Chromatographic column liquid distribution device matched with high performance liquid chromatography analyzer

The chromatographic column liquid distribution device addresses the single-injector limitation of high-performance liquid chromatography analyzers by enabling simultaneous detection and automated cleaning of multiple columns, enhancing detection efficiency and convenience.

CN222280563UActive Publication Date: 2024-12-31SHANGHAI KEZE BIOCHEMICAL TECH CO LTD
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Patent Information

Application Number
CN202420162536.2
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2024-01-23
Publication Date
2024-12-31
Estimated Expiration
2034-01-23

AI Technical Summary

Technical Problem

Existing high-performance liquid chromatography analyzers are limited by a single injector structure, allowing only one chromatographic column to be detected at a time, necessitating manual cleaning and reducing detection efficiency when multiple columns with different analytes are involved.

Method used

A chromatographic column liquid distribution device with multiple cylinders, solenoid valves, and a control circuit allows simultaneous placement and detection of multiple chromatographic columns, facilitated by a power switch system for efficient liquid transfer and pipeline cleaning.

Benefits of technology

Enables simultaneous detection of multiple chromatographic columns with improved efficiency and convenience by allowing easy switching between columns and automated pipeline cleaning, with real-time liquid level monitoring for prompt refilling.

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Abstract

A chromatographic column liquid distribution device used in cooperation with a high performance liquid chromatography analyzer comprises a supporting plate, a liquid pump, an electromagnetic valve, an electromagnetic valve A, a liquid level switch, a barrel, a shell, a liquid storage tank and a control circuit. The liquid storage tank, the shell and the liquid pump are installed on the supporting plate, the liquid level switch is installed in the liquid storage tank, the electromagnetic valve and the electromagnetic valve A are connected with the liquid pump, the liquid storage tank and the barrel respectively, the barrel is installed in the shell, and the control circuit is installed in the element box. According to the utility model, a plurality of chromatographic columns with different objects to be detected can be put into the plurality of cylinders, and detection personnel can conveniently enable a plurality of chromatographic column liquids brought out by a high-pressure circulating phase output by a liquid pump to respectively enter a detector of a high performance liquid chromatography analyzer through simple switching of the power switch, so that the detection efficiency is improved. A plurality of chromatographic columns are detected one by one, and corresponding cylinders and pipelines can be conveniently cleaned; when the mobile phase liquid in the liquid box is reduced to a certain amount, detection personnel can be prompted to add the liquid in time.
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Description

Technical Field

[0001] The utility model relates to the technical field of auxiliary equipment for liquid chromatographic analyzers, in particular to a chromatographic column liquid distribution device used in conjunction with a high-performance liquid chromatographic analyzer. Background Art

[0002] High performance liquid chromatography analyzer is a device that uses gas chromatography theory to detect and analyze substances based on classical chromatography analyzer. Technically, high performance liquid chromatography analyzer has higher detection sensitivity than ordinary chromatography analyzer and can perform continuous detection of effluent. Specifically, when the high performance liquid chromatograph is working, its supporting liquid pump sucks the solvent (that is, the mobile phase) in the liquid storage tank and then outputs it into the injector. The object to be tested (the object to be tested, the filler and the liquid isopropanol are pre-pressed to form a chromatography column) is pre-installed in the injector of the high performance liquid chromatograph. The mobile phase (the substance that carries the components to be tested forward during the detection process of the chromatography column, such as liquid acetonitrile-water solution, acetonitrile-acetic acid aqueous solution, methanol-water solution, acetonitrile-phosphoric acid aqueous solution, etc.) is injected through the liquid inlet pipe at the upper end of the injector and passes through the chromatography column (chromatography column) located in the injector. After the object to be tested is separated by the chromatography column, it flows out through the liquid outlet pipe at the lower end of the injector into the detector of the high performance liquid chromatograph. The signal detected by the detector is collected and processed by the data processing equipment supporting the high performance liquid chromatograph, and the chromatogram of the object to be tested is recorded, thereby obtaining the composition of the object to be tested.

