CN102375073A - Fully automatic fluorine analyzer and analytical method thereof - Google Patents
Fully automatic fluorine analyzer and analytical method thereof Download PDFInfo
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- CN102375073A CN102375073A CN2010102529581A CN201010252958A CN102375073A CN 102375073 A CN102375073 A CN 102375073A CN 2010102529581 A CN2010102529581 A CN 2010102529581A CN 201010252958 A CN201010252958 A CN 201010252958A CN 102375073 A CN102375073 A CN 102375073A
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Abstract
The invention relates to a fully automatic analyzer for analyzing fluoride ions in environmental water. The analyzer which comprises an automatic injection device (1), a peristaltic pump (19), a detector (11), a computer processing system (17), and an online processing assembly is characterized in that: the automatic injection device (1) comprises a sample injection needle (4), a sample disc (20), a sample injection needle cleaning cell (3), and a pipeline cleaning cell (2); the detector (11) is inserted into a flow cell (12), and the outlet of the flow cell (12) is communicated with a liquid waste cell (16) through a second backpressure regulator (14) by capillary connecting tubes; and the detector (11) is connected with the computer processing system (17) through a signal line (18). By combining an electrode method with a sequential injection analysis method, the analyzer of the invention has the advantages of realization of the automation of the whole process, avoiding of personal errors, detection precision improvement, reagent amount saving, and realization of the timely monitoring of water quality.
Description
Technical field
The present invention relates to a kind of automatical analysis of Environmental Water intermediate ion, particularly a kind of fully-automatic analyzer and the method for using fluorine ion in the automatic analysis environments water of this analyser of measuring fluorine ion in the Environmental Water with sequentical injection analysis.
Background technology
Measure the fluoride ion electrode in the water at present, mainly adopt the fluoride ion selective electrode mensuration, fluoride ion selective electrode is the electrode of fluorine ion activity in the ability Correct Determination solution.It mainly is made up of film, interior reference solution and internal reference electrode three parts, and fluoride ion selective electrode cooperates the contrast electrode tentiometer that Connects Power simultaneously, can measure different kinds of ions concentration, and this assay method is the fluoride ion electrode method.
Not enough below but this method exists:
1, because need manually-operated, so, have artificial error, and each amount of reagent that consumes is more.
2, needing manually-operated, is not to carry out automation mechanized operation, can not be applicable to the real-time monitoring to water quality.
Summary of the invention
The object of the present invention is to provide a kind of sensitivity and accuracy of mensuration high, and simple to operate, and analysis speed is fast, the automatic analytical instrument of fluorine ion in the Environmental Water steady in a long-term.
Another object of the present invention has provided the automatic analysis method of fluorine ion in a kind of Environmental Water.
The fully-automatic analyzer of fluorine ion in a kind of Environmental Water comprises automatic sampling apparatus, peristaltic pump, detecting device, computer processing system, online treatment assembly, and automatic sampling apparatus comprises sample introduction needle, sample disc, sample introduction needle service sink, pipeline service sink; Wherein, detecting device inserts flow cell, and the outlet of flow cell is communicated with waste liquid tank through second back pressure regulator with the capillary connecting pipe; Detecting device is connected with computer processing system through signal wire; The online treatment assembly comprises sample fillup valve, reagent introduction valve, syringe, capillary connecting pipe, peristaltic pump pump line; The sample fillup valve has the interface more than 6, and two states are arranged: sample introduction state and detected state when A interface and B interface connection, C interface and D interface connection, E interface and F interface are communicated with, are the sample introduction state; When A interface and F interface connection, B interface and C interface connection, D interface and E interface are communicated with, be detected state; The interface F of sample fillup valve successively with peristaltic pump on pump line, the upper end of sample introduction needle be communicated with the capillary connecting pipe; The lower end of this sample introduction needle can be stretched in the sample bottle; The interface B of sample fillup valve is connected with the two ends of sampling ring respectively with the capillary connecting pipe with interface E; The interface A of sample fillup valve is communicated with waste liquid tank through first back pressure regulator with the capillary connecting pipe, and the interface D of sample fillup valve is connected with the flow cell inlet with the capillary connecting pipe, and the interface C of sample fillup valve is connected with reagent introduction valve interface A with the capillary connecting pipe; The reagent introduction valve is 3 valves; Two states are arranged: reagent is drawn with reagent and is discharged, and when the A interface led to the S interface, syringe was in the state of downward work reagent absorption; When B interface and S interface were logical, syringe was in the reagent release conditions of upwards working, and sample fillup valve C interface is communicated with reagent introduction valve A interface; When the reagent introduction valve is in the reagent release conditions, the sample in the sampling ring is injected in the flow cell A interface of sample fillup valve; The outlet of flow cell is connected with second back pressure regulator respectively; The other end of second back pressure regulator is communicated with waste liquid tank, and back pressure regulator is used for regulating the pressure in the stream, and the bubble that suppresses in the stream generates; Improve accuracy in detection; The kapillary that is connected with the interface B of reagent introduction valve is communicated with reagent bottle, and the interface B of reagent introduction valve is communicated with reagent bottle through the capillary connecting pipe, and reagent introduction valve S interface and syringe join.
