CN212693799U - Flow injection analysis system with range switching device - Google Patents
Flow injection analysis system with range switching device Download PDFInfo
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- CN212693799U CN212693799U CN202021247873.XU CN202021247873U CN212693799U CN 212693799 U CN212693799 U CN 212693799U CN 202021247873 U CN202021247873 U CN 202021247873U CN 212693799 U CN212693799 U CN 212693799U
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Abstract
The utility model discloses a flow injection analysis system with range auto-induction portion, solution conveying part, the chemical reaction flow path, range auto-induction portion and detector, the auto-induction portion is used for the automatic sample that absorbs, solution conveying part is used for being used for carrying sample, current-carrying, reagent A, reagent B respectively to the chemical reaction flow path, the chemical reaction flow path is used for mixing sample, current-carrying, reagent A, reagent B respectively and obtains mixed solution and with mixed solution input detector, the detector is used for detecting absorbance. The flow injection analysis system with the range switching device of the utility model can continuously and automatically test samples, and can be switched to a single sampling ring by adjusting the four-way switching valve under a high range mode, thereby reducing the sensitivity of the flow injection analysis system and realizing the range of a higher concentration range; and in the low-range mode, the four-way switching valve is adjusted to be switched to a double sampling ring, so that the sensitivity of the flow injection analysis system is improved, and the low-concentration range is realized.
Description
Technical Field
The utility model relates to an analytical chemistry field especially relates to a flow injection analytic system with range auto-change over device.
Background
The Flow Injection Analysis technique has been proposed since 1975 (Ruzicka J, Hansen E H, Flow Injection Analysis, Wiley, New York,1981) and has been widely used in chemical Analysis with the advantages of simplicity, convenience, easy automation, and on-line pretreatment of samples.
The common flow injection analysis system has single function and fixed measuring range and can not meet the detection requirement.
SUMMERY OF THE UTILITY MODEL
The to-be-solved technical problem of the utility model is to provide a flow injection analytic system with range auto-change over device.
The utility model discloses a flow injection analysis system with range auto-feed, including autoinjection portion, solution conveying part, chemical reaction flow path, range auto-feed and detector, autoinjection portion is used for the automatic sample that absorbs, and solution conveying part is used for carrying sample, current-carrying, reagent A, reagent B to the chemical reaction flow path respectively, the chemical reaction flow path is used for mixing sample, current-carrying, reagent A, reagent B in order respectively and obtains mixed solution and will mixed solution input detector, the detector is used for detecting mixed solution's absorbance;
the solution conveying part comprises a multi-channel peristaltic pump, and a sample peristaltic pump tube, a current-carrying peristaltic pump tube, a reagent A peristaltic pump tube and a reagent B peristaltic pump tube which are matched with the multi-channel peristaltic pump;
the chemical reaction flow path comprises a winding reaction tube, a first tee joint, a second tee joint, a first sampling ring, a flow carrying bottle, a reagent A bottle, a reagent B bottle, a waste liquid barrel, a flow cell, a first waste discharge tube, a second waste discharge tube and an electric multi-position valve;
the range switching device comprises a four-way switching valve and a second sampling ring;
the electric multi-position valve comprises a valve shell and a valve core, wherein the valve shell is provided with an interface A, an interface B, an interface C, an interface D, an interface E and an interface F, a first channel, a second channel and a third channel are rotatably arranged in the valve core,
the first channel is used for enabling the interface A to be communicated with the interface B or enabling the interface B to be communicated with the interface C, the second channel is used for enabling the interface C to be communicated with the interface D or enabling the interface D to be communicated with the interface E, and the third channel is used for enabling the interface E to be communicated with the interface F or enabling the interface F to be communicated with the interface A;
one end of the sample peristaltic pump tube is connected with an F interface of the electric multi-position valve through a capillary connecting tube, and the other end of the sample peristaltic pump tube is connected with the automatic sample injection part through the capillary connecting tube;
one end of the current-carrying peristaltic pump tube is communicated with the current-carrying bottle through a capillary connecting tube, and the other end of the current-carrying peristaltic pump tube is communicated with a D interface of the electric multi-position valve through a capillary connecting tube;
one end of the reagent A peristaltic pump tube is communicated with the reagent A bottle through a capillary connecting tube, and the other end of the reagent A peristaltic pump tube is connected with a b port of the first tee joint through the capillary connecting tube;
one end of the reagent B peristaltic pump tube is communicated with the reagent B bottle through a capillary connecting tube, and the other end of the reagent B peristaltic pump tube is connected with a port B of the second tee joint through the capillary connecting tube;
the interface A of the four-way switching valve is connected with the interface B of the electric multi-position valve through a capillary connecting pipe;
the B interface of the four-way switching valve is connected with one end of the second sampling ring;
the C interface of the four-way switching valve is connected with the other end of the second sampling ring;
the D interface of the four-way switching valve is connected with one end of the first sampling ring;
one end of the first sampling ring is in liquid communication with an E interface of the electric multi-position valve, and the other end of the first sampling ring is in liquid communication with a D interface of the four-way switching valve;
one end of the second sampling ring is in liquid communication with a port B of the four-way switching valve, and the other end of the second sampling ring is in liquid communication with a port C of the four-way switching valve;
the interface A of the electric multi-position valve is connected with the waste liquid barrel through a capillary connecting pipe and is used for discharging waste liquid;
the interface C of the electric multi-position valve is connected with the interface a of the first tee joint through a capillary connecting pipe;
the D interface of the electric multi-position valve is communicated with the liquid of the current-carrying peristaltic pump pipe through a capillary connecting pipe;
the F interface of the electric multi-position valve is in liquid communication with the sample peristaltic pump pipe through a capillary connecting pipe;
the port c of the first tee is connected with the port a of the second tee through a capillary connecting pipe;
the interface c of the second tee joint is connected with one end of the winding reaction tube through a capillary connecting tube;
the other end of the winding reaction tube is connected with an a interface of the flow cell;
the interface b of the flow cell is connected to a waste liquid barrel through a capillary connecting pipe for discharging waste liquid;
the flow cell is placed within a detector.
