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CN213715246U - Sample introduction mechanical arm assembly and sample introduction device - Google Patents

Sample introduction mechanical arm assembly and sample introduction device Download PDF

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Publication number
CN213715246U
CN213715246U CN202022356539.4U CN202022356539U CN213715246U CN 213715246 U CN213715246 U CN 213715246U CN 202022356539 U CN202022356539 U CN 202022356539U CN 213715246 U CN213715246 U CN 213715246U
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sample
needle
arm
mechanical arm
sample introduction
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朱建雄
朱光皓
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Guangdong Lianjie Biotechnology Co ltd
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Guangdong Lianjie Biotechnology Co ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N35/00Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
    • G01N35/10Devices for transferring samples or any liquids to, in, or from, the analysis apparatus, e.g. suction devices, injection devices

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Abstract

The utility model belongs to the technical field of analytical instrument, concretely relates to advance appearance robotic arm subassembly and sampling device. This advance a kind of mechanical arm subassembly, including the arm that is used for the installation and dismantles the syringe needle to and with this arm complex horizontal conveyor, this horizontal conveyor has two equipartition points, and is equipped with the needle file of a syringe needle on two equipartition points respectively, this arm be used for with advance a kind of needle install in on the needle file and will advance a kind of needle and take off from the needle file. The utility model provides an arm assembly, simple structure can accomplish the sample fast and advance the appearance. The high-throughput automatic sample injector and the sample injection method have the advantages that all sampling and sample injection operations can be automatically completed, the sample injection speed is high, and one-time sample injection can be completed within 1-5 seconds.

Description

Sample introduction mechanical arm assembly and sample introduction device
Technical Field
The utility model belongs to the technical field of analytical instrument, concretely relates to advance appearance robotic arm subassembly and sampling device.
Background
Modern analytical instruments are generally provided with automatic sample injectors, so that the analysis process is completely automated, manpower is saved, the flux (sample analysis speed) of the analytical instrument is increased, and human errors are avoided.
There are a wide variety of autosamplers available on the market, but the basic structure usually includes a robotic arm, a sample storage device such as a sample tray, a needle pump, and a switching valve (sample injection valve). The sample holder is often provided with a thermostat to reduce and maintain the temperature of the sample at around 4 c, thereby avoiding or slowing down the decomposition of the sample by heat. When the sample storage device is operated, the mechanical arm and the needle pump are matched to convey samples in the sample storage device to the detector one by one for measurement, and the conveying pipeline is cleaned after sample introduction every time to eliminate residues and pollution. If the detection system involves high pressure, such as high performance liquid chromatography, the sample is first delivered to the sample injection valve and then introduced into the high pressure path by switching the sample injection valve for measurement.
Currently, the time required for the autosampler used in almost all analytical chemistries to complete the sample injection for one sample is typically between 1 and 2 minutes. For most of noble detection instruments, such as a chromatograph, a nuclear magnetic resonance spectrometer, a liquid/gas chromatograph-mass spectrometer and the like, the analysis time is long, and the influence on the sample injection speed is little. For cheaper instruments, such as various spectrometers, electrochemical detectors, thermal analyzers and the like, the analysis speed only needs a few seconds, which is not very worthy of increasing the sample injection speed at a high cost, because the automatic sample injector is usually more expensive than the instrument itself, and the purchase of the instruments is more economical when more samples are available.
However, for expensive instruments with fast analysis speed, such as flow injection mass spectrometers, the configuration of the conventional automatic sample injector results in large waste, since the value of the mass spectrometer generally exceeds millions and tens of millions, the analysis time of flow injection is at most about half a minute, and the time required for the automatic sample injector to suck, shift, clean, etc. is at least half a minute, so that the use value of the instrument is reduced by more than half. This situation requires a high throughput (high speed) autosampler.
The biggest drawbacks of the existing high-throughput sample injectors for analytical chemistry are three: (1) the mechanical arm is not fast enough in moving speed, and the sample injection can be completed in 1-2 minutes generally; (2) the sample storage device has small capacity, and most of the sample storage devices can only store hundreds of samples; (3) the volume is large, in order to store more samples, most of the existing automatic sample feeders keep the sample plate flat on a large plane, so that the space occupied by the automatic sample feeder is large, the range of the mechanical arm required to be displaced is also large, and a sample feeding process is completed for a longer time. The CTC automatic sample injector adopts a box type sample storage device, but adopts a mechanical arm to open and close the box, thereby not only greatly slowing down the sample injection speed, but also increasing the length of the mechanical arm and the stability of operation.
Therefore, there is a need for a true high throughput autosampler for flow injection analysis, especially for flow injection mass spectrometry.
