A device and method for detecting consistency of customs clearance goods

Abstract

The present invention discloses a device and method for detecting the consistency of goods for customs clearance. At present, the security inspection of inbound and outbound goods by maritime and customs mainly relies on the customs declaration information of enterprises, the appearance characteristics of goods, and the professional quality of front-line personnel. It is difficult to ensure that the transported goods are consistent with the declared goods on site. Suspicious goods need to be sent to qualified laboratories in the rear for testing and confirmation, which takes a long time and is difficult to meet the needs of high-throughput on-site testing of bulk goods by maritime and customs. The present invention discloses a device and method for detecting the consistency of goods for customs clearance, which can be used for on-site rapid screening of whether the goods for customs clearance are consistent with the declared goods. The device includes: an exhaust adsorption device, an inlet, a sampling device, an ion migration tube, a mass flowmeter, a primary air purification tube, a secondary air purification tube, an air suction pump, an air filter membrane, a signal amplifier, and a signal acquisition and display device.

Description

Technical Field

[0001] The invention relates to a device and method for detecting the consistency of customs clearance goods. Background Art

[0002] At present, the maritime and customs security inspection of inbound and outbound goods mainly relies on checking documents and the appearance of goods step by step, as well as the professionalism of front-line personnel. Once deliberate concealment or document forgery occurs, it is extremely difficult for the regulatory authorities to confirm on the spot. However, it takes a long time to send suspicious goods to qualified laboratories for testing and confirmation, which is difficult to meet the needs of high-throughput on-site testing of bulk goods by maritime and customs. Therefore, customs, maritime, stations and other places are in urgent need of an instrument that can quickly confirm on the spot whether the goods are consistent with the declared goods.

[0003] Domestic and foreign scientific research institutions have done a lot of research on cargo inspection, but the inspection equipment they have developed is large in size and weight and cannot be used for on-site inspections, such as gas chromatography-mass spectrometry technology and high-performance liquid chromatography-mass spectrometry technology; some other methods are not accurate enough, the inspection costs are generally high, and the economic benefits of mass production of equipment are not obvious, such as Raman technology. Summary of the invention

[0004] The present invention develops a new method and device for detecting the consistency of customs-cleared goods based on the ion mobility spectrometry (IMS) technology with high sensitivity and fast response time. The ion mobility spectrum peak of the sample is analyzed by rapid sampling on site, and compared with the spectrum library to confirm whether it is consistent with the spectrum library peak, and then confirm whether it is consistent with the declared substance. The method of the present invention has a minimum detection limit of ppb level, an instrument response time of <1s, and an analysis cycle of the entire sample of <1min.

[0005] The present invention provides a device for detecting the consistency of customs-cleared goods, the device comprising an ion mobility spectrometer, the ion mobility spectrometer comprising a power supply (6), an ultraviolet lamp (7), an ion mobility tube (8), a signal amplifier (13), and a signal acquisition and output device (14) connected in sequence; the device also comprises an air filter (18), an air suction pump (17), a secondary air purification tube (16), and a primary air purification tube (15) connected in sequence;

[0006] The outlet pipeline of the primary air purification pipe (15) is connected to the first mass flow meter (5) and the second mass flow meter (9) respectively;

[0007] The gas outlet of the first mass flow meter (5) is connected to the gas inlet of the sampling device (3); a space for accommodating a sample bottle (4) is provided in the middle of the sampling device (3); the gas outlet of the sampling device (3) is connected to an gas inlet of the injection port (2); and the other two interfaces of the injection port (2) are respectively connected to the sample gas adsorption device (1) and the injection port of the ion migration tube (8) of the ion migration spectrometer;

[0008] The gas outlet of the second mass flow meter (9) is connected to the gas inlet at the tail end of the ion transfer tube (8) close to the Faraday disk;

[0009] The gas outlet of the migration spectrometer in the example is connected in sequence to a third mass flow meter (10), an exhaust gas pump (11), and an exhaust gas adsorption device (12).

