CN110057642A - Online silicon table detection composition and preparation method thereof, online silicon table detection method - Google Patents
Online silicon table detection composition and preparation method thereof, online silicon table detection method Download PDFInfo
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- CN110057642A CN110057642A CN201910380713.8A CN201910380713A CN110057642A CN 110057642 A CN110057642 A CN 110057642A CN 201910380713 A CN201910380713 A CN 201910380713A CN 110057642 A CN110057642 A CN 110057642A
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- 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
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The present invention provides a kind of online silicon table detection compositions and preparation method thereof, online silicon table detection method.The online silicon table detection composition includes color developing agent, screening agent and reducing agent, wherein color developing agent is acidic ammonium molybdate solution comprising concentration is the H of the ammonium molybdate of 49.8~50.2g/L, 79.5~81.2g/L2SO4And the water of surplus；Screening agent is oxalic acid solution comprising concentration is the oxalic acid of 39.8~40.2g/L and the water of surplus；Reducing agent is l ferrous ammonium sulfate solution comprising concentration is the H of the iron ammonium sulfate of 19.8~20.2g/L, 22.1~22.6g/L2SO4And the water of surplus.Outsourcing medicament is replaced to detect for online silicon table using the composition, accuracy is higher, and efficiently solves the problems, such as that outsourcing reagent cost is high, and can guarantee the bringing normally into operation of silicon table, improves the efficiency of thermal power plant's water quality detection and the continuity of associated production.
Description
Technical field
The present invention relates to thermal power plant's technical field of chemical detection, in particular to a kind of online silicon table detection combination
Object and preparation method thereof, online silicon table detection method.
Background technique
With the continuous development in thermal power plant, high parameter, large capacity unit have become the mainstream of thermal power generation, it is right
The requirement of water and steam quality is increasingly strict, and chemical supervision becomes increasingly conspicuous in the status of thermal power plant and effect.Thermal power plant's chemistry is supervised at present
The situation superintended and directed is based on On-line monitor, supplemented by manual alignment.The operational percentage and qualification rate of chemical in-line meter, which have become, to be commented
The important indicator of each power plant chemistry supervision situation of valence.The performance of chemical in-line meter is not only embodied in selection function admirable
Meter, it is also important that later maintenance.Reliable technical maintenance is the important leverage of chemical instruments long-term safety stable operation.
The silicate in thermal power plant's water quality, total-phosphorus detection are mainly detected using online silicon table at present.However, because of silicon
Table medication is the password drug that producer provides, and dosage is big, material supply is slow, and frequently resulting in water process silicon table can not normally throw
With, and cost is also higher.
Summary of the invention
The main purpose of the present invention is to provide a kind of online silicon table detection compositions and preparation method thereof, online silicon table
Detection method, to solve the online silicon medicine administered to bring out the cold agent of thermal power plant in the prior art because influencing caused by dosage is big and producer's supply not in time
Silicon table normally comes into operation the problem excessively high with cost.
To achieve the goals above, according to an aspect of the invention, there is provided a kind of online silicon table detects and uses composition,
It includes color developing agent, screening agent and reducing agent, wherein color developing agent is acidic ammonium molybdate solution comprising concentration be 49.8~
The H of the ammonium molybdate of 50.2g/L, 79.5~81.2g/L2SO4And the water of surplus；Screening agent is oxalic acid solution comprising concentration is
The oxalic acid of 39.8~40.2g/L and the water of surplus；Reducing agent is l ferrous ammonium sulfate solution comprising concentration is 19.8~20.2g/
The H of the iron ammonium sulfate of L, 22.1~22.6g/L2SO4And the water of surplus.
Further, acidic ammonium molybdate solution includes the H that concentration is the ammonium molybdate of 50g/L, 81.14g/L2SO4And surplus
Water；Oxalic acid solution includes the water of the oxalic acid that concentration is 40g/L and surplus；L ferrous ammonium sulfate solution includes the sulphur that concentration is 20g/L
The H of sour ferrous ammonium, 22.54g/L2SO4And the water of surplus.
Further, the water in acidic ammonium molybdate solution, oxalic acid solution and reducing agent is demineralized water.
Further, the volume ratio between color developing agent, screening agent and reducing agent is 3:(2.99~3.02): (1.99~
2.02)。
Further, the volume ratio between color developing agent, screening agent and reducing agent is 3:3:2.
