devices at the same time to carry out direct sample introduction or dilution sample introduction, and the automatic sample introduction device can limit the sample amount of direct sample introduction through a flow limiting gas resistor. According to the utility model, full-automatic standard gas analysis and quality inspection are realized, manual duty is not needed for a long time, and gas standard substance quality inspection work of sample injection gas cylinder replacement, sample injection quantity flow limiting, high-concentration gas dilution analysis, component verification, quantity value traceability, quality inspection document editing and database uploading can be automatically completed.

Description

Technical Field

[0001] The utility model relates to the technical field of preparation, inspection and verification of gas standard substances, in particular to an automatic quality inspection system for gas standard substances. Background Art

[0002] Standard gases are standard substances. Standard substances are highly uniform, stable and accurate measurement standards. They have the basic functions of reproducing, preserving and transferring measurement values. They are used to calibrate measuring instruments and measurement processes in the fields of physics, chemistry, biology and engineering measurement, evaluate the accuracy of measurement methods and the detection capabilities of testing laboratories, determine the characteristic values ​​of materials or products, and conduct value arbitration. They can be used for quality control of gas products, detection and calibration of instruments and meters, detection of atmospheric environmental pollution, medical and health care and clinical testing, etc.

[0003] Due to the limitations of standard gas preparation technology, as a certified national standard material production enterprise, the produced gas materials should be traced, preserved and transmitted from multiple angles and methods; the quality inspection process involves the use of a series of professional testing instruments such as pressure reducing valves, dilution devices, and spectral instruments, which places high demands on the professionalism of the users; at the same time, a series of tasks such as experimental data recording, certificate printing, and gas container registration in the quality inspection process may result in scattered data, resulting in missing data comparison and tracking, causing unnecessary work redundancy, so data facts should be summarized and recorded in conjunction with servers and other communication terminals. Utility Model Content

[0004] In view of the above problems, the purpose of this utility model is to provide an automatic quality inspection system for gas standard materials, realize fully automatic standard gas analysis quality inspection, and can automatically complete the gas standard material quality inspection work such as replacement of injection gas cylinders, injection volume flow limiting, high concentration gas dilution analysis, component verification, value traceability, editing quality inspection documents and uploading them to the database without manual supervision for a long time. The technical solution is as follows:

[0005] An automatic quality inspection system for gas standard substances, comprising a host computer data processing terminal, an automatic sample injection device, two gas chromatographs, a spectrometer direct reader and a dilution device; information communication is transmitted between the components by a data transmission line, and gas is transported by a gas transmission pipeline;

[0006] The host computer data processing terminal is connected to the automatic sample injection device through a data transmission line, sends communication commands of channel selection and dilution parameters to the automatic sample injection device, and simultaneously receives the spectrum direct reading instrument data and dilution device parameters returned by the automatic sample injection device;

[0007] The host computer data processing terminal is also connected to the first gas chromatograph through a data transmission line, sends an injection sequence to the first gas chromatograph through the chromatographic workstation online working mode, and reads the chromatogram and key parameters in the chromatogram from the first gas chromatogram through the chromatographic workstation offline working mode;

[0008] The automatic sampling device is provided with a high-pressure sampling port, a low-pressure sampling port and three outlets, the high-pressure sampling port and the low-pressure sampling port are respectively connected to the high-pressure standard gas cylinder and the low-pressure standard gas cylinder, and the three outlets are respectively connected to the dilution device, the spectrometer direct reader and the second gas chromatograph through the gas transmission pipeline;

[0009] The automatic sampling device is also connected to the dilution device, the spectrum direct reader and the second gas chromatograph through a data transmission line; the automatic sampling device manages the gas sampling sequence in the system according to the instruction signal of the host computer data processing terminal and transmits a start-stop signal to the dilution device according to whether the gas needs to be diluted, and at the same time feeds back the test data in the spectrum direct reader and the second gas chromatograph and the working status information of the dilution device to the host computer data processing terminal; the dilution device receives the dilution demand signal transmitted by the automatic sampling device, and at the same time switches the gas path according to the status of the spectrum direct reader and the second gas chromatograph;

[0010] The dilution device is connected to the first gas chromatograph through a data transmission line, and at the same time transmits the diluted gas to the first gas chromatograph through a gas transmission pipeline for component analysis.

