CN111735882B - High-purity TMAH reagent ion chromatography detection device and detection method thereof - Google Patents
High-purity TMAH reagent ion chromatography detection device and detection method thereof Download PDFInfo
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- CN111735882B CN111735882B CN202010618677.7A CN202010618677A CN111735882B CN 111735882 B CN111735882 B CN 111735882B CN 202010618677 A CN202010618677 A CN 202010618677A CN 111735882 B CN111735882 B CN 111735882B
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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
- G01N30/02—Column chromatography
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- 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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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- 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
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/16—Injection
- G01N30/20—Injection using a sampling valve
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Abstract
The invention discloses a high-purity TMAH reagent ion chromatography detection device and a detection method thereof, wherein the detection device comprises a detection machine body and a detection door plate, the detection door plate is arranged on the front side of the detection machine body and is movably connected to the detection machine body through an edge hinge bolt, a buffer insertion tube is arranged on the surface of the detection door plate close to the left edge, the buffer insertion tube longitudinally penetrates through the detection door plate, an inspector chamber is embedded in the right upper corner of the front end of the detection machine body, a peristaltic pump set is embedded in the front end of the detection machine body below the inspector chamber, an inhibition module is embedded in the front end of the detection machine body on the left side of the peristaltic pump set, a high-pressure pump set is embedded in the front end of the detection machine body below the inhibition module to obtain the maximum contact area, and further when a thin tube directly contacts with an insertion tube edge, because the contact area is small, the liquid bends when bending in a small range, and the problem that the liquid cannot flow is caused.
Description
Technical Field
The invention belongs to the technical field related to chemical equipment, and particularly relates to a high-purity TMAH reagent ion chromatography detection device and a detection method thereof.
Background
The instruments used in chemical experiments are called chemical instruments, the main function of which is to measure or react materials is mainly divided into measuring instruments and reaction instruments, and the functional function of which is to combine the instruments in a specific way to form a device to realize the purpose of chemical experiments.
The prior ion chromatography detection device technology has the following problems: ion chromatography detection device department is used for the tubule direction to set up for no buffering pipe fitting with the intubate, and when the tubule moved for the intubate promptly, very easily the appearance tubule is buckled in intubate pipe edge department because of the exogenic action down, and then leads to the interior liquid of tubule to be difficult to flow, the testing result deviation problem that causes.
Disclosure of Invention
The invention aims to provide a high-purity TMAH reagent ion chromatography detection device and a detection method thereof, and aims to solve the problem of detection result deviation caused by the fact that when an intubation tube for guiding a tubule is arranged without a buffer pipe fitting at the position of the ion chromatography detection device, namely, when the tubule moves relative to the intubation tube, the tubule is easily bent at the position along the intubation tube under the action of external force, and further liquid in the tubule is difficult to flow.
In order to achieve the purpose, the invention provides the following technical scheme:
a high-purity TMAH reagent ion chromatography detection device comprises a detection machine body and a detection door plate, wherein the detection door plate is arranged on the front side of the detection machine body and is movably connected to the detection machine body through an edge hinge bolt, a buffer insertion tube is arranged on the surface of the detection door plate close to the left edge and longitudinally penetrates through the detection door plate, an inspector chamber is embedded into the front end of the detection machine body at the upper right corner, a peristaltic pump set is embedded into the front end of the detection machine body below the inspector chamber, an inhibition module is embedded into the front end of the detection machine body at the left side of the peristaltic pump set, a high-pressure pump set is embedded into the front end of the detection machine body below the inhibition module, a sample injection valve is embedded into the front end of the detection machine body at the right side of the high-pressure pump set, and an exhaust valve is embedded into the front end of the detection machine body below the sample injection valve, the right side of discharge valve and injection valve has the pulse damper in the front end embedding that is located the detection organism, the rear end that detects the organism is located the lower right corner department embedding and has power source, power source's left side has the detection line interface in the rear end embedding that is located the detection organism, the top of detection line interface has bolted the detection apron in the rear end that is located the detection organism, the left side that detects the apron has the heat dissipation honeycomb panel in the rear end joint that is located the detection organism, the buffering intubate includes tube head, intubate and silica gel soft cover, the surface that detects the door plant is being provided with the intubate near left side edge, the intubate vertically runs through in detection door plant department, the tube head has been bolted through the mutual interlock between the screw thread in both ends around the intubate, the outside of tube head bonds through the glue film has the silica gel soft cover.
