Automatic device and method combining full-automatic microwave digestion instrument and ICP-MS (Inductively Coupled Plasma Mass Spectrometry)

Abstract

The invention discloses a full-automatic microwave digestion instrument and ICP-MS combined automation device and method, and belongs to the field of analysis. A combined part in the full-automatic microwave digestion instrument comprises a mechanical arm assembly, a sample holder assembly, a first polytetrafluoroethylene tube, a probe assembly, a peristaltic pump assembly, a second polytetrafluoroethylene tube, a tube joint seat, a combined tube, a liquid taking tube, a reagent bottle, a waste liquid bottle, a waste discharge tube and a cleaning tube. The combined part in the ICP-MS comprises an atomizer assembly, a waste discharge pipe, a seven-way valve assembly, a 12-roller peristaltic pump assembly, a waste discharge pipe, a waste liquid bottle, a sample injection pipe, a peristaltic pipe and a reagent bottle; a combined pipe is arranged, and a probe assembly and the outlet end of a peristaltic pump assembly in the full-automatic microwave digestion instrument are correspondingly communicated with the inlet end of a seven-way valve assembly pipeline in the ICP-MS. A set of coupling structure is arranged between the full-automatic microwave digestion instrument and the ICP-MS, so that the automatic application of the whole system is realized, and a solution for integrating sample pretreatment and automatic analysis is provided.

Description

Technical Field

[0001] The invention belongs to the field of testing or analyzing materials, and in particular relates to an automated device and method for realizing the combination of a microwave digestion instrument and ICP-MS. Background Art

[0002] Microwave digestion is a method of sample pretreatment. It usually uses microwaves to heat the digestion solution and sample in a sealed container with acid. Under the action of high temperature, high pressure and strong acid, the sample matrix is ​​quickly decomposed and destroyed, turning into a liquid solution that is easy to analyze. At present, fully automatic microwave digestion instrument (abbreviated as microwave digestion instrument) has become an efficient sample pretreatment technology.

[0003] ICP-MS (Inductively Coupled Plasma-Mass Spectrometry) is an automated analytical instrument that combines ICP technology with mass spectrometry technology. It can analyze almost all metal elements in the periodic table, and can also analyze most non-metal elements. It uses unique interface technology to combine the high-temperature plasma ionization characteristics of ICP with the high sensitivity and rapid scanning advantages of mass spectrometers, and has become a widely used elemental analysis tool.

[0004] These two technologies / equipment (referring to microwave digestion instrument and inductively coupled plasma mass spectrometer) occupy a large market share in their respective fields.

[0005] Customers who need sample pretreatment usually also need sample analysis at the same time. They often complete sample pretreatment in one laboratory and then turn to a third-party testing agency for sample analysis. Even if there are users of these two technical devices, and these two devices are used independently, the samples need to be transferred back and forth for testing, which is time-consuming and labor-intensive, resulting in a great waste of manpower, material resources and other costs.

[0006] The invention application with the application publication date of 2023.11.24 and the application publication number of CN 117110413 A discloses a method for determining arsenic in sodium oleate by microwave digestion and ICP-MS, including: accurately measuring the internal standard solution to prepare the internal standard solution; accurately measuring the arsenic element standard solution to prepare the linear solution; digesting the sodium oleate as the test solution; digesting nitric acid as the blank solution; using Rh as the internal standard, using the online internal standard method, and mixing it with the sample by a peristaltic pump before entering the ICPMS for detection. In this technical solution, the microwave digestion method is used in the preparation of the test solution and the blank solution. In the detection stage, the linear solution, the test solution, and the blank solution are mixed with the sample by the online internal standard method by a peristaltic pump and then enter the ICP-MS for detection. This technical solution obviously falls into the aforementioned situation of "two technologies / equipment are used independently". The samples also need to be transferred back and forth for testing. It fails to free the testers from the tedious and repetitive work, and does not involve the concept of improving the degree of automation of the analysis system.

[0007] The invention patent with the authorization announcement date of 2015.05.13 and the authorization announcement number of CN 102928500 B discloses a "detection method for directly determining organic selenium, protein selenium or polysaccharide selenium in seafood by microwave digestion-ICP-MS method", including: 1. Sample preparation: shell the sample and put it into a sample bag; (i) separation and purification of organic selenium: continuous dialysis; (ii) separation and purification of selenoprotein; (iii) separation and purification of selenopolysaccharides. 2. Determination of selenium content: (i) microwave digestion; (ii) blank test, treat the reagents that have not been in contact with the sample to be tested according to the method of (i) in the second method; (iii) inductively coupled plasma mass spectrometry. This technical solution still belongs to the situation of "two technologies / equipment are used separately", and does not involve the concept of "realizing the full process automation of elemental analysis".

[0008] If the two technologies / equipment, microwave digester and inductively coupled plasma mass spectrometer, can be automatically combined to realize the automated application of the system, the full process automation of elemental analysis can be realized, which can truly free the testers from tedious and repetitive work, make up for the shortcomings of traditional operations such as complexity, time-consuming and unsatisfactory results, and provide an integrated solution from sample pretreatment to automated analysis. Summary of the invention

[0009] The technical problem to be solved by the present invention is to provide an automatic device and method for the combination of a full-automatic microwave digestion instrument and ICP-MS. By setting a set of combination structures between the full-automatic microwave digestion instrument and the ICP-MS, the sampling, suction and transportation, sample loading, injection, detection and analysis, and cleaning steps can be automatically cycled, and the automatic combination between the full-automatic microwave digestion instrument and the ICP-MS is realized. The cyclic workflow of the full-automatic microwave digestion instrument and the operation process of the ICP-MS are interconnected, and the automatic application of the system is realized, which can realize the full process automation of element analysis.

