Pluggable split sample injection port device

Abstract

The utility model relates to the field of micro coulomb sulfur analyzers, and discloses a plug-in type split sample injection port device which comprises a sample injection pipe, wherein the outlet end of the sample injection pipe is in a straight pipe shape and is provided with a first opening; the inlet end of the sample injection pipe is provided with a second opening, and a rubber plug is hermetically arranged in the second opening; the first opening is used for being inserted into a sample inlet of the quartz tube so as to communicate the quartz tube with the sample inlet tube. According to the plug-in type split sample injection port device, the straight-tube-shaped first opening is directly inserted into the quartz tube, the quartz tube is communicated with the sample injection tube, and the rubber plug at the second opening is used as a sealing gasket of a new sample injection port. The plug-in type split sample injection port device is far away from a high-temperature hearth, the temperature is low, the rubber plug can be replaced by directly touching the split sample injection port with a hand, the rubber plug can be manually replaced at the normal temperature, and the operation is very convenient and rapid; during sample injection, the positioning and orientation of the sample injection needle are accurate, and the accuracy of a sample analysis result is improved.

Description

Technical Field

[0001] The utility model relates to the field of microcoulomb sulfur analyzers, in particular to a plug-in split sample inlet device. Background Art

[0002] Sulfide is one of the main hazards that cause equipment corrosion, catalyst poisoning and engine wear. The determination of sulfur content is of great significance in petroleum refining. Refining and chemical companies generally have hundreds of samples to analyze for sulfur content every day, and it is urgent to increase the speed of sulfur content analysis. At present, the method for determining sulfur content is mainly to use the microcoulometric method, that is, to inject the sample into the gasification section of the quartz tube through the rubber plug of the quartz tube inlet with a syringe. The sample is heated and vaporized in the gasification section, enters the combustion section with the carrier gas and mixes with oxygen to burn, and the combustion products enter the titration cell for detection.

[0003] During the measurement process, the temperature of the quartz tube gasification section is as high as 700℃ or more. Since the injection port of the quartz tube is connected to the gasification section of the quartz tube, the temperature of the injection port is also high and cannot be touched by hand, otherwise it will be hot. In addition, the rubber plug of the traditional quartz tube injection port is easily punctured and leaked after being pierced by the syringe needle many times, which affects the detection accuracy. It is necessary to frequently replace the expired rubber plug from the high-temperature injection port. Due to the high temperature of the quartz tube injection port, gloves must be worn when replacing the rubber plug. Tweezers must be used to operate. The left hand holds the tweezers to clamp the neck of the injection port, and the right hand holds the rubber plug and squeezes it into the injection port. Slowly squeeze the rubber plug into the injection port. There is a safety risk of hand burns during the operation, and the operation is inconvenient. The replacement time of the rubber plug is long, which affects the analysis of the sample. Sometimes, if the laboratory personnel operate carelessly or squeeze the rubber plug too hard, the nitrogen or oxygen inlet pipe will be broken, causing the quartz tube to be scrapped due to damage, and a new quartz tube needs to be replaced, increasing production costs. The injection port of a traditional quartz tube has a large diameter. The direction of the syringe needle cannot be controlled during the insertion of the rubber plug in the injection port. It often deviates and hits the spiral tube in the quartz tube, which prevents the needle from further insertion. In severe cases, the spiral tube in the quartz tube will be broken, causing the quartz tube to be scrapped. In order to avoid high-temperature burns on the hands when changing the rubber plug, the laboratory personnel pull the quartz tube out of the furnace, cool it in the air, and wait until the temperature of the injection port cools to room temperature before changing the rubber plug. This wastes time and causes sample analysis to lag. The sulfide in the sample is adsorbed by the air bag, affecting the accuracy of the analysis results. Utility Model Content

[0004] The purpose of the utility model is to provide a plug-in split sample injection port device, which is used to solve the technical problems of easy scalding of hands when replacing rubber plugs under high temperature conditions, inconvenient operation, and breaking of nitrogen and oxygen inlet pipes when replacing rubber plugs, so that replacing rubber plugs is safer, more convenient and faster, and the positioning and orientation of the syringe needle during injection is more accurate, thereby improving the accuracy of sample analysis results and avoiding damage to the quartz tube during injection that affects sample analysis.

