CN220671363U - Analytical equipment of direct titration nitric acid concentration by acid-base indicator method - Google Patents
Analytical equipment of direct titration nitric acid concentration by acid-base indicator method Download PDFInfo
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- CN220671363U CN220671363U CN202322127095.0U CN202322127095U CN220671363U CN 220671363 U CN220671363 U CN 220671363U CN 202322127095 U CN202322127095 U CN 202322127095U CN 220671363 U CN220671363 U CN 220671363U
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- detector
- optical fiber
- nitric acid
- reaction cavity
- fiber
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- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 229910017604 nitric acid Inorganic materials 0.000 title claims abstract description 29
- 238000004448 titration Methods 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 19
- 239000002696 acid base indicator Substances 0.000 title claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 39
- 239000013307 optical fiber Substances 0.000 claims abstract description 31
- 238000001514 detection method Methods 0.000 abstract description 15
- 230000035945 sensitivity Effects 0.000 abstract description 3
- 238000004458 analytical method Methods 0.000 abstract description 2
- 239000000835 fiber Substances 0.000 abstract 6
- 239000007788 liquid Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 31
- 239000003513 alkali Substances 0.000 description 8
- 239000012086 standard solution Substances 0.000 description 7
- ZXJXZNDDNMQXFV-UHFFFAOYSA-M crystal violet Chemical compound [Cl-].C1=CC(N(C)C)=CC=C1[C+](C=1C=CC(=CC=1)N(C)C)C1=CC=C(N(C)C)C=C1 ZXJXZNDDNMQXFV-UHFFFAOYSA-M 0.000 description 6
- 150000002500 ions Chemical class 0.000 description 6
- 229910002007 uranyl nitrate Inorganic materials 0.000 description 5
- 229910052770 Uranium Inorganic materials 0.000 description 4
- 238000000605 extraction Methods 0.000 description 4
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 230000000873 masking effect Effects 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000003086 colorant Substances 0.000 description 2
- 239000011550 stock solution Substances 0.000 description 2
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- WYICGPHECJFCBA-UHFFFAOYSA-N dioxouranium(2+) Chemical compound O=[U+2]=O WYICGPHECJFCBA-UHFFFAOYSA-N 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000002572 peristaltic effect Effects 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000012780 transparent material Substances 0.000 description 1
- -1 uranyl ions Chemical class 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The utility model discloses an analysis device for directly titrating nitric acid concentration by an acid-base indicator method, which belongs to the technical field of nitric acid concentration detection, wherein a reaction cavity is arranged in the detector, a reflector is arranged in the detector and positioned at one side of the reaction cavity, the mirror surface of the reflector faces the reaction cavity, the transmitting end of the first fiber is obliquely fixed on the side wall of the detector, the other end of the first fiber is connected with the light source, the receiving end of the second fiber is obliquely fixed on the side wall of the detector, the other end of the second fiber is connected with the photocell, and the transmitting end of the first fiber and the receiving end of the second fiber are symmetrical with each other about the normal plane of the reflector. The light generated by the light source enters the reaction cavity through the transmitting end of the first optical fiber, passes through the liquid to be detected, and enters the photocell from the receiving end of the second optical fiber through the reflection of the reflector, and the titration detection of the nitric acid concentration is realized by utilizing different potentials generated by the sensitivity of the photocell to different visible lights.
Description
Technical Field
The utility model belongs to the technical field of nitric acid concentration detection, and particularly relates to an analysis device for directly titrating nitric acid concentration by an acid-base indicator method.
Background
In the current nuclear grade uranium product processing, a high-concentration uranium solution TBP extraction refining process is adopted, nitric acid acidity in the extraction stock solution is an important process control parameter in the process, and has important influence on the blending nitric acid consumption of the extraction stock solution and the uranium extraction rate in the process. A common method for detecting the concentration of nitric acid in the uranium dissolution process in the prior art is a titration method, wherein the titration end point is indicated according to the color change of an indicator, and then the concentration of nitric acid is calculated according to the indicator. However, in the prior art, the color change of the titration end point is judged according to the naked eyes of a person, after the color change, the naked eyes of the person react slowly, and then the indicator is continuously added in the process of stopping the addition of the indicator, so that the calculation result of the concentration of the nitric acid is finally affected inaccurately.
Chinese patent (CN 204613114U) discloses a concentration detection device for acetylene clean waste sulfuric acid, the technical scheme shows a titration device, a pH value detection device is utilized to replace an acid-base indicator in a traditional acid-base indicator chromogenic titration method, the specific structure and principle of the pH value detection device are not given in the technical scheme, and the pH value detection device is not known in the field. It is highly desirable for those skilled in the art to propose an analytical device for improving the accuracy of nitric acid concentration detection for a chromogenic titration method.
Disclosure of Invention
In view of the above, the present utility model provides an analyzer for directly titrating nitric acid concentration by an acid-base indicator method, which is used for solving the above problems.