[0010] The technical solution of the present invention is to provide an automatic device for combining a fully automatic microwave digestion instrument and ICP-MS, comprising a fully automatic microwave digestion instrument and an ICP-MS, characterized in that:

[0011] In the fully automatic microwave digestion instrument and ICP-MS, a set of coupling structures are respectively set;

[0012] The structure of the coupling part in the fully automatic microwave digestion instrument at least includes the following parts: a mechanical arm assembly, a sample rack assembly, a first tetrafluoro tube, a probe assembly, a peristaltic pump assembly, a second tetrafluoro tube, a tube connector, a coupling tube, a liquid collection tube, a reagent bottle, a waste liquid bottle, a waste discharge tube and a cleaning tube;

[0013] The structure of the coupling part in ICP-MS at least includes the following parts: a nebulizer assembly, a waste pipe, a seven-way valve assembly, a 12-roller peristaltic pump assembly, a waste pipe, a waste liquid bottle, a sample injection tube, a peristaltic tube and a reagent bottle;

[0014] A coupling tube is provided to connect the outlet ends of the probe assembly and the peristaltic pump assembly in the fully automatic microwave digestion instrument with the inlet end of the seven-way valve assembly pipeline in the ICP-MS; one end of the coupling tube constitutes the output end of the coupling part of the fully automatic microwave digestion instrument, and the other end constitutes the input end of the coupling part of the ICP-MS, playing the role of a connection / coupling pipeline between the coupling part of the fully automatic microwave digestion instrument and the fully automatic microwave digestion instrument;

[0015] In the fully automatic microwave digestion instrument, after the fully automatic microwave digestion instrument digests the sample, the sample solution is sucked up by the peristaltic pump; it is transported to the inlet end of the pipeline of the ICP-MS seven-way valve assembly through the coupling tube; by controlling the switching of the seven-way valve assembly, the ICP-MS sequentially realizes the operations of injection, sample delivery, and cleaning, and performs detection and analysis on the sample solution, thereby realizing automation and integration from sample pretreatment to analysis; the automatic coupling between the fully automatic microwave digestion instrument and the ICP-MS is realized, and the cyclic workflow of the fully automatic microwave digestion instrument and the operation process of the ICP-MS are interconnected, so that the full process automation of element analysis can be realized; during the ICP-MS injection process, the fully automatic microwave digestion instrument also performs automatic cleaning operations at the same time to prepare for the next injection.

[0016] Specifically, the mechanical arm assembly consists of two parts: a mechanical arm and a clamp. The clamp is fixed to the mechanical arm by screws, and the mechanical arm is fixed in the frame of the microwave digestion instrument. The mechanical arm assembly is used to clamp the sample cup or sample rack. The sample rack assembly consists of a sample cup and a sample rack. The sample cup is a part for holding samples, and the blind hole clearance of the sample rack and the sample cup is matched.

[0017] Specifically, the probe assembly includes a probe fixed on a probe seat, a slider, a guide rail, a synchronous belt, a motor, and a bracket; wherein the motor is fixed at one end of the bracket, a lower synchronous wheel is arranged at the other end of the bracket, and the synchronous belt is sleeved between the motor at the upper end of the bracket and the lower synchronous wheel at the lower end of the bracket; a guide rail is arranged in parallel on one side of the bracket; a slider is movably arranged on the guide rail; the probe seat is fixedly connected to the slider and the synchronous belt; the motor rotates, driving the synchronous belt to pull the probe seat and the probe to slide up and down along the guide rail, thereby realizing the up and down movement function of the probe.

[0018] Furthermore, the peristaltic pump assembly comprises a first peristaltic pump, a second peristaltic pump, a peristaltic tube, a joint assembly, a joint fixing plate, a second polytetrafluoro tube, and a connecting tube; wherein the first peristaltic pump is connected to the peristaltic tube, the joint assembly is fixed on the joint fixing plate, the joint on one side of the joint assembly is connected to the second polytetrafluoro tube at the bottom and to the peristaltic tube at the top, the joint on the other side of the joint assembly is connected to the joint at the top and to the connecting tube at the bottom; the peristaltic pump driver provides power to drive the pump head to operate and realize the suction / output of liquid; after the first peristaltic pump completes the sample delivery, the robotic arm removes the sample tank, the probe assembly moves downward, the probe enters the cleaning tube, the second peristaltic pump works, and the liquid extraction tube connected to the second peristaltic pump draws nitric acid from the reagent bottle, and the nitric acid enters the cleaning tube through the peristaltic tube and the connecting tube to clean the probe, and the waste liquid is discharged into the waste liquid bottle through the waste discharge pipe connected to the cleaning tube.

[0019] Specifically, the nebulizer assembly includes a nebulizer chamber body and a nebulizer chamber, a nebulizer chamber connecting pipe is arranged above the nebulizer chamber body, an injection joint is arranged on the side, and a waste liquid joint is arranged at the bottom; the analytical solution sample is transported to the ICP-MS through the coupling tube and the seven-way valve assembly; when the analytical solution sample enters the nebulizer chamber through the injection joint, nitrogen is simultaneously introduced into the nebulizer chamber structure perpendicular to the sample, and the solution sample at the outlet of the nebulizer capillary central tube is broken into droplets by the impact of the airflow, becoming a primary aerosol, forming the medium required for ICP-MS instrument analysis, and the excess waste liquid will be connected to the waste liquid pipe from the waste liquid joint of the nebulizer chamber body and discharged through the peristaltic pump.