[0003] The existing high performance liquid chromatograph generally has only one injector, which includes a cylindrical barrel (with a cross-shaped support frame at the lower end so that after the chromatographic column is placed in the barrel, the lower end of the chromatographic column does not contact the lower end of the barrel, which is convenient for the mobile phase liquid to flow in and out), a movable cover, and the upper part of the two sides of the barrel has a liquid inlet pipe and a liquid outlet pipe respectively. In application, the chromatographic column is placed in the barrel and then the sealing cover is covered to control the high-pressure liquid pump to pump the mobile phase liquid into the barrel. After the high performance liquid chromatograph detects the sample, the movable cover is opened to take out the sample column after the detection. Although the above method meets the detection needs, it is limited by the structure. Since there is only one injector, only one chromatographic column with different analytes can be detected at a time, and after each sample chromatographic column is detected, the detection personnel need to clean the barrel and the corresponding pipeline, so it will bring great inconvenience to the detection personnel, and when the number of chromatographic columns containing different analytes detected is relatively large, it will also lead to low detection efficiency. In summary, it is particularly necessary to provide a device that can bring convenience to the detection personnel and can relatively improve the detection efficiency. Utility Model Content

[0004] In order to overcome the drawbacks of the sample injector used in conjunction with the existing high performance liquid chromatograph analyzer due to structural limitations as described in the background, the utility model provides a chromatographic column liquid distribution device used in conjunction with the high performance liquid chromatograph analyzer, which can be used to place multiple chromatographic columns with different analytes at one time under the joint action of a related mechanism, and the detection personnel can easily make the liquid brought out of the multiple chromatographic columns by the mobile phase enter the detector of the high performance liquid chromatograph analyzer by simply switching the power switch, and can conveniently clean the corresponding cylinder and pipeline, thereby bringing convenience to the detection personnel and correspondingly improving the detection efficiency.

[0005] The technical solution adopted by the utility model to solve its technical problems is:

[0006] A chromatographic column liquid distribution device for use with a high-performance liquid chromatograph analyzer, comprising a support plate, a liquid pump, a solenoid valve, a solenoid valve A, a liquid level switch, a barrel, a shell, and a liquid storage tank, characterized in that it also has a control circuit; the liquid storage tank is installed on one side of the support plate, and a cover is installed on the upper end of the liquid storage tank; the liquid level switch is installed in the liquid storage tank, the liquid pump is installed on the side end of the liquid storage tank, there are multiple solenoid valves and multiple solenoid valves A respectively, one end of the first solenoid valve A is connected to the liquid outlet end of the liquid storage tank, the other end of the first solenoid valve A and one end of the second solenoid valve A are connected in parallel to the liquid inlet end of the liquid pump, and the other end of the second solenoid valve A is connected to a tap water pipe; there are multiple barrels, the shell is installed Installed on the side end of the liquid pump, multiple cylinders are installed in the shell at intervals; the side ends of the multiple liquid outlet pipes of the multiple cylinders are respectively connected to one end of multiple solenoid valves, the other ends of the multiple solenoid valves are connected in parallel to one end of the third solenoid valve A and the fourth solenoid valve A, and the other ends of the third solenoid valve A and the fourth solenoid valve A are respectively connected to the sewage pipe and the liquid inlet end of the detector of the high-performance liquid chromatography analyzer; the side ends of the multiple liquid inlet pipes of the multiple cylinders are respectively connected to one end of the other multiple solenoid valves, and the other ends of the other multiple solenoid valves are connected in parallel to the liquid outlet end of the liquid pump; the control circuit is installed in the component box, and the signal output end of the liquid level switch is electrically connected to the signal input end of the control circuit.

[0007] Furthermore, the solenoid valve and solenoid valve A are normally closed valve core solenoid valves.

[0008] Furthermore, the liquid storage tank is filled with mobile phase liquid.

[0009] Furthermore, the shell is equipped with a sealing plate, the upper end of the shell and the upper end of the cylinder are in the same plane, the front and rear ends of the shell are provided with wire seats, the lower end of the sealing plate is provided with a sealing plate, the sealing plate is sealed and installed on the shell, and the lower end of the sealing plate and the shell and the upper end of the cylinder are in a sealing structure.

[0010] Furthermore, the control circuit includes an electrically connected resistor, a transistor, and a buzzer, one end of the resistor is connected to the base of the transistor, and the collector of the transistor is connected to the negative power input end of the buzzer.