The fully-automatic analyzer of fluorine ion in the Environmental Water of the present invention, circulate among pond are hollow structure, and it is a pmma material.
The fully-automatic analyzer of fluorine ion in the Environmental Water of the present invention, the length of capillary connecting pipe wherein is 0.1～1m, and the length of sampling ring is 1～4m, and the syringe volume is 1～5ml
The fully-automatic analyzer of fluorine ion in the Environmental Water of the present invention, the dead volume of flow cell wherein are 10～100 μ l.
Use the fully-automatic analyzer of fluorine ion in the Environmental Water of the present invention to detect the method for fluorine ion in the water; Wherein, Sample gets into peristaltic pump through automatic sampling apparatus; Sample pumps into the sample fillup valve through peristaltic pump, and after sampling ring was full of, unnecessary sample got into waste liquid tank through interface A and back pressure regulator; The reagent introduction valve is drawn release reagent, sample fillup valve dislocation, reagent introduction valve dislocation through upwards working of syringe downwards; Syringe is released the sample that is full of in the sampling ring, the pond that circulates, and unnecessary sample gets into waste liquid tank through back pressure regulator; Detecting device detects the potential value of solution in the flow cell; And it is transferred to computer processing system, computer processing system calculates the content of fluorine ion in the test fluid according to the position of potential value on typical curve of sample.
For this automatic analyzer; Can change corresponding ion-selective electrode (selecting electrode), supporting flow cell and corresponding current-carrying reagent, be used for measuring corresponding ion like chlorion, iodide ion, magnesium ion, calcium ion, cyanide ion, anionic surfactant.
Advantage of the present invention is: the present invention adopts electrode method and sequentical injection analysis coupling, has realized the robotization of whole process, has avoided personal error, can improve the precision of test, saves amount of reagent and can realize the timely monitoring for water quality.
Description of drawings
Fig. 1 is the structure diagram of the automatic analyzer of fluorine ion in the Environmental Water provided by the invention.
Embodiment
Further the present invention will be described through embodiment below.
