CN116973324A - System and method for measuring trace silicon content in pure water - Google Patents
System and method for measuring trace silicon content in pure water Download PDFInfo
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- CN116973324A CN116973324A CN202310890663.4A CN202310890663A CN116973324A CN 116973324 A CN116973324 A CN 116973324A CN 202310890663 A CN202310890663 A CN 202310890663A CN 116973324 A CN116973324 A CN 116973324A
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 54
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 39
- 239000010703 silicon Substances 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 54
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 40
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000011347 resin Substances 0.000 claims abstract description 36
- 229920005989 resin Polymers 0.000 claims abstract description 36
- 239000002211 L-ascorbic acid Substances 0.000 claims abstract description 20
- 235000000069 L-ascorbic acid Nutrition 0.000 claims abstract description 20
- 235000018660 ammonium molybdate Nutrition 0.000 claims abstract description 20
- 239000011609 ammonium molybdate Substances 0.000 claims abstract description 20
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims abstract description 20
- 229940010552 ammonium molybdate Drugs 0.000 claims abstract description 20
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 20
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 20
- 239000003480 eluent Substances 0.000 claims abstract description 17
- 230000002572 peristaltic effect Effects 0.000 claims description 61
- GALOTNBSUVEISR-UHFFFAOYSA-N molybdenum;silicon Chemical compound [Mo]#[Si] GALOTNBSUVEISR-UHFFFAOYSA-N 0.000 claims description 38
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- 229910052750 molybdenum Inorganic materials 0.000 claims description 5
- 239000011733 molybdenum Substances 0.000 claims description 5
- 230000001105 regulatory effect Effects 0.000 claims description 3
- 238000005259 measurement Methods 0.000 claims 3
- 238000002835 absorbance Methods 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/405—Concentrating samples by adsorption or absorption
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
Landscapes
- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a system and a method for measuring trace silicon content in pure water, wherein an outlet of a water sample input pipeline is communicated with an inlet of a first reactor after being connected with an outlet of a hydrochloric acid input pipeline through a pipeline, an outlet of an ammonium molybdate input pipeline is communicated with an inlet of a first reactor, an outlet of the first reactor is communicated with an inlet of a resin column, an outlet of an eluent NaOH input pipeline is communicated with an inlet of the resin column, an outlet of a reducing agent L-ascorbic acid input pipeline is communicated with an inlet of a second reactor after being connected with an outlet of the resin column through a pipeline, an outlet of the second reactor is communicated with an inlet of a detector, and an outlet of the detector is communicated with a drainage pipeline.
Description
Technical Field
The invention relates to a measuring system and a measuring method, in particular to a measuring system and a measuring method for trace silicon content in pure water.
Background
In the supervision of the water vapor quality of modern high-parameter steam power equipment, the monitoring of silicon in the negative bed effluent, mixed bed effluent, refined effluent, boiler feed water and saturated steam is of great importance. The silicon content in the water vapor is qualified or not, the safe and economic operation of the steam power equipment is directly affected, the silicate exceeding the standard in the steam is combined with sodium hydroxide, the generated silicate can be deposited in a middle pressure cylinder and a low pressure cylinder of a superheater and a steam turbine, the deposit is insoluble in water, hard in texture, difficult to remove and extremely strong in corrosiveness, the thermodynamic equipment is directly damaged, and the efficiency and the reliability of the steam turbine are seriously affected.
Therefore, on-line monitoring of trace silicon in a water vapor system is indispensable, and an instrument capable of accurately and rapidly measuring trace silicon can definitely bring guarantee to safe and economical operation of a power plant. But the existing domestic program type silicon meter has low analysis speed and low accuracy, and can not meet the requirements of the high-parameter unit of the current power system. The foreign import instrument has complex structure and higher manufacturing cost, the electromagnetic valve is easy to be blocked by dirt, and the application effect of the electric power system is poor.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a system and a method for measuring the trace silicon content in pure water, which can measure the trace silicon content in the pure water and have the characteristics of low cost, high accuracy and high detection efficiency.
