CN111795884B - Fractionation treatment method for analysis of chemical wastewater soluble organic matters - Google Patents
Fractionation treatment method for analysis of chemical wastewater soluble organic matters Download PDFInfo
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Abstract
The invention discloses a fractionation treatment method for analysis of soluble organic matters in chemical wastewater. The processing method comprises the following steps: (1) Leaching the solid phase extraction column by methanol and then leaching by acidified ultrapure water to obtain a treated solid phase extraction column; (2) Injecting the pretreated chemical wastewater water sample into a solid phase extraction column for desalting treatment; (3) Removing water from the desalted solid phase extraction column, eluting with methanol to obtain an extract fraction and a raffinate fraction, uniformly dividing the raffinate fraction into two parts, adding MAX into one part of the raffinate fraction, eluting to obtain a first hydrophilic neutral fraction and a hydrophilic acidic fraction, adding MCX into the other part of the raffinate fraction, and eluting to obtain a second hydrophilic neutral fraction and a hydrophilic alkaline fraction; (4) measuring and analyzing each solid phase extracted component. The treatment method provided by the invention can be used for reserving and separating the strong polar components which are difficult to extract and reserve in the chemical wastewater DOM, so that the hierarchical separation and extraction of the chemical wastewater DOM are realized, and more comprehensive DOM composition information is obtained.
Description
Technical field:
the invention relates to the field of wastewater treatment, in particular to a fractionation treatment method for analyzing soluble organic matters in chemical wastewater.
The background technology is as follows:
the soluble organic matter (DOM) is a mixture of organic matters with very complex structure and composition, different polarity distribution and chemical property. As an important component of the global carbon cycle, it is widely distributed in all aquatic ecosystems such as rivers, lakes, marshes, groundwater, rainwater, sediments and pore water. Plays a very important role in various physical, chemical and biological processes of the surface ecological system, is an important chemical component in various environment mediums of the surface, and is an important way for circulating substances and energy in the ecological system. And a certain amount of soluble organic matters exist in the chemical wastewater, and the existence and composition of the soluble organic matters have important influence on the treatment process and the regeneration performance of the wastewater. Compositionally, soluble organic matter can be divided into Hydrophilic (HI) and Hydrophobic (HO) components, which contain some more hydrophilic organic acids, amino acids, carbohydrates, proteins, polysaccharides, and the like, in addition to the more hydrophobic humus. In addition, the natural organic matter component reacts with organic compounds in the chemical wastewater to form new compounds with changed properties, so that the composition of the new compounds is more complex and various.
Because of the differences in chemical properties and molecular structures, different components in DOM have great influence on migration, adsorption and conversion behaviors of organic pollutants. For example, studies have demonstrated that Hydrophobic (HPOA) and Hydrophilic (HPIA) acids in DOM are the major precursor species that produce the deleterious disinfection by-product Trihalomethane (THM). Therefore, the sub-component separation of components with different properties in the DOM and the analysis of the components are of great significance to the cognition of the DOM and the evaluation of the environmental impact of the DOM. In addition, the diversity and complexity of the overall DOM composition makes the current stage less well known about its composition and structure, mainly due to its incomplete isolation and extraction that makes it impossible to perform a comprehensive characterization analysis.
The traditional separation and extraction method for chemical wastewater DOM basically adopts the extraction method of natural water DOM, namely adopts the method of XAD resin, and the method is proposed by Leenheer and the like, is mainly based on the method of XAD and ion exchange resin, and can separate 6 components from natural water. However, the ionization of ESI is strongly affected by the inhibition of ionization of inorganic ions in each component, and thus it is important to separate DOM by solid phase extraction and to realize a rapid and convenient desalination method. Solid phase extraction has become a widely used method for extracting salt-free DOM from water, wherein the most commonly used method is C18 and PPL columns, which have a certain difference in extract selection. However, in general, due to the limitation of the polarity of the matrix of the solid phase extraction column, the separation method based on the polarity difference of different compounds in the mixture can effectively retain and separate the organic matters with weak polarity to medium polarity in the water body, but cannot effectively retain the compound with strong polarity. Therefore, the research on water soluble organic matters at the present stage mainly focuses on extractable hydrophobic components, and the deep knowledge of the components with strong hydrophilicity in DOM is lacking. Therefore, there is an urgent need for a fractionation extraction treatment method capable of aiming at the DOM of a water body, particularly the DOM of strong hydrophilicity.