The utility model discloses a flow injection analytic system with range auto-change over device, wherein, still include the data processing workstation, the data processing workstation with the detector is connected, and is right the absorbance that the detector detected is handled.
The utility model discloses a flow injection analytic system with range auto-change over device, wherein, the length of winding reaction tube is 1-10m, and the internal diameter is 0.3-1.5 mm.
The utility model discloses a flow injection analytic system with range auto-change over device, wherein, the length of capillary connecting pipe is 0.1-10m, and the internal diameter is 0.3-1.0 mm.
The utility model discloses a flow injection analytic system with range auto-change over device, wherein, the internal diameter of sample peristaltic pump pipe, current-carrying peristaltic pump pipe, reagent A peristaltic pump pipe, reagent B peristaltic pump pipe is 0.38-1.52mm, multichannel peristaltic pump speed is 20-40 rpm/min.
The utility model discloses a flow injection analytic system with range auto-change over device, wherein, the length of first row of waste pipe, second row of waste pipe is 1-5m, and the internal diameter is 0.3-1.0 mm.
The utility model discloses a flow injection analysis system with range auto-change over device, wherein, autoinjection portion includes the sample dish of bearing test tube and is used for driving the first motor that the sample dish rotated, the output shaft of first motor is connected with the rotation axis of sample dish, be provided with a plurality of round holes that are used for placing the test tube on the sample dish, the test tube that holds sample and standard solution respectively inserts respectively in the round hole, autoinjection portion still includes the sampling needle that can insert in the test tube and with be used for driving the second motor that the sampling needle reciprocated, the output of second motor with the sampling needle is connected, the second motor with the sampling needle is installed on the sampling arm, the sampling arm is connected with the output shaft of third motor, the third motor is used for driving the sampling arm is in the sample dish top is rotatory swing, so that the sampling needle can get into in the test tube of selecting, the outer end of the sampling needle is connected with the sample peristaltic pump pipe through a pipeline.
The flow injection analysis system with the range switching device of the utility model can continuously and automatically test samples, and can be switched to a single sampling ring by adjusting the four-way switching valve under a high range mode, thereby reducing the sensitivity of the flow injection analysis system and realizing the range of a higher concentration range; and in the low-range mode, the four-way switching valve is adjusted to be switched to a double sampling ring, so that the sensitivity of the flow injection analysis system is improved, and the low-concentration range is realized. The utility model discloses a flow injection analytic system with range auto-change over device can change the sample volume, realizes the range of two different concentrations on same set of flow injection analytic system, adapts to the detection demand under the different conditions.
Drawings
Fig. 1 is a schematic structural diagram of a flow injection analysis system with a range switching device according to the present invention.
