CN117288884A - Titration flow path of automatic analyzer and titration analysis method - Google Patents
Titration flow path of automatic analyzer and titration analysis method Download PDFInfo
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- CN117288884A CN117288884A CN202311222932.6A CN202311222932A CN117288884A CN 117288884 A CN117288884 A CN 117288884A CN 202311222932 A CN202311222932 A CN 202311222932A CN 117288884 A CN117288884 A CN 117288884A
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- 238000004448 titration Methods 0.000 title claims abstract description 130
- 238000004458 analytical method Methods 0.000 title claims abstract description 22
- 230000029087 digestion Effects 0.000 claims abstract description 77
- 239000007788 liquid Substances 0.000 claims abstract description 70
- 238000002347 injection Methods 0.000 claims abstract description 64
- 239000007924 injection Substances 0.000 claims abstract description 64
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 63
- 239000003814 drug Substances 0.000 claims abstract description 48
- 238000002835 absorbance Methods 0.000 claims abstract description 44
- 239000002699 waste material Substances 0.000 claims abstract description 43
- 230000002572 peristaltic effect Effects 0.000 claims abstract description 22
- 239000000523 sample Substances 0.000 claims description 55
- 239000012488 sample solution Substances 0.000 claims description 54
- 238000005086 pumping Methods 0.000 claims description 34
- 239000003153 chemical reaction reagent Substances 0.000 claims description 28
- 239000000243 solution Substances 0.000 claims description 26
- 238000004140 cleaning Methods 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 8
- 239000012496 blank sample Substances 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000012360 testing method Methods 0.000 claims description 6
- 238000012937 correction Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 239000012086 standard solution Substances 0.000 claims description 3
- 238000000605 extraction Methods 0.000 claims description 2
- 238000007599 discharging Methods 0.000 claims 3
- 238000001514 detection method Methods 0.000 abstract description 20
- 239000000126 substance Substances 0.000 description 8
- 101150041326 air-2 gene Proteins 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000002372 labelling Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000010892 non-toxic waste Substances 0.000 description 1
- 239000010891 toxic waste Substances 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/18—Water
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Abstract
The invention discloses a titration flow path of an automatic analyzer, which comprises a control valve group, an injection pump, a peristaltic pump, a digestion unit and a reaction unit; the control valve group is provided with a plurality of communicated ports, and is connected with a burette, a standard liquid pipe, a pure water pipe, a sample pipe, a first air pipe, a first waste liquid pipe and a plurality of medicament pipes through the ports; one end of the injection pump, one end of the peristaltic pump, the bottom of the digestion unit and the bottom of the reaction unit are respectively connected with the control valve group through ports, the other end of the peristaltic pump is connected with a second waste liquid pipe, and the digestion unit is connected with a second air pipe. The top of the reaction unit is connected with a burette, and the side edge of the reaction unit is provided with a light generator for emitting light and a detector for detecting absorbance. On the basis, the invention also discloses a titration analysis method, which uses the automatic analyzer to perform analysis. The invention is suitable for water sample detection with large concentration span, and saves labor and is convenient to detect.
Description
Technical Field
The invention relates to the technical field of water quality analysis, in particular to a titration flow path of an automatic analyzer and a titration analysis method.
Background
The water is a life source, the quality of the water is closely related to human health, and along with the development of social economy, scientific progress and the improvement of the living standard of people, the requirements of people on the water are also continuously improved, and the water quality detection is more and more strict. At present, an automatic analyzer is adopted to analyze a water sample when detecting water quality, and the content of various chemical components in the water is measured, but the water sample is limited by a concentration range, and the existing automatic analyzer can only measure the water sample with the concentration in the range when in use.
When detecting certain water samples, high concentration detection and low concentration detection are needed, and the concentration difference is large. In this regard, it is generally inconvenient to detect by using a high-range analyzer and a low-range analyzer, or by using a analyzer capable of switching between a high range and a low range, and then cleaning the switched range to detect after the range is found out to be over-standard in the detection process.