[0020] Specifically, the seven-way valve assembly at least includes a motor and a valve body; the valve body includes a valve head and a valve core; the seven-way valve assembly has seven channels 1#-7#, the motor drives the valve body to rotate, and the switching of the required channels is achieved through the valve head and the valve core; the solution sample enters the quantitative ring through one of the channels, and the solution exceeding the storage volume of the quantitative ring is discharged through the seven-way valve switching channel; the connection between each switching channel of the seven-way valve and the 12-roller peristaltic pump can respectively realize the functions of ICP-MS injection, sample delivery, and cleaning.

[0021] Furthermore, the 12-roller peristaltic pump assembly includes a drive motor, a movable roller, a fixed roller, an elastic delivery hose and a shell; the drive motor drives the movable roller to rotate, and the movable roller squeezes the peristaltic tube arranged between the movable roller and the fixed roller, and a negative pressure is formed in the peristaltic tube, and the liquid in the tube flows accordingly; the sample solution is pumped by alternately squeezing and releasing the elastic delivery hose arranged around the movable and fixed rollers.

[0022] Specifically, the automatic device for combining the fully automatic microwave digester and ICP-MS, by respectively setting a set of combination structures between the fully automatic microwave digester and the ICP-MS, and uniformly controlling through a program, enables the automatic cycle of sampling, suction and transportation, sample loading, injection, detection and analysis, and cleaning steps, thereby realizing the automatic combination between the fully automatic microwave digester and the ICP-MS, and realizing the interconnection between the cyclic workflow of the fully automatic microwave digester and the operation process of the ICP-MS, thereby realizing the automated application of the system and being able to realize the full process automation of elemental analysis.

[0023] The technical solution of the present invention also provides an automated operation method of the above-mentioned fully automatic microwave digestion instrument + ICP-MS combined automation device, which is characterized by comprising the following steps or procedures:

[0024] Step 1: After the fully automatic microwave digestion instrument digests the sample, the robotic arm clamps the sample cup to the probe assembly, the guide rail probe assembly moves down, and the sample is taken from the sample cup; the sample passes through the second PTFE tube to the peristaltic pump assembly, and the sample is sucked and transported through the peristaltic pump;

[0025] Step 2: The sample solution is transmitted through the coupling tube to the seven-way valve assembly of the ICP-MS. At this time, the seven-way valve switches the channel and sends the sample solution to the quantitative loop for storage;

[0026] Step 3: The seven-way valve cuts the quantitative loop into the flow path. At the same time, the 12-roller peristaltic pump of the ICP-MS draws the carrier fluid into the flow path and pushes the sample solution into the nebulizer assembly for detection and analysis.

[0027] Step 4: Insert the injection needle of the fully automatic microwave digestion instrument into the cleaning tube, and absorb the cleaning liquid to clean the injection needle pipeline;

[0028] Step 5: After the ICP-MS analysis is completed, the seven-way valve quantitative loop is kept in the flow path for 3 seconds and the quantitative loop is cleaned with carrier liquid. At this point, a cycle of fully automatic microwave digestion instrument + ICP-MS automation is completed;

[0029] At the same time, the injection needle of the fully automatic microwave digestion instrument is inserted into the next standard or sample solution, so that the process cycle and ICP-MS can be interconnected.

[0030] Further, the steps and processes of combining the key components of the ICP-MS to work are as follows:

[0031] 1) Sample loading stage: The liquid output from the fully automatic microwave digestion instrument coupling tube is pumped into the seven-way valve assembly and stored in the quantitative loop; during the sample loading process, the 12-roller peristaltic pump assembly pumps the carrier liquid into the nebulizer cleaning channel;

[0032] In the loading phase, ICP-MS completes the process of loading, draining, cleaning, and draining;

[0033] 2) Injection stage: The seven-way valve assembly switches the channel, the sample in the quantitative loop enters the peristaltic tube, and the 12-roller peristaltic pump assembly pumps the carrier liquid into the peristaltic tube, pushing the sample into the nebulizer to complete the analysis;

[0034] 3) During the ICP-MS sampling process, the fully automatic microwave digester also performs automatic cleaning to prepare for the next step of sampling.

[0035] Compared with the prior art, the advantages of the present invention are:

[0036] 1. The technical solution of the present invention realizes the automation application of the whole system by setting a coupling structure between the fully automatic microwave digestion instrument and the ICP-MS, and provides an integrated solution from sample pretreatment to automated analysis;

[0037] 2. The technical solution of the present invention is that the connection between the two machines is fully automated, which makes it unattended, saves labor costs, truly liberates the hands of laboratory personnel, and saves 50% of analysis time;

[0038] 3. The technical solution of the present invention can realize one-key setting, which is more convenient to operate and the two machines are interconnected, saving time and effort;

[0039] 4. The technical solution of the present invention realizes the fully automatic coupling between the fully automatic microwave digestion instrument and ICP-MS, forming a set of efficient sampling-analysis system, and the testing process is more stable, efficient and reliable. BRIEF DESCRIPTION OF THE DRAWINGS

[0040] Figure 1 It is a structural schematic diagram of the combined part of the fully automatic microwave digestion instrument of the present invention;

