CN113340834A - Method for rapidly determining content of sodium acetate in industrial-grade sodium acetate solution - Google Patents
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- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 title claims abstract description 106
- 239000001632 sodium acetate Substances 0.000 title claims abstract description 105
- 235000017281 sodium acetate Nutrition 0.000 title claims abstract description 105
- 238000000034 method Methods 0.000 title claims abstract description 41
- 239000000243 solution Substances 0.000 claims abstract description 67
- 238000002835 absorbance Methods 0.000 claims abstract description 41
- 239000003381 stabilizer Substances 0.000 claims abstract description 27
- 239000000523 sample Substances 0.000 claims abstract description 26
- 239000012086 standard solution Substances 0.000 claims abstract description 14
- 238000010521 absorption reaction Methods 0.000 claims abstract description 13
- 239000012488 sample solution Substances 0.000 claims abstract description 10
- 238000002798 spectrophotometry method Methods 0.000 claims abstract description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- LWIHDJKSTIGBAC-UHFFFAOYSA-K tripotassium phosphate Chemical compound [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 claims description 4
- 239000004471 Glycine Substances 0.000 claims description 2
- 229910021538 borax Inorganic materials 0.000 claims description 2
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 2
- 239000004327 boric acid Substances 0.000 claims description 2
- 229910000160 potassium phosphate Inorganic materials 0.000 claims description 2
- 235000011009 potassium phosphates Nutrition 0.000 claims description 2
- 239000001488 sodium phosphate Substances 0.000 claims description 2
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 2
- 239000004328 sodium tetraborate Substances 0.000 claims description 2
- 235000010339 sodium tetraborate Nutrition 0.000 claims description 2
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 2
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-UHFFFAOYSA-N 0.000 claims 1
- 238000001514 detection method Methods 0.000 abstract description 8
- 239000000126 substance Substances 0.000 abstract description 5
- 238000004458 analytical method Methods 0.000 abstract description 2
- 230000003595 spectral effect Effects 0.000 abstract description 2
- 238000002479 acid--base titration Methods 0.000 description 7
- 238000005259 measurement Methods 0.000 description 6
- 239000007983 Tris buffer Substances 0.000 description 4
- 239000011550 stock solution Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000011088 calibration curve Methods 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 230000002401 inhibitory effect Effects 0.000 description 2
- 238000004255 ion exchange chromatography Methods 0.000 description 2
- KJFMBFZCATUALV-UHFFFAOYSA-N phenolphthalein Chemical compound C1=CC(O)=CC=C1C1(C=2C=CC(O)=CC=2)C2=CC=CC=C2C(=O)O1 KJFMBFZCATUALV-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 229940040526 anhydrous sodium acetate Drugs 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000012470 diluted sample Substances 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000005337 ground glass Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000007974 sodium acetate buffer Substances 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
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- Health & Medical Sciences (AREA)
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Abstract
The invention discloses a method for rapidly determining the content of sodium acetate in an industrial-grade sodium acetate solution, belongs to the technical field of chemical analysis, and solves the problems of complex operation, high cost and long time consumption in the prior art for determining sodium acetate. The method adopts an ultraviolet spectrophotometry for determination, and the determination process comprises the following steps: drawing a standard curve: respectively measuring sodium acetate standard use solutions with different concentrations, adding a stabilizer, and respectively measuring the absorbance at the characteristic absorption wavelength; taking the concentration of the standard solution as an abscissa and the corrected absorbance of the standard solution as an ordinate, and drawing a standard curve; taking a sample of industrial-grade sodium acetate solution, adding a stabilizer, and measuring the absorbance of the industrial-grade sodium acetate solution at a characteristic absorption wavelength; substituting the corrected absorbance into a standard curve fitting equation, and calculating to obtain the concentration of the sodium acetate in the sample solution. The invention has simple, convenient and quick operation and low cost; the spectrophotometric method for detecting the content of the sodium acetate solution is invented by creatively utilizing the spectral characteristics of the sodium acetate solution in a specific wavelength range, and the stabilizing agent is added into a detection system, so that the accuracy of a detection result and the interference resistance of the detection system are improved.
Description
Technical Field
The invention belongs to the technical field of chemical analysis, and particularly relates to a method for rapidly determining the content of sodium acetate in an industrial-grade sodium acetate solution.
Background
Sodium acetate is a common chemical and has been widely used in various fields such as medicine, printing and dyeing, industrial catalysis, sewage treatment and the like. In practical application, enterprises generally directly purchase industrial-grade sodium acetate solution for adding. Meanwhile, in the using process, the using amount of sodium acetate is often larger, the adding frequency is high, and the content of sodium acetate is used as a key index for quality control of industrial sodium acetate solution in the using process and needs to be rapidly analyzed and detected.