Disclosure of Invention
The invention aims to provide a titration flow path of an automatic analyzer and a titration analysis method so as to improve detection convenience.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a titration flow path of an automatic analyzer comprises a control valve group, an injection pump, a peristaltic pump, a digestion unit and a reaction unit; the control valve group is provided with a plurality of communicated ports, and is connected with a burette, a standard liquid pipe, a pure water pipe, a sample pipe, a first air pipe, a first waste liquid pipe and a plurality of medicament pipes through the ports; the injection pump, one end of the peristaltic pump, the bottom of the digestion unit and the bottom of the reaction unit are respectively connected with the control valve group through the ports, and the other end of the peristaltic pump is connected with a second waste liquid pipe; the top of the reaction unit is connected with the burette, the side edge of the reaction unit is provided with a light generator and a detector relatively, the light generator is used for emitting light rays and directing the light rays to liquid contained in the reaction unit, and the detector is used for detecting absorbance of the liquid contained in the reaction unit.
Further, the control valve group comprises a multi-way valve, a two-position two-way valve, a first three-way valve and a second three-way valve, and the ports comprise a first end, a tenth end, two public ends, a normal open end and a normal closed end, wherein the first end, the tenth end and the public ends are positioned on the multi-way valve, the normal open end and the normal closed end are positioned on the first three-way valve, and the normal open end and the normal closed end are positioned on the second three-way valve; two common ends on the multi-way valve are respectively connected with the injection pump and one end on the two-position two-way valve; the reagent tube comprises a first reagent tube, a second reagent tube, a third reagent tube, a fourth reagent tube, a sample tube, a digestion unit, a reaction unit and a third reagent tube, wherein the first end and the tenth end are respectively connected with the burette, the standard liquid tube, the pure water tube, the sample tube, the first reagent tube, the second reagent tube, the digestion unit and the reaction unit; the common end of the first three-way valve is connected with the other end of the two-position two-way valve, and the normally open end of the first three-way valve is connected with the first air pipe; and a normally open end of the second three-way valve is connected with the first waste liquid pipe, and a normally closed end of the second three-way valve is connected with the peristaltic pump.
Further, the reactor also comprises a stirrer, wherein the stirrer is used for stirring and uniformly mixing the liquid contained in the reaction unit.
A titration analysis method for performing an analysis using the automatic analyzer titration flow path, comprising the steps of:
s1, sample injection digestion: and extracting a sample solution, pumping the sample solution into the digestion unit for heating and digestion, and cooling after the digestion is completed.
S2, feeding: the reagents required for the titration reaction are withdrawn and pumped into the reaction unit.
S3, titration and calculation: determining a minimum value V of the titration volume of the burette H With titration volume maximum V L And continuously dripping the sample solution after the determination and the extraction and the cooling into the reaction unit, and judging according to the following steps:
s31, if the titration amount value is equal to the minimum titration volume value V H And when the titration end point appears, the reaction unit is cleaned, the sample solution is diluted or the precision of the burette is improved, then the steps S2 and S3 are repeated,until the sample concentration C is obtained by calculation S 。
S32, if the titration amount value is at the minimum titration volume value V H With the titration volume maximum V L In between, and when a titration end point occurs, the sample titration amount V when the titration end point is reached is recorded S And according to the sample, the amount V is dropped S Calculating to obtain sample concentration C S 。
S33, if the titration amount value is equal to the titration volume maximum value V L And if the titration end point does not appear, the absorbance of the solution contained in the measuring reaction unit is recorded as the absorbance A of the sample S And based on the absorbance A of the sample S Calculating to obtain sample concentration C S 。
Further, the step S1 specifically includes:
s11, extracting a sample solution from the injection pump and the sample tube, and washing the injection pump by the extracted sample solution; after rinsing, the waste liquid generated by rinsing is pushed to the first waste liquid pipe by the injection pump and discharged.
S12, extracting a sample solution from the sample tube through the injection pump, and pumping the sample solution into the digestion unit; and extracting the medicament required by digestion through the injection pump and the medicament tube, and pumping the medicament into the digestion unit.
S13, pumping air through the injection pump and the first air pipe, and driving the air into the digestion unit.
S14, heating and digesting the solution contained in the digestion unit, and cooling the digestion unit after digestion is completed.
Further, the step S2 specifically includes:
s21, extracting pure water through the injection pump and the pure water pipe, and cleaning the injection pump by the extracted pure water; after washing, the generated waste liquid is pushed to the first waste liquid pipe by the syringe pump and discharged.
S22, pumping pure water through the injection pump and the pure water pipe, and pumping the pure water into the reaction unit.
S23, extracting the medicament required by the titration reaction through the injection pump and the medicament tube, and pumping the medicament into the reaction unit.
S24, extracting pure water through the injection pump and the pure water pipe, and pumping into the reaction unit until the solution contained in the reaction unit submerges the light rays emitted by the light generator.