The invention comprises the following steps:
aiming at the problems existing in the prior art, the invention provides a fractionation treatment method for analyzing the soluble organic matters of the chemical wastewater, breaks the limit of the conventional separation solid-phase extraction method on the retention of the polarity of the soluble organic matters of the chemical wastewater, and is hopeful to be an effective reduction of the complexity of DOM analysis of a water body and a fractionation pretreatment method for other water bodies by combining anion-cation exchange with polarity separation.
The invention provides a fractionation treatment method for analysis of soluble organic matters in chemical wastewater, which comprises the following steps:
(1) Eluting the solid phase extraction column with methanol, and eluting with acidified ultrapure water to obtain a treated solid phase extraction column;
(2) Injecting the pretreated chemical wastewater water sample into the solid phase extraction column treated in the step (1) for enrichment, and leaching the solid phase extraction column with ultrapure water for desalting treatment;
(3) Removing water from the desalted solid phase extraction column, eluting with methanol to obtain an extraction fraction (hydrophobic fraction) and a raffinate fraction, equally dividing the raffinate fraction into two parts, adding one part of the raffinate fraction into the mixed anion solid phase extraction column, adjusting pH=9.5-10.5, eluting with methanol with mass fraction of 100% to obtain a first hydrophilic neutral fraction, eluting with methanol with mass fraction of 4-6% of formic acid to obtain a hydrophilic acidic fraction, adding the other part of the raffinate fraction into the mixed cation solid phase extraction column, adjusting pH=1.5-2.5, eluting with methanol with mass fraction of 100% to obtain a second hydrophilic neutral fraction, and eluting with methanol with mass fraction of ammonium hydroxide to obtain a hydrophilic alkaline fraction;
(4) Mixing the obtained first hydrophilic neutral component and second hydrophilic neutral component, measuring the Total Organic Carbon (TOC) content of the hydrophilic neutral component, the hydrophilic acidic component and the hydrophilic alkaline component, drying the hydrophilic neutral component, the hydrophilic acidic component and the hydrophilic alkaline component by nitrogen, and then re-dissolving the hydrophilic neutral component, the hydrophilic acidic component and the hydrophilic alkaline component by methanol to obtain a sample for ESIFT-ICRMS analysis.
The method is characterized in that the method comprises the steps of carrying out secondary extraction on the soluble organic matters of the strong-polarity hydrophilic chemical wastewater which cannot be obtained by extraction through common polarity separation by using a method of polarity separation and ion exchange separation to obtain three additional components, namely hydrophilic acid component (HIA), hydrophilic neutral component (HIN) and hydrophilic alkaline component (HIB), and carrying out total organic carbon analysis (TOC) and anion Electrospray (ESI) Fourier transform ion cyclotron resonance mass spectrometry (FT-ICRMS) on the obtained components.
Preferably, the specific steps of step (1) are: and eluting the solid phase extraction column with methanol with the volume of which is three times that of the solid phase extraction column in advance, and eluting the solid phase extraction column with acidified ultrapure water with the pH=2 after being acidified by high-purity hydrochloric acid with the volume of which is three times that of the solid phase extraction column to obtain the treated solid phase extraction column.