[0041] Figure 2 It is a structural schematic diagram of the mechanical arm assembly of the present invention;

[0042] Figure 3 is a schematic structural diagram of a sample rack assembly of the present invention;

[0043] Figure 4 It is a schematic diagram of the structure of the polytetrafluoroethylene tube of the present invention;

[0044] Figure 5 is a schematic structural diagram of the probe assembly of the present invention;

[0045] Figure 5a is a schematic diagram of the structure of the probe seat;

[0046] Figure 5b It is a structural schematic diagram of the needle seat fixing plate;

[0047] Figure 5c It is a structural schematic diagram of the synchronous belt pressure plate;

[0048] Figure 5d is a structural schematic diagram of the rotating shaft;

[0049] Figure 5e It is a structural schematic diagram of the synchronous wheel;

[0050] Figure 6 It is a schematic diagram of the piping structure of the peristaltic pump assembly of the present invention;

[0051] Figure 7 It is a schematic diagram of the positional relationship between the coupling part of the fully automatic microwave digestion instrument of the present invention and the complete machine of the fully automatic microwave digestion instrument;

[0052] Figure 8 It is a schematic diagram of the structure of the ICP-MS coupling part of the present invention;

[0053] Figure 9a is a schematic diagram of the structure of the atomizer assembly;

[0054] Figure 9b It is a schematic diagram of the working process of the atomizer assembly;

[0055] Fig.10a Schematic diagram of the appearance structure of the seven-way valve assembly;

[0056] Fig.10b is a schematic cross-sectional view of a seven-way valve assembly;

[0057] Fig.11 is a schematic diagram of the structure of a roller peristaltic pump assembly;

[0058] Fig.12 It is a schematic diagram of the ICP-MS loading steps;

[0059] Fig.13 It is a schematic diagram of the ICP-MS injection steps;

[0060] Fig.14 It is a schematic diagram of the working principle of the combination of fully automatic microwave digestion instrument and ICP-MS.

[0061] In the figure, 1 is a mechanical arm assembly, 2 is a sample rack assembly, 3 is a first tetrafluoro tube, 4 is a probe assembly, 5 is a peristaltic pump assembly, 6 is a second tetrafluoro tube, 7 is a tube connector, 8 is a coupling tube, 9 is a liquid collection tube, 10 is a reagent bottle, 11 is a waste liquid bottle, 12 is a waste discharge tube, 13 is a cleaning tube, and 14 is a housing assembly of the coupling part of the full-automatic microwave digestion instrument;

[0062] 1.1 is a mechanical arm, 1.2 is a clamping claw, 2.1 is a sample dissolution cup, 2.2 is a sample rack, 4.1 is a probe, 4.2 is a probe seat, 4.3 is a movable pressure column, 4.4 is a needle seat fixing plate, 4.5 is a bracket, 4.6 is a guide rail, 4.7 is a belt, 4.8 is a motor, 4.9 is a rotating shaft, 4.10 is a lower synchronous wheel, 4.11 is a bearing fixing seat, 4.12 is a probe through hole, 4.13 is a probe seat fixing hole, 4.14 is a needle seat fixing plate fixing hole, 4.15 is a probe seat fixing hole, 4.16 is a synchronous wheel rotating shaft through hole, 5.1 is a first peristaltic pump, 5.2 is a second peristaltic pump, 5.3 is a peristaltic tube, 5.4 is a joint assembly, 5.5 is a joint fixing plate, 5.6 is a connecting tube, and 5.7 is a pump chamber bracket;

[0063] 1' is the nebulizer assembly, 2' is the waste pipe, 3' is the seven-way valve assembly, 4' is the 12-roller peristaltic pump assembly, 5' is the waste pipe, 6' is the waste liquid bottle, 7' is the injection tube, 8' is the peristaltic tube, 9' is the reagent bottle, 10' is the housing of the ICP-MS, and 11' is the quantitative loop;

[0064] 1.1' is the spray chamber body, 1.2' is the spray chamber, 1.3' is the spray chamber connecting pipe, 1.4' is the injection joint, 1.5' is the waste liquid joint, 1.6' is the sample, 1.7' is the nitrogen, 3.1' is the motor, 3.2' is the valve body, 3.2.1' is the valve head, 3.2.2' is the valve core, 4.1' is the motor, 4.2' is the moving roller, 4.3' is the fixed roller, and B' is the automatic sampler;

[0065] A is ICP-MS, and B is fully automatic microwave digestion instrument. DETAILED DESCRIPTION

[0066] The present invention will be further described below in conjunction with the accompanying drawings.

[0067] like Figure 1 As shown in the figure, the structure of the combined part of the fully automatic microwave digestion instrument mainly consists of the following parts:

[0068] Robotic arm assembly 1, sample rack assembly 2, first polytetrafluoroethylene tube 3, probe assembly 4, peristaltic pump assembly 5, second polytetrafluoroethylene tube 6, tube connector 7, connecting tube 8, liquid collection tube 9, reagent bottle 10, waste liquid bottle 11, waste discharge tube 12, cleaning tube 13, outer shell assembly 14.

[0069] Specifically, the structure of the robot arm assembly 1 is as follows: Figure 2 As shown in , the robot arm assembly 1 consists of two parts: a robot arm 1.1 and a clamping jaw 1.2. The clamping jaw is fixed to the robot arm by screws, and the robot arm is fixed in the frame of the microwave digestion instrument.