S25, pumping air through the injection pump and the first air pipe, and pumping the air into the reaction unit.
Further, step S3 further includes: extracting a portion of the cooled sample solution from the digestion unit by the syringe pump prior to dropping the sample solution to rinse the syringe pump; after rinsing, the waste liquid generated by rinsing is pushed to the first waste liquid pipe by the injection pump and discharged. And (3) dropwise adding the sample solution, stirring the solution contained in the reaction unit, and detecting the absorbance of the solution contained in the reaction unit in real time.
Further, in step S32, the sample concentration C S The calculation formula of (2) is as follows:
wherein V is S Dripping and quantifying a sample; v (V) H Is the minimum titration volume; v (V) L Is the maximum titration volume; c (C) H To and titrate volume minimum V H Corresponding concentration values; c (C) L Is equal to the maximum value V of titration volume L Corresponding concentration values; k (k) V The coefficient was corrected for titration volume.
Further, in step S33, the sample concentration C S The calculation formula of (2) is as follows:
wherein A is S Absorbance for the sample; a is that B The absorbance is the absorbance of a blank sample, namely, in a blank test, after all the blank samples are dripped, the absorbance obtained by the solution contained in the reaction unit is measured; a is that C For titration of end point absorbance, i.e. at standardIn the test, the minimum value V of the titration volume is added dropwise H Measuring absorbance of the solution contained in the reaction unit after the standard solution with the same volume; c (C) L Is equal to the maximum value V of titration volume L Corresponding concentration values; k (k) A Is the absorbance correction coefficient.
Further, the determining step of the titration endpoint is as follows: and starting the light generator when the sample solution is dripped, detecting the absorbance of the solution contained in the reaction unit in real time through the detector, and judging that the titration end point is reached when the detected absorbance value is equal to a preset absorbance value.
The invention has the following beneficial effects:
1. the invention provides a titration flow path of an automatic analyzer and a titration analysis method, which are applied to the automatic analyzer for detecting a water sample, wherein a sample solution to be detected can be digested in a digestion unit and gradually dripped into a reaction unit as a titration solution for reaction, high concentration detection and low concentration detection of the sample solution can be completed in fewer titration processes along with continuous dripping of the sample solution, the detection is convenient, and the concentration of the sample solution can be accurately calculated and obtained according to the titration amount or absorbance when the titration is stopped.
2. The invention provides a titration flow path and a titration analysis method of an automatic analyzer, which can measure a large concentration range, are suitable for detecting water samples with large concentration spans, are convenient to detect, and have a wide application range.
3. The titration flow path structure of the automatic analyzer provided by the invention is simple and convenient to maintain.
Drawings
FIG. 1 is a schematic view of a titration flow path of an automatic analyzer according to the present invention.
Description of main reference numerals: 1. a multi-way valve; 2. a first end; 3. a second end; 4. a third end; 5. a fourth end; 6. a fifth end; 7. a sixth end; 8. a seventh end; 9. an eighth end; 10. a ninth end; 11. a tenth end; 12. a two-position two-way valve; 13. a first three-way valve; 14. a second three-way valve; 15. a syringe pump; 16. a peristaltic pump; 17. a digestion unit; 18. a reaction unit; 19. a light generator; 20. a detector; 21. a stirrer; 22. a burette; C. a liquid labeling pipe; H. a pure water pipe; s, a sample tube; r1, a first medicament tube; r2, a second agent tube; r3, a third agent tube; r4, a fourth medicament tube; air1, a first Air tube; air2, a second Air tube; air3, a third Air tube; NW, first waste liquid tube; TW, second waste liquid pipe.
Detailed Description
The invention will be further described with reference to the drawings and detailed description.
Example 1
As shown in fig. 1, the invention discloses a titration flow path of an automatic analyzer, which comprises a control valve group, an injection pump 15, a peristaltic pump 16, a digestion unit 17 and a reaction unit 18. The control valve group is provided with a plurality of communicated ports, and is connected with a burette 22, a standard liquid pipe C, a pure water pipe H, a sample pipe S, a first Air pipe Air1, a first waste liquid pipe NW and a plurality of medicament pipes through the ports. One end of liquid inlet on the injection pump 15 and peristaltic pump 16, the bottom of the digestion unit 17 and the bottom of the reaction unit 18 are respectively connected with a control valve group through ports, and one end of liquid outlet on the peristaltic pump 16 is connected with a second waste liquid pipe TW.