Preferably, the pretreatment step of the pretreated chemical wastewater in the step (2) is as follows: filtering the chemical wastewater by a filter membrane with the aperture of 0.45 μm, and acidifying the filtered water sample by high-purity hydrochloric acid until the pH value is=2 to obtain a pretreated chemical wastewater water sample. Injecting the pretreated chemical wastewater water sample into the solid phase extraction column treated in the step (1) for enrichment, and leaching the solid phase extraction column with acidified water and ultrapure water for desalting treatment;
preferably, the specific steps of step (3) are: and (3) after the solid phase extraction column subjected to desalting treatment is dehydrated, eluting with methanol to obtain an extract fraction and a raffinate fraction, equally dividing the raffinate fraction into two parts, adding one part of the raffinate fraction into the mixed anion solid phase extraction column, adjusting the pH value to be 10, eluting with methanol with the mass fraction of 100% to obtain a first hydrophilic neutral fraction, eluting with methanol with the mass fraction of 5% of formic acid to obtain a hydrophilic acidic fraction, adding the other part of the raffinate fraction into the mixed cation solid phase extraction column, adjusting the pH value to be 2, eluting with methanol with the mass fraction of 100% to obtain a second hydrophilic neutral fraction, and eluting with methanol with the mass fraction of 5% of ammonium hydroxide to obtain a hydrophilic alkaline fraction.
Preferably, in step (3), a 2% ammonium hydroxide solution is used to adjust a portion of the raffinate ph=10.
Preferably, in step (3), the ph=2 of the other part of the raffinate is adjusted with a formic acid solution with a mass fraction of 2%.
The beneficial effects of the invention are as follows:
(1) The classification separation treatment method provided by the invention reveals the composition information of the DOM with strong hydrophilicity in the chemical wastewater, deepens the knowledge depth of DOM in the current stage, expands the research range of the composition of the water body, especially the chemical wastewater, and improves the understanding of organic matters of the water body. The method can break the limit of the conventional separation solid-phase extraction method on the retention of the polarity of the soluble organic matters in the chemical wastewater, and is hopeful to be a fractionation pretreatment method for other water bodies by combining anion-cation exchange with polarity separation to effectively reduce the complexity of DOM analysis of the water bodies.
(2) The fractionation treatment method provided by the invention can be used for retaining and separating the strong polar components which are difficult to extract and retain in the chemical wastewater DOM, and can be used for effectively analyzing and identifying the strong polar DOM by combining means of organic carbon analysis, anion electrospray Fourier transform ion cyclotron resonance mass spectrometry and the like, and the result shows that the recovery rate can be increased by 9.36%, the number of molecular formulas can be increased by 2275, and the molecular formulas can be increased by 62.62% compared with the traditional solid-phase extraction method.
(3) According to the fractionation treatment method provided by the invention, the pH condition of the extraction process is inspected and optimized, and the result proves that the pH condition selected by the method has the optimal extraction yield in a proper pH range.
Description of the drawings:
FIG. 1 is a flow chart of the combined solid phase extraction according to example 1 of the present invention;
FIG. 2 is a-ESIFT-ICRMS plot of the components of the combined solid phase extraction of example 1 of the present invention.
The specific embodiment is as follows:
the invention will be further elucidated with reference to specific examples. It should be understood that these examples are illustrative of the present invention and are not intended to limit the scope of the present invention. Modifications and adaptations of the invention that will occur to those skilled in the art in light of the present disclosure are intended to be within the scope of the invention.
The equipment and reagents used in the present invention are conventional commercially available products in the art, unless specifically indicated.
