CN113340834B - Method for rapidly determining sodium acetate content in industrial sodium acetate solution - Google Patents
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- CN113340834B CN113340834B CN202110655057.5A CN202110655057A CN113340834B CN 113340834 B CN113340834 B CN 113340834B CN 202110655057 A CN202110655057 A CN 202110655057A CN 113340834 B CN113340834 B CN 113340834B
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- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 title claims abstract description 107
- 239000001632 sodium acetate Substances 0.000 title claims abstract description 106
- 235000017281 sodium acetate Nutrition 0.000 title claims abstract description 106
- 238000000034 method Methods 0.000 title claims abstract description 38
- 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 25
- 238000010521 absorption reaction Methods 0.000 claims abstract description 13
- 239000012086 standard solution Substances 0.000 claims abstract description 13
- 239000012488 sample solution Substances 0.000 claims abstract description 12
- 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
- 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
- 238000002156 mixing Methods 0.000 claims description 4
- 239000007983 Tris buffer Substances 0.000 claims description 3
- LWIHDJKSTIGBAC-UHFFFAOYSA-K tripotassium phosphate Chemical compound [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 claims description 3
- 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
- 238000007865 diluting Methods 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
- 229910000160 potassium phosphate Inorganic materials 0.000 claims 1
- 235000011009 potassium phosphates Nutrition 0.000 claims 1
- 239000001488 sodium phosphate Substances 0.000 claims 1
- 229910000162 sodium phosphate Inorganic materials 0.000 claims 1
- 238000001514 detection method Methods 0.000 abstract description 8
- 238000002798 spectrophotometry method Methods 0.000 abstract description 6
- 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
- 238000005259 measurement Methods 0.000 description 10
- 238000002479 acid--base titration Methods 0.000 description 7
- 230000000052 comparative effect Effects 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
- 238000011088 calibration curve Methods 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 239000011521 glass Substances 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
- 239000003513 alkali Substances 0.000 description 1
- 229940040526 anhydrous sodium acetate Drugs 0.000 description 1
- 239000002585 base Substances 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
- 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
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000002360 preparation method Methods 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
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing 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
- 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
Abstract
The invention discloses a method for rapidly determining the content of sodium acetate in an industrial 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 of sodium acetate determination. The method adopts ultraviolet spectrophotometry to measure, and the measuring process comprises the following steps: drawing a standard curve: measuring sodium acetate standard use solutions with different concentrations respectively, adding a stabilizer, and measuring the absorbance of the standard use solutions at characteristic absorption wavelengths respectively; 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; taking an industrial sodium acetate solution sample, adding a stabilizer, and measuring the absorbance of the sample at a characteristic absorption wavelength; substituting the corrected absorbance into a standard curve fitting equation, and calculating to obtain the sodium acetate concentration of the sample solution. The invention has simple and rapid operation and low cost; the spectrophotometry for detecting the content of the sodium acetate solution is creatively invented by utilizing the spectral characteristics of the sodium acetate solution in a specific wavelength range, and a stabilizer is added into a detection system, so that the accuracy of a detection result and the anti-interference capability 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 sodium acetate solution.
Background
Sodium acetate is used as a common chemical and is widely applied to various fields of medicine, printing and dyeing, industrial catalysis, sewage treatment and the like. In practical application, enterprises generally directly purchase industrial sodium acetate solution for adding and using. Meanwhile, in the use process, the use amount of sodium acetate is often larger, the adding frequency is high, and the sodium acetate content is used as a key index for quality control of the industrial sodium acetate solution in the use process, so that the industrial sodium acetate solution needs to be rapidly analyzed and detected.
In the prior art, the sodium acetate content is generally measured by an acid-base titration method and an ion chromatography method. When the acid-base titration method is adopted, phenolphthalein is used as an indicator, sodium hydroxide is used for back titration, and the sodium acetate content is calculated. The method is easy to be interfered by impurities, has poor selectivity and is complex to operate. The sodium acetate content was measured by ion chromatography, the leacheate was suppressed by a suppressor, the background conductance was subtracted, and the measurement was performed by a conductivity meter. The method is time-consuming and has high cost.