The control valve group comprises four parts of a multi-way valve 1, a two-position two-way valve 12, a first three-way valve 13 and a second three-way valve 14, wherein the ports comprise a first end 11 to a tenth end 11 which are positioned on the multi-way valve 1 and two public ends communicated with the first end 11, a normally open end positioned on the first three-way valve 13 and normally open and normally closed ends positioned on the second three-way valve 14. The medicine pipes connected with the control valve group comprise four first to fourth medicine pipes R4.
Specifically, the multi-way valve 1 adopts ten rows of valves, one of two public ends on the multi-way valve 1 is connected with a port of liquid inlet and outlet on the injection pump 15, the other end of the multi-way valve 1 is connected with one end on the two-position two-way valve 12, the first end 2 on the multi-way valve 1 is connected with the bottom of the reaction unit 18, the second end 3 is connected with the buret 22, the third end 4 is connected with the standard liquid pipe C, the fourth end 5 is connected with the pure water pipe H, the fifth end 6 is connected with the sample pipe S, the sixth end 7 is connected with the first reagent pipe R1, the seventh end 8 is connected with the second reagent pipe R2, the eighth end 9 is connected with the third reagent pipe R3, the ninth end 10 is connected with the fourth reagent pipe R4, and the tenth end 11 is connected with the digestion valve at the bottom of the digestion unit 17. The common end of the first three-way valve 13 is connected with the other end of the two-position two-way valve 12, and the normally open end is connected with the first Air pipe Air1. The normally open end of the second three-way valve 14 is connected to the first waste liquid pipe NW, and the normally closed end is connected to the peristaltic pump 16. The first waste liquid pipe NW connected to the second three-way valve 14 is a non-toxic waste liquid pipe, and the second waste liquid pipe TW connected to the peristaltic pump 16 is a toxic waste liquid pipe.
The top of the reaction unit 18 is connected with a buret 22 and a third Air pipe Air3, and is connected with a second end 3 on the multi-way valve 1 through the buret 22. The side of the reaction unit 18 is provided with a light generator 19 and a detector 20, the light generator 19 is used for emitting light and directing the light to the liquid contained in the reaction unit 18, and the detector 20 is used for detecting the absorbance of the liquid contained in the reaction unit 18. The bottom of the reaction unit 18 is provided with a magnetic stirrer 21, a stirrer is arranged in the reaction unit, and the stirrer can be driven to rotate by the magnetic stirrer 21 so as to stir and mix the liquid contained in the reaction unit 18.
In the titration flow path, the digestion unit 17 and the reaction unit 18 are mutually independent and can be communicated through the control valve group, so that the purposes of obtaining the titration solution by digesting the sample solution and titrating in the reaction unit 18 can be fulfilled, the whole titration flow path has a simple structure, and the maintenance is convenient.
Example two
On the basis of the first embodiment, the invention also discloses a titration analysis method which uses the automatic analyzer titration flow path for analysis.
Before the detection analysis is performed, the syringe pump 15, the digestion unit 17 and the reaction unit 18 are cleaned. Pure water is typically left in the digestion unit 17 prior to cleaning. During cleaning, the tenth end 11 is firstly opened, and pure water in the digestion unit 17 is pumped by the injection pump 15; then, the peristaltic pump 16 is started, residual pure water in the digestion unit 17 is pumped out through the tenth end 11 of the multi-way valve 1, the two-position two-way valve 12, the first three-way valve 13 and the second three-way valve 14, and the pure water is discharged through the second waste liquid pipe TW; then the second end 3 is opened, the injection pump 15 is pushed to push pure water stored in the injection pump 15 into the reaction unit 18 through the burette 22, and the burette 22 and the reaction unit 18 are cleaned; then opening the tenth end 11, pumping Air through the injection pump 15 and the second Air pipe Air2 on the digestion unit 17, opening the second end 3 after pumping, pumping Air into the reaction unit 18 through the burette 22, and completely exhausting liquid possibly remained through the Air; finally, peristaltic pump 16 and first end 2 are turned on, and reaction unit 18 is emptied through peristaltic pump 16 and second waste tube TW. So far, the whole titration flow path is clean, and can meet detection requirements.