According to another aspect of the present invention, a kind of preparation method of online silicon table detection composition is additionally provided, is wrapped
It includes:
S1 is added a part of water in marking graduated container according to the ratio, the concentrated sulfuric acid is added dropwise in water with dropper；Then
Container is cooled to room temperature, ammonium molybdate is added, stirring supplements another part water, obtains acidic ammonium molybdate solution to after dissolving,
Namely color developing agent；
S2 is added a part of water in marking graduated container according to the ratio, oxalic acid is added under the state that is stirred continuously, until
Another part water is added after dissolution, obtains oxalic acid solution namely screening agent；
S3 is added a part of water in marking graduated container according to the ratio, ferrous sulfate is added under the state that is stirred continuously
The concentrated sulfuric acid is added dropwise in water until container is placed in cold bath after dissolution with dropper by ammonium, after being cooled to room temperature, is added
Another part water obtains l ferrous ammonium sulfate solution namely reducing agent.
According to another aspect of the present invention, additionally provide a kind of online silicon table detection method, the silicon medicine administered to bring out the cold agent used for
Composition is used in above-mentioned online silicon table detection.
It further, should detection method includes the following steps: it is accurate to measure 100mL water sample to be measured, accurately added with pipette
Enter the color developing agent 3mL in online silicon table detection composition, is waited 5 minutes after shaking up, add after screening agent 3mL shakes up and wait
1 minute, reducing agent 2mL is ultimately joined, is waited 8 minutes after shaking up, it is dense using the activated silica in silicon table on-line checking water sample to be measured
Degree.
Online silicon table detection composition provided by the invention includes color developing agent, screening agent and reducing agent, wherein color developing agent
For acidic ammonium molybdate solution comprising concentration is the H of the ammonium molybdate of 49.8~50.2g/L, 79.5~81.2g/L2SO4And surplus
Water；Screening agent is oxalic acid solution comprising concentration is the oxalic acid of 39.8~40.2g/L and the water of surplus；Reducing agent is sulfuric acid
Ferrous ammonium salt solution comprising concentration is the H of the iron ammonium sulfate of 19.8~20.2g/L, 22.1~22.6g/L2SO4And surplus
Water.Using the composition replace outsourcing medicament for online silicon table detection, accuracy is higher, and efficiently solve outsourcing medicament at
This high problem, and can guarantee the bringing normally into operation of silicon table, improve the efficiency of thermal power plant's water quality detection and the company of associated production
Continuous property.
Specific embodiment
It should be noted that in the absence of conflict, the features in the embodiments and the embodiments of the present application can phase
Mutually combination.Below in conjunction with embodiment, the present invention will be described in detail.
As described in background technology part, the online silicon medicine administered to bring out the cold agent of thermal power plant is because dosage is big and producer supplies in the prior art
Normally coming into operation for silicon table should be will affect not in time, and reagent cost is excessively high.
To solve the above-mentioned problems, the present invention provides a kind of online silicon table detection compositions comprising color developing agent is covered
Cover agent and reducing agent, wherein color developing agent is acidic ammonium molybdate solution comprising concentration be 49.8~50.2g/L ammonium molybdate,
The H of 79.5~81.2g/L2SO4And the water of surplus；Screening agent is oxalic acid solution comprising concentration is the grass of 39.8~40.2g/L
The water of acid and surplus；Reducing agent is l ferrous ammonium sulfate solution comprising concentration be 19.8~20.2g/L iron ammonium sulfate,
The H of 22.1~22.6g/L2SO4And the water of surplus.
Outsourcing medicament is replaced to detect for online silicon table using the composition, accuracy is higher, and efficiently solves outsourcing
The high problem of reagent cost, and can guarantee the bringing normally into operation of silicon table, efficiency and the correlation for improving thermal power plant's water quality detection are raw
The continuity of production.It is highly preferred that acidic ammonium molybdate solution includes the H that concentration is the ammonium molybdate of 50g/L, 81.14g/L2SO4And it is remaining
The water of amount；Oxalic acid solution includes the water of the oxalic acid that concentration is 40g/L and surplus；L ferrous ammonium sulfate solution includes that concentration is 20g/L
Iron ammonium sulfate, 22.54g/L H2SO4And the water of surplus.Detection accuracy can be further increased in this way.