[0005] In order to achieve the above-mentioned purpose, the utility model provides a pluggable split injection port device, including an injection tube: the outlet end of the injection tube is a straight tube and has a first opening; the inlet end of the injection tube has a second opening, and a rubber plug is sealed in the second opening; the first opening is used to be inserted into the injection port of a quartz tube to connect the quartz tube and the injection tube.

[0006] As a preferred solution, the sample injection tube includes a straight tube body and an inlet tube integrally formed with the tube body, the first opening is located at the outlet end of the tube body, and the second opening is located at the inlet end of the inlet tube.

[0007] As a preferred solution, there is an integrally formed inlet pipe between the tube body and the second opening tube, the diameter of the inlet pipe is larger than the diameter of the tube body, and the diameter of the inlet pipe gradually increases and then decreases from the end connected to the tube body to the end connected to the second opening.

[0008] As a preferred solution, a sealing sleeve is sleeved at the connection between the tube body and the inlet pipe, and the sealing sleeve extends from the vicinity of the first opening on the tube body to the connection between the tube body and the inlet pipe.

[0009] As a preferred solution, the sealing sleeve is a silicone rubber sleeve.

[0010] As a preferred embodiment, the length of the tube is 1 cm to 1.7 cm;

[0011] The length of the sealing sleeve is 0.7 cm to 0.9 cm.

[0012] Compared with the prior art, the plug-in split sample inlet device of the utility model has the following beneficial effects:

[0013] The plug-in split injection port device of the embodiment of the utility model includes an injection tube: the outlet end of the injection tube is a straight tube and has a first opening; the inlet end of the injection tube has a second opening, and a rubber plug is sealed in the second opening; the first opening is used to be inserted into the injection port of the quartz tube to connect the quartz tube and the injection tube; when it is used, the straight tube-shaped first opening is directly inserted into the quartz tube to connect the quartz tube and the injection tube. The rubber plug at the second opening is used as a sealing gasket for the new injection port. The plug-in split injection port device of the present application is far away from the high-temperature furnace and the temperature is relatively low. The rubber plug can be directly replaced by touching the split injection port with hands, or the split injection port can be pulled out and reinserted into the original place after replacing the rubber plug at room temperature, so that the rubber plug can be manually replaced at room temperature. The operation is very convenient, and there will be no safety accidents of scalding hands, and no accidents of damaging the quartz tube. At the same time, the straight tube body guides the injection needle, making the needle orientation more accurate and the insertion smoother during injection. The measurement results are consistent with the traditional methods. It has a good application effect in sulfur content analysis in petrochemical enterprises and improves the accuracy of sample analysis results. BRIEF DESCRIPTION OF THE DRAWINGS

[0014] Figure 1 Schematic diagram of a plug-in split sample inlet device according to an embodiment of the utility model;

[0015] Figure 2 It is a schematic diagram of the connection between the plug-in split injection port device and the quartz tube in the embodiment of the utility model;

[0016] Figure 3 It is a spectrum diagram of measuring the sulfur content in a sample by using the utility model.

[0017] In the figure, 10, sample injection tube, 11, first opening, 12, second opening, 13, tube body, 14, inlet tube, 20, rubber plug, 30, sealing sleeve. DETAILED DESCRIPTION

[0018] The following is a further detailed description of the specific implementation of the present invention in conjunction with the accompanying drawings and examples. The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention.