In order to achieve the above purpose, the present utility model adopts the following technical scheme:
an analytical device for directly titrating nitric acid concentration by an acid-base indicator method, comprising: the detector is provided with a reaction cavity, the reflector is arranged in the detector and positioned on one side of the reaction cavity, the mirror surface of the reflector faces the reaction cavity, the emitting end of the first optical fiber is obliquely fixed on the side wall of the detector, the other end of the first optical fiber is connected with the light source, the receiving end of the second optical fiber is obliquely fixed on the side wall of the detector, the other end of the second optical fiber is connected with the photocell, and the emitting end of the first optical fiber and the receiving end of the second optical fiber are symmetrical with respect to the normal plane of the reflector.
Further, the detector also comprises a magnetic stirrer, wherein the magnetic stirrer stretches into the reaction cavity and is arranged at the bottom end of the detector.
Further, the detector is provided with a solution inlet and a solution outlet, and the solution inlet and the solution outlet are communicated with the reaction cavity.
Further, the detector and the reaction chamber are cylindrical.
The utility model has the beneficial effects that:
the method comprises the steps that light irradiates a solution to be detected in a reaction cavity in real time at the emitting end of a first optical fiber, the light enters from the receiving end of a second optical fiber after being reflected by a reflecting mirror, enters a photocell through the second optical fiber, titrates an alkali standard solution into the reaction cavity, the color in the reaction cavity changes at the titration end point, the sensitivity of the photocell to visible light of different colors generates different electromotive forces, and the characteristic of the photocell is utilized to realize accurate detection of nitric acid concentration; after the magnetic stirrer can drop the indicator into the reaction cavity, the reaction of the alkali standard solution and nitric acid in the solution to be detected is quickened, the indicator is monitored timely to change in color, the concentration of nitric acid at the titration end point is accurately determined, and the detection efficiency and the detection precision are improved.
Drawings
In order to more clearly illustrate the embodiments of the present utility model or the technical solutions in the prior art, the drawings that are required to be used in the embodiments or the description of the prior art will be briefly described below, and it is obvious that the drawings in the following description are only embodiments of the present utility model, and that other drawings can be obtained according to the provided drawings without inventive effort for a person skilled in the art.
Fig. 1 is a schematic structural diagram of an analyzer for directly titrating nitric acid concentration by an acid-base indicator method.
Fig. 2 is a top view of the detector.
Wherein, in the figure:
10-detector, 11-reaction chamber, 12-solution inlet and outlet, 20-reflector, 30-first optical fiber, 31-transmitting end, 40-second optical fiber, 41-receiving end, 50-light source, 60-photocell and 70-magnetic stirrer.
Detailed Description
The following description of the embodiments of the present utility model will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present utility model, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the utility model without making any inventive effort, are intended to be within the scope of the utility model.
Referring to FIGS. 1-2, the present utility model provides an analyzer for directly titrating nitric acid concentration by an acid-base indicator method, comprising: the detector 10 is made of transparent materials, the reflector 20 is arranged in the detector 10 and positioned on one side of the reaction cavity 11, the mirror surface of the reflector 20 faces the reaction cavity 11, the transmitting end 31 of the first optical fiber 30 is obliquely fixed on the side wall of the detector 10, the other end of the first optical fiber 30 is connected with the light source 50, the receiving end 41 of the second optical fiber 40 is obliquely fixed on the side wall of the detector 10, the other end of the second optical fiber 40 is connected with the photocell 60, and the transmitting end 31 of the first optical fiber 30 and the receiving end 41 of the second optical fiber 40 are symmetrical with respect to the normal plane of the reflector 20. The light source 50 generates visible light, the light continuously irradiates the solution to be detected in the reaction cavity 11 from the emitting end 31 in real time through the first optical fiber 30, the light enters from the receiving end 41 of the second optical fiber 40 after being reflected by the reflecting mirror, and enters the photocell 60 through the second optical fiber 40; the alkali standard solution is titrated into the reaction cavity 11, the color in the reaction cavity 11 changes at the titration end point, the electromotive force generated by the sensitivity of the photocell 60 to the visible light with different colors is different, the use amount of the alkali standard solution at the titration end point is determined by utilizing the characteristic of the photocell 60, the concentration of nitric acid is calculated, and the detection result of the concentration of nitric acid is accurate.
The preferred embodiment further comprises a magnetic stirrer 70, wherein the magnetic stirrer 70 stretches into the reaction cavity 11 and is arranged at the bottom end of the detector 10, the magnetic stirrer 70 can accelerate the reaction of the alkali standard solution and nitric acid in the solution to be detected after the indicator is dripped into the reaction cavity 11, the indicator is timely monitored to change in color, the concentration of nitric acid at the titration end point is accurately determined, and the detection efficiency and the detection accuracy are improved.