Detailed Description
As shown in fig. 1, the utility model discloses a flow injection analysis system with range auto-sampler, solution conveying portion, chemical reaction flow path, range auto-sampler and detector, auto-sampler is used for automatic absorption sample, and solution conveying portion is used for carrying sample, current-carrying, reagent A, reagent B respectively to the chemical reaction flow path, the chemical reaction flow path is used for mixing sample, current-carrying, reagent A, reagent B respectively according to the order and obtains mixed solution and with mixed solution input detector, the detector is used for detecting the absorbance of mixed solution;
the solution conveying part comprises a multi-channel peristaltic pump, and a sample peristaltic pump tube, a current-carrying peristaltic pump tube, a reagent A peristaltic pump tube and a reagent B peristaltic pump tube which are matched with the multi-channel peristaltic pump;
the chemical reaction flow path comprises a winding reaction tube, a first tee joint, a second tee joint, a first sampling ring, a flow carrying bottle, a reagent A bottle, a reagent B bottle, a waste liquid barrel, a flow cell, a first waste discharge tube, a second waste discharge tube and an electric multi-position valve;
the range switching device comprises a four-way switching valve and a second sampling ring;
the electric multi-position valve comprises a valve shell and a valve core, wherein the valve shell is provided with an interface A, an interface B, an interface C, an interface D, an interface E and an interface F, a first channel, a second channel and a third channel are rotatably arranged in the valve core,
the first channel is used for enabling the interface A to be communicated with the interface B or enabling the interface B to be communicated with the interface C, the second channel is used for enabling the interface C to be communicated with the interface D or enabling the interface D to be communicated with the interface E, and the third channel is used for enabling the interface E to be communicated with the interface F or enabling the interface F to be communicated with the interface A;
one end of the sample peristaltic pump tube is connected with an F interface of the electric multi-position valve through a capillary connecting tube, and the other end of the sample peristaltic pump tube is connected with the automatic sample injection part through the capillary connecting tube;
one end of the current-carrying peristaltic pump tube is communicated with the current-carrying bottle through a capillary connecting tube, and the other end of the current-carrying peristaltic pump tube is communicated with a D interface of the electric multi-position valve through a capillary connecting tube;
one end of the reagent A peristaltic pump tube is communicated with the reagent A bottle through a capillary connecting tube, and the other end of the reagent A peristaltic pump tube is connected with a b port of the first tee joint through the capillary connecting tube;
one end of the reagent B peristaltic pump tube is communicated with the reagent B bottle through a capillary connecting tube, and the other end of the reagent B peristaltic pump tube is connected with a port B of the second tee joint through the capillary connecting tube;
the interface A of the four-way switching valve is connected with the interface B of the electric multi-position valve through a capillary connecting pipe;
the B interface of the four-way switching valve is connected with one end of the second sampling ring;
the C interface of the four-way switching valve is connected with the other end of the second sampling ring;
the D interface of the four-way switching valve is connected with one end of the first sampling ring;
one end of the first sampling ring is in liquid communication with an E interface of the electric multi-position valve, and the other end of the first sampling ring is in liquid communication with a D interface of the four-way switching valve;
one end of the second sampling ring is in liquid communication with a port B of the four-way switching valve, and the other end of the second sampling ring is in liquid communication with a port C of the four-way switching valve;
the interface A of the electric multi-position valve is connected with the waste liquid barrel through a capillary connecting pipe and is used for discharging waste liquid;
the interface C of the electric multi-position valve is connected with the interface a of the first tee joint through a capillary connecting pipe;
the D interface of the electric multi-position valve is communicated with the liquid of the current-carrying peristaltic pump pipe through a capillary connecting pipe;
the F interface of the electric multi-position valve is in liquid communication with the sample peristaltic pump pipe through a capillary connecting pipe;
the port c of the first tee is connected with the port a of the second tee through a capillary connecting pipe;
the interface c of the second tee joint is connected with one end of the winding reaction tube through a capillary connecting tube;
the other end of the winding reaction tube is connected with an a interface of the flow cell;
the interface b of the flow cell is connected to a waste liquid barrel through a capillary connecting pipe for discharging waste liquid;
the flow cell is placed in a detector for measuring absorbance.
The utility model discloses a flow injection analytic system with range auto-change over device, wherein, still include the data processing workstation, the data processing workstation with the detector is connected, and is right the absorbance that the detector detected is handled.
The utility model discloses a flow injection analytic system with range auto-change over device, wherein, the length of winding reaction tube is 1-10m, and the internal diameter is 0.3-1.5 mm.
The utility model discloses a flow injection analytic system with range auto-change over device, wherein, the length of capillary connecting pipe is 0.1-10m, and the internal diameter is 0.3-1.0 mm.
The utility model discloses a flow injection analytic system with range auto-change over device, wherein, the internal diameter of sample peristaltic pump pipe, current-carrying peristaltic pump pipe, reagent A peristaltic pump pipe, reagent B peristaltic pump pipe is 0.38-1.52mm, multichannel peristaltic pump speed is 20-40 rpm/min.
The utility model discloses a flow injection analytic system with range auto-change over device, wherein, the length of first row of waste pipe, second row of waste pipe is 1-5m, and the internal diameter is 0.3-1.0 mm.
The utility model discloses a flow injection analysis system with range auto-change over device, wherein, autoinjection portion includes the sample dish of bearing test tube and is used for driving the first motor that the sample dish rotated, the output shaft of first motor is connected with the rotation axis of sample dish, be provided with a plurality of round holes that are used for placing the test tube on the sample dish, the test tube that holds sample and standard solution respectively inserts respectively in the round hole, autoinjection portion still includes the sampling needle that can insert in the test tube and with be used for driving the second motor that the sampling needle reciprocated, the output of second motor with the sampling needle is connected, the second motor with the sampling needle is installed on the sampling arm, the sampling arm is connected with the output shaft of third motor, the third motor is used for driving the sampling arm is in the sample dish top is rotatory swing, so that the sampling needle can get into in the test tube of selecting, the outer end of the sampling needle is connected with the sample peristaltic pump pipe through a pipeline.