In the prior art, an acid-base titration method and an ion chromatography method are generally adopted to measure the content of sodium acetate. When an acid-base titration method is adopted, phenolphthalein is used as an indicator, back titration is carried out by using sodium hydroxide, and the content of sodium acetate is calculated. The method is easily interfered by impurities, has poor selectivity and is relatively complicated to operate. Measuring sodium acetate content by ion chromatography, inhibiting leacheate by using an inhibitor, deducting background conductivity, and measuring by using a conductivity measuring device. The method is long in time consumption and high in cost.
Therefore, the method which is rapid, accurate and simple to operate and is suitable for measuring the content of sodium acetate in the industrial-grade sodium acetate solution is provided, and the problem to be solved by the technical personnel in the field is solved urgently.
Disclosure of Invention
The invention aims to provide a method for rapidly determining the content of sodium acetate in an industrial-grade sodium acetate solution, and solves the problems of complex operation, high cost and long time consumption in the prior art for determining sodium acetate.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the invention provides a method for rapidly determining the content of sodium acetate in an industrial-grade sodium acetate solution, which adopts an ultraviolet spectrophotometry to determine and comprises the following steps:
s1, drawing a standard curve: respectively measuring sodium acetate standard use solutions with different concentrations, adding a stabilizer, and uniformly mixing to obtain standard solutions to be detected with different concentrations; measuring the absorbance at the characteristic absorption wavelengths respectively; taking deionized water as a blank control, and measuring the absorbance by the same method; subtracting the absorbance of the blank control from the absorbance of the obtained sodium acetate standard use solution with different concentrations to obtain the corrected absorbance of the standard solution, and drawing a standard curve by taking the concentration of the standard solution as an abscissa and the corrected absorbance of the standard solution as an ordinate;
s2, taking an industrial-grade sodium acetate solution sample, adding a stabilizer, and uniformly mixing to obtain a sample solution to be detected; measuring the absorbance of the solution of the sample to be measured at the characteristic absorption wavelength; taking deionized water as a blank control, and measuring the absorbance by the same method; subtracting the absorbance of the blank control from the absorbance of the sample to obtain the corrected absorbance of the sample;
and S3, substituting the corrected absorbance of the sample obtained in the S2 into a standard curve fitting equation of the S1, and calculating to obtain the concentration of the sample solution.
In some embodiments of the invention, the stabilizer comprises a solution formulated from one or more of potassium hydroxide, sodium hydroxide, potassium phosphate, sodium phosphate, tris, glycine, borax, boric acid, hydrochloric acid.
In some embodiments of the invention, the stabilizer solution has a pH >7 and a blank absorbance <0.100 at the characteristic absorption wavelength.
In some embodiments of the invention, the stabilizer is a sodium hydroxide solution or a tris solution at a pH of 9.
The invention discovers that sodium acetate as a strong base and a weak acid salt is easy to hydrolyze in water:
when the spectrophotometry is used for measuring the content of sodium acetate in an industrial-grade sodium acetate solution, a sample is often required to be diluted, so that the sodium acetate is hydrolyzed to a certain degree, balanced type is moved to the right, and the sodium acetate is converted into acetic acid, so that the property of the solution is changed, and the accuracy of a measuring result is influenced. In addition, industrial sodium acetate may have a certain amount of residual raw material present in the production process, which also interferes with the determination of the sodium acetate content. Therefore, the invention creatively adds a certain amount of sodium acetate stabilizer into the detection system to establish a sodium acetate buffer system so as to achieve the purposes of stabilizing the solution property, inhibiting the hydrolysis of sodium acetate and improving the accuracy of the measurement result and the anti-interference capability of the system.
In some embodiments of the invention, the characteristic absorption wavelength range is 190-210 nm.
In some embodiments of the invention, the characteristic absorption wavelength is 191 nm. .
In the invention, the superior pure sodium acetate is scanned by a spectrophotometer within the wavelength range of 190-210nm, and the wavelength at the characteristic absorption peak is selected as the wavelength for measuring the content of the sodium acetate.
The correlation coefficient r of the standard curve of the invention is greater than or equal to 0.999.
In some embodiments of the invention, the concentration of the standard curve is in the range of 0 to 100 mg/L.
In some embodiments of the invention, each 50mL of standard solution to be tested contains 0.5-5 mL of stabilizer; preferably 1 mL;
each 50mL of sample solution to be detected contains 0.5-5 mL of stabilizer; preferably 1 mL.
In order to reduce the chemical interference of an added substance to a system as much as possible and improve the detection accuracy, a proper amount of a stabilizer needs to be added. The inventors found that the addition of 1mL of stabilizer was satisfactory.
In some embodiments of the present invention, in S2, a technical grade sodium acetate solution sample is diluted and then added with a stabilizer.
In some embodiments of the present invention, after the corrected absorbance of the sample obtained in S2 exceeds the concentration range of the standard curve, the industrial grade sodium acetate solution sample is diluted and then measured.