SUMMERY OF THE UTILITY MODEL
An object of the embodiment of the utility model is to provide a advance kind robotic arm assembly and including this robotic arm assembly's high flux autoinjection device aims at solving the slow problem of kind speed among the prior art.
The embodiment of the utility model provides a kind mechanical arm component advances, including the arm that is used for the installation and dismantles the syringe needle to and with this arm complex horizontal conveyor, this horizontal conveyor has two equipartition points, and is equipped with the needle file of a syringe needle on two equipartition points respectively, this arm be used for with advance the syringe needle install in on the needle file and take off from the needle file with advancing the syringe needle.
Furthermore, the needle base is an omega-shaped buckle, and a U-shaped magnet or an electromagnet buckle.
Further, the mechanical arm is an XYZ trilinear arm, or an XYR, XRZ and RYZ two linear rotating shafts, or an XRR, RYR and RRZ one linear rotating shaft and two rotating shafts, or an RRR three rotating shaft mechanical arm.
Further, the mechanical arm comprises a vertical shaft and a horizontal moving arm, one end of the horizontal moving arm is vertically connected with the vertical shaft, the horizontal moving arm can rotate around the vertical shaft, and the rotation of the vertical shaft is driven by driving a worm gear through a spline shaft. Another object of the embodiment of the utility model is to provide a high flux autoinjection device, including above-mentioned robotic arm assembly.
Furthermore, the sample injection device also comprises a sample injection needle arranged on a needle seat of the mechanical arm, a standard bin for placing a standard sample, and a sample circulating bin for automatically conveying the sample to be detected.
Furthermore, the sample circulating bin comprises a mechanical pushing device for pushing the sample to be tested to move and a storage bin for storing the sample to be tested.
Further, the standard bin is located below the sample introduction mechanical arm assembly.
Further, the standard bin top height is substantially the same as the sample circulating bin top height.
Further, a top plate is arranged above the sample circulating bin and used for pressing the sample plate to avoid displacement when a sample is pricked by the sample injection needle.
Further, the top plate is provided with an opening hole at a position corresponding to a sample in the sample tray, and the opening hole is used for allowing a sample injection needle to pass through so as to suck the sample.
The utility model provides a mechanical arm component has simple structure, and the sample can be accomplished fast and advance the appearance to the quick advantage of convenient operation. The utility model provides a high flux autosampler and advance a kind method, whole sample advance kind operation all can accomplish automatically, and advance kind fastly, realize accomplishing once advance kind in 1-5 seconds, are showing the efficiency that has improved the detection sample.
Drawings
FIG. 1 is a block diagram of a robot arm assembly provided in one embodiment of the present application;
figures 2 and 3 are a block diagram and a rear view, respectively, of the robot assembly of figure 1;
FIG. 4 is another block diagram of the robot arm assembly of FIG. 1;
FIGS. 5 and 6 are partial block diagrams of a robot arm assembly provided in accordance with an embodiment of the present application;
FIG. 7 is a partial block diagram of a robot arm assembly provided in another embodiment of the present application;
FIG. 8 is a schematic diagram of a high throughput autosampler according to an embodiment of the present application;
FIGS. 9 and 10 are perspective views of sample wells of a high throughput autosampler provided herein, respectively;
FIG. 11 is a rear view of a sample compartment of a high throughput autosampler as provided herein;
FIG. 12 is a partial block diagram of a sample chamber of the high throughput autosampler provided herein;
fig. 13 is a schematic flow diagram of a high throughput autosampling method provided herein.
Detailed Description
In order to make the technical problem, technical solution and advantageous effects to be solved by the present invention more clearly understood, the following description is given in conjunction with the accompanying drawings and embodiments to further explain the present invention in detail. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The embodiment of the utility model provides a mechanical arm subassembly, this mechanical arm subassembly are used as the application of sample arm subassembly of high flux autosampler, and the arm among this mechanical arm subassembly can be for XYZ trilinear, or XYR, XRZ, two linear rotation axes that add of RYZ, or XRR, RYR, RRZ are linear to add two rotation axes, or the combination arm of RRR three rotation axes. Preferably, one embodiment is an XRZ combined three-axis mechanical arm, the longest arm is taken as an X axis, and the two ends in the horizontal direction are fixed and driven by a synchronous belt; the up-and-down motion is taken as a Z axis, the Z axis is connected to a synchronous belt of an X axis, and a spline shaft parallel to the X axis drives a synchronous belt in the vertical direction to drive. Preferably, the rotating shaft is driven by a group of worm gears driven by a spline shaft parallel to the X axis, the rotating shaft is coupled with the Z axis driving device at the top of the spline shaft, can rotate under the driving of the worm gears and can move up and down under the driving of the Z axis driving device, the coupling is fixed on the Z axis driving device by a strong magnet, the south pole or the north pole of the strong magnet is tightly attached to the top plane of the iron rotating shaft in a coupling mode, and the top of the rotating shaft is tightly sleeved into a bearing fixed in the Z axis driving device in another coupling mode. When used in a high throughput autosampler, the number of robotic arms may be one or two, and in the case of two robotic arms, the two robotic arms may be the same three-axis combination or different three-axis combinations. Specifically, the left and right operation range of each mechanical arm is 250-800 mm, the front and back operation range is 40-100 mm, the up and down operation range is about 15-150 mm, and the displacement precision is controlled to be about 0.1mm, so that accurate sample introduction is realized.
