CN114371165B - Method for detecting silicon dioxide content in high-chroma and reductive wastewater - Google Patents

Method for detecting silicon dioxide content in high-chroma and reductive wastewater Download PDF

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CN114371165B
CN114371165B CN202210001771.7A CN202210001771A CN114371165B CN 114371165 B CN114371165 B CN 114371165B CN 202210001771 A CN202210001771 A CN 202210001771A CN 114371165 B CN114371165 B CN 114371165B
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silicon dioxide
solution
wastewater
color development
chroma
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CN114371165A (en
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刘欢
吕晓辉
朱丽清
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Hangzhou Enpr Environmental Technology Co ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N21/78Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W10/00Technologies for wastewater treatment
    • Y02W10/30Wastewater or sewage treatment systems using renewable energies
    • Y02W10/37Wastewater or sewage treatment systems using renewable energies using solar energy

Abstract

The invention discloses a method for detecting the content of silicon dioxide in high-chroma and reductive wastewater, which comprises the following steps: and (3) an acidification step: taking water samples such as domestic sewage, landfill leachate or sewage with over-high concentration and dilutable concentration, and the like, adding a sulfuric acid solution with a certain concentration into a conical flask for acidification, and oxidizing: adding ammonium persulfate solution, shaking, heating and boiling the water sample for 5 minutes under an acidic condition, oxidizing and decomposing the original interference components such as reducing substances, color-developing substances and the like in the water sample by utilizing the oxidizing property of the ammonium persulfate, cooling the water sample to room temperature for volume setting, thereby shielding various color-developing interference in the wastewater, and transferring the water sample to a plastic beaker after volume setting. The invention shields the interference of high-interference wastewater such as domestic sewage, landfill leachate or diluted sewage with high concentration and the like with high chromaticity and reducing substances, so compared with the traditional silicon-molybdenum blue color development method, the added operation steps are simple and convenient, and the detection conditions are easy to control.