Preferably, the number of the buffer insertion tubes is two, the specification and the size of the buffer insertion tubes are consistent, and the buffer insertion tubes are arranged at the detection door plate up and down.
Preferably, the bottom end of the detection machine body is embedded with foot pads at the peripheral corners, and the foot pads at the bottom end of the detection machine body are in a rectangular distribution state.
Preferably, detect the door plant and can rotate for detecting the organism under the effect of power, detect the door plant and can carry out the angle range and be zero to one hundred eighty degrees rotation for detecting the organism under the effect of power.
Preferably, the high-pressure pump group is connected with the exhaust valve through a pipeline, the exhaust valve is connected with the pulse damper through a pipeline, and the pulse damper is connected with the sample injection valve through a pipeline.
Preferably, the power supply connected with the power interface is a two-hundred and twenty-volt ground power supply.
Preferably, the soft silica gel sleeve is made of a soft material, the soft silica gel sleeve can be elastically deformed under the action of force, and the soft silica gel sleeve is restored to the original set shape after the force is applied.
A high-purity TMAH reagent ion chromatography detection method comprises the following steps:
the method comprises the following steps: accurately weighing 5-10 g of 25% TMAH sample, diluting the solution in a PFA bottle by 9-10 times with high-purity water, passing through a cationic resin column (001 x 7 type strong acid resin), filtering out the first 20ml, inoculating 10ml of sample, and performing detection and analysis;
step two: preparing 1ppm Cl and NO3 mixed solution as stock solution, preserving at constant temperature, preparing 10, 20, 50 and 100ppb mixed standard solution by adopting a stepwise dilution method, and preparing the standard solution for use in situ;
step three: making an external standard curve by using 10, 20, 50 and 100ppb mixed standard solution, wherein the correlation coefficient is more than or equal to 0.999;
step four: clicking a red button 'Stop' of the 863 automatic sample injector when the baseline is stable, and starting the automatic sample injector;
step five: placing a series of samples to be measured in a certain sequence, clicking a column in a sample table row in a 'measurement sequence' of a Magic Net 'working platform' interface, changing the column into yellow, then double clicking the column, selecting a 'new mixed standard method' in a 'method' of a popup dialog box, selecting a 'standard' mode for measurement if a standard curve is measured in a sample type, selecting a 'sample' mode for measurement if the sample is measured, filling the position of the automatic sample feeder where the sample to be measured is placed in a sample position, and filling '1' in a sample amount column;
step six: after all samples are edited, clicking 'start' to start measurement;
step seven: regenerating the used resin by using a sulfuric acid solution with the concentration of about 2%, soaking the resin in the sulfuric acid solution according to the volume ratio of 1:1.5, soaking the resin for 2 hours, and washing the resin with high-purity water until the pH value is 7.