[0011] Furthermore, the liquid level switch includes a fixed rod, a reed switch and a float, the float is movably sleeved on one side of the fixed rod, a magnet is installed on the outside of the float, and the reed switch is installed on the other side of the fixed rod.

[0012] Compared with the prior art, the present invention has the following beneficial effects: (1) the present invention has a plurality of cylinders, so before testing, a plurality of chromatographic columns with different objects to be tested can be placed in the plurality of cylinders for testing. By simply switching the power switch, the testing personnel can conveniently allow the various chromatographic column liquids brought out by the high-pressure flow phase output by the liquid pump to enter the detector of the high-performance liquid chromatography analyzer respectively, and test the plurality of chromatographic columns one by one, and can conveniently clean the corresponding cylinders and pipelines; (2) when the mobile phase liquid in the liquid box is reduced to a certain amount, the testing personnel can be promptly prompted to add it in time, which brings convenience to the testing personnel and correspondingly improves the testing efficiency. BRIEF DESCRIPTION OF THE DRAWINGS

[0013] The present invention will be further described below with reference to the accompanying drawings and embodiments.

[0014] Figure 1 It is a schematic diagram of the overall structure and the partially enlarged structure of the utility model.

[0015] Figure 2 This is a circuit diagram of the utility model. DETAILED DESCRIPTION

[0016] Figure 1 , 2As shown, a chromatographic column liquid distribution device for use with a high-performance liquid chromatographic analyzer includes a support plate 1, a liquid pump M (220V, 400W), a power supply mechanism T1, a solenoid valve, a liquid level switch, a cylinder 3, a shell 4, a liquid storage tank 5, a power switch, and a control circuit 6; the lower end of the liquid storage tank 5 is installed on the right end of the support plate 1, and a movable cover 51 (open the movable cover to add liquid) is threadedly installed on the upper end of the liquid storage tank 5, and a one-way air valve 52 is installed on the upper end of the movable cover 51, and the air inlet pipe of the one-way air valve 52 (allowing external air to enter the liquid storage tank 5 to prevent negative pressure from being generated in the liquid storage tank) is interconnected with the upper end of the movable cover 51; the liquid level switch is installed on the lower left end of the liquid storage tank 5, the liquid pump M is installed on the support plate 1 located at the left end of the liquid storage tank 5, there are twenty solenoid valves, one end of the first solenoid valve DC1 is threadedly connected to the liquid outlet pipe outside the lower left end of the liquid storage tank 5 (interconnected with the liquid storage tank), and the first solenoid valve DC1 is threadedly connected to the liquid outlet pipe outside the lower left end of the liquid storage tank 5 (interconnected with the liquid storage tank). The other end of the valve DC1, one end of the second solenoid valve DC2 and a three-way pipe, both ends of which are connected via pipe joints respectively, the other end of the second solenoid valve DC2 is connected to the tap water pipe via a pipe, and the third end of the three-way pipe is connected to the liquid inlet end of the liquid pump M via a threaded connection; there are eight cylinders 3 (the lower end of which has a M-shaped support frame 31 so that after the chromatographic column is placed in the cylinder 3, the lower end of the chromatographic column does not contact the lower end of the cylinder 3, which is convenient for the mobile phase liquid to flow in and out), and the lower end of the shell 4 (an open-top and closed-bottom structure) is welded to the support plate 1 located at the left end of the liquid pump M. The upper end of the cylinder 3 is an open structure and the lower end is a closed structure. The lower ends of the eight cylinders 3 are distributed at a front-to-back distance and are longitudinally welded to the lower end of the shell 4. The liquid inlet pipe 32 on the right end of the eight cylinders 3 and the liquid outlet pipe 33 under the left end are respectively located on the outside of the upper right end and the lower part of the lower left end of the shell 4; the left side of the eight liquid outlet pipes at the lower left side of the cylinder 3 and the other eight solenoid valves DC1 N are connected by threads respectively, and the other ends of the other eight solenoid valves DC1 N and the outer sides of the eight openings on the right side of a connecting pipe A34 are connected together by pipe joints (the other ends of the other eight solenoid valves DC1 N are interconnected with the inside of the connecting pipe A34), the connecting pipe welded on the left side of the connecting pipe A34 and the first end of the second three-way pipe are connected by threads, the second end and the third end of the second three-way pipe are connected with one end of the third solenoid valve DC3 and the fourth solenoid valve DC4 respectively by pipe joints, and the other ends of the third solenoid valve DC3 and the fourth solenoid valve DC4 are connected with the sewage pipe on the upper part of the wastewater tank in the detection area and the liquid inlet end of the detector of the high performance liquid chromatography analyzer respectively by flanges; the right sides of the liquid inlet pipes on the right sides of the eight cylinder bodies 3 are connected with one end of the remaining eight solenoid valves DCN respectively by threads, and the other ends of the remaining eight solenoid valves DCN and the outer sides of the eight openings on the left side of a connecting pipe 35 are connected together by branch pipes respectively (the branch pipes are interconnected with the inside of the connecting pipe), and the connecting pipe welded on the right side of the connecting pipe 35 and the liquid outlet end of the liquid pump M are connected by threads;The power supply mechanism T1, the power switch and the control circuit 6 are installed in the component box 7, and the component box 7 is installed at the front outer end of the liquid storage tank 5.