[0010] The present invention provides a method for detecting the consistency of customs clearance goods, using the above-mentioned device, comprising the following steps:

[0011] ① Under the action of the suction pump (17), the outside air passes through the air filter (18) to remove particulate matter in the air, and then is discharged through the suction pump (17) and the air secondary purification pipe (16) and the air primary purification pipe (15) in sequence, forming two paths of clean air, which are respectively controlled by the first mass flow meter (5) and the second mass flow meter (9) for use by the ion mobility spectrometer;

[0012] ② The clean air enters the ion transfer tube (8) through the second mass flow meter (9) to form a clean gas atmosphere;

[0013] ③ The sample placed in the sample bottle (4) is carried by the clean air flowing through the first mass flow meter (5) and the sampling device (3), a portion of which enters the ion transfer tube (8) through the injection port (2) for analysis, and the excess sample gas is processed by the sample gas adsorption device (1) and then discharged;

[0014] ④ The sample entering the ion transfer tube (8) generates ions under the action of the ultraviolet lamp (7), which are separated and detected by the ion transfer tube (8), and the output electrical signal is received and displayed by the signal acquisition and output device (14) after passing through the signal amplifier (13);

[0015] ⑤ After the analysis is completed, the exhaust gas is discharged from the tail gas port of the ion transfer tube (8) together with the sample gas. The tail gas enters the tail gas adsorption device (12) at a constant flow rate through the mass flow meter (10) and the tail gas pump (11) and is then discharged after being processed.

[0016] Furthermore, in the above technical solution, the sampling device (3) is made of polytetrafluoroethylene material, the upper part is a rotatably sealed bottle cap, and a silicone O-ring seal is lined between the bottle cap and the bottle body; the air inlet of the sampling device (3) is located at the upper end of the device, and the air outlet is located at the lower end of the device, so that the gas input into the sampling device (3) carries the sample from the top and then flows out from the bottom of the device and is transported to the sampling port (2).

[0017] Furthermore, in the above technical solution, under the action of the tail gas pump (11), the flow rate of the third mass flow meter (10) is greater than the flow rate of the second mass flow meter (9), so that the ion transfer tube (8) can absorb the required sample from the injection port (2). The injection volume of the ion transfer tube (8) is the flow rate obtained there, and the injection volume can be changed by changing the difference between the flow rates of the second and third mass flow meters (9, 10).

[0018] Furthermore, in the above technical solution, the sample enters the ionization zone of the ion transfer tube (8) and is discharged from the outlet close to the ultraviolet lamp (7). The distance between the air outlet of the ion transfer tube (8) and the ultraviolet lamp (7) is between 0.2-1 cm, so that the sample is closest to the ultraviolet lamp, ensuring that the sample is fully ionized, thereby improving the sensitivity of detection.

[0019] Furthermore, in the above technical solution, the sample ions in the ion transfer tube (8) reach the migration zone through the periodically opened ion gate, and are separated according to the difference in ion mobility, and then reach the Faraday disk in turn; different samples can be detected according to the arrival time of different ions.

[0020] Furthermore, in the above technical solution, the method of the present invention has a minimum detection limit of ppb level, an instrument response time of <1s, and an analysis cycle of the entire sample of <1min.

[0021] Furthermore, in the above technical solution, this method uses ion migration spectrometry as a basis for judgment, compares the sample spectrum obtained by real-time measurement with the standard spectrum of the declared goods, confirms whether the peak position and peak number are consistent, and thus confirms on-site whether the cleared goods are consistent with the declared goods.

[0022] The advantages of the present invention are as follows:

[0023] The method of the present invention has a minimum detection limit of ppb level, an instrument response time of less than 1s, and an analysis cycle of the entire sample of less than 1min. Using the ion migration spectrum as a basis for judgment, the sample spectrum obtained by real-time measurement is compared with the standard spectrum of the declared goods to confirm whether the peak position and peak number are consistent, and whether the customs clearance goods are consistent with the declared goods can be confirmed on site.

[0024] 1. The detection limit of the method of the present invention is extremely low, which can reach ppb level, and low-volatility liquids and solids can be sampled and analyzed on site.

[0025] The instrument response time is less than 1s, which is much higher than the requirements of the national standard (GB50493-2009). It can issue an early warning when the concentration level of hazardous chemical leakage is far below the lower explosion limit or toxic level.

