CN112666160B - Multi-element online titration method and device - Google Patents
Multi-element online titration method and device Download PDFInfo
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- CN112666160B CN112666160B CN202011614084.XA CN202011614084A CN112666160B CN 112666160 B CN112666160 B CN 112666160B CN 202011614084 A CN202011614084 A CN 202011614084A CN 112666160 B CN112666160 B CN 112666160B
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- 238000004448 titration Methods 0.000 title claims abstract description 106
- 238000005070 sampling Methods 0.000 claims abstract description 24
- 238000001514 detection method Methods 0.000 claims abstract description 20
- 238000003756 stirring Methods 0.000 claims abstract description 20
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 24
- 239000012086 standard solution Substances 0.000 claims description 17
- 238000004140 cleaning Methods 0.000 claims description 16
- 239000003153 chemical reaction reagent Substances 0.000 claims description 11
- 238000002835 absorbance Methods 0.000 claims description 8
- 238000007599 discharging Methods 0.000 claims description 4
- 239000012530 fluid Substances 0.000 claims 1
- 239000007788 liquid Substances 0.000 description 8
- 238000000034 method Methods 0.000 description 6
- 238000012544 monitoring process Methods 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 238000003760 magnetic stirring Methods 0.000 description 3
- 238000012423 maintenance Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 238000012864 cross contamination Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000009854 hydrometallurgy Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000002572 peristaltic effect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000005375 photometry Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
Abstract
The invention provides a multi-element online titration method and a device, wherein the multi-element online titration device comprises a sampling unit, a titration cup, a stirring unit and a heating unit; the light source is only one, and emits wavelengths corresponding to various elements to be detected respectively, and the detector is used for receiving detection light emitted by the light source and passing through the titration cup; one end of the first pipeline is communicated with the sampling pool, and the other end of the first pipeline is communicated with the titration cup; one end of the second pump is communicated with the titration cup, the other end of the second pump is communicated with a common end of the multi-channel direction-selecting valve, and the multi-channel direction-selecting valve is communicated with a plurality of containers. The invention has the advantages of low cost and the like.
Description
Technical Field
The invention relates to detection, in particular to a multi-element online titration method and device.
Background
At present, the on-line monitoring of reaction conditions and intermediate product components in the production process of industries such as hydrometallurgy, chemical industry and the like is a requirement of high-quality and high-efficiency modern production. In the process of monitoring process parameters, the temperature, the pressure, the flow speed and the like are easier to realize on-line monitoring, and are widely applied in the actual production process. However, the online monitoring process of the material components is complex, and the influence factors are many, but the method has wide application in actual production activities.
The traditional detection process of the material components in the industries of hydrometallurgy, chemical industry and the like is field sampling and laboratory analysis. The existing defects are high working strength and high difficulty; the monitoring data is lagged, the quality control of the process is not timely, and huge economic loss can be brought to the production process. At present, the online titration process can only realize online titration of single or few elements, and has low analysis speed and low monitoring integration level. In view of this, there is an urgent need to develop an online titration method that is simple, fast, highly integrated, and satisfies multi-element measurement.
Disclosure of Invention
In order to solve the defects in the prior art scheme, the invention provides a multi-element online titration method.
The invention aims at realizing the following technical scheme:
the multi-element online titration method comprises the following steps:
(A1) Adding a sample to be tested into the titration cup;
(A2) Adding a reagent and an indicator into the titration cup and stirring;
(A3) Adding excessive standard solution to make the solution in the titration cup develop color;
(A4) Only one light source emits detection light with different wavelengths corresponding to a plurality of elements to be detected, and the detection light passes through the solution in the titration cup to obtain the wavelength lambda of the detection light which is absorbed by the solution to be strongest 0 ；
(A5) Cleaning a titration cup, sampling from a sampling groove and adding the titration cup;
(A6) Adding a reagent and an indicator into the titration cup and stirring;
(A7) The light source emits a wavelength lambda 0 Continuously adding standard solution into the titration cup, recording initial absorbance A 0 And a continuously varying absorbance A;
(A8) Comparing the difference value |A 0 -a| and threshold a 1 If the difference value |A 0 -A| is greater than threshold A 1 Stopping adding the standard solution;
(A9) And obtaining the concentration or mass fraction of the sample to be detected according to the amount of the added standard solution.