The fully-automatic analyzer of fluorine ion in embodiment 1 Environmental Water
The automatic analyzer of fluorine ion in the Environmental Water as shown in Figure 1; Comprise automatic sampling apparatus 1, peristaltic pump 19, detecting device 11, computer processing system 17, online treatment assembly, automatic sampling apparatus comprises sample introduction needle 4, sample disc 20, sample introduction needle service sink 3, pipeline service sink 2; Detecting device 11 inserts flow cell 12, and flow cell 12 is the protruding structure of middle recessed side, and the dead volume of flow cell is 10～100 μ l, and it is a pmma material, and the outlet of flow cell 12 is communicated with waste liquid tank 16 through second back pressure regulator 14 with the capillary connecting pipe; Detecting device 11 is connected with computer processing system 17 through signal wire 18; The online treatment assembly comprises sample fillup valve 8, reagent introduction valve 9, syringe 10, capillary connecting pipe, peristaltic pump pump line 6; Syringe 10 volumes are 1-5ml; Capillary connecting pipe length is 0.1-1m; Sample fillup valve 8 tools have A, B, C, D, E, six interfaces of F, the interface F of sample fillup valve 8 successively with peristaltic pump 19 on pump line 6, the upper end of sample introduction needle 4 be communicated with the capillary connecting pipe, the lower end of this sample introduction needle 4 can be stretched in the sample hose 5; The interface B of sample fillup valve 8 is connected with the two ends of sampling ring 7 with interface E; The length of sampling ring 7 is 1～4m, and the interface A of sample fillup valve 8 is communicated with waste liquid tank 16 through first back pressure regulator 13 with the capillary connecting pipe, and the interface D of sample fillup valve 8 is connected with flow cell 12 inlets with the capillary connecting pipe; The interface C of sample fillup valve 8 is connected with reagent introduction valve 9 interface A with the capillary connecting pipe; Reagent introduction valve 9 is 3 valves, and the interface B of reagent introduction valve 9 is communicated with reagent bottle 15 through the capillary connecting pipe, and reagent bottle 15 reagent introduction valve 9S interfaces and syringe 10 join.
The course of work of automatic analyzer is:
Sample gets into peristaltic pump through automatic sampling apparatus 1; Sample pumps into sample fillup valve 8 through peristaltic pump; At this moment, when the A interface of sample fillup valve 8 and B interface connection, C interface and D interface connection, E interface and F interface are communicated with, be the sample introduction state; After sampling ring 7 was full of, unnecessary sample was through interface A and back pressure regulator 13 entering waste liquid tanks 16; When the B interface of reagent introduction valve 9 and S interface led to, syringe 10 is in downwards drew current-carrying from reagent bottle 15; When reagent introduction valve 9A interface and S interface were logical, syringe 10 was in the reagent release conditions of upwards working, and the C interface of sample fillup valve 8 is communicated with reagent introduction valve A interface; At this moment; The A interface of sample fillup valve 8 and F interface connection, B interface and C interface connection, D interface and E interface are communicated with, and sample is injected in the flow cell, the pressure that back pressure regulator 13,14 is used for regulating in the stream; The bubble that suppresses in the stream generates, and improves accuracy in detection.Detecting device 11 detects the potential value of solution in the flow cell 12, and it is transferred to computer processing system 17, and computer processing system 17 calculates the content of fluorine ion in the test fluid according to the position of potential value on typical curve of sample.
The fully-automatic analyzer of fluorine ion is measured the method for fluorine ion in the water in the Environmental Water that embodiment 2 uses among the embodiment 1
(1) preparation of standard specimen
11 standard models preparation: take by weighing 0.2210g benchmark sodium fluoride (NaF) (,, cooling off), change in the 1000ml volumetric flask after the water dissolving, be diluted to graticule, shake up perhaps in 500～600 ℃ of dry 40min in advance in 105～110 ℃ of dry 2h.Be transferred in the polyethylene bottle of dried and clean at once and store.(100mg/L is (with F for the fluoride standard reserving solution
-Meter)).
1.2 fluoride standard reserving solution 100mg/L with equal-volume TISAB solution stepwise dilution, is configured to 0.2,0.5,1.0,2.0,5.0,10.0, the 20.0mg/L standard series.
1.3 the sodium chloride volumetric molar concentration is 1.5mol/L in the total ionic strength adjustment buffer degree buffer solution (being called for short TISAB solution); The sodium acetate volumetric molar concentration is 1.5mol/L; The sodium citrate volumetric molar concentration is 0.5mol/L, and 36% acetic acid volumetric molar concentration is 0.5mol/L, is diluted to 1L with deionized water.
1.4 being isopyknic TISAB solution, mixes current-carrying with water.
Need to use domestic reagent in the use, the purity of reagent is minimum pure for analyzing.
Adopt automatic analyzer shown in Figure 1 to test.
(2) sample introduction
Sample is pumped to sampling ring 7, after sampling ring 7 is full of, gets into waste liquid tank 16.