[0026] 2. The analysis speed of the method of the present invention is extremely fast, and the analysis cycle of the entire sample is less than 1 minute, which can meet the needs of on-site bulk cargo customs clearance inspection.

[0027] 3. The device of the method of the present invention has a small size, a small mass, and a low power consumption, and can be placed at the detection site for use. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] Figure 1 It is a design schematic diagram of a device and method for detecting the consistency of customs-cleared goods, wherein 1 is a sample gas adsorption device, 2 is a sample inlet, 3 is a sampling device, 4 is a sample bottle, 5 is a first mass flow meter, 6 is a power supply, 7 is an ultraviolet lamp, 8 is an ion migration tube, 9 is a second mass flow meter, 10 is a third mass flow meter, 11 is an exhaust pump, 12 is an exhaust gas adsorption device, 13 is a signal amplifier, 14 is a signal acquisition and output device, 15 is a primary air purification tube, 16 is a secondary air purification tube, 17 is an air suction pump, and 18 is an air filter membrane;

[0029] Figure 2 is the standard spectrum of ion mobility spectrometry of acetone;

[0030] Figure 3 This is the standard ion mobility spectrum of p-xylene;

[0031] Figure 4 is the standard spectrum of ion mobility spectrometry of styrene;

[0032] Figure 5 This is the standard ion mobility spectrum of o-xylene. DETAILED DESCRIPTION

[0033] ] The following examples illustrate the use of the present invention but do not limit the scope of application described.

[0034] like Figure 1 As shown, a device for detecting the consistency of goods passing customs, the device includes an ion mobility spectrometer, the ion mobility spectrometer includes a power supply 6, an ultraviolet lamp 7, an ion migration tube 8, a signal amplifier 13, and a signal acquisition and output device 14 connected in sequence; the device also includes an air filter 18, an air suction pump 17, a secondary air purification tube 16, and a primary air purification tube 15 connected in sequence;

[0035] The outlet pipeline of the primary air purification pipe 15 is connected to the first mass flow meter 5 and the second mass flow meter 9 respectively;

[0036] The gas outlet of the first mass flowmeter 5 is connected to the gas inlet of the sampling device 3. A space for accommodating a sample bottle 4 is provided in the middle of the sampling device 3. The gas outlet of the sampling device 3 is connected to an gas inlet of the injection port 2. The other two interfaces of the injection port 2 are respectively connected to the injection ports of the sample gas adsorption device 1 and the ion migration tube 8 of the ion migration spectrometer;

[0037] The gas outlet of the second mass flow meter 9 is connected to the gas inlet at the tail of the ion transfer tube 8 close to the Faraday disk;

[0038] The gas outlet of the migration spectrometer in the example is connected to a third mass flow meter 10, an exhaust gas pump 11, and an exhaust gas adsorption device 12 in sequence.

[0039] The present invention provides a method for detecting the consistency of customs clearance goods, using the above-mentioned device, comprising the following steps:

[0040] ① Under the action of the suction pump 17, the outside air passes through the air filter 18 to remove particulate matter in the air, and then is discharged through the suction pump 17 and the air secondary purification pipe 16 and the air primary purification pipe 15 in sequence, forming two paths of clean air, which are respectively controlled by the first mass flow meter 5 and the second mass flow meter 9 for use by the ion mobility spectrometer;

[0041] ② Clean air enters the ion transfer tube 8 through the second mass flow meter 9 to form a clean gas atmosphere;

[0042] ③ The sample placed in the sample bottle 4 is carried by the clean air flowing through the first mass flow meter 5 and the sampling device 3, a part of which enters the ion transfer tube 8 through the inlet 2 for analysis, and the excess sample gas is processed by the sample gas adsorption device 1 and then discharged;

[0043] ④ The sample entering the ion transfer tube 8 generates ions under the action of the ultraviolet lamp 7, which are separated and detected by the ion transfer tube 8, and the output electrical signal is received and displayed by the signal acquisition and output device 14 after passing through the signal amplifier 13;

[0044] ⑤ After the analysis is completed, the exhaust gas is discharged from the tail gas port of the ion transfer tube 8 together with the sample gas. The tail gas enters the tail gas adsorption device 12 at a constant flow rate through the mass flow meter 10 and the tail gas pump 11 and is then discharged after being treated.