In order to achieve the aim, the invention discloses a measuring system for the trace silicon content in pure water, which comprises a water sample input pipeline, a hydrochloric acid input pipeline, a first reactor, an ammonium molybdate input pipeline, a resin column, an eluent NaOH input pipeline, a reducing agent L-ascorbic acid input pipeline, a second reactor, a detector and a drainage pipeline;
the outlet of the water sample input pipeline is communicated with the inlet of the first reactor after being connected with the outlet of the hydrochloric acid input pipeline through a pipeline, the outlet of the ammonium molybdate input pipeline is communicated with the inlet of the first reactor, the outlet of the first reactor is communicated with the inlet of the resin column, the outlet of the eluent NaOH input pipeline is communicated with the inlet of the resin column, the outlet of the reducing agent L-ascorbic acid input pipeline is communicated with the inlet of the second reactor after being connected with the outlet of the resin column through a pipeline, the outlet of the second reactor is communicated with the inlet of the detector, and the outlet of the detector is communicated with the drainage pipeline.
The outlet of the water sample input pipeline is communicated with the inlet of the first peristaltic pump, the outlet of the hydrochloric acid input pipeline is communicated with the inlet of the second peristaltic pump, and the outlet of the first peristaltic pump and the outlet of the second peristaltic pump are communicated with the inlet of the first reactor after being connected through a pipeline.
The outlet of the ammonium molybdate input pipeline is communicated with the inlet of the first reactor through a third peristaltic pump.
The outlet of the eluent NaOH input pipeline is communicated with the inlet of the resin column through a fourth peristaltic pump.
The outlet of the reducing agent L-ascorbic acid input pipeline is communicated with the inlet of a fifth peristaltic pump, and the outlet of the fifth peristaltic pump is communicated with the inlet of the second reactor after being connected with the outlet of the resin column through the pipeline.
The peristaltic pump also comprises a time program controller which is connected with the first peristaltic pump, the second peristaltic pump, the third peristaltic pump, the fourth peristaltic pump and the fifth peristaltic pump.
The outlet of the first reactor is communicated with the inlet of the resin column through a silicon-molybdenum yellow input pipeline.
The outlet of the second reactor is communicated with the inlet of the detector through a silicon-molybdenum blue input pipeline.
The invention discloses a method for measuring the content of trace silicon in pure water, which comprises the following steps:
1) Mixing the hydrochloric acid output by the hydrochloric acid input pipeline with the pure water sample output by the water sample input pipeline, regulating the pH value of the pure water sample to 1.1-1.3 by the hydrochloric acid, and then entering the first reactor;
2) The ammonium molybdate solution output by the ammonium molybdate input pipeline enters the first reactor;
3) The pure water sample reacts with ammonium molybdate solution in a first reactor to generate silicon-molybdenum yellow, and the silicon-molybdenum yellow output by the first reactor 5 is input into a resin column and is enriched in the resin column;
4) After the preset time of the silicon-molybdenum Huang Fuji, the eluent NaOH is input into a pipeline to output the eluent NaOH into a resin column, and the silicon-molybdenum yellow enriched on the resin column is eluted;
5) The eluted silicon molybdenum yellow enters a second reactor, a reducing agent L-ascorbic acid output by a reducing agent L-ascorbic acid input pipeline enters the second reactor, the silicon molybdenum yellow reacts with the reducing agent L-ascorbic acid in the second reactor under the citric acid environment to generate silicon molybdenum blue, and then the silicon molybdenum blue is sent into a detector, and the silicon content is detected by the detector;
6) And calculating the trace silicon content of the pure water sample according to the silicon content detected by the detector.