[0019] like Figure 1 to Figure 2As shown, a plug-in split injection port device of a preferred embodiment of the utility model comprises an injection tube 10, which is specifically a quartz tube; the outlet end of the injection tube 10 is a straight tube and has a first opening 11; the inlet end of the injection tube 10 has a second opening 12, and a rubber plug 20 is sealed in the second opening 12; the first opening 11 is used to be inserted into the injection port of the quartz tube to connect the quartz tube and the injection tube 10. When in use, the straight first opening 11 is directly inserted into the quartz tube to connect the quartz tube and the injection tube 10. The rubber plug 20 at the second opening 12 is used as a sealing gasket for a new injection port. The plug-in split injection port device of the present application is far away from the high-temperature furnace, and the temperature is relatively low. The split injection port can be directly touched by hand to replace the rubber plug 20, or the split injection port can be pulled out, replaced at room temperature and then reinserted back to its original position, so as to achieve the purpose of manually replacing the rubber plug 20 at room temperature. The operation is very convenient, and there will be no safety accidents of scalding hands, and the waiting time for cooling is avoided. The whole operation time is short, and the timely analysis of the sample is not affected, and there will be no accidental incidents of damaging the quartz tube. At the same time, through the guiding effect of the tube body on the injection needle, the needle orientation is more accurate during injection, and the insertion is smoother. The measurement results are consistent with the traditional method, and the application effect is good in the sulfur content analysis of petrochemical enterprises, which improves the accuracy of the sample analysis results.

[0020] In a specific embodiment of the present application, the injection tube 10 includes a straight tube body 13 and an inlet tube integrally formed with the tube body 13, the first opening 11 is located at the outlet end of the tube body 13, and the second opening 12 is located at the inlet end of the inlet tube. The tube body 13 of the injection tube 10 guides the insertion of the injection needle, ensuring that the analysis result of the sample remains stable and preventing the needle from deviating in direction during the insertion process and hitting or breaking the spiral tube in the quartz tube.

[0021] In a specific embodiment of the present application, there is an inlet pipe 14 formed integrally between the tube body 13 and the second opening, the diameter of the inlet pipe is larger than the diameter of the tube body 13, and the diameter of the inlet pipe 14 gradually increases and then gradually decreases from the end connected to the tube body 13 to the end connected to the second opening. The inlet pipe 14 in the present application is conical or funnel-shaped, which facilitates the insertion of the rubber plug 20 into the inlet pipe and seals the inlet pipe at the same time.

[0022] In a specific embodiment of the present application, a sealing sleeve 30 is sleeved at the connection between the tube body 13 and the inlet tube, and the sealing sleeve 30 extends from the vicinity of the first opening 11 along the tube body to the connection between the tube body 13 and the inlet tube 14. The sealing sleeve 30 can ensure that the silicone rubber sleeve is sealed and connected to the injection port of the traditional quartz tube without air leakage. The depth of the inlet tube can be determined according to the length requirement of the rubber plug 20 inserted into the inlet tube.

[0023] In a specific embodiment of the present application, the sealing sleeve 30 is a silicone rubber sleeve having a certain elasticity to enhance its sealing performance.

[0024] In a specific embodiment of the present application, the total length of the split injection port is 1.8 cm to 2.5 cm, the length of the tube body is 1 cm to 1.7 cm; the length of the sealing sleeve is 0.7 cm to 0.9 cm, the inner diameter is 2 mm to 3 mm, and the outer diameter is 3 mm to 4 mm.

[0025] like Figure 2 As shown, the present application improves the injection port integrated with the quartz tube into a plug-in split injection port, and the split injection port and the injection port of the traditional quartz tube are seamlessly connected through a non-heat-conducting silicone rubber sleeve. The injection port of the present application is far away from the furnace, the temperature is low, and it can be touched directly by hand without being hot. The rubber plug can be replaced at room temperature, and the operation is safe, fast and convenient. The entire plug-in split injection port can also be directly rotated and pulled out from the injection port of the traditional quartz tube, and the spare new split injection port of the present application, which has been covered with a silicone rubber sleeve and plugged with a rubber plug, can be reinserted into its original place. The method of replacing the rubber plug of the plug-in split injection port device of the present application will not burn the hands or damage the quartz tube; the operation time is short and does not affect the analysis of the sample. The traditional time for replacing the rubber plug is about 3 minutes, and the time for replacing the rubber plug after the improvement is only 15 seconds, and it is easy to operate, which is deeply loved by laboratory personnel.

