CN113820418A - Method for determining content of sodium acetate and 8 inorganic anions of water treatment agent - Google Patents
Method for determining content of sodium acetate and 8 inorganic anions of water treatment agent Download PDFInfo
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- CN113820418A CN113820418A CN202111114485.3A CN202111114485A CN113820418A CN 113820418 A CN113820418 A CN 113820418A CN 202111114485 A CN202111114485 A CN 202111114485A CN 113820418 A CN113820418 A CN 113820418A
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- 238000000034 method Methods 0.000 title claims abstract description 35
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 title claims abstract description 34
- 239000001632 sodium acetate Substances 0.000 title claims abstract description 34
- 235000017281 sodium acetate Nutrition 0.000 title claims abstract description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 23
- 150000001449 anionic compounds Chemical class 0.000 title claims abstract description 16
- 229910001412 inorganic anion Inorganic materials 0.000 title claims abstract description 16
- 238000001514 detection method Methods 0.000 claims abstract description 16
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims abstract description 8
- 238000004255 ion exchange chromatography Methods 0.000 claims abstract description 8
- 239000012535 impurity Substances 0.000 claims description 15
- -1 fluoride ions Chemical class 0.000 claims description 12
- 239000000523 sample Substances 0.000 claims description 12
- 238000010828 elution Methods 0.000 claims description 10
- 239000012488 sample solution Substances 0.000 claims description 8
- 239000000706 filtrate Substances 0.000 claims description 6
- 229910002651 NO3 Inorganic materials 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 239000012528 membrane Substances 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 4
- 239000004677 Nylon Substances 0.000 claims description 4
- 229920001778 nylon Polymers 0.000 claims description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 3
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 3
- XTEGARKTQYYJKE-UHFFFAOYSA-M chlorate Inorganic materials [O-]Cl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-M 0.000 claims description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 238000011002 quantification Methods 0.000 claims description 2
- 150000001450 anions Chemical class 0.000 abstract description 6
- 238000005259 measurement Methods 0.000 abstract description 5
- 238000003912 environmental pollution Methods 0.000 abstract description 3
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 150000002500 ions Chemical class 0.000 description 19
- 239000000243 solution Substances 0.000 description 14
- 239000000047 product Substances 0.000 description 10
- 238000004458 analytical method Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 4
- 238000004448 titration Methods 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 244000005700 microbiome Species 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 238000010200 validation analysis Methods 0.000 description 3
- HNSDLXPSAYFUHK-UHFFFAOYSA-N 1,4-bis(2-ethylhexyl) sulfosuccinate Chemical compound CCCCC(CC)COC(=O)CC(S(O)(=O)=O)C(=O)OCC(CC)CCCC HNSDLXPSAYFUHK-UHFFFAOYSA-N 0.000 description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- TVWHTOUAJSGEKT-UHFFFAOYSA-N chlorine trioxide Chemical compound [O]Cl(=O)=O TVWHTOUAJSGEKT-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 238000012795 verification Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 238000005571 anion exchange chromatography Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012496 blank sample Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000013375 chromatographic separation Methods 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 239000003480 eluent Substances 0.000 description 1
- 238000010829 isocratic elution Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 230000001360 synchronised effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Images
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/34—Control of physical parameters of the fluid carrier of fluid composition, e.g. gradient
Abstract
The invention discloses a method for determining the content of sodium acetate and 8 inorganic anions in a water treatment agent, and relates to the technical field of chemical detection. The invention utilizes ion chromatography to detect 8 common inorganic anions which are easy to cause environmental pollution in the water treatment agent sodium acetate and carbonate which are used as main components, and realizes the accurate measurement of the contents of the 8 inorganic anions and the sodium acetate by optimizing the concentration ratio of a standard sample. The method has high reliability and low experimental cost, can detect anions which can cause potential pollution in the water treatment agent sodium acetate, and has practical significance for improving the quality of the water treatment agent sodium acetate product.
Description
Technical Field
The invention belongs to the technical field of chemical detection, and particularly relates to a method for determining the content of sodium acetate and 8 inorganic anions in a water treatment agent.