The invention has the following beneficial effects:
when the system and the method for measuring the trace silicon content in the pure water are specifically operated, the pure water sample and the ammonium molybdate solution are used for generating the silicon-molybdenum yellow, then the silicon-molybdenum yellow is enriched in the resin column, after the silicon-molybdenum yellow enriched on the resin column is enriched for a period of time, the silicon-molybdenum yellow is eluted through the eluent NaOH, the reducing agent L-ascorbic acid is reacted with the silicon-molybdenum yellow to generate the silicon-molybdenum blue, and then the detector is used for detecting the silicon content, so that the trace silicon content of the pure water sample is calculated, and the detection accuracy and the detection efficiency are higher, the structure is simpler, and the cost is lower.
Drawings
Fig. 1 is a structural diagram of the present invention.
Wherein, 1 is a water sample input pipeline, 2 is a hydrochloric acid input pipeline, 3 is an ammonium molybdate input pipeline, 41 is a first peristaltic pump, 42 is a second peristaltic pump, 43 is a third peristaltic pump, 5 is a first reactor, 6 is a silico-molybdenum yellow input pipeline, 7 is a time program controller, 8 is a resin column, 91 is a fourth peristaltic pump, 92 is a fifth peristaltic pump, 10 is an eluent NaOH input pipeline, 11 is a reducing agent L-ascorbic acid input pipeline, 12 is a second reactor, 13 is a silico-molybdenum blue input pipeline, and 14 is a detector.
Detailed Description
In order to make the present invention better understood by those skilled in the art, the following description will clearly and completely describe the technical solutions in the embodiments of the present invention with reference to the accompanying drawings, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments, but not intended to limit the scope of the present disclosure. In addition, in the following description, descriptions of well-known structures and techniques are omitted so as not to unnecessarily obscure the concepts of the present disclosure. All other embodiments, which can be made by those skilled in the art based on the embodiments of the present invention without making any inventive effort, shall fall within the scope of the present invention.
In the accompanying drawings, there is shown a schematic structural diagram in accordance with a disclosed embodiment of the invention. The figures are not drawn to scale, wherein certain details are exaggerated for clarity of presentation and may have been omitted. The shapes of the various regions, layers and their relative sizes, positional relationships shown in the drawings are merely exemplary, may in practice deviate due to manufacturing tolerances or technical limitations, and one skilled in the art may additionally design regions/layers having different shapes, sizes, relative positions as actually required.
Referring to fig. 1, the measuring system for trace silicon content in pure water according to the present invention comprises a water sample input pipe 1, a hydrochloric acid input pipe 2, an ammonium molybdate input pipe 3, a first peristaltic pump 41, a second peristaltic pump 42, a third peristaltic pump 43, a first reactor 5, a silico-molybdenum yellow input pipe 6, a time program controller 7, a resin column 8, a fourth peristaltic pump 91, a fifth peristaltic pump 92, an eluent NaOH input pipe 10, a reducing agent L-ascorbic acid input pipe 11, a second reactor 12, a silico-molybdenum blue input pipe 13 and a detector 14;
the outlet of the water sample input pipeline 1 is communicated with the inlet of a first peristaltic pump 41, the outlet of a hydrochloric acid input pipeline 2 is communicated with the inlet of a second peristaltic pump 42, the outlet of an ammonium molybdate input pipeline 3 is communicated with the inlet of a third peristaltic pump 43, the outlet of the first peristaltic pump 41 is communicated with the inlet of a first reactor 5 after being connected with the outlet of the second peristaltic pump 42 through a pipeline, the outlet of the third peristaltic pump 43 is communicated with the inlet of the first reactor 5, the outlet of the first reactor 5 is communicated with the inlet of a resin column 8 through a silicon molybdenum yellow input pipeline 6, the outlet of an eluent NaOH input pipeline 10 is communicated with the inlet of the resin column 8 through a fourth peristaltic pump 91, the outlet of a reducing agent L-ascorbic acid input pipeline 11 is communicated with the inlet of a fifth peristaltic pump 92, the outlet of the fifth peristaltic pump 92 is communicated with the inlet of a second reactor 12 after being connected with the outlet of the resin column 8 through a pipeline, the outlet of the second reactor 12 is communicated with the inlet of a detector 14 through a silicon molybdenum blue input pipeline 13, and the outlet of the detector 14 is communicated with the drain pipeline.