[0026] In addition, the injection tube of the plug-in split injection port has a positioning and guiding function for the insertion of the syringe needle, avoiding the injection direction of the needle from being offset during injection, which would cause the spiral tube of the quartz tube to be broken; the position and direction of the syringe needle insertion are basically fixed during injection, ensuring that the analysis results remain stable. After the injection port is improved, the injection is smooth, the repeatability of the measurement results is slightly better than that of the traditional method, and the measurement results are consistent with the traditional method.

[0027] The embodiments performed after the plug-in split injection port of the present application is connected to the quartz tube are as follows:

[0028] 1. Experimental process

[0029] 1.1 The relevant instruments and equipment used are: microcoulometric sulfur analyzer (including temperature flow controller, amplifier, titration cell, stirrer); ZWK-2001A microcomputer sulfur and chlorine analyzer.

[0030] 1.2 The experimental operating conditions and analysis methods are the same as those for determining sulfur content using the traditional microcoulometry method.

[0031] 1.3 The injection port of the traditional quartz tube is seamlessly connected with the silicone rubber sleeve of the plug-in split injection port. A rubber plug is inserted into the plug-in split injection port to ensure that the entire quartz tube device is leak-proof. Figure 2 shown.

[0032] 1.4 Connect the quartz tube connected to the plug-in split sampling port of the present application to the sulfur titration cell. The quartz tube connected to the plug-in split sampling port of the present application can be connected to the sulfur titration cell for instant and continuous replenishment of electrolyte as well as to the traditional sulfur titration cell.

[0033] 1.5 Comparison of the time of changing rubber plugs with traditional methods

[0034] 1.6 Determine the repeatability of the standard sample and the sample, continuously determine the conversion rate of the standard sample and the analysis results of the sample, and calculate the relative standard deviation.

[0035] 1.7 Determine the accuracy of the samples and compare the analysis results of the samples determined by the improved method with those of the traditional method to determine the accuracy of the method.

[0036] 1.8 Carry out spike recovery test.

[0037] 2. Results and Discussion

[0038] 2.1 Shape and size of injection port

[0039] like Figure 1 As shown, the shape and wall thickness of the plug-in split injection port are the same as those of the traditional quartz tube, with a wall thickness of 2 mm. The wall thickness cannot be too thin, otherwise it is easy to break. The depth of the split injection port entrance is suitable so that three quarters of the rubber plug is inserted into the injection port and one quarter is exposed to the air. The rubber plug is cylindrical, with a height of 7 mm and a diameter of 8 mm. Experiments were conducted on plug-in split injection ports of different depths to determine that the depth of the split injection port entrance is 8 mm. The depth of the split injection port entrance cannot be too deep, otherwise, the rubber plug will be squeezed into the split injection port by the syringe during injection, and it is difficult to pull it out by hand. The diameter of the rubber plug is 8 mm, and the caliber (diameter) of the plug-in split injection port is 7 mm. After the rubber plug is inserted into the split injection port, it is completely sealed with the inner wall of the split injection port.

[0040] The injection tube is the insertion channel for the syringe needle during injection. The inner diameter of the syringe needle is about 1mm. To facilitate the insertion of the syringe needle, the inner diameter of the injection tube is 2mm~3mm. The inner diameter cannot be too large, otherwise, after the silicone rubber sleeve is put on, the outer diameter of the sleeve is too large and cannot be plugged into the split injection port; it cannot be too small, and cannot be less than the outer diameter of the needle, otherwise, the needle cannot be inserted. The outer diameter of the injection tube is preferably 3mm~4mm. The wall thickness of the injection tube cannot be too thin, otherwise, it is easy to break; the wall thickness cannot be too thick, otherwise, after the silicone rubber sleeve is put on, the sleeve will not be plugged into the split injection port, or the outer diameter of the injection tube is too large and cannot be inserted into the silicone rubber sleeve. The wall thickness of the injection tube is preferably 0.5mm. The length of the silicone rubber sleeve is 8mm, the inner diameter is 2mm, and the outer diameter is 6mm. After the silicone rubber sleeve is put on the injection tube, the two are completely sealed. Insert the plug-in split injection port covered with a silicone rubber sleeve into the injection port of the traditional quartz tube, and plug it tightly into the injection port to ensure complete sealing. Test to confirm that there is no leakage.