(3) response measurement
Reagent introduction valve 9 is drawn to syringe 10 with current-carrying, and current-carrying is released the sample in the sampling ring 7, and the pond 12 that circulates is detected, and the data of generation can be by record.Potential value according to the standard solution that writes down is done typical curve, on typical curve, calculates the content of fluorine ion according to the suction potential value of sample.
The test result of table 1 standard model:
| Concentration known mg/L | logC | Potential value (mv) | Return and calculate concentration mg/L |
| 0.2 | -0.69897 | 197.6 | 0.208 |
| 0.5 | -0.30103 | 176.6 | 0.481 |
| 1 | 0 | 158.7 | 0.982 |
| 2 | 0.30103 | 140.8 | 2.005 |
| 5 | 0.69897 | 117.7 | 5.041 |
| 10 | 1 | 100.3 | 10.092 |
The test result of the different samples of table 2 (n=3)
Can know that from this embodiment it is accurate to adopt this method to record the result.
Above embodiment describes preferred implementation of the present invention; Be not that scope of the present invention is limited; Design under the prerequisite of spirit not breaking away from the present invention; Various distortion and improvement that those of ordinary skills make technical scheme of the present invention all should fall in the definite protection domain of claims of the present invention.
Claims (7)
1. the fully-automatic analyzer of fluorine ion in the Environmental Water; Comprise automatic sampling apparatus (1), peristaltic pump (19), detecting device (11), computer processing system (17), online treatment assembly, said automatic sampling apparatus comprises sample introduction needle (4), sample disc (20), sample introduction needle service sink (3), pipeline service sink (2); It is characterized in that said detecting device (11) inserts flow cell (12), the outlet of flow cell (12) is communicated with waste liquid tank (16) through second back pressure regulator (14) with the capillary connecting pipe; Detecting device (11) is connected with computer processing system (17) through signal wire (18); Said online treatment assembly comprises sample fillup valve (8), reagent introduction valve (9), syringe (10), capillary connecting pipe, peristaltic pump pump line (6); Said sample fillup valve (8) has the interface more than 6; The interface F of sample fillup valve (8) successively with peristaltic pump (19) on pump line (6), the upper end of sample introduction needle (4) be communicated with the capillary connecting pipe; The interface B of sample fillup valve (8) is connected with the two ends of sampling ring (7) respectively with interface E; The interface A of sample fillup valve (8) is communicated with waste liquid tank (16) through first back pressure regulator (13) with the capillary connecting pipe; The interface D of sample fillup valve (8) is connected with flow cell (12) inlet with the capillary connecting pipe, and the interface C of sample fillup valve (8) is connected with reagent introduction valve (9) interface A with the capillary connecting pipe, and reagent introduction valve (9) is 3 valves; The interface B of reagent introduction valve (9) is communicated with reagent bottle (15) through the capillary connecting pipe, and the S interface of reagent introduction valve (9) and syringe (10) join.
2. the fully-automatic analyzer of fluorine ion in the Environmental Water as claimed in claim 1 is characterized in that: circulate among pond (12) are the protruding structure of middle recessed side, and it is a pmma material.
3. the fully-automatic analyzer of fluorine ion in according to claim 1 or claim 2 the Environmental Water, it is characterized in that: the length of described capillary connecting pipe is 0.1～1m, and the length of sampling ring (7) is 1～4m, and the syringe volume is 1～5ml
4. the fully-automatic analyzer of fluorine ion in according to claim 1 or claim 2 the Environmental Water, it is characterized in that: the dead volume of described flow cell (12) is 10～100 μ l.
5. use the fully-automatic analyzer of fluorine ion in claim 1 or the 2 described Environmental Water to detect the method for fluorine ion in the water; It is characterized in that; Sample gets into peristaltic pump through automatic sampling apparatus (1); Sample pumps into sample fillup valve (8) through peristaltic pump, and after sampling ring (7) was full of, unnecessary sample got into waste liquid tank (16) through interface A and back pressure regulator (13); Reagent introduction valve (9) is upwards worked downwards through syringe the sample that is full of in the sampling ring (7) is released; The pond circulates; Unnecessary sample gets into waste liquid tank (16) through back pressure regulator (14), and detecting device (11) detects the potential value of solution in the flow cell, and it is transferred to computer processing system (17); According to the position of potential value on typical curve of sample, computer processing system (17) calculates the content of fluorine ion in the test fluid.