The time program controller 7 is connected to the first peristaltic pump 41, the second peristaltic pump 42, the third peristaltic pump 43, the fourth peristaltic pump 91 and the fifth peristaltic pump 92.
The method for measuring the trace silicon content in the pure water comprises the following steps of:
1) The hydrochloric acid output by the hydrochloric acid input pipeline 2 is mixed with the pure water sample output by the first peristaltic pump 41 through the second peristaltic pump 42, the pH value of the pure water sample is regulated to be 1.1-1.3 through the hydrochloric acid, and then the pure water sample enters the first reactor 5;
2) The ammonium molybdate solution output from the ammonium molybdate input pipe 3 enters the first reactor 5 through the second peristaltic pump 42;
3) The pure water sample reacts with ammonium molybdate solution in a first reactor 5 to generate a yellow silicon-molybdenum complex, namely silicon-molybdenum yellow, and the silicon-molybdenum yellow output by the first reactor 5 is input into a resin column 8 through a silicon-molybdenum yellow input pipeline 6 and is enriched in the resin column 8;
4) After the preset time of the silicon molybdenum Huang Fuji, the eluent NaOH is output by the eluent NaOH input pipeline 10 and enters the resin column 8 through the fourth peristaltic pump 91, and the silicon molybdenum yellow enriched on the resin column 8 is eluted;
5) The eluted silicon molybdenum yellow enters the second reactor 12, the reducing agent L-ascorbic acid output by the reducing agent L-ascorbic acid input pipeline 11 enters the second reactor 12 through the fifth peristaltic pump 92, the silicon molybdenum yellow reacts with the reducing agent L-ascorbic acid in the second reactor 12 under the citric acid environment to generate silicon molybdenum blue, and then the silicon molybdenum blue is sent into the detector 14, and the silicon content is detected by the detector 14;
6) The trace silicon content of the pure water sample is calculated according to the detected silicon content by the detector 14.
The detector 14 measures the absorbance of the molybdenum-silicon blue at the wavelength 815nm using a spectrophotometer, and substitutes into the linear relation of the silicon content and the absorbance, where y=ax+b, y is the silicon content, x is the absorbance, a is a coefficient, and b is an intercept.
The first peristaltic pump 41, the second peristaltic pump 42, the third peristaltic pump 43, the fourth peristaltic pump 91 and the fifth peristaltic pump 92 are controlled to be intermittently started and stopped through the time program controller 7, so that the structure is simple, and the control is convenient.
Finally, it should be noted that: the above embodiments are only for illustrating the technical aspects of the present invention and not for limiting the same, and although the present invention has been described in detail with reference to the above embodiments, it should be understood by those of ordinary skill in the art that: modifications and equivalents may be made to the specific embodiments of the invention without departing from the spirit and scope of the invention, which is intended to be covered by the claims.
Claims (9)
1. The measuring system for the trace silicon content in the pure water is characterized by comprising a water sample input pipeline (1), a hydrochloric acid input pipeline (2), a first reactor (5), an ammonium molybdate input pipeline (3), a resin column (8), an eluent NaOH input pipeline (10), a reducing agent L-ascorbic acid input pipeline (11), a second reactor (12), a detector (14) and a drainage pipeline;
the outlet of the water sample input pipeline (1) is communicated with the inlet of the first reactor (5) after being connected with the outlet of the hydrochloric acid input pipeline (2) through a pipeline, the outlet of the ammonium molybdate input pipeline (3) is communicated with the inlet of the first reactor (5), the outlet of the first reactor (5) is communicated with the inlet of the resin column (8), the outlet of the eluent NaOH input pipeline (10) is communicated with the inlet of the resin column (8), the outlet of the reducing agent L-ascorbic acid input pipeline (11) is communicated with the inlet of the second reactor (12) after being connected with the outlet of the resin column (8) through a pipeline, the outlet of the second reactor (12) is communicated with the inlet of the detector (14), and the outlet of the detector (14) is communicated with the drainage pipeline.