[0070] Figure 3 In the figure, the sample rack assembly 2 is composed of a sample cup 2.1 and a sample rack 2.2. The sample cup is a part for holding samples. The fully automatic microwave digestion instrument needs to work in a high temperature, high pressure and high acid environment, and has high requirements on the material of the dissolved oxygen cup. Generally, corrosion-resistant modified PTFE is used. Because of the large-scale testing environment, the sample rack needs to consider corrosion resistance and portability, and the blind hole clearance between the sample rack and the sample cup is matched.

[0071] Figure 4 In the figure, the first tetrafluoro tube 3 is a connecting piece between the probe and the peristaltic pump, and it is a channel for direct sampling in the linkage structure.

[0072] See also Figure 5 , Figure 5a to Figure 5eIn the figure, the probe assembly 4 is the core component of the combined structure, the probe 4.1 is a tube connector, which is fixed to the probe seat by a movable pressure column 4.3 through the probe through hole 4.12 of the probe seat 4.2, and the probe seat is fixed to the needle seat fixing plate 4.4 by screws. The probe seat is fixed to the slider bracket (not shown in the figure), and the fixing hole 4.14 of the needle seat fixing plate and the bracket is a U-shaped hole, which can indirectly adjust the position of the probe tube. The needle seat fixing plate is fixed to the slider (not shown in the figure) of the guide rail 4.6, and the needle seat fixing plate is also fixed together with a synchronous belt (referred to as belt 4.7) by fasteners; the motor 4.8 is fixed to one end of the bracket, and a rotating shaft 4.9 is set at the other end of the bracket, and a lower synchronous wheel 4.10 is set on the rotating shaft, and the belt is set between the motor at the upper end of the bracket and the lower synchronous wheel at the lower end of the bracket. The motor rotates, driving the belt to pull the needle seat assembly to slide up and down along the guide rail to realize the up and down movement function of the probe.

[0073] The rotating shaft 4.9 is fixed to the lower end of the bracket through the bearing fixing seat 4.11.

[0074] See also Figure 6 As shown in the figure, the peristaltic pump assembly 5 includes a first peristaltic pump 5.1 and a second peristaltic pump 5.2. The first peristaltic pump is connected to a peristaltic tube 5.3. A joint assembly 5.4 is fixed on a joint fixing plate 5.5. The lower side of the joint on one side of the joint assembly is connected to the second polytetrafluoro tube 6 and the upper side is connected to the peristaltic tube 5.3. The upper side of the joint on the other side of the joint assembly is connected to the joint and the lower side is connected to the connecting tube 8.

[0075] The first peristaltic pump, the second peristaltic pump, the connector assembly and the connector fixing plate are all fixed on the pump compartment bracket 5.7.

[0076] The peristaltic pump driver provides power to drive the pump head to operate and realize the suction and output of liquid. The second peristaltic pump 5.2 is used to clean the probe. After the first peristaltic pump completes the sample delivery, the robot arm removes the sample tank, the probe assembly 4 moves downward, the probe enters the cleaning tube 13, the second peristaltic pump works, and the liquid collection tube 9 connected to the second peristaltic pump draws nitric acid from the reagent bottle 10. The nitric acid enters the cleaning tube through the peristaltic tube and the connecting tube 5.6 to clean the probe. The waste liquid is discharged to the waste liquid bottle 11 through the waste discharge tube 12 connected to the cleaning tube.

[0077] like Figure 7 As shown in , the above-mentioned fully automatic microwave digestion instrument coupling part is integrally installed in the housing of the fully automatic microwave digestion instrument, leaving a coupling tube 8 for connecting with the coupling part of the ICP-MS through a pipeline.

[0078] exist Figure 8 In this technical solution, the structure of the ICP-MS coupling part mainly consists of the following parts:

[0079] Atomizer assembly 1', waste pipe 2', seven-way valve assembly 3', 12-roller peristaltic pump assembly 4', waste pipe 5', waste liquid bottle 6', sample injection tube 7', peristaltic tube 8', reagent bottle 9', shell 10'.

[0080] like Figure 9a and Figure 9b As shown in the figure, the nebulizer assembly 1' is a sample injection system assembly and is an extremely important component of ICP-MS; it includes a nebulizer chamber body 1.1' and a nebulizer chamber 1.2', a nebulizer chamber connecting pipe 1.3' is arranged above the nebulizer chamber body, a sample injection connector 1.4' is arranged on the side, and a waste liquid connector 1.5' is arranged at the bottom.

[0081] The workflow of the nebulizer assembly is as follows Figure 9b As shown, the analytical solution sample 1.6' enters the nebulizer chamber through the injection connector, and nitrogen gas 1.7' is introduced into the nebulizer chamber structure perpendicular to the sample. The carrier gas flow rate is very fast at the outlet of the capillary center tube of the nebulizer, while the solution sample flow rate is relatively slow, and friction is generated between the two, so that the liquid flow is stretched and broken into droplets by the impact of the air flow to become a primary aerosol, forming the medium required for ICP-MS instrument analysis. Excess waste liquid will be connected to the waste liquid pipe from the waste liquid connector of the nebulizer body and discharged through the peristaltic pump.

[0082] See also Fig.10a and Fig.10b As shown in , the seven-way valve assembly 3' comprises at least a motor 3.1' and a valve body 3.2'; the valve body comprises a valve head 3.2.1' and a valve core 3.2.2'.