Description

Method for detecting silicon dioxide content in high-chroma and reductive wastewater
Technical Field
The invention relates to the technical field of silicon dioxide detection, in particular to a method for detecting the content of silicon dioxide in high-chromaticity and reducing wastewater.
Background
At present, the detection of silicon dioxide in water is mainly aimed at water samples with poor water quality such as industrial wastewater, domestic sewage and the like, when the silicon dioxide content is detected by adopting a silicomolybdenum blue spectrophotometry in GBT12149-2017 industrial circulating cooling water and determination of silicon in boiler water, larger errors and interference can be brought by higher chromaticity and turbidity of the water sample in the color development process, most of sewage contains higher-concentration sulfide and other reducing substances, silicomolybdenum yellow and phosphomolybdenum Huang Hui generated during the addition of ammonium molybdate are immediately reduced into silicomolybdenum blue and phosphomolybdenum blue, and the phosphomolybdenum blue cannot be removed by tartaric acid or oxalic acid, so that the interference of the phosphorus content cannot be shielded, and accurate detection results are difficult to obtain, therefore, the detection of the silicon dioxide content in the wastewater and the method have complex operation steps, difficult control of detection conditions, poor repeatability and low accuracy of detection results.
Disclosure of Invention
In order to solve the problems in the background art, the invention aims to provide a method for detecting the content of silicon dioxide in high-chroma and reductive wastewater, which has the advantages of accurate and efficient detection results and solves the problems of low accuracy of the detection results of the method and the detection results of the method, complex operation steps, difficult control of detection conditions and poor repeatability.
In order to achieve the above purpose, the present invention provides the following technical solutions: a method for detecting the content of silicon dioxide in high-chroma and reductive wastewater comprises the following steps:
and (3) an acidification step: taking water samples such as domestic sewage, landfill leachate or sewage with over-high concentration and dilutable concentration and the like, adding sulfuric acid solution with certain concentration into a conical flask for acidification;
an oxidation step: adding ammonium persulfate solution, shaking uniformly, heating and boiling a water sample for 5 minutes under an acidic condition, oxidizing and decomposing original reducing substances, chromogenic substances and other interference components in the water sample by utilizing the oxidizing property of ammonium persulfate, cooling the water sample to room temperature for constant volume, thereby shielding various chromogenic interference in wastewater, and transferring the water sample to a plastic beaker after constant volume;
and (3) color development: transferring the sample with fixed volume into a plastic beaker, adding 1ml of hydrochloric acid solution and 2ml of ammonium molybdate solution for color development for 8 minutes, adding 3ml of tartaric acid solution for 5 minutes, adding 2ml of 1-amino-2 naphthol-4 sulfonic acid solution for color development for 10 minutes, adding a color development agent for color development, and measuring absorbance at 640nm by using a 1cm cuvette;
standard curve making step: and (3) using a silica standard solution as a standard curve, wherein the steps are the same as the color development step, and the silica content in the water sample is calculated by adopting a standard curve method.
Preferably, in the acidification step, the conical flask is a transparent flask with scales, and the user can conveniently observe the volume inside the conical flask through the scales on the conical flask.
As a preferable mode of the invention, in the oxidation step, the ammonium persulfate solution and domestic sewage, landfill leachate or sewage with over-high concentration and dilutable concentration are stirred through a glass rod, so that the ammonium persulfate solution and the wastewater are uniformly mixed together.
As the preferred color development step, the plastic beaker is a transparent plastic beaker, and the domestic sewage with constant volume, garbage percolate or the diluted sewage with too high concentration and ammonium persulfate solution can be clearly observed through the transparent plastic beaker.
As the preferred method, the step of preparing the silica is carried out, the numerical value calculated by adopting the standard curve method for the silica content in the water sample is expressed by an electronic report, and the content of the silica is known in a clear report expression form.
As a preferable mode of the invention, the concentration of sulfuric acid in the acidification step is 0.5mol/L, and the sulfuric acid concentration is 0.5mol/L, so that the acidification step can be fully mixed with domestic sewage, landfill leachate or sewage with over-high concentration and dilutable concentration, and the oxidizing property of ammonium persulfate is enhanced by utilizing the acidity of sulfuric acid solution.
As a preferable mode of the invention, the concentration of the ammonium persulfate is 20 g/L-50 g/L, the addition amount is 2 ml-5 ml, the ammonium persulfate is prepared and added according to the strong interference degree, and the acid solution and the ammonium persulfate solution are added first, boiled and then developed.
As a preferred embodiment of the present invention, the 1ml hydrochloric acid solution is 1+1 hydrochloric acid, 2ml ammonium molybdate solution is 75g/L ammonium molybdate solution, 3ml tartaric acid solution is 200g/L tartaric acid solution, and 1-amino-2-naphthol-4-sulfonic acid solution is prepared by dissolving 0.75g of 1-amino-2-naphthol-4-sulfonic acid in 100ml aqueous solution containing 3.5g of sodium sulfite, adding the solution to 300ml aqueous solution containing 45g of sodium bisulfite, and fixing the volume to 500ml.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the invention, through setting the acidification step, the oxidation step and the color development step, the interference of higher chromaticity and reducing substances in domestic sewage, landfill leachate or high-interference wastewater such as wastewater with high concentration and dilution is shielded, so that compared with the traditional silicon-molybdenum blue color development method, the method has the advantages of simple and direct operation steps, easy control of detection conditions, good repeatability and higher accuracy, and can realize batch detection in a laboratory with lower detection cost under the condition of no advanced precision equipment, and under the condition of ensuring precision and accuracy, thereby achieving the advantages of accurate and high efficiency of detection results, and solving the problems of low accuracy rate of detection results, complex operation steps, difficult control of detection conditions and poor repeatability of the silicon dioxide content in the wastewater.
Detailed Description
The following description will clearly and fully describe the technical solutions of the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