The detection and analysis method comprises the following steps:
s1, sample injection digestion: and extracting the sample solution, pumping the sample solution into the digestion unit 17 for heating digestion, and cooling the digestion unit 17 after the digestion is completed. The step S1 specifically comprises the following steps:
s11, opening the fifth end 6 of the multi-way valve 1, extracting sample solution through the injection pump 15 and the sample tube S, and washing the injection pump 15 and the internal pipelines of the multi-way valve 1 through the extracted sample solution. After the completion of the rinsing, the syringe pump 15 is pushed, and the waste liquid generated by the rinsing is pushed to the first waste liquid pipe NW via the two-position two-way valve 12, the first three-way valve 13, and the second three-way valve 14 and discharged.
S12, opening the fifth end 6 of the multi-way valve 1, extracting the sample solution from the sample tube S through the injection pump 15, opening the tenth end 11 of the multi-way valve 1, and pumping the extracted sample solution into the digestion unit 17. Thereafter, the medicine required for digestion is extracted from the medicine tube by the syringe pump 15 and is injected into the digestion unit 17.
In this embodiment, the medicaments required for digestion include a first medicament and a second medicament, and the corresponding medicament tube includes a first medicament tube R1 and a second medicament tube R2. When the first medicament is added, the sixth end 7 of the multi-way valve 1 is firstly opened, the first medicament is extracted through the injection pump 15 and the first medicament tube R1, and then the tenth end 11 is opened, so that the first medicament is injected into the digestion unit 17. After the first chemical is injected, a certain amount of Air is extracted by the syringe pump 15 and the first Air tube Air1, the tenth end 11 is opened, the extracted Air is injected into the digestion unit 17, and the sample solution and the first chemical are sufficiently mixed. Similarly, when the second chemical is added, the seventh end 8 of the multi-way valve 1 is opened, the second chemical is pumped through the injection pump 15 and the second chemical tube R2, and then the second chemical is pumped into the digestion unit 17.
S13, after the last medicament is injected, air is pumped by the injection pump 15 and the first Air pipe Air1, the tenth end 11 is opened, and the Air is injected into the digestion unit 17, so that the sample solution to be digested is fully mixed with the medicament required for digestion.
S14, heating the solution contained in the digestion unit 17, wherein in the embodiment, the sample solution in the digestion unit 17 is heated to 100 ℃ for 500S. After digestion is completed, the digestion unit 17 is cooled to a specified temperature, and then a titration solution to be titrated is obtained.
S2, feeding: the reagents required for the titration reaction are withdrawn and pumped into the reaction unit 18. The method specifically comprises the following steps:
s21, opening the fourth end 5 of the multi-way valve 1, pumping pure water through the injection pump 15 and the pure water pipe H, and cleaning the injection pump 15 by the pumped pure water. After washing, the syringe pump 15 is pushed to push the generated waste liquid to the first waste liquid pipe NW and discharge the same.
S22, opening the fourth end 5 of the multi-way valve 1, pumping a certain amount of pure water through the injection pump 15 and the pure water pipe H, and pumping the pure water into the reaction unit 18 through the first end 2 of the multi-way valve 1.
S23, extracting the medicament required by the titration reaction from the medicament tube through the injection pump 15, and pumping the medicament into the reaction unit 18 through the first end 2 of the multi-way valve 1. In this embodiment, the reagents required for the titration reaction include a third reagent and a fourth reagent, and the corresponding reagent tubes include a third reagent tube R3 and a fourth reagent tube R4. When the third medicine is added, the eighth end 9 of the multi-way valve 1 is opened first, the third medicine is pumped through the injection pump 15 and the third medicine tube R3, and then the first end 2 of the multi-way valve 1 is opened, and the third medicine is injected into the reaction unit 18. When the fourth medicine is added, the ninth end 10 of the multi-way valve 1 is opened, the fourth medicine is pumped through the injection pump 15 and the fourth medicine tube R4, and then the fourth medicine is pumped into the reaction unit 18 through the first end 2 of the multi-way valve 1.
S24, in step S22, after the chemical required for the reaction is pumped into the reaction unit 18, pure water is pumped into the reaction unit 18 until the solution contained in the reaction unit 18 submerges the light emitted by the light generator 19.
And S25, finally, pumping a certain amount of Air through the injection pump 15 and the first Air pipe Air1, and pumping the Air into the reaction unit 18 through the first end 2 of the multi-way valve 1 to ensure that the added medicament and pure water are both pumped into the reaction unit 18.
S3, titration and calculation: determining a minimum value V of the titration volume of burette 22 H With titration volume maximum V L Wherein the titration volume minimum value V H I.e. upper limit of titration amount, maximum titration volume V L I.e. the lower limit of the titration amount.
