CN112816611A - Combustion online ion chromatography system and use method thereof - Google Patents
Combustion online ion chromatography system and use method thereof Download PDFInfo
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- CN112816611A CN112816611A CN202011636573.5A CN202011636573A CN112816611A CN 112816611 A CN112816611 A CN 112816611A CN 202011636573 A CN202011636573 A CN 202011636573A CN 112816611 A CN112816611 A CN 112816611A
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- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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- G—PHYSICS
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- G01N31/12—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using combustion
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Abstract
The invention discloses a combustion online ion chromatography system and a using method thereof.A sample boat chamber is fixedly connected and communicated with two ends of a combustion tube and a guide quartz tube respectively, a sample boat is arranged in the sample boat chamber, a filter plate is fixedly connected in the combustion tube, a plurality of through holes are formed on the filter plate, two sides of the filter plate are communicated only through the through holes, and the through holes allow gas to pass through but not allow solids to pass through. The invention prevents the small solid particles of the sample from passing through the filter plate while the gas smoothly passes through the through hole by the filter plate made of ceramics, so that the small solid particles of the sample can not enter the ion chromatograph through the combustion tube, but are continuously heated and cracked on the filter plate until the gas is formed, thereby eliminating the small solid particles of the sample in the combustion tube, solving the problems of difficult cleaning and interference on next detection caused by the small solid particles of the sample remaining in the combustion tube and the ion chromatograph, and simultaneously ensuring the sufficient combustion of the sample.
Description
Technical Field
The application belongs to the field of chemical detection, and particularly relates to a combustion online ion chromatography system and a using method thereof.
Background
The prior pretreatment mainly adopts a single-tube furnace direct combustion method, and has rough treatment and lower recovery rate. The existing halogen detection is to detect gas cracked by a sample after the gas enters absorption liquid to be absorbed by an ion chromatograph, the gas often carries part of solid particles of the sample to flow out, the combustion is insufficient, the solid particles of the sample can pollute the inside of a combustion tube and the ion chromatograph, and the residual particles can interfere the next detection.
Disclosure of Invention
In view of the above problems, the present application proposes a combustion online ion chromatography system and a method for using the same, which solve the problems of small solid particles of a sample remaining inside a combustion tube, insufficient combustion, difficulty in cleaning caused in an ion chromatograph, and interference with the next detection.
The online combustion ion chromatography system comprises a combustion tube, a sample boat chamber and a guide quartz tube, wherein two ends of the sample boat chamber are fixedly connected with the combustion tube and the guide quartz tube respectively and communicated with each other, the sample boat is arranged in the sample boat chamber, a filter plate is fixedly connected with the inside of the combustion tube, a plurality of through holes are formed in the filter plate, two sides of the filter plate are communicated with each other only through the through holes, and the through holes allow gas to pass through and do not allow solids to pass through.
Further, the combustion pipe comprises an inner pipe and an outer pipe, the inner pipe is arranged in the outer pipe, one end of the inner pipe is provided with a first connecting port, and the other end of the inner pipe is provided with a second connecting port; the second connecting port is communicated with the interior of the sample boat chamber, a third connecting port is formed at one end of the outer tube, which is close to the first connecting port, and the filter plate is positioned between the first connecting port and the third connecting port.
Furthermore, a first oxygen inlet pipe and a water inlet pipe are formed on the outer side of the outer pipe, and the first oxygen inlet pipe and the water inlet pipe are communicated with the inside of the outer pipe respectively.
Furthermore, the water inlet pipe is communicated with a water supply capillary pipe, the water supply capillary pipe is positioned between the inner pipe and the outer pipe, the water supply capillary pipe comprises a first axial pipe, a circumferential pipe and a second axial pipe, the first axial pipe and the second axial pipe are respectively positioned at two sides of the outer part of the inner pipe, two ends of the circumferential pipe are respectively communicated with the first axial pipe and the second axial pipe, and the second axial pipe is communicated with the inner part of the inner pipe; the circumference pipe encircles the circumference of half inner tube, the one end that first axial pipe kept away from water and advanced the pipe extends to the direction that is close first connector, the one end that first connector was kept away from to the second axial pipe extends to the direction that is close the second connector.