Example 1
In order to verify the influence of the pH value selected in the experiment, a plurality of experiments are carried out by selecting different pH values, and the method is specifically as follows:
as shown in fig. 1, a fractionation treatment method for analysis of soluble organic matters in chemical wastewater comprises the following steps:
(1) The solid phase extraction column (PPL column, 1g,6 mL) was rinsed with 20mL of methanol (LC-MS grade) in advance, and then rinsed with 20mL of acidified ultrapure water with ph=2 after acidification with high purity hydrochloric acid;
(2) Passing 50mL of chemical wastewater through a filter membrane with the aperture of 0.45 μm, acidifying the filtered water sample to pH=2 by using high-purity hydrochloric acid (the molar concentration of the hydrochloric acid is 1M), injecting the acidified water sample into a solid-phase extraction column, and passing the water sample through the column at the rate of 5mL/min (using a peristaltic pump or a negative pressure device and the like);
(3) Immediately after the water sample passes through the solid phase extraction column, eluting with 20mL of acidified ultrapure water with pH=2 after being acidified by high-purity hydrochloric acid, wherein the step is to remove the salt remained on the column; after the desalting treatment, completely removing the moisture in the column by nitrogen blowing;
(4) After nitrogen stripping, the organics were eluted with 10mL methanol (LC-MS grade) to give an extract fraction (i.e., hydrophobic in fig. 1) and a raffinate fraction; dividing the extract residual phase into two parts, respectively adding the two parts into MAX (500 mg,6 mL) and MCX (500 mg,6 mL) solid-phase extraction columns, respectively adjusting pH=9.5, 10 and 10.5 of the extract residual phase entering the MAX columns by adopting an ammonium hydroxide solution with the mass fraction of 2%, eluting by adopting 100% methanol to obtain a first hydrophilic neutral component during the final elution, and eluting by adopting methanol with the mass fraction of 5% formic acid to obtain a hydrophilic acidic component; for the raffinate entering the MCX column, formic acid solution with mass fraction of 2% is adopted to respectively adjust the pH=1.5, 2 and 2.5, and finally, 100% methanol is adopted for elution to obtain a second hydrophilic neutral fraction during elution, and then 5% methanol with mass fraction of ammonium hydroxide is adopted for elution to obtain a hydrophilic alkaline fraction;
mixing the obtained first hydrophilic neutral fraction and second hydrophilic neutral fraction, measuring the Total Organic Carbon (TOC) content of the hydrophilic neutral fraction, the hydrophilic acidic fraction and the hydrophilic alkaline fraction, and calculating the yield of DOM obtained by experiment. The yield results are shown in Table 1:
TABLE 1 total organic carbon yield (%)
From table 1, it can be derived that: the pH condition of the anion-cation exchange column selected by the invention is the condition with higher yield, and for the MAX column, the extraction yield of the hydrophilic acid component and the hydrophilic neutral component can be reduced due to too high or too low pH; likewise, too high or too low a pH for the MCX column will also affect the extraction yields of the hydrophilic alkaline fraction and the hydrophilic neutral fraction. Therefore, the pH conditions selected in the present invention are more suitable.
Example 2
As shown in fig. 1, a fractionation treatment method for analysis of soluble organic matters in chemical wastewater comprises the following steps:
(1) The solid phase extraction column (PPL column, 1g,6 mL) was rinsed with 20mL of methanol (LC-MS grade) in advance, and then rinsed with 20mL of acidified ultrapure water with ph=2 after acidification with high purity hydrochloric acid;
(2) Passing 50mL of chemical wastewater through a filter membrane with the aperture of 0.45 μm, acidifying the filtered water sample to pH=2 by using high-purity hydrochloric acid (the molar concentration of the hydrochloric acid is 1M), injecting the acidified water sample into a solid-phase extraction column, and passing the water sample through the column at the rate of 5mL/min (using a peristaltic pump or a negative pressure device and the like);
(3) Immediately after the water sample passes through the solid phase extraction column, eluting with 20mL of acidified ultrapure water with pH=2 after being acidified by high-purity hydrochloric acid, wherein the step is to remove the salt remained on the column; after the desalting treatment, completely removing the moisture in the column by nitrogen blowing;
(4) After nitrogen stripping, the organics were eluted with 10mL methanol (LC-MS grade) to give an extract fraction (i.e., hydrophobic in fig. 1) and a raffinate fraction; equally dividing the raffinate into two parts, respectively adding the two parts into a MAX (500 mg,6 mL) solid-phase extraction column and an MCX (500 mg,6 mL) solid-phase extraction column, adjusting pH=10 for the raffinate entering the MAX column by adopting an ammonium hydroxide solution with the mass fraction of 2%, eluting by adopting 100% methanol to obtain a first hydrophilic neutral fraction during the final elution, and eluting by adopting methanol with the mass fraction of 5% formic acid to obtain a hydrophilic acidic fraction; for the raffinate entering the MCX column, the pH=2 is adjusted by adopting a formic acid solution with the mass fraction of 2%, and finally, a second hydrophilic neutral fraction is obtained by adopting 100% methanol for elution, and then, a hydrophilic alkaline fraction is obtained by adopting 5% methanol for elution with the mass fraction of ammonium hydroxide;
mixing the obtained first hydrophilic neutral fraction and second hydrophilic neutral fraction, measuring the Total Organic Carbon (TOC) content of the hydrophilic neutral fraction, the hydrophilic acidic fraction and the hydrophilic alkaline fraction, drying the hydrophilic neutral fraction, the hydrophilic acidic fraction and the hydrophilic alkaline fraction by nitrogen, and re-dissolving the hydrophilic neutral fraction, the hydrophilic acidic fraction and the hydrophilic alkaline fraction by 5mL of methanol to obtain a sample for ESIFT-ICRMS analysis.