[0017] Figure 1 , 2 As shown, the solenoid valve is a normally closed valve core solenoid valve (2W). The liquid storage tank 5 is filled with mobile phase liquid. The shell is equipped with a sealing plate 8. The upper end of the shell 4 and the upper end of the barrel 3 are in the same plane. A wire seat 9 is welded to the upper part of the front and rear ends of the shell 4 respectively. There is an opening in the middle of the front and rear ends of the sealing plate 8 respectively. A sealing rubber plate 81 is glued to the lower end of the sealing plate. Two manual screws 10 vertically pass through the front and rear end openings of the sealing plate and are respectively screwed into the two wire holes of the wire seat 9 at the upper end of the shell, and the sealing plate 8 is sealed and installed on the shell 4. The lower end of the sealing plate 8 and the upper end of the shell 4 and the barrel 3 are in a sealed structure. The control circuit includes a resistor R1, a transistor Q1, and a buzzer B connected by circuit board wiring. One end of the resistor R1 is connected to the base of the transistor Q1, and the collector of the transistor Q1 is connected to the negative power input end of the buzzer B1. The liquid level switch includes a "U"-shaped fixed rod 21, a reed switch GH and an annular rubber float 22. The hollow part of the float 22 is movably sleeved on the right outer end of the fixed rod 21. A limit plate 23 with an outer diameter larger than the outer diameter of the float is welded on the right end of the fixed rod 21. An annular hollow permanent magnet sheet 24 is glued to the outside of the float 22. A shell is installed at the lower end of the left right part of the fixed rod 21. The reed switch GH (normally open contact reed switch) is vertically distributed and glued to the right part of the shell, and the moving contact of the reed switch is vertically located at the left end. The left side of the fixed rod is welded to the lower left end in the liquid storage tank (the reed switch GH and the magnet are 2 mm apart when they are in the same plane). The power input end of the liquid pump M is connected in series through a power switch ASK, and the power input ends 1 and 2 of the power mechanism T1 are connected to the two poles of the AC 220V power supply through wires respectively. The power output end of the power mechanism T1 and twenty power switches, the power input end of the control circuit, the positive power input end of the buzzer B and the emitter of the transistor Q1 are connected through wires respectively. The power output ends of the twenty power switches S1, S2, S3, S4, SN (representing eight), S1 N (representing eight) and the 4th foot of the power mechanism T1 and the power input ends of twenty solenoid valves DC1, DC2, DC3, DC4, DCN (representing eight), DC1 N (representing eight) are connected through wires respectively. The two ends of the reed switch GH at the signal output end of the liquid level switch and the positive power input end of the buzzer B at the signal input end of the control circuit and the emitter of the transistor Q1 are connected through wires respectively.