Therefore, the method for determining the sodium acetate content in the industrial sodium acetate solution is quick, accurate and simple to operate, and is a problem to be solved urgently by those skilled in the art.
Disclosure of Invention
The invention aims to provide a method for rapidly determining the content of sodium acetate in an industrial sodium acetate solution, which solves the problems of complicated operation, high cost and long time consumption in the prior art.
In order to achieve the above 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 sodium acetate solution, which is determined by adopting an ultraviolet spectrophotometry and comprises the following steps:
s1, drawing a standard curve: respectively measuring standard use solutions of sodium acetate with different concentrations, adding a stabilizing agent, and uniformly mixing to obtain standard solutions to be tested with different concentrations; measuring the absorbance at the characteristic absorption wavelength respectively; deionized water is used as a blank control, and absorbance is measured by the same method; the absorbance of the standard use solution of sodium acetate with different concentrations is subtracted from the absorbance of the blank control to obtain standard solution corrected absorbance, the standard solution concentration is taken as an abscissa, the standard solution corrected absorbance is taken as an ordinate, and a standard curve is drawn;
s2, taking an industrial sodium acetate solution sample, adding a stabilizer, and uniformly mixing to obtain a sample solution to be detected; measuring the absorbance of the sample solution to be measured at the characteristic absorption wavelength; deionized water is used as a blank control, and absorbance is measured by the same method; subtracting the blank control absorbance from the sample absorbance to obtain a sample corrected absorbance;
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 present invention, the stabilizer comprises a solution formulated from one or more of potassium hydroxide, sodium hydroxide, potassium phosphate salt, sodium phosphate salt, tris, glycine, borax, boric acid, and 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 present invention, the stabilizer is a sodium hydroxide solution or a tris (hydroxymethyl) aminomethane solution having a pH of 9.
The invention discovers that sodium acetate is used as strong alkali weak acid salt, and is extremely easy to hydrolyze in water:
when the sodium acetate content in the industrial sodium acetate solution is measured by utilizing a spectrophotometry, a sample is often required to be diluted, so that sodium acetate is hydrolyzed to a certain extent, the equilibrium is shifted to the right, and sodium acetate is converted into acetic acid, so that the property of the solution is changed, and the accuracy of a measurement result is affected. In addition, industrial sodium acetate may have some residual raw material during the production process, which may also interfere with the determination of 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 sodium acetate hydrolysis, improving the accuracy of the measurement result and improving the anti-interference capability of the system.
In some embodiments of the invention, the characteristic absorption wavelength ranges from 190 to 210nm.
In some embodiments of the invention, the characteristic absorption wavelength is 191nm. .
The invention scans the sodium acetate with high purity by using a spectrophotometer within the wavelength range of 190-210nm, and selects the wavelength at the characteristic absorption peak as the wavelength for measuring the sodium acetate content.
The correlation coefficient r of the standard curve is more than or equal to 0.999.
In some embodiments of the invention, the concentration of the standard curve ranges from 0 to 100mg/L.
In some embodiments of the invention, each 50mL of standard solution to be tested contains 0.5-5 mL of stabilizer; preferably 1mL;
each 50mL of the sample solution to be measured contains 0.5-5 mL of stabilizer; preferably 1mL.
In order to reduce the chemical interference of the external substances to the system as much as possible, the detection accuracy needs to be improved, and the addition amount of the stabilizer needs to be proper. The inventors found that the addition of 1mL of stabilizer can meet the requirements.
In some embodiments of the present invention, in S2, the stabilizer is added after the industrial sodium acetate solution sample is diluted.
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 sample of the technical grade sodium acetate solution is diluted and then measured.