Furthermore, a first oxygen inlet pipe valve is installed on the first oxygen inlet pipe, a water inlet pipe valve is installed on the water inlet pipe, the third connecting port is respectively communicated with the first valve and the second valve, the first valve is communicated with a U-shaped pipe, the U-shaped pipe is communicated with an absorption pipe, and the absorption pipe is communicated with an ion chromatograph.
Furthermore, a heating furnace is arranged outside the combustion tube and is divided into a box body and a box cover, heating devices are respectively arranged in the box body and the box cover, the box body is fixed relative to the combustion tube, and the box cover is hinged with the box body; the filter plate and the first connecting port are located inside the heating furnace, and the water supply capillary part is located inside the heating furnace.
Furthermore, the sample boat is detachably connected with a push rod, one end, far away from the sample boat, of the push rod is fixedly connected with a sliding block, the sliding block is located in the guide quartz tube and is in sliding connection with the guide quartz tube, and the guide quartz tube is provided with a second oxygen inlet tube.
The magnetic field generator comprises a lead screw, a nut, magnets, a magnetic block, a motor, a magnetic block and a magnetic block, wherein the lead screw is connected with the nut and drives the nut to move along the lead screw; and a second oxygen inlet pipe valve is arranged on the second oxygen inlet pipe.
Further, the filter plate is made of ceramic.
The use method of the combustion online ion chromatography system comprises the following steps:
step S1: preparing equipment;
step S2: containing a sample;
step S3: removing residual gas;
step S4: preheating a sample;
step S5: heating the sample;
step S6: and (5) fixing the volume and detecting the absorption liquid.
The invention has the following advantages:
1. the filter plate made of ceramics prevents small solid particles of the sample from passing through the filter plate while enabling the gas to smoothly pass through the through hole, so that the small solid particles of the sample cannot enter the ion chromatograph through the combustion tube, but are continuously heated and cracked on the filter plate until the gas is formed, the small solid particles of the sample in the combustion tube are eliminated, the problems of difficult cleaning and interference on next detection caused by the fact that the small solid particles of the sample remain in the combustion tube and the ion chromatograph are solved, and meanwhile, the sufficient combustion of the sample is ensured;
2. oxygen entering from the second oxygen inlet pipe can not only supply oxygen to the sample in the inner pipe for reaction, but also form airflow flowing to the direction of the filter plate, so that pyrolysis gas formed by the pyrolysis of the sample is driven to flow to the third connecting port; the oxygen part entering the first oxygen inlet pipe enters the inner pipe to carry out cracking reaction, and the oxygen part does not enter the inner pipe and directly carries out cracking reaction with the small test solid particles on the filter plate, so that sufficient oxygen can be provided for the small test solid particles on the filter plate, and the situation that the small test solid particles on the filter plate cannot fully react due to the reduction of the oxygen content caused by the fact that the oxygen entering the second oxygen inlet pipe participates in the cracking reaction is avoided;
3. the water entering from the water inlet pipe is heated in the water supply capillary tube to form water vapor, so that the water inlet pipe is not required to be heated, a heating device for heating the water inlet pipe is omitted, and the structure is simple.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present application, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present application, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1: the front view structure of the invention is schematic (the combustion tube is not sectioned);
FIG. 2: the invention discloses a schematic structural diagram of a combustion tube in a top view;
FIG. 3: the invention is a partial enlarged structure schematic diagram at A;
FIG. 4: the invention is a partial enlarged structure schematic diagram at B;
FIG. 5: the invention is a schematic sectional structure at C.
Detailed Description
The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are only a part of the embodiments of the present application, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
The first embodiment is as follows:
as shown in fig. 1 to 5, the present embodiment provides a combustion online ion chromatography system, including a combustion tube 1, a sample boat chamber 2 and a guide quartz tube 3, two ends of the sample boat chamber 2 are respectively fixedly connected and communicated with the combustion tube 1 and the guide quartz tube 3, a sample boat 4 is disposed in the sample boat chamber 2, a filter plate 7 is fixedly connected inside the combustion tube 1, the filter plate 7 is formed with a plurality of through holes 71, two sides of the filter plate 7 are communicated only through the through holes 71, and the through holes 71 allow gas to pass through and do not allow solids to pass through.