6. use the fully-automatic analyzer of fluorine ion in the described Environmental Water of claim 3 to detect the method for fluorine ion in the water; It is characterized in that; Sample gets into peristaltic pump through automatic sampling apparatus (1); Sample pumps into sample fillup valve (8) through peristaltic pump, and after sampling ring (7) was full of, unnecessary sample got into waste liquid tank (16) through interface A and back pressure regulator (13); Reagent introduction valve (9) is drawn release reagent through upwards working of syringe downwards; Sample fillup valve (8) dislocation, reagent introduction valve (9) dislocation, syringe is released the sample that is full of in the sampling ring (7); The pond circulates; Unnecessary sample gets into waste liquid tank (16) through back pressure regulator (14), and detecting device (11) detects the potential value of solution in the flow cell, and it is transferred to computer processing system (17); Computer processing system (17) calculates the content of fluorine ion in the test fluid according to the position of potential value on typical curve of sample.
7. use the fully-automatic analyzer of fluorine ion in the described Environmental Water of claim 4 to detect the method for fluorine ion in the water; Sample gets into peristaltic pump through automatic sampling apparatus (1); Sample pumps into sample fillup valve (8) through peristaltic pump; After sampling ring (7) was full of, unnecessary sample was through interface A and back pressure regulator (13) entering waste liquid tank (16); Reagent introduction valve (9) is drawn release reagent through upwards working of syringe downwards; Sample fillup valve (8) dislocation, reagent introduction valve (9) dislocation, syringe is released the sample that is full of in the sampling ring (7); The pond circulates; Unnecessary sample gets into waste liquid tank (16) through back pressure regulator (14), and detecting device (11) detects the potential value of solution in the flow cell, and it is transferred to computer processing system (17); Computer processing system (17) calculates the content of fluorine ion in the test fluid according to the position of potential value on typical curve of sample.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103267795A (en) * | 2013-05-02 | 2013-08-28 | 中国科学院合肥物质科学研究院 | On-line monitoring analyzer for fluorinion in water and detection method thereof |
| CN103776889A (en) * | 2013-11-20 | 2014-05-07 | 北京华安奥特科技有限公司 | Automatic ion electrode detection module |
| CN104730216A (en) * | 2015-04-16 | 2015-06-24 | 肖巍 | Analyzing and measuring device and liquid analyzing system |
| CN104764861A (en) * | 2015-04-16 | 2015-07-08 | 肖巍 | Analyzing and metering device and liquid analysis system |
| CN105738361A (en) * | 2016-05-03 | 2016-07-06 | 北京宝德仪器有限公司 | Automatic analyzer for index of permanganate in water and analysis method |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103267795A (en) * | 2013-05-02 | 2013-08-28 | 中国科学院合肥物质科学研究院 | On-line monitoring analyzer for fluorinion in water and detection method thereof |
| CN103267795B (en) * | 2013-05-02 | 2015-04-22 | 中国科学院合肥物质科学研究院 | On-line monitoring analyzer for fluorinion in water and detection method thereof |
| CN103776889A (en) * | 2013-11-20 | 2014-05-07 | 北京华安奥特科技有限公司 | Automatic ion electrode detection module |
| CN104730216A (en) * | 2015-04-16 | 2015-06-24 | 肖巍 | Analyzing and measuring device and liquid analyzing system |
| CN104764861A (en) * | 2015-04-16 | 2015-07-08 | 肖巍 | Analyzing and metering device and liquid analysis system |
| CN104730216B (en) * | 2015-04-16 | 2016-12-07 | 肖巍 | A kind of analysis metering device and liquid analysis system |
| CN105738361A (en) * | 2016-05-03 | 2016-07-06 | 北京宝德仪器有限公司 | Automatic analyzer for index of permanganate in water and analysis method |
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