[0011] Furthermore, the spectrometer is directly connected to the host computer data processing terminal through a data transmission line to upload the type, concentration and flow data information of the detected gas in real time; the spectrometer is also connected to the dilution device and the automatic sampling device through the gas pipeline to absorb the samples submitted by the automatic sampling device and the dilution device.

[0012] Furthermore, the host computer data processing terminal is provided with a signal line interface, a host computer host, a PC display screen, a mobile touch display screen and a signal transmission line; the signal transmission line uses TCP / IP communication to send commands to the automatic sampling device, and at the same time reads the data in the spectrometer and the first gas chromatograph through TCP / IP communication for processing; the host computer data processing terminal is also connected to a barcode scanner, an industrial tablet computer, a marking machine and an RFID reader.

[0013] Furthermore, the automatic sampling device has a built-in sampling selection valve, a high-pressure critical flow component and a low-pressure critical flow component;

[0014] The low-pressure injection port is connected to the gas inlet end of the injection selection valve, and the gas outlet end of the injection selection valve is connected to the spectrometer and the second gas chromatograph through two outlets respectively;

[0015] The high-pressure inlet is first connected to the high-pressure critical flow component to reduce the pressure of the sample for the first round, and then connected to the low-pressure critical flow component and the air inlet end of the pressure relief valve to control the injection flow rate. The air outlet end of the low-pressure critical flow component is connected to the dilution device.

[0016] Furthermore, the high-pressure critical flow group and the low-pressure critical flow group are tubular pressure differential flow control components with gradually decreasing diameters at the inlet and gradually increasing diameters at the outlet.

[0017] Furthermore, the injection selection valve is a multi-selection multi-injection valve which has been subjected to an inert treatment inside.

[0018] Furthermore, a signal processing module is provided inside the automatic sampling device, which is used to complete TCP / IP protocol communication with the host computer and communicate with the dilution device, the spectrometer and the second gas chromatograph respectively through RS232 or 485 protocol.

[0019] The beneficial effects of the utility model are as follows: the utility model realizes fully automatic standard gas analysis quality inspection, which can be done without manual supervision for a long time, and can automatically complete the replacement of sampling gas cylinders, sampling volume limiting, high-concentration gas dilution analysis, component verification, value traceability, and editing of quality inspection documents and uploading of gas standard material quality inspection work to the database; in the inspection and verification of standard gases, the components of standard materials are determined and quantified through devices such as spectrometer direct readers and gas chromatograph analyzers to identify whether the gas quality reaches the level of national standard materials, thereby improving the overall quality and standardization of gas enterprises; a complete set of automated quality inspection systems is adopted to reduce manual intervention in production processes, work tasks and operating procedures; autonomous operation and control processes are achieved through automatic equipment and systems, making the production process continuous, high-speed and accurate, improving efficiency while reducing labor costs, and factual records avoid fraud and effectively reduce the possibility of safety accidents during gas inspections. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] Figure 1 This is a structural diagram of the automatic quality inspection system for gas standard substances of the utility model.

[0021] Figure 2 This is the structural diagram of the automatic sampling device. DETAILED DESCRIPTION

[0022] The utility model is further described in detail below with reference to the accompanying drawings and specific embodiments.

[0023] like Figure 1As shown, the automatic quality inspection system for gas standard substances of the utility model is composed of a host computer data processing terminal, a spectrometer direct reader, a gas chromatograph, a dilution device and an automatic sampling device. Information communication is transmitted between the components via data transmission lines, and the gas transmission lines are connected using gas transmission pipelines made of anti-adsorption materials.

[0024] The host data processing terminal includes a host computer, data transmission lines and peripherals. The host computer is connected to the diluter, direct reader, peripherals and automatic sampling device through data transmission lines; the control signal is transmitted through the data connection line to allocate sampling channels, create sampling methods, preset dilution and injection sequences, read analysis data, feedback control signals and finally complete the archiving of analysis data.