Further, the combustion pipe 1 includes an inner pipe 11 and an outer pipe 12, the inner pipe 11 is inside the outer pipe 12, one end of the inner pipe 11 is formed with a first connection port 111, and the other end is formed with a second connection port 112; the second connection port 112 is communicated with the inside of the sample boat chamber 2, a third connection port 121 is formed at one end of the outer tube 12 close to the first connection port 111, and the filter plate 7 is located between the first connection port 111 and the third connection port 121. The setting of double-deck body is that solid sample gets into the furnace body and can not directly get into the maximum temperature position, can make the sample burning insufficient like this, so need preheat earlier, and inner tube 11 needs argon gas, rather than oxygen when preheating, so, this is the needs that satisfy the difference of inside and outside gas kind, and different gas and velocity of flow are required to different combustion stages promptly. Another reason is that the water supply capillary 15 needs to be left in the space, and the cracked water needs to have a ring of capillary to vaporize it, which is convenient to implement between the inner and outer tubes.
Further, a first oxygen inlet pipe 13 and a water inlet pipe 14 are formed outside the outer pipe 12, and the first oxygen inlet pipe 13 and the water inlet pipe 14 are respectively communicated with the inside of the outer pipe 12.
Further, the water inlet pipe 14 is communicated with a water supply capillary 15, the water supply capillary 15 is located between the inner pipe 11 and the outer pipe 12, the water supply capillary 15 includes a first axial pipe 151, a circumferential pipe 152 and a second axial pipe 153, the first axial pipe 151 and the second axial pipe 153 are respectively located at two sides of the outer portion of the inner pipe 11, two ends of the circumferential pipe 152 are respectively communicated with the first axial pipe 151 and the second axial pipe 153, and the second axial pipe 153 is communicated with the inner portion of the inner pipe 11; the circumferential pipe 152 surrounds a half of the circumference of the inner pipe 11, the first axial pipe 151 extends from an end of the water inlet pipe 14 to a direction approaching the first connection port 111, and the second axial pipe 153 extends from an end of the first axial pipe 111 to a direction approaching the second connection port 112. The cracked water is carried by gas to enter a water supply capillary 15 between an inner pipe 11 and an outer pipe 12 of the combustion pipe 1, the water supply capillary 15 passes through the highest temperature zone and then returns to the front end of the combustion pipe 1, namely, the water can completely vaporize through the highest temperature zone and then enters the inner pipe, and the water is vaporized to become small molecules. On one hand, the function of the cracking water can participate in the leaching of inorganic ions in the sample; on the other hand, the release of ions from the organic ionic compound can be assisted.
Further, a first oxygen inlet pipe valve 131 is installed on the first oxygen inlet pipe 13, a water inlet pipe valve 141 is installed on the water inlet pipe 14, the third connecting port 121 is respectively communicated with the first valve 122 and the second valve 123, the first valve 122 is communicated with the U-shaped pipe 8, the U-shaped pipe 8 is communicated with the absorption pipe 9, and the absorption pipe 9 is communicated with the ion chromatograph.
Further, a heating furnace 6 is arranged outside the combustion tube 1, the heating furnace 6 is divided into a box body and a box cover, heating devices 61 are respectively arranged in the box body and the box cover, the box body is fixed relative to the combustion tube 1, and the box cover is hinged with the box body; the filter sheet 7 and the first connection port 111 are located inside the heating furnace 6, and the water supply capillary 15 is partially located inside the heating furnace 6.