The electric multi-position valve has at least six interfaces and has two states; the first state is a sample loading state, and the second state is a sample injection state; the four-way switching valve has four interfaces and has two states: the first state is a single sampling ring state; the second state is a double sampling loop state.
The flow injection analysis system with the range switching device of the utility model can continuously and automatically test samples, and can be switched to a single sampling ring by adjusting the four-way switching valve under a high range mode, thereby reducing the sensitivity of the flow injection analysis system and realizing the range of a higher concentration range; and in the low-range mode, the four-way switching valve is adjusted to be switched to a double sampling ring, so that the sensitivity of the flow injection analysis system is improved, and the low-concentration range is realized.
When the sampling loop is switched to the single sampling loop state, the interface A of the four-way switching valve is communicated with the interface D, the interface B of the four-way switching valve is communicated with the interface C, a sample flows into the interface A from the interface E of the electric multi-position valve and is filled in the first sampling loop, then the sample flows into the interface A from the interface D of the four-way switching valve, and redundant sample solution flows into the interface B of the electric multi-position valve and is discharged; when the sampling loop is switched into the double-sampling loop state, an interface A of the four-way switching valve is communicated with an interface B, an interface C of the four-way switching valve is communicated with an interface D, a sample flows into the interface C from the interface D of the four-way switching valve and then enters and fills a second sampling loop after flowing into and filling up a first sampling loop from an interface E of the electric multi-position valve, the sample flows into the interface A from the interface B of the four-way switching valve, and redundant sample solution flows into the interface B of the electric multi-position valve and is discharged; the electric multi-position valve has two states: the first state is a sample loading state, wherein the interface A is communicated with the interface B, the interface C is communicated with the interface D, and the interface E is communicated with the interface F; the second state is a sample injection state, wherein the interface B is communicated with the interface C, the interface D is communicated with the interface E, and the interface F is communicated with the interface A. The carrier flow is water or other solution taking water as solvent; the reagent a and the reagent B are each a solution used in the flow injection analysis method, and are not limited to a solution.
The device sensitivity and the degree of accuracy are high, use single sampling ring, or two sampling rings are established ties to change the sample volume, select by oneself according to the concentration of the measured object matter in the actual water sample. In the flow injection analysis system, the sample sampling amount of the sampling ring has positive correlation with the detection sensitivity, so the operation is simple, the analysis speed is high, and the precision is high.
The technical solution of the present invention will be further explained with reference to the following embodiments and accompanying drawings.
Example 1
The embodiment provides a flow injection analysis system with a range switching device, which comprises an automatic sample introduction part, a solution conveying part, a chemical reaction flow path, a detector and a data processing workstation.
The automatic sample introduction part comprises a sample introduction arm, a sample introduction needle 3, a sample disc 2, a test tube 1, a first motor, a second motor and a third motor.
The test tube 1 is used for placing a standard solution with a known concentration or a sample to be tested, and the sample introduction arm and the sampling needle 3 are used for collecting the sample in the sample test tube 1 and conveying the collected sample to the solution conveying part through the sample introduction arm.
The sampling arm is used for fixing the sampling needle; the sample plate 2 is used for placing test tubes; the second motor is used for moving the sampling needle up and down, when the sampling needle moves down, the sampling needle is used for sucking the standard solution with known concentration or the sample to be detected which is placed in the test tube, and when the sampling needle moves up, the sucking is stopped; the third motor is used for driving the sample feeding arm and the sample needle 3 to rotate; the first motor is used for driving the sample plate 2 to rotate.
The solution conveying part comprises a multi-channel peristaltic pump 11, and liquid in a sample peristaltic pump pipe 7, a current-carrying peristaltic pump pipe 8, a reagent A peristaltic pump pipe 9 and a reagent B peristaltic pump pipe 10 is conveyed through the multi-channel peristaltic pump;
the chemical reaction flow path comprises a sample peristaltic pump pipe 7, a current-carrying peristaltic pump pipe 8, a reagent A peristaltic pump pipe 9, a reagent B peristaltic pump pipe 10, a winding reaction pipe 26, a first tee joint 23, a second tee joint 24, a capillary connecting pipe, a first sampling ring 18, a second sampling ring 19, a container bottle, a flow cell 27, a first waste discharge pipe 15, a second waste discharge pipe 28, a four-way switching valve 17 and an electric multi-position valve 14;
the container bottles comprise a flow carrying bottle 4, a reagent A bottle 6, a reagent B bottle 5 and a waste liquid barrel; the electric multi-position valve 14 has at least six ports, which are a port a, a port B, a port C, a port D, a port E and a port F. The electric multi-position valve 6 has two states: the first state is a sample loading state, at the moment, the interface A is communicated with the interface B, the interface C is communicated with the interface D, and the interface E is communicated with the interface F; the second state is a sample injection state, wherein the interface B is communicated with the interface C, the interface D is communicated with the interface E, and the interface F is communicated with the interface A.