In a preferred embodiment, the water in acidic ammonium molybdate solution, oxalic acid solution and reducing agent is desalination
Water.Medicament is configured using demineralized water, micro salts substances in water is can be avoided and measurement is impacted.
In order to further increase test accuracy, in a preferred embodiment, color developing agent, screening agent and reducing agent
Between volume ratio be 3:(2.99~3.02): (1.99~2.02).It is highly preferred that between color developing agent, screening agent and reducing agent
Volume ratio be 3:3:2.
According to another aspect, the present invention also provides a kind of preparation method of above-mentioned online silicon table detection composition,
The following steps are included: S1, is added a part of water in marking graduated container according to the ratio, the concentrated sulfuric acid is added dropwise to water with dropper
In；Then container is cooled to room temperature, adds ammonium molybdate, stirring supplements another part water, obtain acid molybdic acid to after dissolving
Ammonium salt solution namely color developing agent；A part of water is added in marking graduated container according to the ratio in S2, adds under the state that is stirred continuously
Enter oxalic acid, until adding another part water after dissolution, obtains oxalic acid solution namely screening agent；S3 is indicating scale according to the ratio
Container in a part of water is added, iron ammonium sulfate is added under the state that is stirred continuously, until container is placed in cold water after dissolution
In bath, the concentrated sulfuric acid is added dropwise in water with dropper, after being cooled to room temperature, another part water is added, it is molten to obtain iron ammonium sulfate
Liquid namely reducing agent.
Easy to operate using the preparation method, safety, concentration is accurate, and obtained composition replaces outsourcing medicament to be used for
The detection of line silicon table, accuracy is higher, and efficiently solves the problems, such as that outsourcing reagent cost is high, and can guarantee the normal throwing of silicon table
Fortune, improves the efficiency of thermal power plant's water quality detection and the continuity of associated production.
According to another aspect of the present invention, additionally provide a kind of online silicon table detection method, the silicon medicine administered to bring out the cold agent used for
Composition is used in above-mentioned online silicon table detection.
It is specifically, above-mentioned that detection method includes the following steps: it is accurate to measure 100mL water sample to be measured, accurately added with pipette
Enter the color developing agent 3mL in the online silicon table detection composition, waited 5 minutes after shaking up, is added after screening agent 3mL shakes up
It waits 1 minute, ultimately joins reducing agent 2mL, waited 8 minutes after shaking up, utilize the activity in silicon table on-line checking water sample to be measured
Silicon concentration.
The application is described in further detail below in conjunction with specific embodiment, these embodiments should not be understood as limitation originally
Apply for range claimed.
Embodiment 1
The embodiment is prepared for online silicon table detection composition, specific as follows: color developing agent acidic ammonium molybdat: carving indicating
About 1500 milliliters of demineralized waters are added in the container of degree, with the 90 milliliters of concentrated sulfuric acid (H of addition that buret is careful2SO4Content is
98%, density 1.84g/cm3), then after the container is put into being cooled to room temperature in water-bath, 100 grams of ammonium molybdates are added, sufficiently stir
It mixes to being completely dissolved, is finally settled to 2 liters with demineralized water.Being equivalent to acidic ammonium molybdate solution includes the molybdic acid that concentration is 50g/L
The H of ammonium, 81.14g/L2SO4And the water of surplus.
Screening agent oxalic acid: about 1200 milliliters of demineralized waters are added in marking graduated container, are added under constant stirring
80 grams of oxalic acid add demineralized water and are diluted to 2 liters until being completely dissolved.Being equivalent to oxalic acid solution includes the grass that concentration is 40g/L
The water of acid and surplus.
Reducing agent iron ammonium sulfate: about 1200 milliliters of demineralized waters are added in marking graduated container, are stirred continuously down
40 grams of iron ammonium sulfates are added, until be completely dissolved, then the container are put into water-bath, with careful 25 milliliters of addition of buret
The concentrated sulfuric acid (H2SO4Content is 98%, density 1.84g/cm3), after solution is cooled to room temperature, demineralized water is added to be diluted to 2 liters.
Being equivalent to l ferrous ammonium sulfate solution includes the H that concentration is the iron ammonium sulfate of 20g/L, 22.54g/L2SO4And the water of surplus.