[0041] The shortest syringe needle length used by staff on a daily basis is 3 cm, and the total length of the plug-in split injection port should be 1.8 cm to 2.5 cm. Ensure that the needle passes through the outlet of the injection tube during injection, otherwise the sample will remain in the injection tube and affect the measurement results.

[0042] 2.2 Effect of plug-in split injection port on injection

[0043] The injection port of the traditional quartz tube is sealed by a rubber plug. The inner diameter of the neck of the injection port is about 5mm. The area where the syringe needle is inserted from the rubber plug during injection is large. The direction of the injection needle is relatively random and difficult to control. It often hits the spiral tube of the quartz tube and needs to be pulled out and reinserted. Sometimes the staff will bend the needle when inserting too hard, or even break the spiral tube in the quartz tube, causing the quartz tube to be scrapped. Different injection positions and directions also have a certain impact on the repeatability of the measurement results. The rubber plug of the traditional quartz tube is easily squeezed into the injection port and is difficult to pull out by hand. It needs to be picked out with a needle. In order to prevent the rubber plug from falling into the injection port of the traditional quartz tube during injection, the staff inserts a needle horizontally into the rubber plug exposed outside the injection port, and the needle is used to block the rubber plug from being completely squeezed into the injection port, but the needle across the middle of the rubber plug will hinder the injection.

[0044] After inserting the plug-in injection port into the injection port of the traditional quartz tube, because the inner diameter of the injection tube is only 2mm to 3mm, the needle can only be inserted horizontally from the center of the rubber plug during injection. The needle enters along the direction of the injection tube and passes through the outlet of the injection tube. The direction of the needle is basically fixed, the injection position is accurate, and it will not touch the spiral tube of the quartz tube. The injection is smooth and easy to operate. The entrance depth of the split injection port is only 8mm and is funnel-shaped. The rubber plug will not be completely squeezed into the split injection port, and a small part is still exposed, which is convenient for replacing the rubber plug.

[0045] The temperature of the traditional quartz tube vaporization section is as high as 700℃ or more, and the temperature of the injection port is relatively high. When changing the rubber plug, you cannot touch the injection port with your hands, otherwise your hands will be burned. When changing the rubber plug under high temperature conditions, the staff usually wear gloves and use tweezers to operate. Sometimes when squeezing the rubber plug into the injection port too hard, the nitrogen or oxygen injection tube will be broken, causing the quartz tube to be damaged and unable to analyze the sample, so you have to replace it with a new quartz tube. The temperature of the split injection port is low, so you can directly replace the rubber plug by hand, or directly replace the entire split injection port by hand.

[0046] 2.3 Method and time of changing rubber plug

[0047] Compared with the traditional injection port, the plug-in split injection port of the present application has an extended length of 1.6 cm in the air, is 1.6 cm farther from the furnace of the heating furnace, and is connected to the high-temperature quartz tube through a non-heat-conducting silicone rubber sleeve. The temperature of the plug-in split injection port is relatively low, and no high-temperature protection measures are required when changing the rubber plug, and it can be touched directly by hand. When changing the rubber plug, just hold the plug-in split injection port with your hand and gently rotate it to pull it out, replace it with a new rubber plug at room temperature, and insert it back to its original place. Or replace it with a spare new split injection port, or you can directly replace the rubber plug in the plug-in split injection port by hand. New employees who were afraid of changing the rubber plug no longer have to ask someone to do it for them. The three methods of changing the rubber plug are safe, fast and easy to operate. The traditional time to change the rubber plug is about 3 minutes, and the time to change the rubber plug after the improvement is only 15 seconds, and it will not damage the quartz tube, and there is no safety risk of scalding, which is deeply loved by post personnel.

[0048] 2.4 Effect of plug-in split injection port on measurement results

[0049] After the plug-in split injection port is inserted into the injection port of the traditional quartz tube, the position and direction of the needle insertion during injection are basically fixed. As the length of the injection port is extended, the distance that the needle is inserted into the vaporization section of the quartz tube becomes shorter, that is, the insertion depth becomes shallower, which has a certain impact on the conversion rate of the standard sample.