In particular, for the case of at least one linear axis, the robot arm is preferably mounted on a slide and is movable along the slide, the robot arm being horizontally displaceable by a conveyor belt controlled by a stepper motor or a servo motor. Preferably, the conveyor belt is in a track shape, and is provided with a latch thereon for correspondingly engaging with a slot on the mechanical arm to perform precise displacement and positioning, or the conveyor belt is provided with a slot, and the mechanical arm is provided with a latch at a corresponding position.
Specifically, the mechanical arm assembly can control the up-and-down displacement and the axial rotation of the sample injection needle through a spline shaft, for example, the rotation and the up-and-down movement of the mechanical arm are synchronously controlled through two spline shafts, so that the mechanical arm assembly can move to an injection port of a mass spectrometer for injection after the sample injection needle sucks a sample.
In particular, for a high throughput autosampler with two robotic arms, one is used for the sample injection of standard samples and the other is used for the sample injection of samples to be tested. In order to accelerate the mechanical movement speed, the dead weight of the moving part of the mechanical arm, namely the moving arm part, must be reduced as much as possible to reduce the inertia, the moving part is preferably made of light materials such as aluminum alloy and titanium alloy, and the movement in each direction is transmitted in the fastest transmission mode as much as possible, such as a synchronous belt, long arm rotation, a large-proportion gear and the like, so that the operation speed of the mechanical arm is improved, and one sample injection is completed within 1-5 seconds.
In one embodiment, the mechanical arm is an XRZ-combined three-axis mechanical arm, as shown in fig. 1, in which the horizontal direction (the direction in which the upper slide rail 33 and the lower slide rail 34 are arranged) in fig. 1 is the X axis, and the upper and lower directions are the Z axis, each mechanical arm is arranged on one slide rail, a motor arranged on the end side drives a spline shaft to drive the mechanical arm to move horizontally along the upper and lower slide rails, and a synchronous belt drives the mechanical arm to move up and down and rotate.
Figure 1 shows a block diagram of a robot arm assembly according to an embodiment of the present application, in which 2 sample introduction robot arm assemblies (4, 5) are shown, the two robot arm assemblies are structurally different, the robot arm assembly 4 is an XRZ combined three-axis robot arm, and the robot arm assembly 5 is an XR robot arm and cannot move up and down. The two sample feeding mechanical arm assemblies (4, 5) are simultaneously arranged on a group of track structures, the horizontal moving direction of the two sample feeding mechanical arm assemblies is used as an X axis, the sample feeding mechanical arm assemblies 4 can also move up and down (move along a Z axis) and can rotate around the self axis (R axis), and therefore sampling and injection are completed by controlling the displacement of the sample feeding needle. The tail ends of the mechanical arm assemblies (4, 5) are used for arranging a sample injection needle for injecting and sucking samples,
in another embodiment, the two robot arm assemblies are identical in structure and are both XRZ-combined three-axis robot arms.
Fig. 2 and 3 are a block diagram and a rear view of the robot arm assembly of fig. 1, which includes the enclosure 1 and the drive structure in addition to the above-described rail structures (the upper rail 33 and the lower rail 34). The whole enclosure structure is a rectangular frame structure and serves as a mounting frame of the track structure. The two ends of the upper sliding rail 33 and the lower sliding rail 34 are fixedly arranged on the enclosure structure, and the driving structure is arranged on one side of the enclosure structure, so that the integral structure is compact, and the installation and the disassembly are convenient.