The composition is used for the silicon table on-line checking of chemistry water anion bed outlet Huo Niwei Lovell processed, it is specifically, accurate to measure
The color developing agent 3mL in online silicon table detection composition is accurately added with pipette for 100mL water sample to be measured, and 5 points are waited after shaking up
Clock adds after screening agent 3mL shakes up and waits 1 minute, ultimately join reducing agent 2mL, waits 8 minutes after shaking up, utilize silicon table
Active silicon concentration in on-line checking water sample to be measured.The result is as follows:
Table 1
It can be seen from the above description that the above embodiments of the present invention realized the following chievements:
Composition provided by the invention is detected for online silicon table, greatly reduces purchase medicine cost, it is important that improve
The operational percentage of online silicon table, provides safety guarantee for Water Treatment reliability service.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (8)
1. a kind of online silicon table detection composition, which is characterized in that the online silicon table detection composition include color developing agent,
Screening agent and reducing agent, wherein
The color developing agent is acidic ammonium molybdate solution comprising concentration is ammonium molybdate, the 79.5~81.2g/ of 49.8~50.2g/L
The H of L2SO4And the water of surplus；
The screening agent is oxalic acid solution comprising concentration is the oxalic acid of 39.8~40.2g/L and the water of surplus；
The reducing agent be l ferrous ammonium sulfate solution comprising concentration be 19.8~20.2g/L iron ammonium sulfate, 22.1~
22.6g/L H2SO4And the water of surplus.
2. online silicon table detection composition according to claim 1, which is characterized in that
The acidic ammonium molybdate solution includes the H that concentration is the ammonium molybdate of 50g/L, 81.14g/L2SO4And the water of surplus；
The oxalic acid solution includes the water of the oxalic acid that concentration is 40g/L and surplus；
The l ferrous ammonium sulfate solution includes the H that concentration is the iron ammonium sulfate of 20g/L, 22.54g/L2SO4And the water of surplus.
3. online silicon table detection composition according to claim 1, which is characterized in that the acidic ammonium molybdate solution,
Water in the oxalic acid solution and the reducing agent is demineralized water.
4. according to claim 1 to online silicon table detection composition described in 3, which is characterized in that the color developing agent described is covered
Covering the volume ratio between agent and the reducing agent is 3:(2.99~3.02): (1.99~2.02).
5. online silicon table detection composition according to claim 4, which is characterized in that the color developing agent, the masking
Volume ratio between agent and the reducing agent is 3:3:2.
6. the online silicon table detection preparation method of composition, feature described in a kind of any one of claims 1 to 5 exist
In,
S1 is added a part of water in marking graduated container according to the ratio, the concentrated sulfuric acid is added dropwise in water with dropper；Then will hold
Device is cooled to room temperature, and adds ammonium molybdate, and stirring supplements another part water, obtain acidic ammonium molybdate solution to after dissolving, namely
Color developing agent；
S2 is added a part of water in marking graduated container according to the ratio, oxalic acid is added under the state that is stirred continuously, until dissolution
After add another part water, obtain oxalic acid solution namely screening agent；
S3 is added a part of water in marking graduated container according to the ratio, iron ammonium sulfate is added under the state that is stirred continuously, directly
Container is placed in cold bath after to dissolution, the concentrated sulfuric acid is added dropwise in water with dropper, after being cooled to room temperature, another portion is added
Divide water, obtains l ferrous ammonium sulfate solution namely reducing agent.
7. a kind of online silicon table detection method, which is characterized in that the silicon medicine administered to bring out the cold agent that the detection method uses for claim 1 to
Composition is used in online silicon table detection described in any one of 5.
8. online silicon table detection method according to claim 7, which is characterized in that the detection method includes following step
It is rapid:
It is accurate to measure 100mL water sample to be measured, the color developing agent in the online silicon table detection composition is accurately added with pipette
3mL is waited 5 minutes after shaking up, and is added after screening agent 3mL shakes up and is waited 1 minute, reducing agent 2mL is ultimately joined, after shaking up etc.
To 8 minutes, the active silicon concentration in silicon table on-line checking water sample to be measured is utilized.
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Cited By (2)
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| CN111060499A (en) * | 2019-11-29 | 2020-04-24 | 河北冀研能源科学技术研究院有限公司 | On-line silicate surface anti-fouling and anti-blocking additive for thermal power plant |
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