[0083] The seven-way valve assembly has seven channels 1#-7#. The motor drives the valve body to rotate, and the required channels are switched through the valve head and valve core. The sample solution enters the quantitative ring 11' through one of the channels (see Fig.12 The quantitative loop serves as a temporary storage for the sample solution, and the solution exceeding the storage volume of the quantitative loop will be discharged through the seven-way valve switching channel. The connection between each switching channel of the seven-way valve and the 12-roller peristaltic pump can realize the functions of ICP-MS injection, sample delivery, and cleaning.

[0084] See also Fig.11 As shown in the figure, the 12-roller peristaltic pump assembly 4' is mainly composed of a drive motor 4.1', a moving roller 4.2', a fixed roller 4.3', and an elastic delivery hose (also called a peristaltic tube). The motor drives the moving roller to rotate, and the moving roller squeezes the peristaltic tube arranged between the moving roller and the fixed roller. Negative pressure is formed in the peristaltic tube, and the liquid in the tube flows accordingly. The sample solution is pumped by alternately squeezing and releasing the elastic delivery hose arranged around the moving and fixed rollers, and it can accurately control the flow rate.

[0085] 12-roller peristaltic pumps are also commercially available products. Any 12-channel peristaltic pump such as Omron peristaltic pump, Aiko peristaltic pump, and Telmei peristaltic pump can be used. As long as the pump flow meets the needs, there are no special requirements.

[0086] Introduction to the working principle of the three key components in ICP-MS:

[0087] Sampling: The liquid of the automatic sampler is pumped into the seven-way valve assembly 3' and stored in the quantitative loop. The excess sample solution will be discharged from the channel 6 of the seven-way valve. During the sampling process, the roller peristaltic pump assembly 4' pumps the carrier liquid (equivalent to Figure 8 The nitric acid or other solution in the reagent bottle 9' is pumped into the atomizer cleaning channel.

[0088] In the loading stage, the process of loading, discharging, cleaning and discharging is completed, as shown in the following figure. Fig.12 as shown in .

[0089] Injection: The seven-way valve assembly 3' switches the channel, the sample in the quantitative loop enters the peristaltic tube, and the 12-roller peristaltic pump assembly 4' transfers the carrier liquid (equivalent to Figure 8 The nitric acid in the reagent bottle 9' is pumped into the peristaltic tube to push the sample into the atomizer to complete the analysis. Fig.13 as shown in .

[0090] During the injection process, the autosampler also performs automatic cleaning to prepare for the next injection.

[0091] exist Fig.12 and Fig.13 In the figure, the automatic sampler B' located on the left side is implemented by the full-automatic microwave digester B in the present technical solution. The coupling tube 8 output from the coupling part of the full-automatic microwave digester constitutes the output end of the coupling part of the full-automatic microwave digester on the one hand, and the input end of the ICP-MS coupling part on the other hand, playing the role of a connecting / coupling pipeline between the coupling part of the full-automatic microwave digester and the full-automatic microwave digester.

[0092] In the technical solution of the present invention, the connection relationship and working principle of the fully automatic microwave digestion instrument and ICP-MS are as follows: Figure 1 , Figure 7 , Figure 8 and Figure 12 to Figure 14 As shown in:

[0093] Step 1: After the fully automatic microwave digestion instrument digests the sample, the robot arm 1 clamps the sample cup to the probe assembly 4, the guide rail probe assembly 4 moves down, and the sample is taken from the sample cup; the sample passes through the polytetrafluoroethylene tube 6 to the peristaltic pump assembly 5, and the sample is sucked and transported through the peristaltic pump.

[0094] Step 2: The sample solution is transmitted through the coupling tube 8 and first reaches the seven-way valve assembly 3' of the ICP-MS. At this time, the seven-way valve switches the channel and sends the sample solution to the quantitative loop for storage.

[0095] In fact, the fully automatic microwave digestion instrument at this time is equivalent to the automatic sampler B' in Figures 9 and 10.

[0096] Excess sample liquid will be discharged through the seven-way valve outlet.

[0097] Step 3: The seven-way valve cuts the quantitative loop into the flow path. At the same time, the 12-roller peristaltic pump of the ICP-MS draws the carrier fluid (1% nitric acid) into the flow path and pushes the sample solution into the nebulizer assembly 1' for detection and analysis.

[0098] Step 4: Then the injection needle of the fully automatic microwave digestion instrument is inserted into the cleaning tube 13, and the cleaning liquid (2% nitric acid) is sucked to clean the injection needle pipeline.

[0099] Step 5: After the ICP-MS analysis is completed, the seven-way valve quantitative loop remains in the flow path for 3 seconds and is cleaned with a carrier liquid (1% nitric acid), thus completing one cycle of the coupling.

[0100] The sampling needle of the fully automatic microwave digestion instrument is inserted into the next standard or sample solution, so that the process cycle and ICP-MS can be interconnected.

[0101] In the above technical solution, there are no special requirements for the fully automatic microwave digester, ICP-MS, peristaltic pump, seven-way valve, etc., and commercially available products that meet the usage requirements can be used.

[0102] In summary, the technical solution of the present invention has the following advantages:

[0103] 1. Realize the automated application of the system and provide an integrated solution from sample pre-treatment to automated analysis;

[0104] 2. The two machines are fully automated and can be operated unattended, saving labor costs, truly freeing the hands of laboratory personnel, and saving 50% of analysis time;

[0105] 3. The operation is more convenient, one-key setting, two machines are interconnected, saving time and effort;

[0106] 4. Efficient sampling system makes the testing process more stable, efficient and reliable.