[0018] Figure 1 , 2As shown, before the new detection, the sealing plate 8 is opened, and then eight or less chromatographic columns are placed in the eight barrels 3. Then, the sealing plate 8 is covered on the outer shell 4, and then the manual screw 10 is tightened. The 220V AC power supply enters the power input end of the power supply mechanism T1, and the 3rd and 4th feet of the power supply mechanism T1 output a stable DC 12V power supply to enter the power input end of the twenty power switches and the control circuit. After the inspector turns on the power switch SK of the liquid pump M, the liquid pump M is powered on to work and the mobile phase liquid in the liquid tank (liquid storage tank 5) is drawn out through the solenoid valve DC1 with the valve core opened, pressurized and pumped out from the liquid outlet pipe (the power switch of the solenoid valve DC1 is turned on, and the valve core of the solenoid valve DC1 is powered on and opened). When the testing personnel turn on the power switch SN of one of the solenoid valves DCN and the power switch S1 N of one of the solenoid valves DC1 N, the valve cores of one of the solenoid valves DCN and one of the solenoid valves DC1 N are electrified and opened, and the mobile phase (the substance that carries the component to be tested forward during the chromatographic column detection process, such as liquid acetonitrile-water solution, acetonitrile-acetic acid aqueous solution, methanol-water solution, acetonitrile-phosphoric acid aqueous solution, etc.) is injected into the chromatographic column (chromatographic column) located in the cylinder through the upper liquid inlet pipe of one of the cylinders 3, and the test object is separated by the chromatographic column and then flows out through the lower liquid outlet pipe of the cylinder, and then enters the detector of the high performance liquid chromatograph through the solenoid valve DC4 with the valve core opened (turn on the power switch of the solenoid valve DC4, and the valve core of the solenoid valve DC4 is electrified and opened), and the signal detected by the detector is collected and processed by the data processing equipment supporting the high performance liquid chromatograph, and the chromatogram of the tested substance is recorded, so as to obtain the composition of the tested substance. Specifically, in actual testing, the staff turns on the eight power switches DCN and DC1 N one by one, so that the mobile phase pumped out by the liquid pump M can enter eight cylinders (actually more cylinders can be set up), and the chromatographic columns in the eight cylinders are tested by high performance liquid chromatography analyzer.

[0019] Figure 1 , 2As shown, after actually testing each chromatographic column in a cylinder 3, in order to ensure that the residue in the cylinder will not affect the detection of another chromatographic column with a different detection object during the next detection, and after the chromatographic column in the corresponding cylinder is tested, when it is necessary to discharge the residual liquid in the pipeline connected to the corresponding solenoid valve DC1N and the solenoid valve DC3, the tester turns on the power switch of the solenoid valve DC2, and its energized valve core opens, turns off the power switch of the solenoid valve DC1, and its de-energized valve core closes, turns on the power switch of the solenoid valve DC3, and its valve core opens, turns off the power switch of the solenoid valve DC4, and its de-energized valve core closes. In this way, tap water is drawn into the pressure pump through the liquid pump M (with its power switch A turned on) and then goes out through the corresponding solenoid valve DCN into the corresponding cylinder, and is discharged through the sewage pipe through the corresponding solenoid valve DC1N after flushing the cylinder. During the process of water flowing in and out, the corresponding cylinder and the pipeline will be effectively cleaned. After cleaning, the inspector first turns off the power switch of the electromagnetic valve DC2, then turns off the power switch of the liquid pump M, and finally turns off the power switch of the electromagnetic valve DC3. Then, consistent with all the above processes, the next column detection process can be entered until all the columns in the cylinder are detected. When the amount of liquid in the liquid tank 5 is large, the float 22 is higher than the height of the reed switch GH as the liquid level is high, and the internal contact of the reed switch GH will not close. In this way, the transistor Q1 will not be turned on, and the buzzer B will not be powered on to sound, indicating that the amount of liquid is large and does not need to be added. When the amount of liquid in the liquid tank is small, the float moves along with the liquid level, and the height is level with the height of the reed switch GH. The magnetism of the magnet 24 causes the internal contacts of the reed switch GH to close. In this way, the 12V power supply will enter the base of the transistor Q1 through the resistor R1 current limiting and voltage reduction. The transistor Q1 conducts and the collector outputs a low level and enters the negative power input terminal of the buzzer B. The buzzer B is powered and sounds to promptly remind the inspector to add mobile phase liquid, thus ensuring the need for liquid in the detection process. Through the above, the new inspector can conveniently allow the liquids of multiple chromatographic columns brought out by the high-pressure flow phase output by the liquid pump to enter the detector of the high-performance liquid chromatograph analyzer one by one through a simple power switch conversion, detect multiple chromatographic columns, and conveniently clean the corresponding cylinders and pipelines; when the mobile phase liquid in the liquid tank is reduced to a certain amount, it can promptly remind the inspector to add, which brings convenience to the inspector and correspondingly improves the detection efficiency. Figure 2 In the figure, the resistance of resistor R1 is 1K; the model of transistor Q is 9013 (NPN type); the buzzer B is an active continuous sound buzzer alarm of model MF12V; the power supply unit T1 is an AC 220V to DC 12V switching power supply module.