[0025] The host computer data processing terminal is connected to the automatic sampling device, gas chromatograph, barcode scanner and other peripherals at the same time; it sends communication commands such as sampling channel selection and dilution parameters to the automatic sampling device through the TCP / IP protocol, and accepts the direct reading instrument data and dilution device parameters returned by the automatic sampling device; the host computer data processing terminal sends the injection sequence to the gas chromatograph through the online working mode of the chromatographic workstation, and reads the chromatogram from the gas chromatograph through the offline working mode of the chromatographic workstation and brings the key parameters in the graph into the established table for qualified judgment.

[0026] In a short period of time, users can achieve unattended gas quality inspection throughout the entire process simply by issuing operating instructions such as standard gas concentration, target concentration and injection channel from the host computer or setting the injection sequence through the chromatographic workstation.

[0027] The host computer can also be connected to peripheral instruments such as barcode scanners, marking machines, industrial tablets, etc., and basic information such as gas cylinder number and gas order date can be input to the host computer data terminal. Entering the basic information of the standard substance gas cylinder into the system can form a real-time testing and real-time recording working mode.

[0028] The host computer data processing terminal is composed of a signal line interface, a host computer, a PC display screen, a mobile touch display screen, and a signal transmission line; the host computer serves as the highest control unit of the entire system to perform analytical operations on the data signals of the overall gas standard material quality inspection; the multi-screen design allows the operator to program the operation of the entire system through independent control software in the traditional PC Windows system, or to control the entire automatic quality inspection system through the app in the touch screen of the mobile terminal; the signal transmission line connects the automatic sampling device, uses TCP / IP communication to send commands to the sampling device, etc., and can also read the data in the direct reader and chromatograph analyzer through TCP / IP for processing; the host computer data processing terminal can also connect to many peripherals, including but not limited to barcode scanners, industrial tablet computers, marking machines, RFID readers, etc., and add information acquisition paths according to needs.

[0029] The automatic sampling device is connected to the host computer data terminal through upward communication, and is connected to the dilution device, spectrometer and gas chromatograph through RS-232 and RS-485 protocol communication and returns relevant analysis data. The hardware gas circuit connection is connected to the high-pressure standard gas cylinder and the low-pressure standard gas cylinder from the high-pressure sampling port and the low-pressure sampling port respectively.

[0030] The dilution device is connected to the automatic sampling device through RS-232 serial communication, and is connected to the gas chromatograph through RS-485 serial communication. At the same time, the diluted gas is transported to the gas chromatograph through the hardware gas pipeline for component analysis. Specifically, the dilution device receives the dilution demand signal transmitted by the automatic sampling device through the data transmission line, and is compatible with three sets of experimental coefficients of nitrogen base gas standard gas, hydrogen base gas standard gas and air base gas standard gas. The dilution sequence can be preset through the host computer data terminal or manual setting to achieve the injection concentration that changes over time. At the same time, the gas line is switched according to the status of the direct reader and the chromatograph; it covers a wide range of single or multi-component gases, and can be injected after diluting up to 1 million times according to experimental requirements. At the same time, the injection flow rate is controlled to stabilize the repeatability of each injection experimental condition.

[0031] The dilution device can continuously dilute the standard substance or the raw gas for configuration, while limiting the gas flow rate for analysis, and input it into the spectrometer for fixed value analysis. The dilution device can select the dilution device with different materials according to the different gas paths of the analyzed gas. For example, if it is a non-toxic, harmless and anti-adsorption gas, a dilution device built with MFC (thermal mass flowmeter) can be used. If toxic gas or high negative absorption gas is used, the critical flow sharp hole gas dilution method is used. The inside of the dilution device can be specially coated or built with anti-adsorption and anti-corrosion materials.