Compared with the prior art, the invention provides a high-purity TMAH reagent ion chromatography detection device and a detection method thereof, and the detection device has the following beneficial effects:
the novel buffering intubation tube is arranged, the buffering intubation tube comprises a tube head, an intubation tube and a silica gel soft sleeve, when the three structures are combined for use, the thin tube can be protected through the silica gel soft sleeve connected to the tube head when inserted into the intubation tube to move, the thin tube can be supported through soft materials during the bending of the thin tube to obtain the maximum contact area, and therefore the problem that liquid cannot flow due to the fact that the thin tube is bent when being in direct contact with the edge of the intubation tube due to the small contact area is avoided.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention without limiting the invention in which:
FIG. 1 is a schematic front view of an ion chromatography detection device for high purity TMAH reagent according to the present invention;
FIG. 2 is a schematic diagram of the internal structure of the ion chromatography detection device for high purity TMAH reagent according to the present invention;
FIG. 3 is a schematic diagram of a rear view structure of the ion chromatography detection device for high purity TMAH reagent according to the present invention;
FIG. 4 is a schematic structural diagram of a buffer cannula in the high purity TMAH reagent ion chromatography detection apparatus of the present invention;
in the figure: 1. detecting a body; 2. detecting the door panel; 3. buffering the cannula; 31. a pipe head; 32. inserting a tube; 33. a silica gel soft sleeve; 4. an inspector room; 5. a peristaltic pump set; 6. a suppression module; 7. a high pressure pump package; 8. a sample injection valve; 9. an exhaust valve; 10. a pulse damper; 11. a power interface; 12. detecting a line interface; 13. a heat dissipating honeycomb panel; 14. and detecting the cover plate.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, 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 invention.
In the description of the present invention, it should be noted that the terms "upper", "lower", "inner", "outer", "front", "rear", "both ends", "one end", "the other end", and the like indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it is to be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "disposed," "connected," and the like are to be construed broadly, and for example, "connected" may be a fixed connection, a detachable connection, or an integral connection; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Referring to fig. 1-4, the present invention provides a high purity TMAH reagent ion chromatography detection device and a detection method thereof, wherein the detection method comprises the following steps:
the utility model provides a high-purity TMAH reagent ion chromatography detection device, including detecting organism 1 and detection door plant 2, the front side that detects organism 1 is provided with detection door plant 2, it articulates swing joint in detecting organism 1 department through the marginal hinge bolt to detect door plant 2, it can rotate for detecting organism 1 under the effect of force to detect door plant 2, it can carry out the angular range for zero to one hundred eighty degrees rotation for detecting organism 1 under the effect of force to detect door plant 2, the surface that detects door plant 2 is being close to left side edge and is being provided with buffering intubate 3, buffering intubate 3 vertically runs through in detecting door plant 2 department, buffering intubate 3 is provided with two altogether, the specification and size of buffering intubate 3 is unanimous, buffering intubate 3 is arranged in detecting door plant 2 departments from top to bottom, the bottom that detects organism 1 inlays and has the pad foot in the edge department all around being located, it is the rectangle distribution state to detect organism 1 department and fill up the foot.
The utility model provides a high pure TMAH reagent ion chromatogram detection device, it has inspector room 4 to be located the embedding of upper right corner department including the front end that detects organism 1, the below of inspector room 4 has peristaltic pump group 5 in the front end embedding that is located detection organism 1, the left side of peristaltic pump group 5 has suppression module 6 in the front end embedding that is located detection organism 1, the below of suppression module 6 has high-pressure pump group 7 in the front end embedding that is located detection organism 1, the right side of high-pressure pump group 7 has injection valve 8 in the front end embedding that is located detection organism 1, the below of injection valve 8 has discharge valve 9 in the front end embedding that is located detection organism 1, discharge valve 9 and the right side of injection valve 8 have pulse damper 10 in the front end embedding that is located detection organism 1, high-pressure pump group 7 is connected with discharge valve 9 through the pipeline, discharge valve 9 is connected with pulse damper 10 through the pipeline, pulse damper 10 is connected with injection valve 8 through the pipeline.
A high-purity TMAH reagent ion chromatography detection device comprises a power supply interface 11 embedded at the lower right corner of the rear end of a detection machine body 1, a power supply connected with the power supply interface 11 is a two hundred twenty-ten volt ground power supply, a detection line interface 12 embedded at the rear end of the detection machine body 1 is arranged at the left side of the power supply interface 11, a detection cover plate 14 is bolted at the rear end of the detection machine body 1 above the detection line interface 12, a heat dissipation cellular board 13 is clamped at the rear end of the detection cover plate 14 at the left side of the detection machine body 1, a buffer insertion tube 3 comprises a tube head 31, an insertion tube 32 and a silica gel soft sleeve 33, the insertion tube 32 is arranged on the surface of the detection door plate 2 near the edge of the left side, the insertion tube 32 longitudinally penetrates through the detection door plate 2, the tube head 31 is bolted at the front end and the rear end of the insertion tube 32 through mutual meshing between threads, and the silica gel soft sleeve 33 is bonded at the outer side end of the tube head 31, the soft silica gel sleeve 33 is made of soft materials, the soft silica gel sleeve 33 can be elastically deformed under the action of force, and the soft silica gel sleeve 33 returns to the original set shape after the force is applied.