Fig. 3 and 4 further show the driving structure of the robot arm assembly in the above embodiment. The drive structure includes four motor mounting blocks (21, 22, 23, 24), a motor mount 25 (see fig. 1), a servo or stepper motor 26, a first shaft motor 27 and a second shaft motor 28. Four motor installation cushion blocks are respectively installed on the left side and the right side, and each side respectively sets up 2 motor installation cushion blocks, respectively through motor installed part 25 interconnect. As shown in fig. 1, the first shaft motor 27 and the second shaft motor 28 are mounted on the outer side of the left end plate 12 and are used for connecting and driving a first spline shaft 31 and a second spline shaft 32, wherein the first spline shaft 31, the second spline shaft 32, the upper slide rail 33 and the lower slide rail 34 are all arranged in parallel. All driving motor fixed mounting are in the end of X axle in above-mentioned structure, do not remove along with the motion arm, have both reduced the dead weight of motion arm, do not have the tow line again, and the structure is more stable moreover, and the rate of motion can accelerate as far as possible.
For the mechanical arm assembly 4, the mechanical arm is sleeved on only one rail (the upper slide rail 33 or the lower slide rail 34), but is connected with the first spline shaft 31 and the second spline shaft 32 at the same time. The right ends of the first spline shaft 31 and the second spline shaft 32 are fixedly connected with a right end plate through an upper spline bearing and a lower spline bearing respectively. The servo motor 26 penetrates the front cover and is mounted on the motor mounting member 25. As shown in fig. 4, the track structure further includes an X-axis timing belt, a timing belt drive pulley 352, a timing belt driven pulley mounting member, a timing belt driven pulley 354, a timing belt driven pulley screw 355, and a timing belt driven pulley washer. And the two sides of the upper sliding rail 33 and the lower sliding rail 34 are respectively fixedly connected with motor mounting cushion blocks positioned on the left side and the right side. The servo or stepping motor 26 is connected to the synchronous belt driving wheel 352 through a rotating shaft, and drives the synchronous belt driving wheel 352 to rotate, thereby driving the X-axis synchronous belt to move and driving the mechanical arm to move along the upper sliding rail 33 or the lower sliding rail 34. The inside of the X-axis synchronous belt is in a rodent shape and is in meshing transmission with the synchronous belt driving wheel 352 and the synchronous belt driven wheel 354.
Fig. 5 and fig. 6 are schematic diagrams showing an embodiment of the present invention. The sample injection mechanical arm device comprises a sliding block mechanism, a vertical transmission structure, a pressure spring 44, a pressure spring retaining sheet 45, a rotating arm 46 and a sample injection needle interface 47. Wherein the slider mechanism comprises an upper slider 411, a lower slider 412, a connecting block 413, a mounting slider (414, 415, 416, 417, 418, 419) and a short slide rail slider 4191. The vertical transmission structure comprises a Z-axis synchronous belt 421, a spline driving wheel 422, a spline driven wheel 423, an X-axis synchronous belt toothed plate 424, a Z-axis synchronous belt toothed plate 425, a short slide rail 426, a turbine 427, a screw sleeve 428, an upper turbine bearing 4291, a lower turbine bearing 4292, a first screw bearing 4293, a second screw bearing 4294 and a short spline 43. The upper slider 411 and the lower slider 412 are engaged with the upper rail 33 and the lower rail 34, respectively. As shown in fig. 5, the upper spline shaft 31 rotates to drive the vertical transmission structure 42, thereby controlling the mechanical arm to move up and down; the lower spline shaft 31 rotates to drive the turbine 427 to rotate, thereby controlling the mechanical arm to rotate axially.
Fig. 7 is a schematic structural diagram of a robot arm assembly according to another embodiment of the present invention, which shows the structure of the robot arm assembly 5 on the left side in fig. 1. The robot arm assembly reduces the need for an up and down moving conveyor belt assembly relative to the robot arm shown in figures 5 and 6, which is only axially rotatable and cannot move up and down. Specifically, the mechanical arm device comprises a transmission mechanism, a screw sleeve 511, a first screw bearing 512, a second screw bearing 513, a turbine 514, a fixing mechanism 52, a mounting block 521, an upper bearing 522, a lower bearing 523, a sliding block 524, a zero position disk 525, a zero position spline 53, a rotating arm 54 and a sample injection needle interface 55, and the axial rotation principle of the mechanical arm device is the same as that of the mechanical arm assembly shown in fig. 5 and 6.
In a specific embodiment, if a mechanical arm assembly is used, the unknown sample and the standard sample are both fed by using the same mechanical arm, and the operation range of the mechanical arm only covers the area where the standard sample and the unknown sample are located, which is about 200x200mm, preferably about 180x150 mm. If two robotic arms are used, one for the unknown sample (sample to be tested) and the other for the standard sample, the footprint of each robotic arm is consistent with the dimensions of the sample tray. The three-axis structure of the mechanical arm is the same as the mechanical arm structure, and can be any combination of rotation and linear motion, and the preferred structure is an XRZ combination of two spline shafts and a synchronous belt drive, which is consistent with the embodiment. Other robotic arm configurations may also be employed.