One end of the sample peristaltic pump tube 7 is connected with an F interface of the electric multi-position valve 14 through a capillary connecting tube, and the other end of the sample peristaltic pump tube is connected with a sample injection arm and a sample injection needle 3 through the capillary connecting tube;
one end of the current-carrying peristaltic pump pipe 8 is in liquid communication with the current-carrying bottle 4 through a capillary connecting pipe, and the other end of the current-carrying peristaltic pump pipe is in liquid communication with a D interface of the electric multi-position valve 14 through a capillary connecting pipe;
one end of the reagent A peristaltic pump tube 9 is in liquid communication with the reagent A bottle 5 through a capillary connecting tube, and the other end of the reagent A peristaltic pump tube is connected with a port b of the first tee 23 through the capillary connecting tube;
one end of the reagent B peristaltic pump tube 10 is in liquid communication with the absorption liquid reagent bottle 6 through a capillary connecting tube, and the other end of the reagent B peristaltic pump tube is connected with a B interface of a second tee 25 through a capillary connecting tube;
the interface A of the four-way switching valve 17 is connected with the interface B of the electric multi-position valve 14 through a capillary connecting pipe;
the interface B of the four-way switching valve 17 is connected with a second sampling ring 19;
the C interface of the four-way switching valve 17 is connected with the other end of the second sampling ring 19;
the interface D of the four-way switching valve 17 is connected with the interface B of the electric multi-position valve 14 through a capillary connecting pipe; one end of the first waste discharge pipe 15 is connected with an A interface of the electric multi-position valve 14, and the other end is connected with a waste liquid barrel.
One end of the winding reaction tube 26 is communicated with the c interface of the second tee 25 through a capillary connecting tube, and the other end is communicated with the flow cell 17 through a capillary connecting tube;
the data processing workstation 30 is connected to the detector 29 to process the absorbance detected by the detector.
The wound reaction tube 26 has a length of 1 to 10m and an inner diameter of 0.3 to 1.5 mm.
The length of the capillary connecting pipe of the first waste discharge pipe 15 and the second waste discharge pipe 28 is 1-5m, and the inner diameter is 0.3-1.0 mm.
The capillary connecting pipe has a length of 0.1-1m and an inner diameter of 0.3-1.0 mm.
The first sampling ring and the second sampling ring have a length of 0.1-5m and an inner diameter of 0.3-1.0 mm.
The inner diameters of the sample peristaltic pump tube 7, the current-carrying peristaltic pump tube 8, the reagent A peristaltic pump tube 9 and the reagent B peristaltic pump tube 10 are 0.38-1.52mm, and the pump speed of the multi-channel peristaltic pump 11 is 20-40 rpm/min.
The optical path of the flow cell 27 is 10-50 mm.
In the low range mode, the interface a of the four-way switching valve 17 communicates with the interface B, and the interface C communicates with the interface D. The electric multi-position valve 14 is firstly in a sample loading state, when the electric multi-position valve 14 is in the sample loading state, a sample enters the sample peristaltic pump pipe 7 through the driving of the multi-channel peristaltic pump 11, then flows into an F interface of the electric multi-position valve 14, then flows out of an E interface, enters and fills the first sampling ring 18, and then flows into a D interface of the four-way switching valve 17; at this time, the interface D of the four-way switching valve 17 is communicated with the interface C, the sample solution flows out from the interface C, enters and fills the second sampling ring 19, then flows into the interface B, flows out from the interface A, flows into the interface B of the electric multi-position valve 14 through the capillary connecting pipe, and the redundant solution is discharged from the interface A through the waste discharge pipe. Then, the electric multi-position valve 21 is switched to the sample injection state. When the electric multi-position valve 21 is in a sample injection state, a carrier flow enters the carrier flow peristaltic pump pipe 8 through the driving of the multi-channel peristaltic pump 1 and further flows into a D interface of the electric multi-position valve 21, the D interface is communicated with an E interface at the moment, the carrier flow pushes a sample in the first sampling ring 18, then the sample in the second sampling ring 19 is pushed to enter a B interface of the electric multi-position valve 21, the B interface is communicated with a C interface at the moment, and the sample enters an A interface of the first tee 23 through the C interface to perform subsequent reaction.