[0020] It is obvious to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above, and that the present invention can be implemented in other specific forms without departing from the spirit or essential features of the present invention. Therefore, the embodiments should be regarded as exemplary and non-restrictive from any point of view, and the scope of the present invention is defined by the appended claims rather than the above description, and it is intended that all changes falling within the meaning and scope of the equivalent elements of the claims be included in the present invention. Any reference numeral in a claim should not be regarded as limiting the claim to which it relates.

Claims

1. A chromatographic column liquid distribution device for use with a high performance liquid chromatograph analyzer, comprising a support plate, a liquid pump, a solenoid valve, a solenoid valve A, a liquid level switch, a cylinder, a housing, and a liquid storage tank, characterized in that: It also has a control circuit; the liquid storage tank is installed on one side of the support plate, and a cover is installed on the upper end of the liquid storage tank; the liquid level switch is installed in the liquid storage tank, the liquid pump is installed on the side end of the liquid storage tank, and there are multiple solenoid valves and solenoid valves A respectively, one end of the first solenoid valve A is connected to the liquid outlet end of the liquid storage tank, the other end of the first solenoid valve A and one end of the second solenoid valve A are connected in parallel to the liquid inlet end of the liquid pump, and the other end of the second solenoid valve A is connected to the tap water pipe; there are multiple cylinders, the outer shell is installed on the side end of the liquid pump, and the multiple cylinders are installed in the outer shell at intervals; the multiple outlets of the multiple cylinders The side end of the liquid pipe is respectively connected to one end of multiple solenoid valves, and the other end of the multiple solenoid valves is connected in parallel to one end of the third solenoid valve A and the fourth solenoid valve A, and the other end of the third solenoid valve A and the fourth solenoid valve A is respectively connected to the sewage pipe and the liquid inlet end of the detector of the high performance liquid chromatography analyzer; the side ends of the multiple liquid inlet pipes of the multiple cylinders are respectively connected to one end of the other multiple solenoid valves, and the other end of the other multiple solenoid valves is connected in parallel to the liquid outlet end of the liquid pump; the control circuit is installed in the component box, and the signal output end of the liquid level switch is electrically connected to the signal input end of the control circuit.

2. The chromatographic column liquid dispensing device for use with a high performance liquid chromatograph according to claim 1, characterized in that: Solenoid valve, solenoid valve A is a normally closed valve core solenoid valve.

3. The chromatographic column liquid dispensing device for use with a high performance liquid chromatograph according to claim 1, characterized in that: The liquid reservoir contains mobile phase liquid.

4. The chromatographic column liquid dispensing device for use with a high performance liquid chromatograph according to claim 1, characterized in that: The shell is equipped with a sealing plate. The upper end of the shell and the upper end of the cylinder are in the same plane. The front and rear ends of the shell are provided with wire seats. The lower end of the sealing plate is provided with a sealing plate. The sealing plate is sealed and installed on the shell. The lower end of the sealing plate and the shell and the upper end of the cylinder are in a sealing structure.

5. The chromatographic column liquid dispensing device for use with a high performance liquid chromatograph according to claim 1, characterized in that: The control circuit comprises an electrically connected resistor, a triode and a buzzer, one end of the resistor is connected to the base of the triode, and the collector of the triode is connected to the negative power input end of the buzzer.

6. The chromatographic column liquid distribution device for use with a high performance liquid chromatograph according to claim 1, characterized in that: The liquid level switch comprises a fixed rod, a reed switch and a float. The float is movably sleeved on one end of the fixed rod, a magnet is installed on the outside of the float, and the reed switch is installed on the other end of the fixed rod.