[0045] The sampling device 3 is made of polytetrafluoroethylene material, and the upper part is a rotatably sealed bottle cap, and a silicone O-ring seal is lined between the bottle cap and the bottle body; the air inlet of the sampling device 3 is located at the upper end of the device, and the air outlet is located at the lower end of the device, so that the gas input into the sampling device 3 carries the sample from the top and then flows out from the bottom of the device and is transported to the sampling port 2.

[0046] Under the action of the tail gas pump 11, the flow rate of the third mass flow meter 10 is greater than the flow rate of the second mass flow meter 9, so that the ion transfer tube 8 can absorb the required sample from the injection port 2. The injection volume of the ion transfer tube 8 is the flow rate obtained there, and the injection volume can be changed by changing the difference between the flow rates of the second and third mass flow meters 9 and 10.

[0047] The sample enters the ionization zone of the ion transfer tube 8 and is discharged from the outlet near the ultraviolet lamp 7. The distance between the outlet of the ion transfer tube 8 and the ultraviolet lamp 7 is between 0.2-1 cm, which makes the sample closest to the ultraviolet lamp to ensure that the sample is fully ionized, thereby improving the sensitivity of detection.

[0048] In the ion transfer tube 8, the sample ions reach the migration zone through the periodically opened ion gate, and after being separated according to the difference in ion mobility, they reach the Faraday disk one after another; different samples can be detected according to the arrival time of different ions.

[0049] The method of the present invention has a minimum detection limit of ppb level, an instrument response time of less than 1s, and an analysis cycle of the entire sample of less than 1min.

[0050] This method uses ion migration spectrometry as a basis for judgment. The sample spectrum obtained by real-time measurement is compared with the standard spectrum of the declared goods to confirm whether the peak position and peak number are consistent. This can confirm on-site whether the cleared goods are consistent with the declared goods.

[0051] Example 1

[0052] A device and method for detecting the consistency of customs clearance goods, when a VUV lamp is used as an ionization source, the migration zone voltage is set to 600V / cm, the drift gas flow rate is set to 400ml / min, the tail gas flow rate is set to 600ml / min, and the sampling volume is 200ml / min. Figure 2 As shown in the figure, the standard ion migration spectrum of acetone is a single peak at 5.7ms. Therefore, it is possible to judge whether the transported goods are acetone based on the position and quantity of the peak.

[0053] Example 2

[0054] A device and method for detecting the consistency of customs clearance goods, when a VUV lamp is used as an ionization source, the migration zone voltage is set to 600V / cm, the drift gas flow rate is set to 400ml / min, the tail gas flow rate is set to 600ml / min, and the sampling volume is 200ml / min. Figure 3 As shown in the figure, the standard ion migration spectrum of p-xylene is a single peak at 5.36ms. Therefore, it is possible to judge whether the transported goods are p-xylene based on the position and quantity of the peak.

[0055] Example 3

[0056] A device and method for detecting the consistency of customs clearance goods, when a VUV lamp is used as an ionization source, the migration zone voltage is set to 600V / cm, the drift gas flow rate is set to 400ml / min, the tail gas flow rate is set to 600ml / min, and the sampling volume is 200ml / min. Figure 4 As shown, the standard ion migration spectrum of styrene has two peaks at 7.34ms and 9.27ms. Therefore, it is possible to determine whether the transported goods are styrene based on the position and number of the peaks.

[0057] Example 4

[0058] A device and method for detecting the consistency of customs clearance goods, when a VUV lamp is used as an ionization source, the migration zone voltage is set to 600V / cm, the drift gas flow rate is set to 400ml / min, the tail gas flow rate is set to 600ml / min, and the sampling volume is 200ml / min. Figure 5 As shown in the figure, the standard ion migration spectrum of o-xylene is a single peak at 5.38ms. Therefore, it is possible to judge whether the transported goods are o-xylene based on the position and quantity of the peak.