In the high range mode, the a port of the four-way switching valve 17 communicates with the D port, and the C port communicates with the B port. The electric multi-position valve 14 is firstly in a sample loading state, when the electric multi-position valve 14 is in the sample loading state, a sample enters the sample peristaltic pump pipe 7 through the driving of the multi-channel peristaltic pump 11, then flows into an F interface of the electric multi-position valve 14, then flows out of an E interface, enters and fills the first sampling ring 18, and then flows into a D interface of the four-way switching valve 17; at this time, the port D of the four-way switching valve 17 communicates with the port a, flows out from the port a, flows into the port B of the electric multi-position valve 14 through the capillary connection pipe, and discharges the excess solution from the port a through the waste discharge pipe. Then, the electric multi-position valve 21 is switched to the sample injection state. When the electric multi-position valve 21 is in a sample injection state, a carrier flow enters the carrier flow peristaltic pump pipe 8 through the driving of the multi-channel peristaltic pump 1 and further flows into a D interface of the electric multi-position valve 21, the D interface is communicated with an E interface at the moment, the carrier flow pushes a sample in the first sampling ring 18 to flow into an A interface through a four-way switching valve 17D interface, the sample enters a B interface of the electric multi-position valve 21 through a capillary connecting pipe, the B interface is communicated with a C interface at the moment, and the sample enters the A interface of the first tee joint 23 through the C interface to perform subsequent reaction.
The reagent A solution is driven by the multi-channel peristaltic pump 11, enters the reagent A peristaltic pump tube 9, enters the first tee 23 through the interface B of the first tee 23, is mixed with a sample pushed by a current-carrying agent in the first tee 23, and then enters the interface A of the second tee 25.
The reagent B solution is driven by a multi-channel peristaltic pump 11, enters a reagent B solution peristaltic pump pipe 10, enters a second tee 25 through a B interface of the second tee 25 to be mixed with the previous solution, then enters a first winding reactor 26 for mixing reaction, and enters a flow cell 27 for detection.
The utility model discloses a flow injection analytic system with range auto-change over device can test the sample automatically in succession, and the test rate is fast to can select low-range mode (high sensitivity) or high-range mode (low sensitivity) to the sample concentration of difference, satisfy the demand among the actual detection.
Example 2
And (3) making a standard curve according to the peak height or peak area of the absorbance of the measured standard solution and the concentration of the standard solution, and calculating the concentration of the ammonia nitrogen in the sample on the standard curve according to the peak height or peak area of the absorbance of the sample.
(Note: absorbance)Definition of (1)
Wherein A is the absorbance, I0Is the intensity of incident light, I is the intensity of emergent light, and ε is the molar absorptivity (cm)-1·mol-1L), b is the liquid layer thickness (cm); c is the solution concentration (mol. L)-1))
The reagent used in the flow injection analysis system with the range switching device of the invention is as follows:
the reagents are all commercially available reagents made in China, and the lowest purity of the reagents is analytical purity.
Wherein the pH value of the buffer solution is 5.2 +/-0.1, and the buffer solution is prepared by mixing potassium sodium tartrate, sodium citrate and hydrochloric acid.
The sodium salicylate solution is prepared by mixing 25g/L of sodium hydroxide and 80g/L of sodium salicylate.
The distilling reagent is prepared by mixing potassium dihydrogen phosphate, dipotassium hydrogen phosphate, tetrasodium ethylene diamine tetraacetate and sodium hydroxide.
The absorption solution was a 0.6% (volume ratio) sulfuric acid solution.
The sodium nitroprusside solution is 5g/L sodium nitroferricyanide solution.
The sodium dichloroisocyanate solution is 4g/L sodium dichloroisocyanurate.
The carrier fluid is deionized water.
The standard ammonia nitrogen solution in water is purchased from the national standard center, and the concentration is 1000 mg/L. Diluting 1000mg/L ammonia nitrogen standard solution into 100mg/L and 10mg/L with deionized water, and preparing 0.02, 0.05, 0.10, 0.50, 1.00, 2.00, 3.00, 4.00 and 5.00mg/L standard sample series with 10mg/L ammonia nitrogen stock solution in water in sequence; the ammonia nitrogen stock solution in water of 100mg/L is prepared into standard sample series of 0.1, 0.5, 1.0, 2.0, 5.0, 10.0, 20.0, 30.0, 40.0 and 50.0mg/L in sequence.
The flow injection analysis system with the range switching device is tested by adopting standard samples of ammonia nitrogen in water with the concentrations of 0.02, 0.05, 0.10, 0.50, 1.00, 2.00, 3.00, 4.00 and 5.00mg/L in a low-range mode, the length of a first sampling ring is 15cm, the length of a second sampling ring is 135cm, and the first sampling ring and the second sampling ring are connected in series.
The flow injection analysis system with the range switching device of the invention was tested in a high range mode with a first sampling loop of 15cm in length using only the first sampling loop, using standard samples of ammonia nitrogen at concentrations of 0.1, 0.5, 1.0, 2.5, 5.0, 10.0, 20.0, 30.0, 40.0, 50.0mg/L in water.
The standard samples were analyzed using the flow injection analysis system with span switching device of the present invention, and the results are shown in tables 1 and 2.