After the determination, the cooled sample solution is drawn and continuously dropped into the reaction unit 18. Before extracting the sample solution, the tenth end 11 of the multi-way valve 1 is opened, and a portion of the digested and cooled sample solution is extracted from the digestion unit 17 by the syringe pump 15, and the syringe pump 15 is rinsed with the extracted sample solution. After rinsing, the waste liquid generated by rinsing is pushed to the first waste liquid pipe NW by the syringe pump 15 and discharged. Then, the tenth end 11 of the multi-way valve 1 is opened, and the sample solution after digestion cooling in the digestion unit 17 is pumped by the injection pump 15 and used as a titration solution to wait for titration.
After the sample solution is withdrawn, the second end 3 of the multi-way valve 1 is opened and the syringe pump 15 is pushed, so that the sample solution can be slowly dropped into the reaction unit 18 through the burette 22. The stirrer 21 is turned on at the same time of the dropping to stir the solution contained in the mixing reaction unit 18.
In the titration process, three conditions mainly exist, and the determination is specifically carried out according to the following steps:
s31, if the titration amount value of the sample solution is equal to the minimum titration volume value V H And a titration end point appears, namely if the titration end point appears when only one drop of sample solution is dripped, the detection overrange is judged, the reaction unit 18 is required to be cleaned, the sample solution is diluted or the burette 22 is replaced to improve the precision of the burette 22, and then the steps S2 and S3 are repeated until the sample concentration C is obtained by calculation S 。
S32, if the titration amount of the sample solution is at the minimum titration volume value V H With titration volume maximum V L In between, and when a titration end point occurs, the sample titration amount V when the titration end point is reached is recorded S And titrate according to the sampleQuantity V S Calculating to obtain sample concentration C S . In this case, the sample concentration C S The calculation formula of (2) is as follows:
wherein V is S Dripping and quantifying a sample; v (V) H Is the minimum titration volume as described above; v (V) L Is the maximum titration volume as described above; c (C) H To and titrate volume minimum V H Corresponding concentration values, namely high-range standard liquid concentration values of the burette 22; c (C) L Is equal to the maximum value V of titration volume L The corresponding concentration value, namely the low-range concentration value of the target liquid in the buret 22; k (k) V The volume correction factor was calculated for the titration obtained according to standard test.
S33, if the titration amount value of the sample solution is equal to the titration volume maximum value V L And no titration end point is present, i.e. the titration end point is not present in the sample solution at the completion of the titration, the absorbance of the solution contained in the measurement reaction unit 18 is recorded as the sample absorbance A S And according to the absorbance A of the sample S Calculating to obtain sample concentration C S . In this case, the sample concentration C S The calculation formula of (2) is as follows:
wherein A is S Absorbance for the sample; a is that B The absorbance of the blank sample is measured after all the blank sample is dripped in the blank test, and the titration amount at this time is the maximum value V of the titration volume L ；A C For the end point absorbance of the titration, i.e. in standard experiments, the minimum value of the titration volume V is added dropwise H Measuring the absorbance of the solution contained in the reaction unit 18 after an equal volume of the standard solution; c (C) L Is equal to the maximum value V of titration volume L Corresponding concentration values; k (k) A To according to standard testAnd calculating the obtained absorbance correction coefficient.
In the judging process, the judging step of the titration end point is as follows:
the light generator 19 is turned on at the time of dropping the sample solution, and the absorbance of the solution contained in the reaction unit 18 is detected in real time by the detector 20, and when the detected real-time absorbance value is equal to a preset absorbance value, it is determined that the titration end point is reached.
After the detection analysis is completed, the digestion unit 17, the reaction unit 18, the burette 22, etc. are typically cleaned. The method comprises the following specific steps:
s41, evacuating the digestion unit 17: the tenth end 11 of the multi-way valve 1 is opened, and the waste liquid in the digestion unit 17 is pumped by the peristaltic pump 16 and discharged through the second waste liquid pipe TW.
Evacuation syringe pump 15: pushing the syringe pump 15 pushes the liquid remaining in the syringe pump 15 to the first waste liquid tube NW and discharges the liquid.
S42, cleaning and digestion unit 17: the fourth end 5 of the multi-way valve 1 is opened, pure water is pumped through the injection pump 15 and the pure water pipe H, and then the tenth end 11 of the multi-way valve 1 is opened, and the pure water is pumped into the digestion unit 17, so that the digestion unit 17 is cleaned.