Claims

1. A device for detecting the consistency of goods during customs clearance, characterized in that: The device comprises an ion mobility spectrometer, which comprises a power supply (6), an ultraviolet lamp (7), an ion mobility tube (8), a signal amplifier (13), and a signal acquisition and output device (14) connected in sequence; the device also comprises an air filter (18), an air suction pump (17), a secondary air purification tube (16), and a primary air purification tube (15) connected in sequence; The outlet pipeline of the primary air purification pipe (15) is respectively connected to the first mass flow meter (5) and the second mass flow meter (9); The gas outlet of the first mass flow meter (5) is connected to the gas inlet of the sampling device (3); a space for accommodating a sample bottle (4) is provided in the middle of the sampling device (3); the gas outlet of the sampling device (3) is connected to an gas inlet of the injection port (2); and the other two interfaces of the injection port (2) are respectively connected to the sample gas adsorption device (1) and the injection port of the ion migration tube (8) of the ion migration spectrometer; The gas outlet of the second mass flow meter (9) is connected to the gas inlet at the rear end of the ion transfer tube (8) close to the Faraday disk; The gas outlet of the ion mobility spectrometer is connected in sequence to a third mass flow meter (10), an exhaust gas pump (11), and an exhaust gas adsorption device (12); The steps for consistency testing of goods through customs are as follows: ① Under the action of the suction pump (17), the outside air passes through the air filter (18) to remove particulate matter in the air, and then is discharged through the suction pump (17) and the air secondary purification pipe (16) and the air primary purification pipe (15) in sequence, forming two paths of clean air, which are respectively controlled by the first mass flow meter (5) and the second mass flow meter (9) for use by the ion mobility spectrometer; ② The clean air enters the ion transfer tube (8) through the second mass flow meter (9) to form a clean gas atmosphere; ③ The sample placed in the sample bottle (4) is carried by the clean air flowing through the first mass flow meter (5) and the sampling device (3), a portion of which enters the ion transfer tube (8) through the injection port (2) for analysis, and the excess sample gas is discharged after being processed by the sample gas adsorption device (1); ④ The sample entering the ion transfer tube (8) generates ions under the action of the ultraviolet lamp (7), which are separated and detected by the ion transfer tube (8), and the output electrical signal is received and displayed by the signal acquisition and output device (14) after passing through the signal amplifier (13); ⑤ After the analysis is completed, the exhaust gas is discharged from the tail gas port of the ion transfer tube (8) together with the sample gas. The tail gas enters the tail gas adsorption device (12) at a constant flow rate through the third mass flow meter (10) and the tail gas pump (11) and is discharged after being processed; The sampling device (3) is made of polytetrafluoroethylene material, and the upper part is a rotatably sealed bottle cap, and a silicone O-ring is lined between the bottle cap and the bottle body for sealing; the air inlet of the sampling device (3) is located at the upper end of the device, and the air outlet is located at the lower end of the device, so that the gas input into the sampling device (3) carries the sample from the top and then flows out from the bottom of the device and is transported to the sampling port (2); Under the action of the exhaust pump (11), the flow rate of the third mass flow meter (10) is greater than the flow rate of the second mass flow meter (9), so that the ion transfer tube (8) can absorb the required sample from the injection port (2). The injection volume of the ion transfer tube (8) is the flow rate obtained by the ion transfer tube (8) from the injection port (2). The injection volume can be changed by changing the difference between the flow rates of the second and third mass flow meters (9, 10).

2. The device according to claim 1, characterized in that: The sample enters the ionization zone of the ion migration tube (8) and is discharged from the outlet near the ultraviolet lamp (7). The distance between the outlet of the ion migration tube (8) and the ultraviolet lamp (7) is between 0.2 and 1 cm, so that the sample is closest to the ultraviolet lamp, ensuring that the sample is fully ionized, thereby improving the sensitivity of the detection.

3. The device according to claim 1, characterized in that: In the ion transfer tube (8), the sample ions reach the migration zone through the periodically opened ion gate, and are separated according to the difference in ion mobility, and then reach the Faraday disk in sequence; different samples can be detected according to the arrival time of different ions.

4. The device according to claim 1, characterized in that: Using the ion migration spectrum as the basis for judgment, the sample spectrum obtained by real-time measurement is compared with the standard spectrum of the declared goods to confirm whether the peak position and peak number are consistent, so as to confirm on-site whether the cleared goods are consistent with the declared goods.

Images