Background
Sodium acetate is currently the most common, most used source of added carbon. The current market of water treatment agent sodium acetate is in the stage of short supply and short demand, and the price is higher. However, the quality of the product is not uniform, more and less sodium acetate products are produced by using waste acid as a raw material, the COD of the product is difficult to maintain to a higher level, more carbon-containing compounds which are not easy to be absorbed by microorganisms need to be additionally added, the generated COD is called invalid COD, and simultaneously, other waste acid components have more side effects on the microorganisms, so that the product cannot provide energy, but can inhibit the growth of the microorganisms, and therefore, the product quality is required to be accepted and daily product quality control is required.
The method for measuring the content of sodium acetate is still in a blank stage at present in China, and national standards and unified technical specifications about the sodium acetate of a water treatment agent are not formed. When the third-party organization performs task detection, the detection can be performed only according to a detection method provided by an enterprise, and the accuracy is difficult to guarantee; in the case of wastewater treatment plants, detection is also possible only according to the reagent-grade sodium acetate test method (ion membrane exchange method) they provide. As enterprises can also add more other carbon sources in the water treatment agent sodium acetate, when the determination is carried out by adopting a resin exchange method, the time is more consumed, the regeneration of the resin is more difficult, the cost is higher, and a more reliable and simpler method for determining the content is urgently needed to be developed.
Disclosure of Invention
The invention provides a method for determining the content of sodium acetate and 8 inorganic anions of a water treatment agent, and aims to solve the problems that the existing method is high in cost and low in reliability and cannot detect potential pollution inorganic anions.
A method for measuring the contents of sodium acetate and 8 inorganic anions of a water treatment agent comprises the following operation steps:
s1, weighing 1g of water treatment agent sodium acetate sample solution, and fixing the volume of the solution in a 100mL volumetric flask by using deionized water;
s2, filtering a proper amount of sample solution with constant volume by using a 0.22-micron nylon filter membrane, collecting filtrate in a sample bottle, and then carrying out detection and quantification by using an ion chromatography for sample introduction.
Further, the eluent used in the detection process in step S2 is a gradient KOH solution, and the gradient KOH solution is divided into an impurity gradient solution for detecting fluoride ions, chloride ions, nitrate ions, nitrite ions, sulfate ions, phosphate ions, bromide ions, and chlorate ions, and a main component gradient solution for detecting acetate and carbonate ions.
Further, the conditions of gradient elution of the impurity gradient solution are as follows: 0.0-7.5min, 0.5 mmol/L; 7.5-8.0min, 0.5-3.0 mmol/L; 8.0-19.0min, 3.0 mmol/L; 9.0-21.0min, 3.0-20 mmol/L; 21.0-25.0min, 20.0 mmol/L; 25.0-25.5min, 20.0-0.5 mmol/L; 25.5-30.0min, 0.5 mmol/L.
Further, the gradient elution condition of the main component gradient solution is 0.0-5.0min and 10 mmol/L; 5.0-15.5min, 10.0-50.0 mmol/L; 15.5-20.5min, 50.0 mmol/L; 20.5-25.5min, 50.0-10.0 mmol/L; 25.5-30.0min, 10.0 mmol/L.
The method has the advantages that the ion types involved in the detection process are more, 8 anions can not completely generate peaks during isocratic elution, and the concentration of different leacheate is adjusted to carry out gradient elution on impurity ions and main component ions respectively, so that the chromatographic peak pattern can be improved.
Further, in the case of filtration in step S2, the first 2mL of the preliminary filtrate was discarded.
Thus, the detection result is more accurate.
The invention has the beneficial effects that:
1. the invention establishes a method for quickly, efficiently and low-cost determination of the content of sodium acetate, and can identify and identify inferior products.
2. The method utilizes ion chromatography, uses two leacheate gradient elution programs to respectively detect 8 common impurity anions which easily cause environmental pollution in the water treatment agent sodium acetate and carbonate which are used as main components, and realizes the synchronous determination of the contents of the 8 inorganic impurity anions and the sodium acetate by optimizing the preparation concentration ratios of different ions.
3. The method has high reliability and lower experimental cost, can accurately measure 8 inorganic anions and main component ions causing potential pollution in the sample, and has practical significance for monitoring the quality of the water treatment agent sodium acetate product and reducing the potential environmental pollution risk.
Drawings
FIG. 1 is a chromatogram of mixed standard ions at a concentration of 5mg/L chloride ions.