Further, the sample boat 4 is detachably connected with a push rod 32, one end of the push rod 32, which is far away from the sample boat 4, is fixedly connected with a slide block 31, the slide block 31 is positioned inside the guide quartz tube 3 and is slidably connected with the guide quartz tube 3, and a second oxygen inlet tube 33 is formed in the guide quartz tube 3. The sample is always in the inner tube 11, the preheating of the sample needs inert gas, and the inner tube 11 is filled with oxygen to be beneficial to cleaning the residue between the inner tube and the outer tube; when the sample reaches the highest temperature range, the gas in the inner tube 11 is switched to oxygen to assist combustion. All settings were made to fully burn the sample clean, not partially burn.
Further, the quartz tube guiding device comprises a case 5, wherein a motor 51 is fixedly installed inside the case 5, the motor 51 is connected with a lead screw 52 and drives the lead screw 52 to rotate, the lead screw 52 is connected with a nut 53 and drives the nut 53 to move along the lead screw 52, the nut 53 is fixedly connected with a magnetic block 54 through a connecting rod, the magnetic block 54 is positioned outside the guiding quartz tube 3 and is in sliding connection with the guiding quartz tube 3, and the magnetic block 54 drives the sliding block 31 and the magnetic block 54 to move synchronously through magnetic force; the second oxygen inlet pipe 33 is provided with a second oxygen inlet pipe valve 34.
Furthermore, the filter plate 7 is made of ceramic, the ceramic material can resist high temperature, the component of the ceramic material is mainly silicon dioxide, and other interference ions cannot be introduced; the aperture of the filter plate 7 is 180-220 meshes.
The use method of the combustion online ion chromatography system comprises the following steps:
step S1: preparing equipment;
the connection among all pipe fittings is good, the gas leakage detection is normal, the equipment is initialized, the heating furnace 6 is put into the furnace to be heated to the highest temperature, and the absorption tube 9 and the liquid flow path are cleaned;
step S2: containing a sample;
opening the sample boat chamber 2, putting the sample boat 4 containing the sample, sleeving the sample boat on the hook of the push rod 32, and buckling the sealing cover 21;
step S3: removing residual gas;
the second oxygen inlet pipe valve 34 is opened, and argon is introduced into the inner pipe 11; the first oxygen inlet pipe valve 131 is opened, oxygen is introduced between the inner pipe 11 and the outer pipe 12, and the absorption liquid is added into the absorption pipe 9; opening the second valve 123 to discharge the residual gas in the combustion tube 1 from the second valve 123 to the outside until the inner tube 11 is filled with argon gas and the space between the inner tube 11 and the outer tube 12 is filled with oxygen, and then closing the second valve 123;
step S4: preheating a sample;
the motor 51 drives the screw rod 52 to rotate, so as to drive the screw nut 52 and the magnetic block 54 to move, and the magnetic block 54 drives the sliding block 31 and the magnetic block 54 to synchronously move towards the direction of the combustion tube 1 through magnetic force; the push rod 32 drives the sample boat 4 to enter the inner tube 11 to the first heating zone for preheating, at this time, the inner tube 11 is Ar, and oxygen is filled between the inner tube 11 and the outer tube 12;
step S5: heating the sample;
then the sample boat 4 enters a second heating area and a third heating area for further heating and coking, and the air inlet mode is still adopted at the moment; finally, the sample boat 4 enters the highest temperature zone, the retention time of the sample boat 4 is longest, and oxygen is introduced into the second oxygen inlet pipe valve 34 to switch the argon in the inner pipe 11 into oxygen, so that the sample is completely combusted and dissociated; in the whole process from pushing the sample into the first heating area to the highest temperature area for dissociation, the cracked water is synchronously added through the water supply capillary 15 and is driven into the inner tube 11 of the combustion tube 1 by the argon gas; meanwhile, the pyrolysis gas generated by the sample carries part of sample particles to be pushed by the airflow to move towards the third connecting port 121, the pyrolysis gas and part of the sample particles encounter the filter plate 7, the pyrolysis gas enters the absorption liquid through the third connecting port 121 after passing through the through hole 71, the sample particles cannot fall on the surface of the filter plate 7 through the through hole 71, the sample falling on the surface of the filter plate 7 is continuously heated and pyrolyzed on the filter plate 7 until gas passing through the through hole 71 is formed, and then the sample enters the absorption tube 9 to be absorbed by the absorption liquid after being cooled in the U-shaped tube 8, and the combustion pyrolysis process is accompanied with the absorption liquid in the absorption tube 9 to continuously absorb ionic compounds in the pyrolysis gas; thus, the sample is prevented from being washed into the absorbing liquid after being blocked by the filter 7, and the subsequent adhesion to the inner surface of the flow path pipe can be prevented. At the same time, the blocked sample particles can be burned again, releasing ions sufficiently.