Fig. 8 is a schematic structural diagram of a high throughput autosampler according to an embodiment of the present invention. The automatic sample injector comprises a conveying belt for conveying a sample injection needle, and a mechanical arm assembly, wherein the mechanical arm assembly can clamp the sample injection needle on a needle seat of the sample injection needle or take the sample injection needle off the needle seat. Specifically, the robot arm assembly may be the robot arm assembly described above, or may be other combinations of robot arm assemblies. In this embodiment, there is only one mechanical arm, which is used to install the sampled injection needle on the needle seat, the sample injection needle sucking the sample is transmitted from the mechanical arm to the far distance sample inlet of the mass spectrometer through an independent transmission belt, the transmission belt crosses over the standard sample inlet area and the sample inlet area to be measured, one end of the transmission belt is near the sample inlet of the mass spectrometer, the other end is above the sample plate, the needle seats of the sample injection needle are respectively installed on two points of the transmission belt, each needle seat is a device that can make the sample injection needle be easily installed and removed without changing the position and stability of the sample injection needle, such as an omega-shaped buckle, a "U" shaped magnet, an electromagnet, or the like, or a combination of these parts. When the sample injection needle carrying the unknown sample is conveyed to the sample injection port of the mass spectrometer for sample injection, the other sample injection needle is just above the sample plate, at the moment, the mechanical arm takes the needle down and sends the needle to the specified standard sample for sample absorption, then the needle is sent back and returned to the needle seat, once the sample injection of the unknown sample is finished, the conveyor belt immediately runs for half a week, the standard sample is sent to the sample injection port empty needle and sent to the mechanical arm for absorbing the next sample, and all samples are analyzed one by one in such a week. The advantage of the device structure is that a syringe needle is responsible for the sample, and another syringe needle is responsible for annotating the appearance, and both accomplish simultaneously, then the function replacement, and the circulation is reciprocal, compares in a mechanical arm and accomplishes the sample and inject whole cycle and practiced thrift a lot of times. Preferably, a vertical shaft, a Z shaft, can also be additionally arranged at the sample inlet of the mass spectrometer and used for pushing the sample injection needle downwards into the sample inlet for sample injection. If the sample injection needle also plays the role of a mass spectrum spray needle, the Z axis at the sample injection port can be omitted, and the conveying belt can be obliquely arranged at any angle, so that the sample injection needle can be accurately conveyed to the spray position without the assistance of any other mechanism. For the present embodiment, the positions of the standard sample and the sample to be tested can be placed at any position within the coverage of the sampling arm, and preferably, the standard sample tray and the sample injection tray to be tested are placed separately. In the specific operation, the standard sample is concentrated on a sample feeding disc and fixed at a special position, so that the standard sample can be prevented from entering a circulating bin along with the sample to be detected, the arrangement is prevented from being complicated, and the operation is convenient.
The embodiment of the utility model provides an in the injection needle be hollow needle, be connected with a needle pump for absorb and inject the sample.
The embodiment of the utility model provides a still provide a high flux autoinjection system, including advancing kind robotic arm subassembly, advance the needle, place standard sample's standard storehouse, still including the sample circulation storehouse and the control module of automatic sample presentation. The sample introduction robot assembly may be an XYZ trilinear, or XYR, XRZ, RYZ two linear plus one rotation axis, or XRR, RYR, RRZ one linear plus two rotation axes, or RRR three rotation axis combined robot assembly, preferably the robot assembly described above. The sample circulating bin comprises a set of mechanical pushing device for pushing a sample to be tested to move and a storage bin for storing the sample to be tested. The standard bin is located below the sample feeding mechanical arm, the length of the standard bin is approximately equal to the left and right running range of the mechanical arm, the width of the standard bin is basically consistent with the front and back running range of the mechanical arm, the depth of the standard bin is 0-10 mm larger than the downward movement limit of the mechanical arm, and the height of the standard bin is slightly smaller than the up and down running range of the mechanical arm, so long as the standard bin does not block the movement of the mechanical arm. The standard chamber can contain dozens to hundreds of standard samples and Quality Control (QC) samples. The standard bin can also be arranged at the top of the sample circulating bin and at the position with the height approximately the same as that of the sample to be measured.