Detailed Description
The invention is described in further detail in the following with reference to the figures and the detailed description, wherein the technical means and scientific terms used in the invention are all known to those skilled in the art unless otherwise specified:
instruments and reagents
Dionex ICS-2100 ion chromatograph (Thermo Fisher, USA); a conductivity detector, a Chromeleon chromatography workstation; a Dionex Ionpac AS23(250 mm. times.4 mm) separation column; IonPac AG23 (50X 4mm) was protected; ASRS300 type electrochemical self-regenerating suppressors; 0.22 μm nylon filter membrane filter head.
F-、Cl-、NO2 -、Br-、NO3 -、ClO3 -、SO4 2-、PO4 3-、CH3COO-、CO3 2-(Shanghai city, measurement and test institute, 1000mg/L) and laboratory water are secondary deionized water with conductivity greater than 18.2M omega.
Example 1
A method for measuring the contents of sodium acetate and 8 inorganic anions of a water treatment agent comprises the following operation steps: s1, weighing 1g of a water treatment agent sodium acetate sample solution to be measured, accurately measuring the volume to 0.0002g, and fixing the volume by using deionized water in a 100mL volumetric flask; s2, filtering a proper amount of sample solution with constant volume by using a 0.22-micron nylon filter membrane, discarding the first 2mL of primary filtrate, collecting the filtrate in a sample bottle, and then carrying out sample injection and detection by using ion chromatography to obtain a chromatogram shown in figure 1.
The leacheate used in the detection process is a gradient KOH solution, and the gradient KOH solution is divided into an impurity gradient solution and a main component gradient solution. Gradient elution chromatographic conditionsAs shown in Table 1, the impurity gradient solution was used to detect impurity anions (F) in the sample solution to be tested-、Cl-、NO2 -、Br-、NO3 -、ClO3 -、SO4 2-、PO4 3-) The conditions of gradient elution are as follows: 0.0-7.5min, 0.5 mmol/L; 7.5-8.0min, 0.5-3.0 mmol/L; 8.0-19.0min, 3.0 mmol/L; 9.0-21.0min, 3.0-20 mmol/L; 21.0-25.0min, 20.0 mmol/L; 25.0-25.5min, 20.0-0.5 mmol/L; 25.5-30.0min, 0.5 mmol/L; the principal component gradient solution is used for detecting principal component ions (CH) in a sample solution to be detected3COO-、CO3 2-) The conditions of gradient elution are as follows: 0.0-5.0min, 10 mmol/L; 5.0-15.5min, 10.0-50.0 mmol/L; 15.5-20.5min, 50.0 mmol/L; 20.5-25.5min, 50.0-10.0 mmol/L; 25.5-30.0min, 10.0 mmol/L.
TABLE 1 gradient elution conditions for impurity ions and principal component ions
Methodology validation
1. Preparation of standard curve
The impurity ion analysis part is mixed with standard fluoride ions, chloride ions, nitrate ions, nitrite ions, sulfate ions, phosphate ions, bromide ions and chlorate ions to prepare concentration series of 1mg/L, 5mg/L, 10mg/L, 20mg/L and 25 mg/L;
the main component analysis part mixes standard acetate to prepare 15mg/L, 60mg/L, 150mg/L, 200mg/L, 250mg/L and 300mg/L concentration gradients, and carbonate is prepared to prepare 5mg/L, 30mg/L, 50mg/L, 100mg/L, 150mg/L and 200mg/L concentration series.
2. Methodological parameter validation
And (3) taking out the standard curve series of the impurity ions and the main component ions prepared in the step (1), and respectively carrying out sample injection analysis according to respective chromatographic conditions to obtain the data of the standard line series, wherein the peak area parameters of the lowest point peak of the standard line are shown in a table 2. The detection limit of each impurity ion is determined by adopting a method of diluting a standard sample step by step according to the signal to noise ratio of 3 times, and the obtained linear range, linear equation, linear correlation coefficient R and detection limit data of each ion are shown in a table 3.
TABLE 2 different peak heights and peak areas at the same concentrations
TABLE 3 methodological parameter validation results for target anions
3. Stability verification of acetate and carbonate ion chromatographic separation process
The quantitative result of acetate is directly related to the accuracy of the final content result of the product, the first interferent for measuring the content of sodium acetate by the titration method is carbonate, 6 self-prepared solution samples with different concentrations are respectively prepared and subjected to parallel sample injection for 6 times according to respective linear ranges of the acetate and the carbonate, the measurement result is shown in table 4, the experimental result shows that the relative standard deviations of four indexes, namely the peak height, the peak area, the retention time and the quantitative result, of a target ion at different concentration points are all less than 5%, and the method is shown to have higher stability in the actual test process.