The sample may be an adsorbable organohalogen or a rubber. At a high temperature of 800-1000 ℃, an organism reacts with oxygen to generate water and carbon dioxide, element groups grafted on an organic framework, such as chlorine, bromine, fluorine and the like, are combined with hydrogen groups formed by hydrolysis at a high temperature to form acidic free gases, such as hydrogen chloride, hydrogen fluoride, hydrogen bromide and the like, and the gases are easily dissolved in an alkaline absorption liquid in the absorption tube 9, so that the halogens to be detected are completely detected.
Preferably, the U-shaped pipe 8 is cooled by air cooling, that is, the cracked gas which is continuously discharged is also continuously cooled.
Preferably, a temperature distribution curve function is built in the combustion furnace 6, namely, after the center of the furnace body reaches the highest temperature, the temperature is continuously reduced along with the furnace body extends towards two sides, and the whole furnace body is in normal distribution; the half function close to the sample boat chamber 2 is applied. Through the function, the temperature position where the sample boat 4 is desired to stop can be selected arbitrarily, that is, 4 temperature points and 4 residence times can be set (in steps S4 and S5, the first heating zone, the second heating zone, the third heating zone and the highest temperature zone which are sequentially far away from the sample boat chamber 2), and the software will automatically advance the sample boat 4 to the corresponding position and stay for the corresponding time, so as to realize slow, uniform and sufficient cracking of the sample. The sample is preheated firstly, and the temperature of the sample is gradually increased in different temperature regions, so that the sample is prevented from directly entering the highest temperature region to generate deflagration.
Step S6: fixing the volume and detecting the absorption liquid;
after the sample is burnt, absorption is finished, then the injection pump 10 cleans the U-shaped pipe 8 and the pipeline to the absorption pipe 9 by pure water, the cleaning liquid is subjected to constant volume in the absorption pipe, and the volume of all liquid entering the absorption pipe 9 is calculated for standby; and detecting the absorption liquid (containing target ions) with constant volume by ion chromatography.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solutions of the present application, and not to limit the same; although the present application has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; such modifications and substitutions do not necessarily depart from the spirit and scope of the corresponding technical solutions in the embodiments of the present application.
Claims (10)
1. Burning online ion chromatographic system, including combustion tube (1), sample boat room (2) and direction quartz capsule (3), sample boat room (2) both ends respectively with combustion tube (1) and direction quartz capsule (3) fixed connection and be linked together, be provided with sample boat (4), its characterized in that in sample boat room (2): the combustion tube (1) is internally and fixedly connected with a filter plate (7), the filter plate (7) is provided with a plurality of through holes (71), two sides of the filter plate (7) are communicated only through the through holes (71), and the through holes (71) allow gas to pass through and do not allow solids to pass through.
2. The combustion online ion chromatography system of claim 1, wherein: the combustion pipe (1) comprises an inner pipe (11) and an outer pipe (12), the inner pipe (11) is arranged inside the outer pipe (12), one end of the inner pipe (11) is provided with a first connecting port (111), and the other end of the inner pipe is provided with a second connecting port (112); the second connecting port (112) is communicated with the interior of the sample boat chamber (2), a third connecting port (121) is formed at one end, close to the first connecting port (111), of the outer tube (12), and the filter plate (7) is located between the first connecting port (111) and the third connecting port (121).
3. The combustion online ion chromatography system of claim 2, wherein: a first oxygen inlet pipe (13) and a water inlet pipe (14) are formed on the outer side of the outer pipe (12), and the first oxygen inlet pipe (13) and the water inlet pipe (14) are respectively communicated with the inner part of the outer pipe (12).