S43, cleaning the buret 22: the tenth end 11 of the multi-way valve 1 is opened, pure water in the digestion unit 17 is pumped by the injection pump 15, then the second end 3 of the multi-way valve 1 is opened, and the pumped pure water is pumped into the reaction unit 18 by the burette 22, so that the burette 22 is cleaned.
And then, the residual pure water and a large amount of ventilation in the digestion unit 17 are pumped by the injection pump 15 and are pumped into the reaction unit 18 by the burette 22, so that the digestion unit 17 and the burette 22 are clean and have no residual liquid.
S44, cleaning the reaction unit 18: the fourth end 5 of the multi-way valve 1 is opened, pure water is pumped through the injection pump 15 and the pure water pipe H, and then the first end 2 of the multi-way valve 1 is opened to pump the pure water into the reaction unit 18 so as to clean the reaction unit 18.
Evacuating the reaction unit 18: the first end 2 of the multi-way valve 1 is opened, and the waste liquid in the reaction unit 18 is pumped by the peristaltic pump 16 and discharged through the second waste liquid pipe TW.
And S45, finally, opening the fourth end 5 of the multi-way valve 1, pumping pure water through the injection pump 15 and the pure water pipe H, and then opening the first end 2 of the multi-way valve 1 to pump the pure water into the reaction unit 18.
In steps S41 to S44, the number of times of cleaning and draining may be repeated multiple times according to the actual situation.
In summary, since the sample concentration C is usually predicted before detection S When the detection range is selected, the probability of occurrence of the condition in S31 is low when the titration analysis method is used for detection, and along with continuous dripping of the sample solution, high-concentration detection and low-concentration detection of the sample solution can be basically finished at one time. Therefore, the titration analysis method is convenient to detect, is particularly suitable for detection conditions with larger range difference such as 0.05-20mg/L, 0.1-40mg/L and 0.2-80mg/L, and has wide measurable concentration range, convenient use and wide application range.
While the invention has been particularly shown and described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. An automatic analyzer titration flow path, characterized in that:
comprises a control valve group, an injection pump, a peristaltic pump, a digestion unit and a reaction unit;
the control valve group is provided with a plurality of communicated ports, and is connected with a burette, a standard liquid pipe, a pure water pipe, a sample pipe, a first air pipe, a first waste liquid pipe and a plurality of medicament pipes through the ports;
the injection pump, one end of the peristaltic pump, the bottom of the digestion unit and the bottom of the reaction unit are respectively connected with the control valve group through the ports, and the other end of the peristaltic pump is connected with a second waste liquid pipe;
the top of the reaction unit is connected with the burette, the side edge of the reaction unit is provided with a light generator and a detector relatively, the light generator is used for emitting light rays and directing the light rays to liquid contained in the reaction unit, and the detector is used for detecting absorbance of the liquid contained in the reaction unit.
2. An automatic analyzer titration flow path as recited in claim 1, wherein:
the control valve group comprises a multi-way valve, a two-position two-way valve, a first three-way valve and a second three-way valve, and the ports comprise a first end, a tenth end, two public ends, a normal open end, a normal closed end and a normal open end, wherein the first end, the second public end, the normal open end and the normal closed end are positioned on the multi-way valve;
two common ends on the multi-way valve are respectively connected with the injection pump and one end on the two-position two-way valve; the reagent tube comprises a first reagent tube, a second reagent tube, a third reagent tube, a fourth reagent tube, a sample tube, a digestion unit, a reaction unit and a third reagent tube, wherein the first end and the tenth end are respectively connected with the burette, the standard liquid tube, the pure water tube, the sample tube, the first reagent tube, the second reagent tube, the digestion unit and the reaction unit;
the common end of the first three-way valve is connected with the other end of the two-position two-way valve, and the normally open end of the first three-way valve is connected with the first air pipe; and a normally open end of the second three-way valve is connected with the first waste liquid pipe, and a normally closed end of the second three-way valve is connected with the peristaltic pump.
3. An automatic analyzer titration flow path as recited in claim 1, wherein:
the stirrer is used for stirring and uniformly mixing the liquid contained in the reaction unit.