TABLE 1 analysis results of the standard samples in the Low Range mode
| Concentration (mg/L) | Absorbance (Peak area) | Back calculation concentration (mg/L) |
| 0.00 | 15.70505 | -0.00506 |
| 0.02 | 24.00766 | 0.02240 |
| 0.05 | 88.43481 | 0.05890 |
| 0.10 | 114.19528 | 0.08156 |
| 0.50 | 564.41218 | 0.47751 |
| 1.00 | 1112.59221 | 0.95962 |
| 2.00 | 2450.49594 | 2.13627 |
| 3.00 | 3454.36268 | 3.01915 |
| 4.00 | 4513.21930 | 3.95038 |
| 5.00 | 5683.28564 | 4.97942 |
TABLE 2 analysis results of the standard samples in the Low Range mode
| Concentration (mg/L) | Absorbance (Peak area) | Back calculation concentration (mg/L) |
| 0.00 | 0.33266 | 0.15219 |
| 0.10 | 11.11365 | 0.25175 |
| 0.50 | 48.53700 | 0.59738 |
| 1.00 | 101.31530 | 1.08482 |
| 2.50 | 262.02357 | 2.56905 |
| 5.00 | 508.24066 | 4.84301 |
| 10.00 | 1020.49511 | 9.57398 |
| 20.00 | 2121.10556 | 19.73875 |
| 30.00 | 3222.14192 | 29.90746 |
| 40.00 | 4394.80352 | 40.73767 |
| 50.00 | 5359.14587 | 49.64393 |
The working curve is linearly fitted to the concentration according to the peak area of the measured absorbance, and a fitting equation and a correlation coefficient are calculated by software.
The method for measuring ammonia nitrogen in water by using the flow injection analysis system with the range switching device has the advantages that the linear range in the low-range mode is 0.02-5.00mg/L, and the correlation coefficient r is more than or equal to 0.999; the linear range in the high range mode is 0.1-50.0mg/L, and the correlation coefficient r is more than or equal to 0.999.
Detection limit DL ═ t(n-1,α＝0.99)X(s) (where t(n-1,α＝0.99)Is the standard deviation determined in the case of the one-sided t-test with a confidence of 99% when the degree of freedom is n-1, and t when n is 7(n-1,α＝0.99)3.14; s is the standard deviation of the repeated measurements).
The detection limit of the method using the flow injection analysis system with range switching device of the present invention was <0.001 mg/L.
The flow injection analysis system with the range switching device and the analysis method have the advantages that the adding standard recovery rate of the actual water sample is 90-110%.
The sequence of the above embodiments is only for convenience of description and does not represent the advantages and disadvantages of the embodiments.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, a plurality of modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (7)
1. The flow injection analysis system with the range switching device is characterized by comprising an automatic sample introduction part, a solution conveying part, a chemical reaction flow path, the range switching device and a detector, wherein the automatic sample introduction part is used for automatically sucking a sample, the solution conveying part is used for conveying the sample, a current carrying, a reagent A and a reagent B to the chemical reaction flow path respectively, the chemical reaction flow path is used for mixing the sample, the current carrying, the reagent A and the reagent B in sequence respectively to obtain a mixed solution and inputting the mixed solution into the detector, and the detector is used for detecting the absorbance of the mixed solution;
the solution conveying part comprises a multi-channel peristaltic pump, a sample peristaltic pump tube, a current-carrying peristaltic pump tube, a reagent A peristaltic pump tube and a reagent B peristaltic pump tube which are matched with the multi-channel peristaltic pump;
the chemical reaction flow path comprises a winding reaction tube, a first tee joint, a second tee joint, a first sampling ring, a flow carrying bottle, a reagent A bottle, a reagent B bottle, a waste liquid barrel, a flow cell, a first waste discharge tube, a second waste discharge tube and an electric multi-position valve;
the range switching device comprises a four-way switching valve and a second sampling ring;
the electric multi-position valve comprises a valve shell and a valve core, wherein the valve shell is provided with an interface A, an interface B, an interface C, an interface D, an interface E and an interface F, a first channel, a second channel and a third channel are rotatably arranged in the valve core,
the first channel is used for enabling the interface A to be communicated with the interface B or enabling the interface B to be communicated with the interface C, the second channel is used for enabling the interface C to be communicated with the interface D or enabling the interface D to be communicated with the interface E, and the third channel is used for enabling the interface E to be communicated with the interface F or enabling the interface F to be communicated with the interface A;
one end of the sample peristaltic pump tube is connected with an F interface of the electric multi-position valve through a capillary connecting tube, and the other end of the sample peristaltic pump tube is connected with the automatic sample injection part through the capillary connecting tube;
one end of the current-carrying peristaltic pump tube is communicated with the current-carrying bottle through a capillary connecting tube, and the other end of the current-carrying peristaltic pump tube is communicated with a D interface of the electric multi-position valve through a capillary connecting tube;
one end of the reagent A peristaltic pump tube is communicated with the reagent A bottle through a capillary connecting tube, and the other end of the reagent A peristaltic pump tube is connected with a b port of the first tee joint through the capillary connecting tube;