A method for detecting the content of silicon dioxide in high-chroma and reductive wastewater comprises the following steps:
and (3) an acidification step: transferring 10ml of domestic sewage into a 150ml conical flask, adding 15ml of deionized water, and then adding 1ml of sulfuric acid solution and 5ml of ammonium persulfate solution;
an oxidation step: adding 5ml of ammonium persulfate solution into a conical flask, shaking uniformly, boiling for 5 minutes on an electric furnace, taking down, cooling to room temperature, fixing the volume of the residual solution to 50ml, and transferring to a plastic beaker;
and (3) color development: then adding 1ml of hydrochloric acid solution and 2ml of ammonium molybdate solution into a plastic beaker for color development for 8 minutes, adding 3ml of tartaric acid solution for 5 minutes, then adding 2ml of 1-amino-2 naphthol-4 sulfonic acid solution for color development for 10 minutes, and measuring absorbance at 640nm by using a 1cm cuvette;
standard curve making step: taking 0.00ml (blank), 1.00ml, 2.00ml, 4.00ml, 6.00ml, 8.00ml and 10.00ml of standard solutions (corresponding to the silica contents of 0.00mg, 0.01mg, 0.02mg, 0.04mg, 0.06mg, 0.08mg and 0.10 mg) respectively from 10mg/L of silica standard solution, fixing the volume to 50ml, transferring the standard solutions into a plastic beaker, repeating the acidification step, the oxidation step and the color development step, measuring the absorbance as an ordinate, drawing a standard curve with the silica mass as an abscissa, and calculating a regression equation;
the absorbance of the measured sample is brought into a silicon dioxide regression equation, the mass of silicon dioxide in the water sample is calculated, and the mass is divided by the sampling volume to obtain the concentration of the silicon dioxide in the sample;
and then, 5 groups of domestic sewage with different points are taken, the acidification step, the oxidation step and the color development step are repeated, each group of water samples are repeatedly detected for 6 times, and the content of silicon dioxide in the detected samples is as follows:
table 1: silicon dioxide detection precision test meter
As can be seen from Table 1, the standard deviation of the 5 groups of samples was less than 0.5, and the coefficient of variation was less than 2%. The data show that the detection method provided by the invention has good detection precision aiming at the detection method of the silicon dioxide content in high-chroma and reductive domestic sewage, has small dispersion of detection results, and can meet the precision requirement of the silicon dioxide content detection.
Example two
A method for detecting the content of silicon dioxide in high-chroma and reductive wastewater comprises the following steps:
and (3) an acidification step: taking 2ml of landfill leachate into a 150ml conical flask, adding 20ml of deionized water, and adding 1ml of sulfuric acid solution;
an oxidation step: adding 5ml of ammonium persulfate solution into a conical flask, shaking uniformly, boiling for 5 minutes on an electric furnace, taking down, cooling to room temperature, fixing the volume of the residual solution to 50ml, and transferring to a plastic beaker;
and (3) color development: then adding 1ml of hydrochloric acid solution and 2ml of ammonium molybdate solution into a plastic beaker for color development for 8 minutes, adding 3ml of tartaric acid solution for 5 minutes, then adding 2ml of 1-amino-2 naphthol-4 sulfonic acid solution for color development for 10 minutes, and measuring absorbance at 640nm by using a 1cm cuvette;
the adding step: 2ml of the landfill leachate obtained in the acidification step and the oxidation step (repeated extraction) was transferred to a 150ml conical flask, 5ml of a 10mg/L silica standard solution (corresponding to a silica content of 0.05 mg) was added, 20ml of deionized water was added, 1ml of sulfuric acid solution and 5ml of ammonium persulfate solution were added, and the conical flask was placed on an electric furnace to boil for 5 minutes and then cooled to room temperature. The residual solution is transferred to a plastic beaker after the volume is fixed to 50ml, and the color development step is repeated to obtain the measured absorbance which is the absorbance after the standard addition;
the silica is used as a table step: bringing the absorbance of the sample measured in the color development step and the adding step into a silicon dioxide regression equation, and calculating the mass of silicon dioxide in the water sample, wherein the data measured in the color development step are data before adding the standard, and the data measured in the adding step are data after adding the standard;
the addition step was repeated 6 times and the data obtained after the addition of the 6 groups of silica were measured as follows:
table 2: silicon dioxide detection accuracy test meter
As can be seen from Table 2, the standard recovery rate of the method is between 95% and 105%, the RSD (relative standard deviation) of the method is 2.41%, and the data indicate that the detection method provided by the invention has high detection accuracy and small deviation aiming at the silicon dioxide content in the high-chroma and reductive landfill leachate, and can meet the accuracy requirement of laboratory detection.
Example III
A method for detecting the content of silicon dioxide in high-chroma and reductive wastewater comprises the following steps:
and (3) an acidification step: taking a certain amount of diluted sample with too high concentration, sampling, transferring to a 150ml conical flask, adding a proper amount of deionized water, and adding 1ml of sulfuric acid solution and 5ml of ammonium persulfate solution;
an oxidation step: placing the conical flask on an electric furnace, boiling for a few minutes, taking down, cooling to room temperature, fixing the volume of the residual solution to 50ml, and transferring to a plastic beaker;
and (3) color development: then adding 1ml of hydrochloric acid solution and 2ml of ammonium molybdate solution into a plastic beaker for color development for 8 minutes, adding 3ml of tartaric acid solution for 5 minutes, then adding 2ml of 1-amino-2 naphthol-4 sulfonic acid solution for color development for 10 minutes, and measuring absorbance at 640nm by using a 1cm cuvette;
the silica is used as a table step: taking samples of different points of different types, repeating an acidification step, an oxidation step and a color development step to measure the corresponding absorbance postity, introducing the absorbance postity into a silica regression equation, calculating the mass of silica in a water sample, and dividing the mass by a sampling volume to obtain the concentration of the silica in the sample;
each sample was tested in 6 replicates and 5 different high interference wastewater silica content data were measured as follows:
table 3: silicon dioxide detection applicability test meter
As can be seen from Table 3, the method provided by the invention has high adaptability to different types of high-chroma and reductive wastewater, and the detection results SD (standard deviation) and RSD (relative standard deviation) of the content of silicon dioxide in the dilutable wastewater are all smaller than 0.7, respectively.
It is noted that relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (7)