4. A titration analysis method, characterized in that the automatic analyzer according to any one of claims 1-3 is used for analysis, comprising the steps of:
s1, sample injection digestion: extracting a sample solution, pumping the sample solution into the digestion unit for heating and digestion, and cooling after the digestion is completed;
s2, feeding: extracting the medicament required by titration reaction and pumping the medicament into the reaction unit;
s3, titration and titrationAnd (3) calculating: determining a minimum value V of the titration volume of the burette H With titration volume maximum V L And continuously dripping the sample solution after the determination and the extraction and the cooling into the reaction unit, and judging according to the following steps:
s31, if the titration amount value is equal to the minimum titration volume value V H And when the titration end point appears, the reaction unit is cleaned, the sample solution is diluted or the precision of the burette is improved, and then the steps S2 and S3 are repeated until the sample concentration C is obtained by calculation S ；
S32, if the titration amount value is at the minimum titration volume value V H With the titration volume maximum V L In between, and when a titration end point occurs, the sample titration amount V when the titration end point is reached is recorded S And according to the sample, the amount V is dropped S Calculating to obtain sample concentration C S ；
S33, if the titration amount value is equal to the titration volume maximum value V L And if the titration end point does not appear, the absorbance of the solution contained in the measuring reaction unit is recorded as the absorbance A of the sample S And based on the absorbance A of the sample S Calculating to obtain sample concentration C S 。
5. The method of claim 4, wherein step S1 specifically comprises:
s11, extracting a sample solution from the injection pump and the sample tube, and washing the injection pump by the extracted sample solution; after the washing, pushing the waste liquid generated by the washing to the first waste liquid pipe through the injection pump and discharging the waste liquid;
s12, extracting a sample solution from the sample tube through the injection pump, and pumping the sample solution into the digestion unit; extracting a medicament required for digestion through the injection pump and the medicament tube, and pumping the medicament into the digestion unit;
s13, pumping air through the injection pump and the first air pipe, and pumping the air into the digestion unit;
s14, heating and digesting the solution contained in the digestion unit, and cooling the digestion unit after digestion is completed.
6. The method of claim 4, wherein step S2 specifically comprises:
s21, extracting pure water through the injection pump and the pure water pipe, and cleaning the injection pump by the extracted pure water; after cleaning, pushing the generated waste liquid to the first waste liquid pipe through the injection pump and discharging the waste liquid;
s22, pumping pure water through the injection pump and the pure water pipe, and pumping the pure water into the reaction unit;
s23, extracting a medicament required by titration reaction through the injection pump and the medicament tube, and pumping the medicament into the reaction unit;
s24, extracting pure water through the injection pump and the pure water pipe, and pumping into the reaction unit until the solution contained in the reaction unit submerges the light rays emitted by the light generator;
s25, pumping air through the injection pump and the first air pipe, and pumping the air into the reaction unit.
7. The method of claim 4, wherein step S3 further comprises:
extracting a portion of the cooled sample solution from the digestion unit by the syringe pump prior to dropping the sample solution to rinse the syringe pump; after the washing, pushing the waste liquid generated by the washing to the first waste liquid pipe through the injection pump and discharging the waste liquid;
and (3) dropwise adding the sample solution, stirring the solution contained in the reaction unit, and detecting the absorbance of the solution contained in the reaction unit in real time.
8. A titration analysis method according to claim 4, wherein in step S32, the sample concentration C S The calculation formula of (2) is as follows:
wherein V is S Dripping and quantifying a sample; v (V) H Is the minimum titration volume; v (V) L Is the maximum titration volume; c (C) H To and titrate volume minimum V H Corresponding concentration values; c (C) L Is equal to the maximum value V of titration volume L Corresponding concentration values; k (k) V The coefficient was corrected for titration volume.
9. A titration analysis method according to claim 4, wherein in step S33, the sample concentration C S The calculation formula of (2) is as follows:
wherein A is S Absorbance for the sample; a is that B The absorbance is the absorbance of a blank sample, namely, in a blank test, after all the blank samples are dripped, the absorbance obtained by the solution contained in the reaction unit is measured; a is that C For the end point absorbance of the titration, i.e. in a standard test, the minimum value V of the titration volume is added dropwise H Measuring absorbance of the solution contained in the reaction unit after the standard solution with the same volume; c (C) L Is equal to the maximum value V of titration volume L Corresponding concentration values; k (k) A Is the absorbance correction coefficient.
10. The method of claim 4, wherein the step of determining the endpoint of the titration is as follows:
and starting the light generator when the sample solution is dripped, detecting the absorbance of the solution contained in the reaction unit in real time through the detector, and judging that the titration end point is reached when the detected absorbance value is equal to a preset absorbance value.
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