In one embodiment, the storage chamber is a vertical rectangular box, the sample chamber is arranged in the vertical rectangular box, the front surface of the storage chamber is provided with a door, the periphery and the back surface of the storage chamber are formed by hard plates, a top plate is arranged above the storage chamber and presses the sample plate to prevent the sample plate from displacing when a sample is pricked by a sampling needle, and the top plate is provided with an opening corresponding to the sample position in the sample plate for the sampling needle to pass through so as to suck the sample. Two stacks of overlapped sample feeding discs can be placed in parallel in the storage bin, and a vertical partition plate can be added between the two stacks of sample feeding discs to preventThe sample stopping disc moves towards the left side and the right side in the circulation process. Each stack of sample injection trays can be a stack of any number of sample injection trays, but the total height of the stack is preferably close to and slightly lower than the height of the associated detection instrument. For example, when used in conjunction with a mass spectrometer, the height of the mass spectrometer is typically between 400 and 750mm, and the height of the corresponding storage bin is preferably between 350 and 700 mm. Each sample tray can hold 1-384 samples, and the most common standard tray holds 96 samples, namely a 96-well plate structure corresponding to international standards. The calculation formula of the total number of the sample trays stored in the sample bin is as follows:
Figure DEST_PATH_GDA0003080579660000091
where N is the number of sample trays that can be accommodated by the sample compartment, H is the height of the sample compartment, and H is the total height of the sample trays after the samples are loaded. For example, if the height of the sample tray plus sample is 35mm and the sample compartment is 400mm high, then the number of sample trays that can be accommodated by the sample compartment is 20. The tops of the left side and the right side of the sample bin are respectively provided with a vacancy which is communicated with each other and is slightly higher (about 1-5 mm) than the height of the sample disc filled with the sample, and the vacancies are used for circulating the sample disc. When the storage bin door is closed, the bin door and the back plate clamp the sample tray, so that the sample tray cannot move forwards and backwards when pushed. One pile of the two piles of sample trays always moves upwards and the other pile of the two piles always moves downwards in the circulating operation process. The vacant position at the top of the storage bin at the side moving upwards is a sample feeding position, the front and rear vertical walls of the vacant position are provided with a locking mechanism, and the sample tray cannot move up and down when not being pushed by strong force after being pushed into the position; the last but one position department that moves one side up also is equipped with the stopping mechanism, and after whole pile of sample dish up pushed a position, even if withdraw thrust sample pile and can not fall back automatically to leave a vacancy in the below. The inner arm of the downward storage bin is provided with a damping mechanism except the bottommost position, so that the whole stack of sample trays cannot automatically slide downward under the condition of not being pushed. The catch and backstop mechanism may be any means for allowing the sample plate to move up and preventing it from moving down, such as a spring loaded retractable detent pin with a downward slope, a spring detent ball, an L-shaped rear flip, a cross-shaped pivot, or the like. Damping machineThe mechanism can be any mechanism for preventing the sample plate from automatically sliding downwards under the action of the gravity of the sample plate, such as a rough surface on the inner surface of the storage bin, a magnetic material embedded on the inner surfaces of the sample plate and the storage bin, and the like.
The circulating operation process of the sample tray in the storage bin comprises the following steps that (1) the mechanical pushing device firstly pushes the sample tray stacked on one side upwards until the sample tray is pushed to a top plate above the sample tray, the mechanical pushing device returns to the original position immediately, and a vacant position is formed at the bottom of the upward side; (2) the mechanical pushing device pushes the bottommost sample plate on the downward side to the vacant position on the upward side, and the mechanical pushing device returns to the original position immediately; (3) the sample injection mechanical arm samples the top sample plate, and the top sample plate is injected into a mass spectrometer after each sample is taken, once a sample signal appears, the control module compares the sample signal with a stored standard product series, so that the position of the standard product with the closest signal intensity is selected, and the standard product sample injection mechanical arm immediately injects a sample into the standard product; (4) after a disc of samples is finished, the finished sample disc is pushed to the top vacant position on the downward side by a mechanical pushing device and then is pressed downwards for a vertical distance of one position, the vacant position is still left on the uppermost surface, and the vacant position on the lowermost surface is filled; (5) the next cycle of (1) to (4) is started.
Preferably, each sample injection tray is placed in a frame box, the length and the width of the frame box are just capable of accommodating the sample injection tray, the height of the frame box is slightly larger than the total height of the sample injection tray added into the sample container, the front surface of the frame box is opened, the sample injection trays containing samples can be freely placed in and taken out, the frame boxes are mutually overlapped, and the sample injection trays can circulate in the storage bin but cannot be easily taken out of the storage bin.
Fig. 9-12 show specific configurations of the autosampler sample magazine associated with a high throughput autosampler of an embodiment of the present invention. Fig. 9 shows a front view of the sample compartment comprising the sample enclosure 6, the first top panel 61, the intermediate baffle 62, the second top panel 71, the standard foam gasket 72, and the standard box 63. The sample box 63 is used for accommodating a sample to be measured. The first top plate 61 and the second top plate 71 are used for covering the sample box 63 and preventing displacement during sampling, and the first top plate 61 and the second top plate 71 are provided with openings corresponding to the positions of the samples in the box 63 so as to facilitate the insertion of the injection needles. In fig. 9, the right sample moves upward and the left sample moves downward when the sample trays to be tested are moved cyclically, as indicated by arrows in the figure, and all the sample trays move in one direction.