In some embodiments of the present invention, the mass concentration of sodium acetate in the industrial-grade sodium acetate solution is calculated by the following formula:
C＝[(As-Ab-a)/b]×f
in the formula: c, mass concentration of sodium acetate in the industrial sodium acetate solution, mg/L;
As-absorbance of the sample solution;
Ab-absorbance of blank;
a is the intercept of the calibration curve;
b-the slope of the calibration curve;
f is the dilution factor.
Compared with the prior art, the invention has the following beneficial effects:
the method has scientific design and ingenious conception, directly measures the content of sodium acetate in the industrial-grade sodium acetate solution by using a single-wavelength spectrophotometry, and has simple, convenient and quick operation and low cost; the invention creatively utilizes the spectral characteristic of the sodium acetate solution under the ultraviolet light with specific wavelength to invent the spectrophotometry method for detecting the content of the sodium acetate solution, and adds the stabilizing agent into the detection system, thereby improving the accuracy of the detection result and the interference resistance of the detection system.
Drawings
FIG. 1 is a wavelength scan of sodium acetate of superior purity according to the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Example 1
The implementation provides the method for measuring the content of sodium acetate in the industrial-grade sodium acetate solution, which specifically comprises the following steps:
1. preparation of sodium acetate standard stock solution: 0.5000g of anhydrous sodium acetate is weighed, dissolved in water, transferred to a 1000mL volumetric flask, diluted with water to the marked line and mixed evenly. The concentration of sodium acetate in the stock solution was 2000 mg/L.
2. Preparation of sodium acetate standard use solution: 50.00mL of sodium acetate standard stock solution is weighed into a 100mL volumetric flask, diluted to a marked line by water, mixed evenly and prepared immediately. The concentration of the standard sodium acetate solution is 1000 mg/L.
3. Preparation of sodium acetate stabilizer solution: sodium hydroxide was weighed and dissolved in water and the pH was adjusted to 9.
4. Selection of measurement wavelength: scanning a guaranteed grade pure sodium acetate (100mg/L) in a wavelength range of 190-210nm by using a spectrophotometer, and showing that the absorption peak is maximum at 191 nm. 191nm was chosen as the measurement wavelength.
5. Drawing a standard curve: 0.00mL, 0.50 mL, 1.00mL, 2.00 mL, 3.00 mL, 4.00 mL, and 5.00mL of standard solutions of sodium acetate were measured in 50mL glass cuvettes with plugs, and the corresponding sodium acetate contents were 0.00 mg, 0.50 mg, 1.00 mg, 2.00 mg, 3.00 mg, 4.00 mg, and 5.00mg, respectively. Then respectively adding 1.00mL of sodium hydroxide solution with the pH value of 9, adding water to dilute to 50mL of marked line, covering and plugging, and uniformly mixing. The absorbance was determined on a spectrophotometer using a 10mm quartz cuvette with deionized water as a reference, selecting a single wavelength of 191 nm. After subtracting the absorbance of the blank experiment, a standard working curve was drawn with the corresponding sodium acetate concentration:
the standard curve fitting equation obtained is: a is 0.00555c-0.00954, and r is 0.9990.
6. And (3) sample determination: diluting 1250 times a sample of industrial-grade sodium acetate solution (the pH value is 8.2), measuring 20.00mL of the diluted sample into a 50mL glass colorimetric tube with a plug and a ground port, adding 1.00mL of sodium hydroxide solution with the pH value of 9, measuring the pH value to be 7.7, and measuring according to the step 5 to obtain the absorbance of 0.423;
7. blank test: and (3) replacing an industrial-grade sodium acetate solution sample with deionized water, and measuring according to the same steps of the industrial-grade sodium acetate solution sample to obtain blank absorbance of 0.011.
8. In this embodiment, the mass concentration of sodium acetate in the industrial-grade sodium acetate solution sample is:
[(0.423-0.011)+0.00954]/0.00555×3125＝237253.60mg/L。
the converted mass fraction is:
[(237253.60×10-3)/(1000+237253.60×10-3)]×100％＝19.2％。
the industrial grade sodium acetate solution sample in the embodiment is determined by an acid-base titration method, and the mass fraction of the sodium acetate is measured to be 19.4%.
Example 2
The implementation provides the method for measuring the content of sodium acetate in the industrial-grade sodium acetate solution,
in this example, in comparison with example 1, a tris solution (tris solution) was used as the stabilizer, the pH of the solution being about 9, the other conditions being the same.
The standard curve fitting equation obtained in this example is: a is 0.00546c +0.01131 and r is 0.9997.
The absorbance of the sample in this example was 0.528;
the blank absorbance was 0.006.