The invention also aims to provide a multi-element online titration device for realizing the method, and the aim of the invention is realized through the following technical scheme:
the multi-element online titration device comprises a titration cup, a sampling unit, a stirring unit and a heating unit; the multi-element online titration apparatus further comprises:
the light source is only one and emits wavelengths respectively corresponding to a plurality of elements to be detected, and the detector is used for receiving detection light emitted by the light source and passing through the titration cup;
one end of the first pipeline is communicated with the sampling pool, and the other end of the first pipeline is communicated with the titration cup;
the system comprises a multichannel direction selecting valve and a second pump, wherein one end of the second pump is communicated with the titration cup, the other end of the second pump is communicated with a common end of the multichannel direction selecting valve, and the multichannel direction selecting valve is communicated with a plurality of containers.
Compared with the prior art, the invention has the following beneficial effects:
1. the cost is low;
only one light source is used, so that the on-line titration of a multi-element photometry can be simultaneously satisfied, the self-adaption of the light source is realized, and the required light source is switched according to a sample; the cost is low, the maintenance is simple, and the content of elements can be monitored in real time;
2. the maintenance period is long;
and part of the sample to be detected of the sampling pool is pumped out and returned to the sampling pool, so that a circulation loop is formed, high-concentration sample crystallization is prevented, and the maintenance period is prolonged.
Drawings
The present disclosure will become more readily understood with reference to the accompanying drawings. As will be readily appreciated by those skilled in the art: the drawings are only for illustrating the technical scheme of the present invention and are not intended to limit the scope of the present invention. In the figure:
FIG. 1 is a flow chart of a multi-element online titration method in accordance with an embodiment of the present invention;
FIG. 2 is a schematic diagram of the structure of a multi-element online titration apparatus in accordance with an embodiment of the present invention.
Detailed Description
Figures 1-2 and the following description depict alternative embodiments of the invention to teach those skilled in the art how to make and reproduce the invention. In order to teach the technical solution of the present invention, some conventional aspects have been simplified or omitted. Those skilled in the art will appreciate variations or alternatives derived from these embodiments that fall within the scope of the invention. Those skilled in the art will appreciate that the features described below can be combined in various ways to form multiple variations of the invention. Thus, the invention is not limited to the following alternative embodiments, but only by the claims and their equivalents.
Example 1:
fig. 1 schematically shows a flow chart of a multi-element online titration method according to an embodiment of the invention, as shown in fig. 1, comprising the steps of:
(A1) Adding a sample to be tested into the titration cup;
(A2) Adding a reagent and an indicator into the titration cup and stirring;
(A3) Adding excessive standard solution to make the solution in the titration cup develop color;
(A4) Only one light source emits detection light with different wavelengths corresponding to a plurality of elements to be detected, and the detection light passes through the solution in the titration cup to obtain the wavelength lambda of the detection light which is absorbed by the solution to be strongest 0 ；
(A5) Cleaning a titration cup, sampling from a sampling groove and adding the titration cup;
(A6) Adding a reagent and an indicator into the titration cup and stirring;
(A7) The light source emits a wavelength lambda 0 Continuously adding standard solution into the titration cup, recording initial absorbance A 0 And a continuously varying absorbance A;
(A8) Comparing the difference value |A 0 -a| and threshold a 1 If the difference value |A 0 -A| is greater than threshold A 1 Stopping adding the standard solution;
(A9) And obtaining the concentration or mass fraction of the sample to be detected according to the amount of the added standard solution.
In order to detect other samples to be detected and prevent cross contamination, the multi-element online titration method further comprises the following steps:
(A10) Discharging the solution in the titration cup, introducing the cleaning solution into the titration cup, stirring the cleaning solution, and discharging.
In order to prevent crystallization of the high concentration sample to be measured, further, a part of the sample to be measured extracted from the sample cell enters the titration cup and a part returns to the sample cell.
In order to sufficiently mix the plurality of liquids, further, in the step (A2), the solution in the titration cup is magnetically stirred at a stirring speed of 50-400r/min for 10s-5min.
Further, the light source adopts an LED for reducing cost and improving reliability.
FIG. 2 shows a schematic structural diagram of a multi-element online titration apparatus according to an embodiment of the present invention, as shown in FIG. 2, the multi-element online titration apparatus includes:
titration cup, stirring unit and heating unit, sampling unit, all of which are known in the art;
a light source 11 and a detector 12, wherein the light source is only one and emits wavelengths respectively corresponding to a plurality of elements to be detected, and the detector is used for receiving detection light emitted by the light source and passing through the titration cup;
one end of the first pipeline is communicated with the sampling pool, and the other end of the first pipeline is communicated with the titration cup;
the system comprises a multichannel direction selecting valve and a second pump, wherein one end of the second pump is communicated with the titration cup, the other end of the second pump is communicated with a common end of the multichannel direction selecting valve, and the multichannel direction selecting valve is communicated with a plurality of containers.
In order to prevent crystallization of the high-concentration sample to be measured, the multi-element online titration device further comprises:
and one end of the second pipeline is communicated with the sampling pool, and the other end of the second pipeline is communicated with the first pipeline at the downstream of the first pump.