Comparative example 1
The same chemical wastewater is extracted by adopting a traditional solid phase extraction mode, and the steps are as follows:
(1) The solid phase extraction column (PPL column, 1g,6 mL) was rinsed with 20mL of methanol (LC-MS grade) in advance, and then rinsed with 20mL of acidified ultrapure water with ph=2 after acidification with high purity hydrochloric acid;
(2) Passing 50mL of chemical wastewater through a filter membrane with the aperture of 0.45 μm, acidifying the filtered water sample to pH=2 by using high-purity hydrochloric acid (the molar concentration of the hydrochloric acid is 1M), injecting the acidified water sample into a solid-phase extraction column, and passing the water sample through the column at the rate of 5mL/min (using a peristaltic pump or a negative pressure device and the like);
(3) Immediately eluting the water sample with 20mL of acidified ultrapure water with pH of 2 after being acidified by high-purity hydrochloric acid after passing through the solid phase extraction column, and then completely removing the water in the column by nitrogen blowing;
(4) After nitrogen purging, the organics were eluted with 10mL methanol (LC-MS grade) to give an extract fraction (hydrophobic fraction) and a raffinate fraction;
the Total Organic Carbon (TOC) content of each component of the solid phase extraction obtained in example 2 and comparative example 1 was measured while ESIFT-ICRMS analysis was performed on each component.
The organic carbon yields of the components of the combined solid phase extraction of example 2 and comparative example 1 are shown in Table 2. Example 2-ESIFT-ICRMS plot of the fractions from the combined solid phase extraction is shown in FIG. 1 and the statistics of the molecular formula identified for the fractions from the combined solid phase extraction are shown in Table 3.
TABLE 2 total organic carbon yield of the components in combination with solid phase extraction (%)
Table 3 statistics of molecular formula for identification of components by combined solid phase extraction
From tables 2 and 3, it can be derived that: the method can retain and separate the strong polar components which are difficult to extract and retain in the chemical wastewater DOM, and can effectively analyze and identify the strong polar DOM by combining means of organic carbon analysis, anion electrospray Fourier transform ion cyclotron resonance mass spectrometry and the like, compared with the traditional solid phase extraction mode, the recovery rate can be increased by 9.36%, the number of obtained molecular formulas can be increased by 2275, and the molecular formulas are increased by 62.62% compared with the traditional solid phase extraction method.
The foregoing detailed description is directed to a specific embodiment of the invention, which is not intended to limit the scope of the invention, but rather is to be accorded the full scope of the claims without departing from the true spirit and scope of the invention.