In this embodiment, the mass concentration of sodium acetate in the industrial-grade sodium acetate solution is calculated as follows:
[(0.528-0.006)-0.01131]/0.00546×3125＝292290.52mg/L。
the converted mass fraction is:
[(292290.52×10-3)/(1000+292290.52×10-3)]×100％＝22.6％。
the industrial grade sodium acetate solution sample in the embodiment is determined by an acid-base titration method, and the mass fraction of the sodium acetate is 22.4%.
The results of the method of the invention are compared with the results of the classical acid-base titration method, and are shown in the following table:
TABLE 1
As can be seen from the table above, the results obtained by the method of the present invention are consistent with the results obtained by the classical acid-base titration method, which indicates that the method of the present invention has accurate results.
Comparative example 1
Compared with the example 1, the standard solution and the sample solution to be measured are not added with the stabilizing agent, and the pH value of the sample solution which is placed in the plug ground glass colorimetric tube and used for measuring the absorbance is 6.7; the other conditions were consistent.
In this comparative example, the mass content of sodium acetate in the technical-grade sodium acetate solution was measured to be 17.22%.
The stock solution of the same industrial grade sodium acetate solution is measured by an acid-base titration method, and the mass content of sodium acetate is 19.4 percent; the measurement result of the embodiment 1 added with the stabilizer is 19.2% which is consistent with the measurement result of the classical acid-base method; the measurement result of comparative example 1 without adding the stabilizer was 17.2% lower; specifically, as shown in table 2:
TABLE 2
The above-mentioned embodiment is only one of the preferred embodiments of the present invention, and should not be used to limit the scope of the present invention, but all the insubstantial modifications or changes made within the spirit and scope of the main design of the present invention, which still solve the technical problems consistent with the present invention, should be included in the scope of the present invention.
Claims (9)
1. A method for rapidly determining the content of sodium acetate in an industrial-grade sodium acetate solution is characterized in that an ultraviolet spectrophotometry is adopted for determination, and the method comprises the following steps:
s1, drawing a standard curve: respectively measuring sodium acetate standard use solutions with different concentrations, adding a stabilizer, and uniformly mixing to obtain standard solutions to be detected with different concentrations; measuring the absorbance at the characteristic absorption wavelengths respectively; taking deionized water as a blank control, and measuring the absorbance by the same method; subtracting the absorbance of the blank control from the absorbance of the obtained sodium acetate standard use solution with different concentrations to obtain the corrected absorbance of the standard solution, and drawing a standard curve by taking the concentration of the standard solution as an abscissa and the corrected absorbance of the standard solution as an ordinate;
s2, taking an industrial-grade sodium acetate solution sample, adding a stabilizer, and uniformly mixing to obtain a sample solution to be detected; measuring the absorbance of the solution of the sample to be measured at the characteristic absorption wavelength; taking deionized water as a blank control, and measuring the absorbance by the same method; subtracting the absorbance of the blank control from the absorbance of the sample to obtain the corrected absorbance of the sample;
and S3, substituting the corrected absorbance of the sample obtained in the S2 into a standard curve fitting equation of the S1, and calculating to obtain the concentration of the sample solution.
2. The method for rapidly determining the content of sodium acetate in the industrial-grade sodium acetate solution as claimed in claim 1, wherein the stabilizer comprises one or more of potassium hydroxide, sodium hydroxide, potassium phosphate, sodium phosphate, tris (hydroxymethyl) aminomethane, glycine, borax, boric acid and hydrochloric acid.
3. The method of claim 2, wherein the stabilizer solution has a pH >7 and a blank absorbance <0.100 at the characteristic absorption wavelength.
4. The method for rapidly determining the content of sodium acetate in the industrial-grade sodium acetate solution as claimed in claim 1, wherein the characteristic absorption wavelength range is 190-210 nm.
5. The method for rapidly determining the content of sodium acetate in the industrial-grade sodium acetate solution as claimed in claim 4, wherein the concentration range of the standard curve is 0-100 mg/L.
6. The method for rapidly determining the content of sodium acetate in the industrial-grade sodium acetate solution according to claim 5, wherein 0.5-5 mL of a stabilizer is added to every 50mL of a standard solution to be determined; preferably 1 mL.
7. The method for rapidly determining the content of sodium acetate in the industrial-grade sodium acetate solution according to claim 6, wherein 0.5-5 mL of a stabilizer is added into every 50mL of a sample solution to be determined; preferably 1 mL.
8. The method for rapidly determining the content of sodium acetate in the industrial-grade sodium acetate solution as claimed in claim 6, wherein in S2, a stabilizing agent is added after a sample of the industrial-grade sodium acetate solution is diluted.
9. The method for rapidly determining the content of sodium acetate in the industrial-grade sodium acetate solution as claimed in claim 7, wherein the industrial-grade sodium acetate solution sample is diluted and then determined after the corrected absorbance of the sample obtained in S2 exceeds the concentration range of the standard curve.
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