In order to add other liquids into the titration cup, further, the multi-element online titration apparatus further comprises:
and one end of the third pump is communicated with the titration cup, and the other end of the third pump is communicated with the container.
In order to prevent cross contamination between liquids, further, the multi-channel selector valve communicates with the reagent container and the cleaning liquid container, respectively, and the third pump communicates with the indicator container.
In order to reduce the cost and improve the reliability, further, the light source is an LED light source.
Example 2:
application example of the multi-element on-line titration method and apparatus according to embodiment 1 of the present invention.
In this application example, as shown in fig. 2, the first pump is a peristaltic pump, and the second and third pumps are syringe pumps; the multi-channel direction selecting valve is communicated with a plurality of reagent containers and cleaning liquid containers, and the third pump is communicated with an indicator container; the output end of the first pump is communicated with the sampling pool through a second pipeline; a switching module, such as a three-way valve, for selectively connecting the fifth pump to the first pump and the pure water container; the second pump adopts a syringe pump and is communicated with the titration cup; the fourth pump adopts a peristaltic pump and is communicated with the titration cup;
the LED is adopted as only one light source, and the wavelength of the emitted detection light corresponds to various elements to be detected; the stirring unit adopts a magnetic stirring module, and the titration cup is placed on the heating unit.
The multi-element online titration method provided by the embodiment of the invention comprises the following steps of:
(A1) The switching module works, and the fifth pump is communicated with the first pump; the first pump and the fifth pump work, a sample to be detected in the sampling pool passes through the first pipeline and the first pump, then part of the sample to be detected enters the titration cup through the fifth pump, and part of the sample to be detected returns to the sampling pool through the second pipeline;
(A2) The switching module works, the fifth pump is communicated with the pure water container, pure water sequentially passes through the switching module and the fifth pump and enters the titration cup to dilute a sample to be tested;
the second pump and the multi-channel direction selecting valve work to send the reagent into the titration cup;
the third pump works, an indicator is added into the titration cup, the magnetic stirring module works, the sample to be tested and other solutions are uniformly mixed, the stirring speed is 50-400r/min, and the time is 10s-5min;
(A3) Adding excessive standard solution to make the solution in the titration cup develop color;
(A4) The only one light source (LED) emits detection light with different wavelengths corresponding to a plurality of elements to be detected respectively, the detection light passes through the solution in the titration cup, and the detector receives the detection light passing through the solution in the titration cup, thereby obtaining the wavelength lambda of the detection light which is absorbed by the solution (the elements to be detected) to the strongest 0 Different elements to be measured correspond to different wavelengths lambda 0 ；
(A5) Cleaning a titration cup, sampling from a sampling groove and adding the titration cup;
(A6) Adding a reagent and an indicator into the titration cup and stirring;
(A7) The light source emits a wavelength lambda 0 Continuously adding standard solution into the titration cup, recording initial absorbance A 0 And a continuously varying absorbance A; the multi-channel direction selecting valve and the second pump send the standard solution into the titration cup;
(A8) Comparing the difference value |A 0 -a| and threshold a 1 If the difference value |A 0 -A| is greater than threshold A 1 Stopping adding the standard solution;
(A9) Obtaining the concentration of the sample to be detected according to the amount of the added standard solution, wherein the specific calculation mode is the prior art;
(A10) A fourth pump works to discharge the solution in the titration cup;
the second pump and the multi-channel direction selecting valve work, cleaning liquid enters the titration cup, the magnetic stirring module stirs the cleaning liquid in the titration cup and discharges the cleaning liquid, the stirring speed is 50-400r/min, and the stirring time is 10s-5min;
repeatedly cleaning for multiple times until the cleaning is clean.
Claims (10)
1. The multi-element online titration method comprises the following steps:
(A1) Adding a sample to be tested into the titration cup;
(A2) Adding a reagent and an indicator into the titration cup and stirring;
(A3) Adding excessive standard solution to make the solution in the titration cup develop color;
(A4) Only one light source emits detection light with different wavelengths corresponding to a plurality of elements to be detected, and the detection light passes through the solution in the titration cup to obtain the wavelength lambda of the detection light which is absorbed by the solution to be strongest 0 ；
(A5) Cleaning a titration cup, sampling from a sampling groove and adding the titration cup;
(A6) Adding a reagent and an indicator into the titration cup and stirring;
(A7) The light source emits a wavelength lambda 0 Continuously adding standard solution into the titration cup, recording initial absorbance A 0 And a continuously varying absorbance A;
(A8) Comparing the differenceAnd threshold A 1 If the difference->Greater than threshold A 1 Stopping adding the standard solution;
(A9) And obtaining the concentration or mass fraction of the sample to be detected according to the amount of the added standard solution.