A high-purity TMAH reagent ion chromatography detection method comprises the following steps:
the method comprises the following steps: accurately weighing 5-10 g of 25% TMAH sample, diluting the solution in a PFA bottle by 9-10 times with high-purity water, passing through a cationic resin column (001 x 7 type strong acid resin), filtering out the first 20ml, inoculating 10ml of sample, and performing detection and analysis;
step two: preparing 1ppm Cl and NO3 mixed solution as stock solution, preserving at constant temperature, preparing 10, 20, 50 and 100ppb mixed standard solution by adopting a stepwise dilution method, and preparing the standard solution for use in situ;
step three: making an external standard curve by using 10, 20, 50 and 100ppb mixed standard solution, wherein the correlation coefficient is more than or equal to 0.999;
step four: clicking a red button 'Stop' of the 863 automatic sample injector when the baseline is stable, and starting the automatic sample injector;
step five: placing a series of samples to be measured in a certain sequence, clicking a column in a sample table row in a 'measurement sequence' of a Magic Net 'working platform' interface, changing the column into yellow, then double clicking the column, selecting a 'new mixed standard method' in a 'method' of a popup dialog box, selecting a 'standard' mode for measurement if a standard curve is measured in a sample type, selecting a 'sample' mode for measurement if the sample is measured, filling the position of the automatic sample feeder where the sample to be measured is placed in a sample position, and filling '1' in a sample amount column;
step six: after all samples are edited, clicking 'start' to start measurement;
step seven: regenerating the used resin by using a sulfuric acid solution with the concentration of about 2%, soaking the resin in the sulfuric acid solution according to the volume ratio of 1:1.5, soaking the resin for 2 hours, and washing the resin with high-purity water until the pH value is 7.
The working principle and the using process of the invention are as follows: after the device is installed, when acting force is applied to a detection door panel 2 in the detection process, the detection door panel 2 is rotated to the side of a detection machine body 1, then a thin tube for detection is inserted from a buffer insertion tube 3 consisting of a tube head 31, an insertion tube 32 and a silica gel soft sleeve 33, the thin tube at the positions of an eluent and a regeneration liquid bottle is connected to a suppression module 6, after a pipeline is connected, 5-10 g of 25% sample is accurately weighed, the solution is diluted by 9-10 times by using high pure water in a PFA bottle, passes through a cation resin column (001 x 7 type strong acid resin), the previous 20ml is filtered, 10ml of sample is connected for detection and analysis, then 1ppm of Cl and NO3 mixed solution is prepared as a stock solution and stored at constant temperature, 10, 20, 50 and 100ppb mixed standard solutions are prepared respectively by adopting a stepwise dilution method, an external standard curve is prepared by using the 10, 20, 50 and 100ppb mixed standard solutions, when the base line is stable, clicking a red button 'Stop' of an 863 automatic sample injector, starting the automatic sample injector, placing a series of samples to be measured in a certain sequence, clicking a column in a sample table row in a 'measurement sequence' of a Magic Net 'working platform' interface, wherein the column is changed into yellow, then double clicking the column, selecting a 'mixed standard new method' in a 'method' of a popped dialog box, selecting a 'standard' mode for measurement in a 'sample type', selecting a 'sample' mode for measurement if a standard curve is measured, filling a position on the automatic sample injector where the samples to be measured are placed in a sample position, filling '1' in a column of the sample amount, and clicking 'start' to measure after all the samples are edited.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (6)