[0032] The spectrometer is an analytical instrument for the quality inspection system. Through its independently designed optical structure, the excitation stage directly collects light to measure the element content to determine the content of a specific standard substance; the gas chromatograph can separate and analyze multi-component mixtures to achieve accurate qualitative and quantitative analysis of substances. The spectrometer and gas chromatograph can use different analytical instruments such as vacuum X-ray fluorescence spectrometer, Fourier infrared spectrometer, mass spectrometer, SCD (sulfide chromatograph), FPD (flame photometric chromatograph) according to the composition of the analyzed gas to obtain more accurate analysis data; the analytical instrument obtains the communication commands of the injection time and injection channel with the automatic injection device through the RS232 communication protocol, and returns the analysis data to the host computer for processing and setting.

[0033] like Figure 2 As shown, the sampling device can have multiple sampling ports and multiple gas outlets. Different gas cylinders are selected through the sampling selection valve and input into different analytical instruments or different analysis channels. The built-in high-pressure critical flow component and the low-pressure critical flow component can complete the pressure reduction and then steady flow of the gas standard substance in the high-pressure gas cylinder, and the excess gas can be emptied into the waste processor.

[0034] The automatic sampling device has a built-in special plate-through connector as a high-pressure inlet and outlet and a low-pressure inlet and outlet. The low-pressure inlet is connected to the inlet end of the sampling selection valve, and the outlet end of the sampling selection valve is connected to the spectrometer and the second gas chromatograph through two outlets. The high-pressure inlet is first connected to the high-pressure critical flow component to reduce the pressure of the sample for the first round, and then connected to the low-pressure critical flow component and the inlet end of the pressure relief valve to control the injection flow rate. The outlet end of the low-pressure critical flow component is connected to the dilution device.

[0035] The two ends of the air inlet through-plate connector are respectively connected to the injection gas, the inlet end of the gate injection valve or the high-pressure injection channel; the two ends of the air outlet through-plate connector are respectively connected to the outlet end of the gate injection valve, the outlet end of the high-pressure injection, the direct reading instrument and the chromatograph.

[0036] As the core of the whole system, the automatic sampling device manages the gas sampling sequence in the system according to the indication signal of the host computer data processing terminal, transmits the start and stop signals to the dilution device according to whether the gas needs to be diluted, and feeds back the test data in the direct reader or gas chromatograph and the working status information of the dilution device to the host computer data processing terminal.

[0037] The automatic sampling device is composed of a signal processing module, a sampling selection valve, a high-pressure critical flow component, a low-pressure critical flow component, a pressure relief valve and a through-plate joint; it can meet the separate sampling needs of high-pressure and low-pressure gas cylinders. The high-pressure gas cylinder undergoes the first round of pressure reduction through the high-pressure critical flow component, and then the sampling flow is controlled by the low-pressure critical flow component and the pressure relief valve, and the low-pressure gas cylinder is directly connected to the sampling selection valve; the internal signal processing module can complete TCP / IP protocol communication with the host computer, and can also communicate with the dilution device, direct reader, and chromatograph analyzer through RS232 or 485 protocol, as an intermediate platform for signal analysis and forwarding.

[0038] Among them, the high-pressure critical flow component and the low-pressure critical flow component are designed using the critical flow orifice or Venturi sonic nozzle principle. A tubular pressure differential flow control component with an inlet that gradually shrinks to the throat and then gradually expands can be made of but not limited to stainless steel, polytetrafluoroethylene and other materials; its function is to allow high-pressure gas to be output at a reduced pressure and constant flow through a two-stage critical flow orifice within a larger pressure range, so that both high-pressure gas cylinders and low-pressure gas cylinders can be sampled through an automatic sampling device.

[0039] The injection gate valve uses a multi-select multi-injection valve that has been internally inertized. There is basically no dead volume inside the valve, which is convenient for purging with clean gas. The inert coating can effectively prevent corrosive gases from eroding the valve, helping to improve analysis accuracy. The injection gate valve can simultaneously connect multiple bottles of gas to enter the system for analysis, improve analysis efficiency, and realize the function of unattended replacement of gas cylinders.