4. The combustion online ion chromatography system of claim 3, wherein: the water inlet pipe (14) is communicated with a water supply capillary pipe (15), the water supply capillary pipe (15) is located between the inner pipe (11) and the outer pipe (12), the water supply capillary pipe (15) comprises a first axial pipe (151), a circumferential pipe (152) and a second axial pipe (153), the first axial pipe (151) and the second axial pipe (153) are respectively located on two sides of the outer portion of the inner pipe (11), two ends of the circumferential pipe (152) are respectively communicated with the first axial pipe (151) and the second axial pipe (153), and the second axial pipe (153) is communicated with the inner portion of the inner pipe (11); the circumference of half inner tube (11) is encircleed to circumference pipe (152), the one end that first axial pipe (151) kept away from water inlet pipe (14) extends to the direction that is close to first connector (111), the one end that second axial pipe (153) kept away from first connector (111) extends to the direction that is close to second connector (112).
5. The combustion online ion chromatography system of claim 3, wherein: a first oxygen inlet pipe valve (131) is installed on the first oxygen inlet pipe (13), a water inlet pipe valve (141) is installed on the water inlet pipe (14), the third connecting port (121) is communicated with the first valve (122) and the second valve (123) respectively, the first valve (122) is communicated with the U-shaped pipe (8), the U-shaped pipe (8) is communicated with the absorption pipe (9), and the absorption pipe (9) is communicated with the ion chromatograph.
6. The combustion online ion chromatography system of claim 4, wherein: the heating furnace (6) is arranged on the outer side of the combustion pipe (1), the heating furnace (6) is divided into a box body and a box cover, heating devices (61) are respectively arranged in the box body and the box cover, the box body is fixed relative to the combustion pipe (1), and the box cover is hinged with the box body; the filter plate (7) and the first connecting port (111) are positioned inside the heating furnace (6), and the water supply capillary tube (15) is partially positioned inside the heating furnace (6).
7. The combustion online ion chromatography system of claim 1, wherein: sample boat (4) and catch bar (32) can be dismantled and be connected, the one end and slider (31) fixed connection of sample boat (4) are kept away from in catch bar (32), slider (31) are located inside guide quartz tube (3) and with guide quartz tube (3) sliding connection, guide quartz tube (3) are formed with second oxygen and advance pipe (33).
8. The combustion online ion chromatography system of claim 7, wherein: the quartz tube guiding device is characterized by further comprising a case (5), a motor (51) is fixedly mounted inside the case (5), the motor (51) is connected with a lead screw (52) and drives the lead screw (52) to rotate, the lead screw (52) is connected with a nut (53) and drives the nut (53) to move along the lead screw (52), the nut (53) is fixedly connected with a magnetic block (54) through a connecting rod, the magnetic block (54) is located on the outer side of the quartz tube guiding (3) and is in sliding connection with the quartz tube guiding (3), and the magnetic block (54) drives the slider (31) and the magnetic block (54) to move synchronously through magnetic force; and a second oxygen inlet pipe valve (34) is arranged on the second oxygen inlet pipe (33).
9. The combustion online ion chromatography system of claim 1, wherein: the filter plate (7) is made of ceramics.
10. The method of using a combustion online ion chromatography system according to any one of claims 1 to 9, comprising the steps of:
step S1: preparing equipment;
step S2: containing a sample;
step S3: removing residual gas;
step S4: preheating a sample;
step S5: heating the sample;
step S6: and (5) fixing the volume and detecting the absorption liquid.
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| CN114646712A (en) * | 2022-03-22 | 2022-06-21 | 青岛盛瀚色谱技术有限公司 | Novel combustion online ion chromatography system and use method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114646712A (en) * | 2022-03-22 | 2022-06-21 | 青岛盛瀚色谱技术有限公司 | Novel combustion online ion chromatography system and use method thereof |
| CN114646712B (en) * | 2022-03-22 | 2024-01-09 | 青岛盛瀚色谱技术有限公司 | Novel combustion online ion chromatography system and application method thereof |
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