[0107] The technical solution of the present invention, on the basis of the existing fully automatic microwave digestion instrument and ICP-MS, sets up a set of automatic devices for coupling the fully automatic microwave digestion instrument and the ICP-MS, establishes a connecting / coupling pipeline, adopts a program to control the operation and action of components such as a mechanical arm, a peristaltic pump assembly, a seven-way valve assembly, and a 12-roller peristaltic pump, so that the two independent devices / instruments, the fully automatic microwave digestion instrument and the ICP-MS, can be uniformly linked and operated according to a required program, provides an integrated solution from sample pretreatment to automated analysis, completes the automated application of the entire pretreatment-analysis system, realizes the full process automation and fully automatic coupling of element analysis, truly liberates the hands of laboratory personnel, saves labor costs, builds a set of efficient sampling-analysis system, and makes the test process more efficient, stable and reliable.

[0108] The invention can be widely used in the field of material testing or analysis.

Claims

1. An automatic device for combining a fully automatic microwave digestion instrument and ICP-MS, comprising a fully automatic microwave digestion instrument and an ICP-MS, characterized in that: In the fully automatic microwave digestion instrument and ICP-MS, a set of coupling structures are respectively set; The structure of the combined part in the fully automatic microwave digestion instrument includes at least the following parts: A mechanical arm assembly, a sample rack assembly, a first tetrafluoro tube, a probe assembly, a peristaltic pump assembly, a second tetrafluoro tube, a tube connector, a coupling tube, a liquid collection tube, a reagent bottle, a waste liquid bottle, a waste discharge tube and a cleaning tube; The structure of the coupling part in ICP-MS includes at least the following parts: Nebulizer assembly, waste pipe, seven-way valve assembly, 12-roller peristaltic pump assembly, waste pipe, waste liquid bottle, injection tube, peristaltic tube and reagent bottle; A coupling tube is set up to connect the outlet ends of the probe assembly and the peristaltic pump assembly in the fully automatic microwave digestion instrument with the inlet end of the seven-way valve assembly pipeline in the ICP-MS; The coupling tube has one end constituting the output end of the coupling part of the fully automatic microwave digestion instrument, and the other end constituting the input end of the ICP-MS coupling part, and plays the role of a connecting / coupling pipeline between the coupling part of the fully automatic microwave digestion instrument and the fully automatic microwave digestion instrument; In the fully automatic microwave digestion instrument, after the fully automatic microwave digestion instrument digests the sample, the sample solution is sucked up by the peristaltic pump and transported to the inlet end of the ICP-MS seven-way valve assembly pipeline through the coupling tube; by controlling the switching of the seven-way valve assembly, the ICP-MS sequentially realizes the operations of sample injection, sample delivery, and cleaning, and detects and analyzes the sample solution, realizing automation and integration from sample pretreatment to analysis; The automatic connection between the fully automatic microwave digestion instrument and ICP-MS is realized, and the cyclic workflow of the fully automatic microwave digestion instrument and the operation process of the ICP-MS are interconnected, which can realize the full process automation of element analysis; During the ICP-MS sample injection process, the fully automatic microwave digestion instrument also performs automatic cleaning operations simultaneously to prepare for the next step of sample injection.

2. The automatic device for combining full-automatic microwave digestion instrument and ICP-MS according to claim 1, characterized in that The mechanical arm assembly is composed of a mechanical arm and a clamping claw. The clamping claw is fixed to the mechanical arm by screws, and the mechanical arm is fixed in the frame of the microwave digestion instrument. The mechanical arm assembly is used to clamp the sample dissolution cup or sample rack. The sample rack assembly is composed of a sample dissolving cup and a sample rack. The sample dissolving cup is a part for holding samples, and the blind holes of the sample rack and the sample dissolving cup are matched.

3. The automatic device for the combination of fully automatic microwave digestion instrument and ICP-MS according to claim 1, characterized in that The probe assembly includes a probe fixed to a probe seat, a slider, a guide rail, a synchronous belt, a motor, and a bracket; The motor is fixed at one end of the bracket, a lower synchronous wheel is arranged at the other end of the bracket, and the synchronous belt is sleeved between the motor at the upper end of the bracket and the lower synchronous wheel at the lower end of the bracket; a guide rail is arranged parallel to one side of the bracket; a slider is movably arranged on the guide rail; the probe seat is fixedly connected to the slider and the synchronous belt; The motor rotates, driving the synchronous belt to pull the probe seat and the probe to slide up and down along the guide rail, thereby realizing the up and down movement function of the probe.

4. The automatic device for the combination of fully automatic microwave digestion instrument and ICP-MS according to claim 1, characterized in that The peristaltic pump assembly comprises a first peristaltic pump, a second peristaltic pump, a peristaltic tube, a joint assembly, a joint fixing plate, a second polytetrafluoroethylene tube, and a coupling tube; The first peristaltic pump is connected to the peristaltic tube, the joint assembly is fixed on the joint fixing plate, the lower side of the joint on one side of the joint assembly is connected to the second tetrafluoro tube, and the upper side is connected to the peristaltic tube, and the upper side of the joint on the other side of the joint assembly is connected to the joint, and the lower side is connected to the coupling tube; The peristaltic pump driver provides power to drive the pump head to operate and achieve liquid suction / output; After the first peristaltic pump completes sample delivery, the robotic arm removes the sample tank, the probe assembly moves downward, the probe enters the cleaning tube, the second peristaltic pump starts working, and the liquid collection tube connected to the second peristaltic pump draws nitric acid from the reagent bottle. The nitric acid enters the cleaning tube through the peristaltic tube and the connecting tube to clean the probe, and the waste liquid is discharged into the waste liquid bottle through the waste discharge pipe connected to the cleaning tube.