In a preferred embodiment, the detector 10 is provided with a solution inlet and outlet 12, the solution inlet and outlet 12 is communicated with the reaction cavity 11, the solution to be detected is pumped into the reaction cavity 11 from the solution inlet and outlet 12 by using a peristaltic pump in the prior art, and after the detection is finished, the mixed solution of the solution to be detected and the indicator is discharged from the solution inlet and outlet 12.
In a preferred embodiment, the detector 10 and the reaction chamber 11 are cylindrical.
Examples
In addition to nitric acid, the solution contains a large amount of uranyl nitrate ions, which are ions that are easy to hydrolyze, and the existence of the uranyl nitrate ions affects titration to a certain extent, so that the uranyl nitrate ions are often masked by adding a large amount of masking agent, otherwise, data are large because the uranyl ions consume alkali. If the pH of the solution is greater than 3, it is possible that the uranyl ion will hydrolyze (hydrolysis will produce H+ ions, thereby affecting the measurement of the nitric acid concentration in the solution).
In this embodiment, no masking agent is added, the solution is titrated by using an alkali solution, the pH value of the titration end point is controlled to be not more than 3, the use of the masking agent can be reduced, and methyl violet is used as a tool for indicating the titration end point.
Methyl violet has three color-changing ranges.
Methyl violet first color range: the pH value is 0.13-0.5, and the color changes from yellow to green.
Second range of methyl violet: the pH value is 1.0-1.5, and the color is changed from green to blue.
Third range of methyl violet: pH2.0-3.0, the color changes from blue to purple.
The solution to be detected is pumped into the reaction chamber 11 from the solution inlet and outlet 12 of the detector 10, a proper amount of water sample is taken, and the water sample is added with the methyl violet indicator and mixed and then added into the reaction chamber 11. The light source 50 is turned on, so that the visible light generated by the light source 50 irradiates the solution to be detected in the reaction cavity 11 continuously in real time from the emitting end 31 through the first optical fiber 30, and the light enters from the receiving end 41 of the second optical fiber 40 after being reflected by the reflecting mirror and enters the photocell 60 through the second optical fiber 40. Titration of the base standard solution into the reaction chamber 11 with a titration apparatus until the indicator changes from green (yellow of uranyl nitrate solution + blue of indicator) to black (or grey) (yellow of uranyl nitrate solution + purple of indicator) indicates that the titration endpoint is reached. During the titration process, the magnetic stirrer 70 continuously stirs the solution in the reaction chamber 11, accelerating the chemical reaction. The concentration of H+ ions in the solution can be calculated through the consumption of the alkali standard solution and the sampling amount of the water sample to be detected, and the concentration of nitric acid in the solution can be calculated. The photocell 60 is able to detect the change in electromotive force caused by the abrupt change in the solution from green to black (or gray) and thus determine that the titration endpoint is reached.
In the present specification, each embodiment is described in a progressive manner, and each embodiment is mainly described in a different point from other embodiments, and identical and similar parts between the embodiments are all enough to refer to each other. For the device disclosed in the embodiment, since it corresponds to the method disclosed in the embodiment, the description is relatively simple, and the relevant points refer to the description of the method section.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present utility model. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the utility model. Thus, the present utility model is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (4)
1. An analytical device for directly titrating nitric acid concentration by an acid-base indicator method, comprising: the detector is provided with a reaction cavity, the reflector is arranged in the detector and positioned on one side of the reaction cavity, the mirror surface of the reflector faces the reaction cavity, the emitting end of the first optical fiber is obliquely fixed on the side wall of the detector, the other end of the first optical fiber is connected with the light source, the receiving end of the second optical fiber is obliquely fixed on the side wall of the detector, the other end of the second optical fiber is connected with the photocell, and the emitting end of the first optical fiber and the receiving end of the second optical fiber are symmetrical with respect to the normal plane of the reflector.
2. The apparatus according to claim 1, further comprising a magnetic stirrer extending into the reaction chamber and mounted at the bottom end of the detector.
3. The device for analyzing the concentration of nitric acid by direct titration with an acid-base indicator according to claim 1, wherein the detector is provided with a solution inlet and a solution outlet, and the solution inlet and the solution outlet are communicated with the reaction chamber.
4. The apparatus according to claim 1, wherein the detector and the reaction chamber are cylindrical.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202322127095.0U CN220671363U (en) | 2023-08-09 | 2023-08-09 | Analytical equipment of direct titration nitric acid concentration by acid-base indicator method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202322127095.0U CN220671363U (en) | 2023-08-09 | 2023-08-09 | Analytical equipment of direct titration nitric acid concentration by acid-base indicator method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN220671363U true CN220671363U (en) | 2024-03-26 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202322127095.0U Active CN220671363U (en) | 2023-08-09 | 2023-08-09 | Analytical equipment of direct titration nitric acid concentration by acid-base indicator method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN220671363U (en) |
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2023
- 2023-08-09 CN CN202322127095.0U patent/CN220671363U/en active Active
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