Wherein a mechanical pushing device is located behind the sample compartment and is connected to a link pusher 64 for pushing a sample cassette 63, as shown in fig. 10. The two sides of the middle baffle 62 are storage bins for storing samples to be tested.
Fig. 11 shows a rear view of the sample chamber, i.e., a structural view of the mechanical pushing means. The mechanical pushing device comprises: the device comprises a synchronous driven wheel 72, a synchronous belt 73, an electric telescopic rod 74, a vertical sliding block 75, a transverse connecting rod 76 with a fixed center and two rotatable ends, 2 vertical connecting rods 77 with different heights, a direct-current speed reduction motor 78 and a transverse pushing block 79. The cross link 76 is connected at its ends to 2 vertical links 77 to form a generally N-shaped structure. A synchronous drive wheel 721 is provided below the dc gear motor 78 for driving three other synchronous wheels, as shown in fig. 12. The mechanical pushing device further comprises a cold gas channel 8 for maintaining the temperature of the cryogenic sample. The transverse pushing block 79 is provided with a transverse pushing pin 791. Specifically, the driving motor (dc speed-reducing motor 78) drives the synchronizing wheel to drive the synchronizing belt to move, so that the horizontal push pins (two upper and lower horizontal push pins 791) connected with the synchronizing belt can move horizontally, the horizontal push pin 791 at the lower right corner in fig. 11 pushes the sample tray to move left, and the horizontal push pin 791 at the upper left corner pushes the sample tray to move right. Meanwhile, the vertical connecting rod 77 on the left side is driven by the up-and-down driving device (the electric telescopic rod 74) through the connecting block, the vertical connecting rod 77 on the right side is driven by the transverse connecting rod 76 to move up and down, the lower end of the vertical connecting rod 77 on the left side is connected with the supporting plate, the upper end of the vertical connecting rod 77 on the right side is connected with the pressing plate, the sample tray on the left side can be supported by the supporting plate, the sample tray on the right side can be pressed down by the pressing plate, and the supporting and pressing of the sample tray and the left. The specific working principle is as follows: referring to fig. 10, when the upper right sample tray is used up, the electric telescopic handle moves down to drive the right supporting plate to move down, the upper left pressing plate 64 moves up, the motor works immediately, the conveying belt drives the horizontal pushing pin to work, so that the empty sample tray is pushed to the upper left corner, the lower right corner horizontal pushing pin pushes the lower left sample tray to fill the lower right corner vacancy, then the electric telescopic handle resets, the upper left pressing plate 64 presses down the empty sample tray, the lower right supporting plate holds up the right supporting plate, and the upper right corner vacancy is filled.
Specifically, wash after the injection needle sample, traditional autosampler washes the needle required time and is often more than the time of inhaling appearance and injection sample, the embodiment of the utility model provides an in adopt the developments to wash the needle, concrete method is: set up a needle washing groove on the route that the injection needle got back to the sample district, the inslot sets up the waste liquid water conservancy diversion, mobile cleaning liquid, brush and air-drying device, the injection needle after accomplishing the sample injection is sent to the remaining sample liquid of the in-process in sample district fast and the needle washing liquid in the needle pump by pushing into the needle washing groove fast, the quick reverse cleaning liquid of drawing the inslot flow of injection needle simultaneously, the brush, air-dry the air current, reach the sample district just the complete sanitization and the outward appearance does not have the raffinate to leave over, needle washing time is not increased at all, show through the test: the residual sample can be reduced to below 0.1% by dynamic needle washing.
Another embodiment of the present invention provides a method for high-throughput autosampler, which is implemented by the above-mentioned high-throughput autosampler system, as shown in fig. 13. Specifically, after the system is started, initialization is performed, mass spectrum control software and a sample table are started at the same time, then a sample sequence table provided by a user is read, a standard sample data file is started, data collection is performed on the standard samples to record the concentration of each standard sample and the corresponding detection signal intensity and signal origin-destination time, then sample introduction is performed on each sample of the standard sample series twice one by one, after the completion, the data collection is stopped, the standard data file is closed, and sample introduction of samples to be detected (including unknown samples, QC samples, blank samples and the like) is performed (step S1).