Claims (6)
1. A fractionation treatment method for analyzing soluble organic matters in chemical wastewater is characterized by comprising the following steps:
(1) Eluting the solid phase extraction column with methanol, and eluting with acidified ultrapure water to obtain a treated solid phase extraction column;
(2) Injecting the pretreated chemical wastewater water sample into the solid phase extraction column treated in the step (1) for enrichment, and leaching the solid phase extraction column with acidified water and ultrapure water for desalting treatment;
(3) After nitrogen of the solid phase extraction column subjected to desalting treatment is blown out of water, methanol is used for eluting to obtain an extraction fraction and a raffinate fraction, the raffinate fraction is averagely divided into two parts, one part of the raffinate fraction is added into a mixed anion solid phase extraction column, the pH value of one part of the raffinate fraction is regulated to be 9.5-10.5, the methanol with the mass fraction of 100% is used for eluting to obtain a first hydrophilic neutral fraction, the methanol with the mass fraction of 4-6% of formic acid is used for eluting to obtain a hydrophilic acidic fraction, the other part of the raffinate fraction is added into a mixed cation solid phase extraction column, the pH value of the other part of the raffinate fraction is regulated to be 1.5-2.5, the methanol with the mass fraction of 100% is used for eluting to obtain a second hydrophilic neutral fraction, and the methanol with the mass fraction of ammonium hydroxide is used for eluting to obtain a hydrophilic alkaline fraction;
(4) Mixing the obtained first hydrophilic neutral component and second hydrophilic neutral component, measuring the total organic carbon content of the hydrophilic neutral component, the hydrophilic acidic component and the hydrophilic alkaline component, drying the hydrophilic neutral component, the hydrophilic acidic component and the hydrophilic alkaline component by nitrogen, and then re-dissolving the hydrophilic neutral component, the hydrophilic acidic component and the hydrophilic alkaline component by methanol to obtain a sample for ESIFT-ICR MS analysis.
2. The fractionation treatment method for chemical wastewater soluble organic matter analysis according to claim 1, wherein the specific steps of step (1) are as follows: and eluting the solid phase extraction column with methanol with the volume of three times of the solid phase extraction column in advance, and eluting the solid phase extraction column with acidified ultrapure water with the pH of=2 after being acidified by high-purity hydrochloric acid with the volume of three times of the solid phase extraction column to obtain the treated solid phase extraction column.
3. The method for classifying and separating the chemical wastewater soluble organic matters according to claim 1, wherein the pretreatment step of the pretreated chemical wastewater in the step (2) is as follows: filtering the chemical wastewater by a filter membrane with the aperture of 0.45 μm, acidifying the filtered water sample to pH=2 by using high-purity hydrochloric acid to obtain a pretreated chemical wastewater water sample, injecting the pretreated chemical wastewater water sample into the solid phase extraction column treated in the step (1) for enrichment, and leaching the solid phase extraction column by using the acidified water and the ultrapure water for desalting treatment.
4. The fractionation treatment method for chemical wastewater soluble organic matter analysis according to claim 1, wherein the specific steps of step (3) are as follows: after nitrogen of the solid phase extraction column subjected to desalting treatment is blown out to remove water, methanol is used for eluting to obtain an extraction fraction and a raffinate fraction, the raffinate fraction is divided into two parts averagely, one part of the raffinate fraction is added into a mixed anion solid phase extraction column, the pH=10 of the one part of the raffinate fraction is regulated, the methanol with the mass fraction of 100% is used for eluting to obtain a first hydrophilic neutral fraction, the methanol with the mass fraction of 5% is used for eluting to obtain a hydrophilic acidic fraction, the other part of the raffinate fraction is added into a mixed cation solid phase extraction column, the pH=2 of the other part of the raffinate fraction is regulated, the methanol with the mass fraction of 100% is used for eluting to obtain a second hydrophilic neutral fraction, and the methanol with the mass fraction of 5% of ammonium hydroxide is used for eluting to obtain a hydrophilic alkaline fraction.
5. The method for fractionation treatment of chemical wastewater soluble organic matter analysis according to claim 1 or 4, wherein in the step (3), a ph=10 of a part of the raffinate is adjusted with an ammonium hydroxide solution having a mass fraction of 2%.
6. The method for fractionation treatment of chemical wastewater soluble organic matter analysis according to claim 1 or 4, wherein in the step (3), the ph=2 of the other part of the raffinate is adjusted by using a formic acid solution with a mass fraction of 2%.
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