2. The multi-element online titration method of claim 1, further comprising the steps of:
(A10) Discharging the solution in the titration cup, introducing the cleaning solution into the titration cup, stirring the cleaning solution, and discharging.
3. The multi-element on-line titration method of claim 1, wherein a portion of the sample to be tested that is drawn from the sample cell enters the titration cup and a portion returns to the sample cell.
4. The multi-element online titration method according to claim 1, wherein in step (A2), the solution in the titration cup is magnetically stirred at a stirring speed of 50-400r/min for 10s-5min.
5. The multi-element online titration method of claim 1, wherein the light source employs LEDs.
6. A multi-element online titration apparatus for implementing the multi-element online titration method of any of claims 1-5, the multi-element online titration apparatus comprising a sampling unit, a titration cup, a stirring unit, and a heating unit; the multi-element online titration device is characterized by further comprising:
the light source is only one and emits wavelengths respectively corresponding to a plurality of elements to be detected, and the detector is used for receiving detection light emitted by the light source and passing through the titration cup;
one end of the first pipeline is communicated with the sampling pool, and the other end of the first pipeline is communicated with the titration cup;
the system comprises a multichannel direction selecting valve and a second pump, wherein one end of the second pump is communicated with the titration cup, the other end of the second pump is communicated with a common end of the multichannel direction selecting valve, and the multichannel direction selecting valve is communicated with a plurality of containers.
7. The multi-element online titration apparatus of claim 6, further comprising:
and one end of the second pipeline is communicated with the sampling pool, and the other end of the second pipeline is communicated with the first pipeline at the downstream of the first pump.
8. The multi-element online titration apparatus of claim 6, further comprising:
and one end of the third pump is communicated with the titration cup, and the other end of the third pump is communicated with the container.
9. The multi-element online titration apparatus of claim 8, wherein the multi-channel directional valve communicates with the reagent container and the cleaning fluid container, respectively, and the third pump communicates with the indicator container.
10. The multi-element online titration apparatus of claim 6, wherein the light source is an LED light source.
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| CN202011614084.XA CN112666160B (en) | 2020-12-31 | 2020-12-31 | Multi-element online titration method and device |
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| CN202011614084.XA CN112666160B (en) | 2020-12-31 | 2020-12-31 | Multi-element online titration method and device |
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| CN112666160B true CN112666160B (en) | 2024-03-29 |
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| CN113514458A (en) * | 2021-06-15 | 2021-10-19 | 杭州谱育科技发展有限公司 | Online detection device and method based on automatic titration |
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|---|---|---|---|---|
| CN101294907A (en) * | 2008-06-17 | 2008-10-29 | 聚光科技（杭州）有限公司 | Water quality on-line monitoring method and system |
| JP2009075019A (en) * | 2007-09-21 | 2009-04-09 | Dkk Toa Corp | Titration apparatus |
| CN101806715A (en) * | 2010-04-28 | 2010-08-18 | 复旦大学 | Variable-volume microfluidic chip for colorimetric assay |
| CN105352955A (en) * | 2015-09-30 | 2016-02-24 | 王竞 | Spectrophotometric method liquid analysis method and apparatus |
| CN109060786A (en) * | 2018-08-25 | 2018-12-21 | 成都凯天电子股份有限公司 | Measure the detection method of industrial wastewater sulfuric acid concentration content |
| CN112041675A (en) * | 2018-04-09 | 2020-12-04 | 埃科莱布美国股份有限公司 | Method and multiple analyte titration system for colorimetric endpoint detection |
-
2020
- 2020-12-31 CN CN202011614084.XA patent/CN112666160B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009075019A (en) * | 2007-09-21 | 2009-04-09 | Dkk Toa Corp | Titration apparatus |
| CN101294907A (en) * | 2008-06-17 | 2008-10-29 | 聚光科技（杭州）有限公司 | Water quality on-line monitoring method and system |
| CN101806715A (en) * | 2010-04-28 | 2010-08-18 | 复旦大学 | Variable-volume microfluidic chip for colorimetric assay |
| CN105352955A (en) * | 2015-09-30 | 2016-02-24 | 王竞 | Spectrophotometric method liquid analysis method and apparatus |
| CN112041675A (en) * | 2018-04-09 | 2020-12-04 | 埃科莱布美国股份有限公司 | Method and multiple analyte titration system for colorimetric endpoint detection |
| CN109060786A (en) * | 2018-08-25 | 2018-12-21 | 成都凯天电子股份有限公司 | Measure the detection method of industrial wastewater sulfuric acid concentration content |
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