Before each sample to be tested is injected, the software reads the information of the sample group from the sample table, if the sample and the previously injected sample do not belong to the same group, the sample is a new group, the software triggers the data acquisition and storage switch immediately, records and stores the subsequent process, and then starts the mechanical arm to sample and inject the sample; if not, the mechanical arm is directly started to sample and inject the sample. The purpose of this is to store all the detection signals of all the classified samples (of the same group) in one data file, which not only greatly reduces the number of data files, but also facilitates the subsequent data processing. In the specific operation, when each sample to be detected is injected, the type and the group of the sample are still read, and if the type of the sample is a standard product, the step S1 is repeated; if the sample belongs to the same group as the previously tested sample, directly proceeding to the next step S3; if not, indicating that the sample opened a new group, the software then closes the previous data file and stops data collection, then opens a new data file and resumes data collection to store the subsequent sample detection signal and corresponding origin-time (step S2);
in the sampling process, the mechanical arm moves downwards firstly to suck about 10 mu L of air firstly, then to suck a sample, then moves rightwards to reach a mass spectrum sample inlet, the mechanical arm descends to spray, if the sampling is needed to be continued, the mechanical arm ascends, then the detection system stores the peak height and the origin-destination time corresponding to the sample detection result, then a sample injection needle on the mechanical arm is cleaned, and the sample injection needle is cleaned and then ready to be used, and the step of injecting the sample is prepared to be repeated
Step S3 is an operation of not aspirating and injecting the sample to be tested, in which the control module instantly reads the detection signal and compares it with the signal intensity of each of the previously stored series of standard samples, thereby selecting one of the standard samples having the closest signal intensity as the reference of the sample to be tested.
Step S4 is that after a sample to be tested is fed, the selected standard sample is fed immediately, and the control module stores the detection signal values and the origin-destination times of the two samples in the opened data file.
Specifically, after the sample to be detected is injected, the detection system calculates the concentration of the sample to determine the position of the standard sample, then the standard sample is injected, the mechanical arm moves to the corresponding position according to the calculated position of the standard sample, the standard sample is sucked and then sprayed for sample injection, the system stores the peak height and the beginning and end time of the standard sample after sample injection, the mechanical arm moves to a needle washing port for needle washing, and then the sample injection operation is stopped. The mass spectrometer then stores the data file and fills in the sample table, ending the entire operation.
Further, step S1' is also included before step S2 is started: the sample tray is cycled as described above.
The utility model provides a method of high flux autoinjection through setting up one or two robotic arms to and automatic needle washing device, makes to advance kind in batches and can all automatic realization, and through setting up automatic storage storehouse to sample dish automatic cycle, has improved the efficiency of advancing kind.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not intended to limit the present invention, and all modifications, equivalents, improvements and the like that are made within the principles of the present invention are intended to be included within the scope of the present invention.

Claims (9)

1. The utility model provides a advance kind robotic arm subassembly, its characterized in that, including the arm that is used for the installation and dismantles the syringe needle to and with this arm complex horizontal conveyor, this horizontal conveyor has two equipartition points, and is equipped with the needle file of a kind syringe on two equipartition points respectively, this arm be used for with advance kind syringe install in on the needle file and will advance kind syringe and take off from the needle file.
2. The sampling mechanical arm assembly as in claim 1, wherein the needle mount is an omega-shaped snap, a "U" shaped magnet, or an electromagnet snap.
3. The sample introduction robot arm assembly of claim 1, wherein the robot arm is an XYZ trilinear, or an XYR, XRZ, RYZ twolinear plus one rotation axis, or an XRR, RYR, RRZ twolinear plus two rotation axes, or an RRR three rotation axis robot arm.
4. The sampling mechanical arm assembly as claimed in any one of claims 1 to 3, wherein the mechanical arm comprises a vertical shaft and a horizontal moving arm, one end of the horizontal moving arm is vertically connected with the vertical shaft, the horizontal moving arm can rotate around the vertical shaft, and the rotation of the vertical shaft is driven by a spline shaft driving a worm gear.
5. A sample introduction device comprising a sample introduction robot arm assembly according to any of claims 1-4.
6. The sample introduction device according to claim 5, further comprising a sample introduction needle mounted on the needle seat of the mechanical arm, a standard chamber for placing a standard sample, and a sample circulation chamber for automatically conveying a sample to be measured.
7. The sample introduction device according to claim 6, wherein the sample circulating chamber comprises a mechanical pushing device for pushing the sample to be tested to move and a storage chamber for storing the sample to be tested.
8. The sample introduction device according to claim 6, wherein the reference chamber is located below the sample introduction robot arm assembly.
9. The sample introduction device according to claim 6, wherein the standard chamber top height is substantially the same as the sample circulation chamber top height.
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