5. The automatic device for the combination of fully automatic microwave digestion instrument and ICP-MS according to claim 1, characterized in that The atomizer assembly comprises an atomization chamber body and an atomization chamber, an atomization chamber connecting pipe is arranged above the atomization chamber body, an injection joint is arranged on the side, and a waste liquid joint is arranged at the bottom; The analytical solution sample was delivered to the ICP-MS through the coupling tube and the seven-port valve assembly; When the analytical solution sample enters the nebulizer chamber through the injection joint, nitrogen is introduced into the nebulizer chamber structure perpendicular to the sample. The solution sample at the outlet of the nebulizer capillary center tube is broken into droplets by the impact of the airflow and becomes a primary aerosol, forming the medium required for ICP-MS instrument analysis. The excess waste liquid will be connected to the waste liquid pipe from the waste liquid joint of the nebulizer body and discharged through the peristaltic pump.

6. The automatic device for combining full-automatic microwave digestion instrument and ICP-MS according to claim 1, characterized in that The seven-way valve assembly at least includes a motor and a valve body; the valve body includes a valve head and a valve core; The seven-way valve assembly has seven channels, 1#-7#. The motor drives the valve body to rotate, and the required channels are switched through the valve head and valve core. The solution sample enters the quantitative loop through one of the channels, and the solution exceeding the storage volume of the quantitative loop is discharged through the seven-way valve switching channel; The connection between the switching channels of the seven-way valve and the 12-roller peristaltic pump can realize the functions of ICP-MS injection, sample delivery and cleaning respectively.

7. The automatic device for combining full-automatic microwave digestion instrument and ICP-MS according to claim 1, characterized in that The 12-roller peristaltic pump assembly includes a driver motor, a movable roller, a fixed roller, an elastic delivery hose and a housing; The driver motor drives the moving roller to rotate, and the moving roller squeezes the peristaltic tube arranged between the moving roller and the fixed roller, so that negative pressure is formed in the peristaltic tube, and the liquid in the tube flows accordingly; The sample solution is pumped by alternately squeezing and releasing the elastic delivery hose arranged around the moving and fixed rollers.

8. The automatic device for combining full-automatic microwave digestion instrument and ICP-MS according to claim 1, characterized in that The automatic device for combining the fully automatic microwave digester and ICP-MS, by respectively setting a combination structure between the fully automatic microwave digester and the ICP-MS, and uniformly controlling through a program, enables the automatic cycle of the steps of sampling, suction and transportation, sample loading, injection, detection and analysis, and cleaning, thereby realizing the automatic combination between the fully automatic microwave digester and the ICP-MS, and realizing the interconnection between the cyclic workflow of the fully automatic microwave digester and the operation process of the ICP-MS, thereby realizing the automatic application of the system and being able to realize the full process automation of element analysis.

9. An automated operation method for the fully automatic microwave digestion instrument + ICP-MS combined automation device according to claim 1, characterized in that The following steps or procedures are involved: Step 1: After the fully automatic microwave digestion instrument digests the sample, the robotic arm clamps the sample cup to the probe assembly, the guide rail probe assembly moves down, and the sample is taken from the sample cup; the sample passes through the second PTFE tube to the peristaltic pump assembly, and the sample is sucked and transported through the peristaltic pump; Step 2: The sample solution is transmitted through the coupling tube to the seven-way valve assembly of the ICP-MS. At this time, the seven-way valve switches the channel and sends the sample solution to the quantitative loop for storage; Step 3: The seven-way valve cuts the quantitative loop into the flow path. At the same time, the 12-roller peristaltic pump of the ICP-MS draws the carrier fluid into the flow path and pushes the sample solution into the nebulizer assembly for detection and analysis. Step 4: Insert the injection needle of the fully automatic microwave digestion instrument into the cleaning tube, and absorb the cleaning liquid to clean the injection needle pipeline; Step 5: After the ICP-MS analysis is completed, the seven-way valve quantitative loop is kept in the flow path for 3 seconds and the quantitative loop is cleaned with carrier liquid. At this point, a cycle of fully automatic microwave digestion instrument + ICP-MS automation is completed; At the same time, the injection needle of the fully automatic microwave digestion instrument is inserted into the next standard or sample solution, so that the process cycle and ICP-MS can be interconnected.

10. The automated operation method of the fully automated microwave digestion instrument + ICP-MS coupled automated device according to claim 9, characterized in that The steps and process of combining the key components of the ICP-MS to work are as follows: 1) Sample loading stage: The liquid output from the fully automatic microwave digestion instrument coupling tube is pumped into the seven-way valve assembly and stored in the quantitative loop; during the sample loading process, the 12-roller peristaltic pump assembly pumps the carrier liquid into the nebulizer cleaning channel; In the loading phase, ICP-MS completes the process of loading, draining, cleaning, and draining; 2) Injection stage: The seven-way valve assembly switches the channel, the sample in the quantitative loop enters the peristaltic tube, and the 12-roller peristaltic pump assembly pumps the carrier liquid into the peristaltic tube, pushing the sample into the nebulizer to complete the analysis; 3) During the ICP-MS sampling process, the fully automatic microwave digester also performs automatic cleaning to prepare for the next step of sampling.

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