1. A method for detecting the content of silicon dioxide in high-chroma and reductive wastewater is characterized by comprising the following steps: the method comprises the following steps:
and (3) an acidification step: taking domestic sewage, landfill leachate or a sewage water sample with over-high concentration diluted into a conical flask, and adding a sulfuric acid solution with a certain concentration for acidification;
an oxidation step: adding ammonium persulfate solution, shaking uniformly, heating and boiling a water sample for 5 minutes under an acidic condition, using the oxidizing property of ammonium persulfate to oxidize and decompose original reducing substances and color-developing substance interference components in the water sample, cooling the water sample to room temperature for constant volume, thereby shielding various color-developing interferences in the wastewater, and transferring the water sample to a plastic beaker after constant volume;
and (3) color development: transferring the sample with fixed volume into a plastic beaker, adding 1ml of hydrochloric acid solution and 2ml of ammonium molybdate solution for color development for 8 minutes, adding 3ml of tartaric acid solution for 5 minutes, adding 2ml of 1-amino-2 naphthol-4 sulfonic acid solution for color development for 10 minutes, adding a color development agent for color development, and measuring absorbance at 640nm by using a 1cm cuvette;
standard curve making step: and respectively taking 0.00ml (blank), 1.00ml, 2.00ml, 4.00ml, 6.00ml, 8.00ml and 10.00ml of standard solutions (corresponding to the silicon dioxide contents of 0.00mg, 0.01mg, 0.02mg, 0.04mg, 0.06mg, 0.08mg and 0.10 mg) from 10mg/L of silicon dioxide standard solution to 50ml, transferring the standard solutions into a plastic beaker, repeating the acidification step, the oxidation step and the color development step, measuring the absorbance as an ordinate, drawing a standard curve with the silicon dioxide mass as an abscissa, calculating a regression equation, bringing the absorbance of the measured sample into the silicon dioxide regression equation, calculating the mass of silicon dioxide in a water sample, and dividing the mass by the sampling volume to obtain the concentration of the silicon dioxide in the sample.
2. The method for detecting the content of silicon dioxide in high-chroma and reductive wastewater according to claim 1, which is characterized in that: the acidification step, the conical flask is a transparent flask with scales, and the user can observe the capacity inside the conical flask conveniently through the scales on the conical flask.
3. The method for detecting the content of silicon dioxide in high-chroma and reductive wastewater according to claim 1, which is characterized in that: and in the oxidation step, the ammonium persulfate solution is uniformly shaken by a glass rod, and the ammonium persulfate solution, domestic sewage, landfill leachate or sewage with over-high concentration after dilution are stirred by the glass rod, so that the ammonium persulfate solution and the wastewater are uniformly mixed together.
4. The method for detecting the content of silicon dioxide in high-chroma and reductive wastewater according to claim 1, which is characterized in that: the color development step is that the plastic beaker is a transparent plastic beaker, and the transparent plastic beaker is used for carrying out color development.
5. The method for detecting the content of silicon dioxide in high-chroma and reductive wastewater according to claim 1, which is characterized in that: the concentration of sulfuric acid in the acidification step is 0.5mol/L, and the sulfuric acid is fully mixed with domestic sewage, landfill leachate or sewage with over-high concentration dilution.
6. The method for detecting the content of silicon dioxide in high-chroma and reductive wastewater according to claim 1, which is characterized in that: the concentration of ammonium persulfate in the oxidation step is 20 g/L-50 g/L, and the addition amount is 2 ml-5 ml.
7. The method for detecting the content of silicon dioxide in high-chroma and reductive wastewater according to claim 1, which is characterized in that: in the color development step, 1ml of hydrochloric acid solution is 1+1 hydrochloric acid, 2ml of ammonium molybdate solution is 75g/L of ammonium molybdate solution, 3ml of tartaric acid solution is 200g/L of tartaric acid solution, and 1-amino-2-naphthol-4-sulfonic acid solution is prepared by dissolving 0.75g of 1-amino-2-naphthol-4-sulfonic acid in 100ml of aqueous solution containing 3.5g of sodium sulfite, adding the solution into 300ml of aqueous solution containing 45g of sodium bisulfite, and fixing the volume to 500ml.
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