Claims

1. A gas standard material automatic quality inspection system, characterized in that: It includes a host computer data processing terminal, an automatic sampling device, two gas chromatographs, a spectrometer and a dilution device; the components communicate with each other through data transmission lines, and the gas is transported through gas pipelines; The host computer data processing terminal is connected to the automatic sample injection device through a data transmission line, sends communication commands of channel selection and dilution parameters to the automatic sample injection device, and simultaneously receives the spectrum direct reading instrument data and dilution device parameters returned by the automatic sample injection device; The host computer data processing terminal is also connected to the first gas chromatograph through a data transmission line, sends an injection sequence to the first gas chromatograph through the chromatographic workstation online working mode, and reads the chromatogram and key parameters in the chromatogram from the first gas chromatogram through the chromatographic workstation offline working mode; The automatic sampling device is provided with a high-pressure sampling port, a low-pressure sampling port and three outlets, the high-pressure sampling port and the low-pressure sampling port are respectively connected to the high-pressure standard gas cylinder and the low-pressure standard gas cylinder, and the three outlets are respectively connected to the dilution device, the spectrometer direct reader and the second gas chromatograph through the gas transmission pipeline; The automatic sampling device is also connected to the dilution device, the spectrum direct reader and the second gas chromatograph through a data transmission line; the automatic sampling device manages the gas sampling sequence in the system according to the instruction signal of the host computer data processing terminal and transmits a start-stop signal to the dilution device according to whether the gas needs to be diluted, and at the same time feeds back the test data in the spectrum direct reader and the second gas chromatograph and the working status information of the dilution device to the host computer data processing terminal; the dilution device receives the dilution demand signal transmitted by the automatic sampling device, and at the same time switches the gas path according to the status of the spectrum direct reader and the second gas chromatograph; The dilution device is connected to the first gas chromatograph through a data transmission line, and at the same time transmits the diluted gas to the first gas chromatograph through a gas transmission pipeline for component analysis.

2. The automatic quality inspection system for gas standard substances according to claim 1 is characterized in that: The spectrometer is also directly connected to the host computer data processing terminal through a data transmission line to upload the type, concentration and flow data information of the detected gas in real time; the spectrometer is also connected to the dilution device and the automatic sampling device through the gas transmission pipeline to absorb the samples submitted by the automatic sampling device and the dilution device.

3. The automatic quality inspection system for gas standard substances according to claim 2 is characterized in that: The host computer data processing terminal is provided with a signal line interface, a host computer host, a PC display screen, a mobile touch display screen and a signal transmission line; the signal transmission line uses TCP / IP communication to send commands to the automatic sampling device, and at the same time reads the data in the spectrometer and the first gas chromatograph through TCP / IP communication for processing; the host computer data processing terminal is also connected to a barcode scanner, an industrial tablet computer, a marking machine and an RFID reader.

4. The automatic quality inspection system for gas standard substances according to claim 1 is characterized in that: The automatic sampling device is built with a sampling selection valve, a high-pressure critical flow component and a low-pressure critical flow component; The low-pressure injection port is connected to the gas inlet end of the injection selection valve, and the gas outlet end of the injection selection valve is connected to the spectrometer and the second gas chromatograph through two outlets respectively; The high-pressure inlet is first connected to the high-pressure critical flow component to reduce the pressure of the sample for the first round, and then connected to the low-pressure critical flow component and the air inlet end of the pressure relief valve to control the injection flow rate. The air outlet end of the low-pressure critical flow component is connected to the dilution device.

5. The automatic quality inspection system for gas standard substances according to claim 4 is characterized in that: The high-pressure critical flow component and the low-pressure critical flow component are tubular pressure differential flow control components with gradually narrowing diameters at the inlet and gradually widening diameters at the outlet.

6. The automatic quality inspection system for gas standard substances according to claim 4 is characterized in that: The injection selection valve is a multi-selection multi-injection valve that has been subjected to inertization treatment inside.

7. The automatic quality inspection system for gas standard substances according to claim 1 is characterized in that: The automatic sampling device is also provided with a signal processing module, which is used to complete TCP / IP protocol communication with the host computer and communicate with the dilution device, the spectrometer and the second gas chromatograph respectively through RS232 or 485 protocol.

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