2. The measurement system of trace silicon content in pure water according to claim 1, wherein the outlet of the water sample input pipeline (1) is communicated with the inlet of the first peristaltic pump (41), the outlet of the hydrochloric acid input pipeline (2) is communicated with the inlet of the second peristaltic pump (42), and the outlet of the first peristaltic pump (41) and the outlet of the second peristaltic pump (42) are communicated with the inlet of the first reactor (5) after passing through the pipeline.
3. A system for measuring the content of trace amounts of silicon in pure water according to claim 2, characterized in that the outlet of the ammonium molybdate input pipe (3) is in communication with the inlet of the first reactor (5) via a third peristaltic pump (43).
4. A system for measuring the trace silicon content in pure water according to claim 3, characterized in that the outlet of the eluent NaOH input conduit (10) is connected to the inlet of the resin column (8) via a fourth peristaltic pump (91).
5. The system for measuring the trace amount of silicon in pure water according to claim 4, wherein the outlet of the reducing agent L-ascorbic acid input pipe (11) is communicated with the inlet of a fifth peristaltic pump (92), and the outlet of the fifth peristaltic pump (92) is communicated with the inlet of the second reactor (12) after passing through the pipe and the outlet of the resin column (8).
6. The system for measuring the trace silicon content in pure water according to claim 5, further comprising a time program controller (7), wherein the time program controller (7) is connected with the first peristaltic pump (41), the second peristaltic pump (42), the third peristaltic pump (43), the fourth peristaltic pump (91) and the fifth peristaltic pump (92).
7. The system for measuring the trace amount of silicon in pure water according to claim 1, wherein the outlet of the first reactor (5) is communicated with the inlet of the resin column (8) through a silicon molybdenum Huang Shuru pipe (6).
8. The measurement system of the trace silicon content in pure water according to claim 1, characterized in that the outlet of the second reactor (12) is in communication with the inlet of the detector (14) via a silico-molybdenum blue input conduit (13).
9. A method for measuring the trace silicon content in pure water, characterized in that the measurement system based on the trace silicon content in pure water according to claim 1 comprises the following steps:
1) The hydrochloric acid output by the hydrochloric acid input pipeline (2) is mixed with the pure water sample output by the water sample input pipeline (1), the pH value of the pure water sample is regulated to be 1.1-1.3 by the hydrochloric acid, and then the pure water sample enters the first reactor (5);
2) The ammonium molybdate solution output by the ammonium molybdate input pipeline (3) enters the first reactor (5);
3) The pure water sample reacts with ammonium molybdate solution in a first reactor (5) to generate silicon-molybdenum yellow, and the silicon-molybdenum yellow output by the first reactor (5) is input into a resin column (8) and is enriched in the resin column (8);
4) After the preset time of the silicon molybdenum Huang Fuji, the eluent NaOH is output by an eluent NaOH input pipeline (10) and enters a resin column (8), and the silicon molybdenum yellow enriched on the resin column (8) is eluted;
5) The eluted silicon molybdenum yellow enters a second reactor (12), a reducing agent L-ascorbic acid output by a reducing agent L-ascorbic acid input pipeline (11) enters the second reactor (12), the silicon molybdenum yellow reacts with the reducing agent L-ascorbic acid in the second reactor (12) under the citric acid environment to generate silicon molybdenum blue, and then the silicon molybdenum blue is sent to a detector (14), and the silicon content is detected by the detector (14);
6) And calculating the trace silicon content of the pure water sample according to the silicon content detected by the detector (14).
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310826398 | 2023-07-06 | ||
| CN2023108263983 | 2023-07-06 |
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| Publication Number | Publication Date |
|---|---|
| CN116973324A true CN116973324A (en) | 2023-10-31 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202310890663.4A Pending CN116973324A (en) | 2023-07-06 | 2023-07-19 | System and method for measuring trace silicon content in pure water |
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| CN (1) | CN116973324A (en) |
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