one end of the reagent B peristaltic pump tube is communicated with the reagent B bottle through a capillary connecting tube, and the other end of the reagent B peristaltic pump tube is connected with a port B of the second tee joint through the capillary connecting tube;
the interface A of the four-way switching valve is connected with the interface B of the electric multi-position valve through a capillary connecting pipe;
the B interface of the four-way switching valve is connected with one end of the second sampling ring;
the C interface of the four-way switching valve is connected with the other end of the second sampling ring;
the D interface of the four-way switching valve is connected with one end of the first sampling ring;
one end of the first sampling ring is in liquid communication with an E interface of the electric multi-position valve, and the other end of the first sampling ring is in liquid communication with a D interface of the four-way switching valve;
one end of the second sampling ring is in liquid communication with a port B of the four-way switching valve, and the other end of the second sampling ring is in liquid communication with a port C of the four-way switching valve;
the interface A of the electric multi-position valve is connected with the waste liquid barrel through a capillary connecting pipe and is used for discharging waste liquid;
the interface C of the electric multi-position valve is connected with the interface a of the first tee joint through a capillary connecting pipe;
the D interface of the electric multi-position valve is communicated with the liquid of the current-carrying peristaltic pump pipe through a capillary connecting pipe;
the F interface of the electric multi-position valve is in liquid communication with the sample peristaltic pump pipe through a capillary connecting pipe;
the port c of the first tee is connected with the port a of the second tee through a capillary connecting pipe;
the interface c of the second tee joint is connected with one end of the winding reaction tube through a capillary connecting tube;
the other end of the winding reaction tube is connected with an a interface of the flow cell;
the interface b of the flow cell is connected to a waste liquid barrel through a capillary connecting pipe for discharging waste liquid;
the flow cell is placed within a detector.
2. The flow injection analysis system with span switching apparatus of claim 1 further comprising a data processing station connected to the detector for processing the absorbance detected by the detector.
3. The flow injection analysis system with span switching device of claim 2 wherein the wound reaction tube has a length of 1-10m and an inner diameter of 0.3-1.5 mm.
4. The flow injection analysis system with span switching device of claim 3 wherein the capillary connecting tube has a length of 0.1-10m and an inner diameter of 0.3-1.0 mm.
5. The flow injection analysis system with span switching device of claim 4, wherein the internal diameters of the sample peristaltic pump tube, the current-carrying peristaltic pump tube, the reagent A peristaltic pump tube and the reagent B peristaltic pump tube are 0.38-1.52mm, and the multi-channel peristaltic pump has a pumping speed of 20-40 rpm/min.
6. The flow injection analysis system with span switching device of claim 5 wherein the first and second waste pipes have a length of 1-5m and an inner diameter of 0.3-1.0 mm.
7. The flow injection analysis system with range switching device according to claim 6, wherein the automatic sample introduction part comprises a sample tray for holding test tubes and a first motor for driving the sample tray to rotate, an output shaft of the first motor is connected to a rotation shaft of the sample tray, the sample tray is provided with a plurality of circular holes for holding test tubes, the test tubes for holding samples and standard solutions are inserted into the circular holes respectively, the automatic sample introduction part further comprises a sampling needle capable of being inserted into the test tubes and a second motor for driving the sampling needle to move up and down, an output end of the second motor is connected to the sampling needle, the second motor and the sampling needle are installed on a sample introduction arm, the sample introduction arm is connected to an output shaft of a third motor, the third motor is used for driving the sample introduction arm to swing above the sample tray, so that the sampling needle can enter a selected test tube, and the outer end of the sampling needle is connected with the sample peristaltic pump tube through a pipeline.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114324190A (en) * | 2021-12-30 | 2022-04-12 | 杭州谱育科技发展有限公司 | Self-correcting multi-parameter monitoring method |
| CN114965310A (en) * | 2022-04-26 | 2022-08-30 | 上海亚新城市建设有限公司 | Water quality on-line monitoring system measuring range self-switching control method and system |
| CN117031055A (en) * | 2023-08-25 | 2023-11-10 | 北京宝德仪器有限公司 | Flow analysis system with bubble interval continuous flow and flow injection switchable |
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2020
- 2020-06-30 CN CN202021247873.XU patent/CN212693799U/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114324190A (en) * | 2021-12-30 | 2022-04-12 | 杭州谱育科技发展有限公司 | Self-correcting multi-parameter monitoring method |
| CN114965310A (en) * | 2022-04-26 | 2022-08-30 | 上海亚新城市建设有限公司 | Water quality on-line monitoring system measuring range self-switching control method and system |
| CN117031055A (en) * | 2023-08-25 | 2023-11-10 | 北京宝德仪器有限公司 | Flow analysis system with bubble interval continuous flow and flow injection switchable |
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