1. The utility model provides a high-purity TMAH reagent ion chromatogram detection device, includes and detects organism (1) and detection door plant (2), its characterized in that: the detection device is characterized in that a detection door plate (2) is arranged on the front side of the detection machine body (1), the detection door plate (2) is movably connected to the detection machine body (1) through an edge hinge bolt, a buffer insertion tube (3) is arranged on the surface of the detection door plate (2) close to the left edge, the buffer insertion tube (3) longitudinally penetrates through the detection door plate (2), an inspector chamber (4) is embedded into the front end of the detection machine body (1) at the upper right corner, a peristaltic pump set (5) is embedded into the front end of the detection machine body (1) below the inspector chamber (4), an inhibition module (6) is embedded into the front end of the detection machine body (1) at the left side of the peristaltic pump set (5), a high-pressure pump set (7) is embedded into the front end of the detection machine body (1) below the inhibition module (6), a sample introduction valve (8) is embedded into the front end of the detection machine body (1) at the right side of the high-pressure pump set (7), the front end embedding that lies in detecting organism (1) of the below of admission valve (8) has discharge valve (9), the right side of discharge valve (9) and admission valve (8) has pulse damper (10) in the front end embedding that lies in detecting organism (1), the rear end that detects organism (1) is being located the lower right corner department and is having embedded power source (11), the left side of power source (11) is being located the rear end embedding that detects organism (1) has detection line interface (12), the top of detection line interface (12) has been bolted at the rear end that lies in detecting organism (1) and has been detected apron (14), the left side that detects apron (14) has been in the rear end joint that lies in detecting organism (1) and has heat dissipation honeycomb panel (13), buffering intubate (3) include tube head (31), intubate (32) and soft cover of silica gel (33), the surface that detects door plant (2) is being provided with intubate (32) near left side edge, intubate (32) vertically runs through in detection door plant (2) department, tube head (31) have been bolted through the mutual interlock between the screw in both ends around intubate (32), the outside port department of tube head (31) has soft cover of silica gel (33) through the glue film bonding, soft cover of silica gel (33) are soft material, the elasticity deformation can take place under the effect of force in soft cover of silica gel (33), the soft cover of silica gel (33) atress is accomplished the back and is recovered to original settlement shape.
2. The ion chromatography detection device for high-purity TMAH reagent according to claim 1, wherein: the buffer insertion tubes (3) are arranged in two, the specification and the size of the buffer insertion tubes (3) are consistent, and the buffer insertion tubes (3) are arranged at the detection door plate (2) up and down.
3. The ion chromatography detection device for high-purity TMAH reagent according to claim 1, wherein: the bottom of the detection machine body (1) is embedded with pad feet at the corners around the bottom, and the pad feet at the bottom of the detection machine body (1) are in a rectangular distribution state.
4. The ion chromatography detection device for high-purity TMAH reagent according to claim 1, wherein: the detection door plate (2) can rotate by an angle ranging from zero to one hundred and eighty degrees relative to the detection machine body (1) under the action of force.
5. The ion chromatography detection device for high-purity TMAH reagent according to claim 1, wherein: the high-pressure pump unit (7) is connected with the exhaust valve (9) through a pipeline, the exhaust valve (9) is connected with the pulse damper (10) through a pipeline, and the pulse damper (10) is connected with the sample injection valve (8) through a pipeline.
6. The ion chromatography detection device for high-purity TMAH reagent according to claim 1, wherein: the power supply connected with the power supply interface (11) is a two-hundred and twenty-volt grounding power supply.
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| US4699718A (en) * | 1986-01-21 | 1987-10-13 | Millipore Corporation | Ion chromatography method and apparatus |
| CN106814151A (en) * | 2015-11-30 | 2017-06-09 | 江苏核电有限公司 | The measurement apparatus and measuring method of trace anion in a kind of strong basic reagent |
| CN106198800A (en) * | 2016-07-08 | 2016-12-07 | 中国石油化工股份有限公司 | Based on the device of anion and detection method in flowing dialysis sulfate by ion chromatography acrylic fiber solvent |
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