[0050] Table 1 Effect of the quartz tube connected to the plug-in split injection port device of the present application on the instrument conversion rate

[0051]

[0052] As can be seen from Table 1, the repeatability of the standard sample conversion rate after the method is improved is slightly better than that of the traditional injection port, and the conversion rate is slightly lower, but both can meet the method requirements (SH / T 0253-2021 method requires a conversion rate greater than 75%). The sulfur content of the raw material carbon four after MTBE (II) water washing was measured three times in a row using a quartz tube connected to the plug-in split injection port device of the present application and a traditional quartz tube, and the results are shown in Table 2.

[0053] Table 2 Effect of the quartz tube connected to the plug-in split injection port device of the present application on the repeatability of the results

[0054]

[0055] It can be seen from Table 2 that the repeatability of the measurement results of the improved injection port is better than that of the traditional injection port. This is because the injection tube of the improved injection port has a guiding effect on the injection needle, making the positioning of the injection needle more accurate, so the repeatability of the measurement results is slightly better.

[0056] Table 3 The influence of the quartz tube connected to the plug-in split injection port device of the present application on the measurement results

[0057]

[0058] It can be seen from Table 3 that the improved injection port has no effect on the measurement results, and the difference between the improved injection method and the traditional injection method is much smaller than the method allowable error. This is because the instrument has been calibrated with standard samples, so the results of the two methods are in good agreement.

[0059] Figure 3 The spectrum of sulfur content in hydrogenated diesel is measured by the improved injection port. Figure 3 It can be seen that the improved method of the present application has good repeatability in measuring samples.

[0060] A certain amount of 10 mg / m3 H2S standard gas (nitrogen as the balance gas) was added to the desulfurization-deodorization A, and the sample recovery rate of the sulfur content in the desulfurization-deodorization A was determined to be 104%, which shows that the improved method has high accuracy and reliable measurement results.

[0061] 3. Conclusion

[0062] (1) A plug-in split injection port is inserted into the injection port of the traditional quartz tube, making the operation of replacing the rubber plug safe, fast and simple.

[0063] (2) The plug-in split injection port connection method makes injection smoother, orientation and positioning more accurate, and the repeatability of the measurement results is slightly better than that of the traditional method, and the measurement results are consistent with those of the traditional method.

[0064] In the description of this specification, the description with reference to the terms "one embodiment", "some embodiments", "illustrative embodiments", "examples", "specific examples", or "some examples" means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representation of the above terms does not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described may be combined in any one or more embodiments or examples in a suitable manner.

[0065] Although the embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the claims and their equivalents.

[0066] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and substitutions can be made without departing from the technical principles of the present invention. These improvements and substitutions should also be regarded as the protection scope of the present invention.

Claims

1. A plug-in split sample inlet device, characterized in that : It includes an injection tube, the outlet end of which is in the shape of a straight tube and has a first opening; the inlet end of the injection tube has a second opening, and a rubber plug is sealed in the second opening; the first opening is used to be inserted into the injection port of a quartz tube to connect the quartz tube and the injection tube; the injection tube includes a straight tube body and an inlet tube, the first opening is located at the outlet end of the tube body, and the second opening is located at the inlet end of the inlet tube; a sealing sleeve is sleeved on the tube body, and the sealing sleeve extends from the vicinity of the first opening on the tube body to the connection between the tube body and the inlet tube; the total length of the split injection port is 1.8cm to 2.5cm; the length of the tube body is 1cm to 1.7cm; the length of the sealing sleeve is 0.7cm to 0.9cm.

2. The plug-in split sample inlet device according to claim 1, characterized in that :The tube body and the inlet pipe are integrally formed.

3. The plug-in split sample inlet device according to claim 2, characterized in that: There is also an integrally formed inlet pipe between the tube body and the second opening; the diameter of the inlet pipe is larger than the diameter of the tube body, and gradually increases and then gradually decreases from the end connected with the tube body to the end connected with the inlet pipe.

4. The plug-in split sample inlet device according to claim 1, characterized in that : The sealing sleeve is a silicone rubber sleeve.

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