Table 4 verification of stability of main component anion chromatography process
4. Simulation of sample measurement results
In order to simulate the possible content difference of actual samples, 5%, 10%, 15%, 20% and 25% of analytically pure sodium acetate and deionized water are respectively prepared, 5 simulated samples with different concentrations are respectively subjected to parallel determination experiments of a titration method and an ion chromatography, the test results are average values of 6 determinations, and the results are shown in table 5.
TABLE 5 comparison of the results of the titration and ion chromatography measurements of sodium acetate samples
From table 5, it can be seen that the quantitative accuracy of the method of the present invention for sodium acetate samples of different contents can meet the product analysis requirements, and the quantitative results of ion chromatography and the relative standard deviation of parallel samples are generally superior to those of titration.
5. Determination of impurity ion standard recovery rate
Pure water is used as a blank sample of the standard adding recovery rate experiment, two horizontal inorganic mixed standard samples of 1.0mg/L and 5mg/L are added (the rest ions are increased in proportion), the reliability of the method is verified in the test step and the sample analysis step, and the experimental results are shown in the following table 6.
Table 6 recovery and standard deviation of addition of inorganic standards at two levels
The foregoing is merely an example of the present invention and common general knowledge of the specific structures and characteristics of the processes, etc., is not set forth herein in any greater detail. It should be noted that, for those skilled in the art, without departing from the structure of the present invention, several changes and modifications can be made, which should also be regarded as the protection scope of the present invention, and these will not affect the effect of the implementation of the present invention and the practicability of the patent. The scope of the claims of the present application shall be determined by the contents of the claims, and the description of the embodiments and the like in the specification shall be used to explain the contents of the claims.
Claims (5)
1. A method for measuring the content of sodium acetate and 8 inorganic anions of a water treatment agent is characterized by comprising the following operation steps:
s1, weighing 1g of water treatment agent sodium acetate sample solution, and fixing the volume of the solution in a 100mL volumetric flask by using deionized water;
s2, filtering a proper amount of sample solution with constant volume by using a 0.22-micron nylon filter membrane, collecting filtrate in a sample bottle, and then carrying out detection and quantification by using an ion chromatography for sample introduction.
2. The method for determining the contents of sodium acetate and 8 inorganic anions in a water treatment agent according to claim 1, which is characterized in that: the leacheate used in the detection process of the step S2 is a gradient KOH solution, and the gradient KOH solution is an impurity gradient solution for detecting fluoride ions, chloride ions, nitrate ions, nitrite ions, sulfate ions, phosphate ions, bromide ions and chlorate ions, and a main component gradient solution for detecting acetate and carbonate ions.
3. The method for determining the contents of sodium acetate and 8 inorganic anions in a water treatment agent according to claim 2, wherein the conditions of gradient elution of the impurity gradient solution are as follows: 0.0-7.5min, 0.5 mmol/L; 7.5-8.0min, 0.5-3.0 mmol/L; 8.0-19.0min, 3.0 mmol/L; 9.0-21.0min, 3.0-20 mmol/L; 21.0-25.0min, 20.0 mmol/L; 25.0-25.5min, 20.0-0.5 mmol/L; 25.5-30.0min, 0.5 mmol/L.
4. The method for determining the contents of sodium acetate and 8 inorganic anions in a water treatment agent according to claim 2, wherein the conditions of gradient elution of the principal component gradient solution are as follows: 0.0-5.0min, 10 mmol/L; 5.0-15.5min, 10.0-50.0 mmol/L; 15.5-20.5min, 50.0 mmol/L; 20.5-25.5min, 50.0-10.0 mmol/L; 25.5-30.0min, 10.0 mmol/L.
5. The method for determining the content of sodium acetate and 8 inorganic anions in a water treatment agent according to claim 1, wherein the first 2mL of primary filtrate is discarded during the filtration in the step S2.
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2021
- 2021-09-23 CN CN202111114485.3A patent/CN113820418A/en active Pending
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