In some embodiments of the present invention, the mass concentration of sodium acetate in the technical grade sodium acetate solution is calculated as:
C＝[(A s -A b -a)/b]×f
wherein: c, the mass concentration of sodium acetate in the industrial sodium acetate solution, mg/L;
A s -absorbance of the sample solution;
A b absorbance of a blank control;
a-intercept of the calibration curve;
b-slope of the calibration curve;
f-dilution factor.
Compared with the prior art, the invention has the following beneficial effects:
the invention has scientific design and ingenious conception, and uses a single-wavelength spectrophotometry to directly measure the sodium acetate content in the industrial sodium acetate solution, and has simple and quick operation and low cost; the invention creatively utilizes the spectral characteristics of the sodium acetate solution under ultraviolet light with specific wavelength to invent a spectrophotometry method for detecting the content of the sodium acetate solution, and adds a stabilizer into a detection system to improve the accuracy of a detection result and the anti-interference capability 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 more clear, the technical solutions of the embodiments of the present invention will be clearly and completely described below. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
Example 1
The implementation provides a method for measuring sodium acetate content in an industrial sodium acetate solution, which comprises the following steps:
1. preparation of sodium acetate standard stock solution: 0.5000g of anhydrous sodium acetate is weighed and dissolved in water, transferred to a 1000mL volumetric flask, diluted with water to marked line and mixed well. The concentration of sodium acetate in the stock solution was 2000mg/L.
2. Standard use solution for preparing sodium acetate: 50.00mL of standard sodium acetate stock solution is measured into a 100mL volumetric flask, diluted with water to marked lines, and mixed uniformly for immediate use. The standard use solution concentration of sodium acetate is 1000mg/L.
3. Preparing a sodium acetate stabilizer solution: weighing sodium hydroxide, dissolving in water, and adjusting the pH to 9.
4. Selection of measurement wavelength: scanning of sodium acetate (100 mg/L) of superior purity with a spectrophotometer over the wavelength range 190-210nm showed maximum absorption peak at 191nm. 191nm was chosen as the measurement wavelength.
5. Drawing a standard curve: standard use solutions of 0.00, 0.50, 1.00, 2.00, 3.00, 4.00 and 5.00mL of sodium acetate are respectively measured and put into a 50mL of glass colorimetric tube with a stopper, and the corresponding sodium acetate contents are respectively 0.00, 0.50, 1.00, 2.00, 3.00, 4.00 and 5.00mg. Then 1.00mL of sodium hydroxide solution with pH value of 9 is added respectively, water is added for dilution to 50mL of marked line, and the mixture is covered and uniformly mixed. The absorbance was measured using a 10mm quartz cuvette with deionized water as reference and a single wavelength of 191nm on a spectrophotometer. After subtracting the absorbance of the blank experiment, a standard working curve is drawn with the corresponding sodium acetate concentration:
the resulting standard curve fitting equation is: a=0.00555 c-0.00954, r=0.9990.
6. Sample measurement: diluting an industrial sodium acetate solution sample (pH=8.2) 1250 times, measuring 20.00mL of the diluted sample in a 50mL glass colorimetric tube with a stopper, adding 1.00mL sodium hydroxide solution with a pH value of 9, measuring the pH value to be 7.7, and measuring according to the step 5 to obtain the absorbance to be 0.423;
7. blank test: deionized water was used instead of the technical grade sodium acetate solution sample, and the measurement was carried out in the same procedure as the technical grade sodium acetate solution sample, and the blank absorbance was measured to be 0.011.
8. In this example, the mass concentration of sodium acetate in the industrial sodium acetate solution sample is calculated as follows:
[(0.423-0.011)+0.00954]/0.00555×3125＝237253.60mg/L。
the mass fraction of the product is as follows:
[(237253.60×10 -3 )/(1000+237253.60×10 -3 )]×100％＝19.2％。
the industrial sodium acetate solution sample in this example was measured by acid-base titration to determine that the mass fraction of sodium acetate was 19.4%.
Example 2
The implementation provides the method for measuring the sodium acetate content in the technical sodium acetate solution,
in this example, compared with example 1, a tris solution was used as a stabilizer, and the pH of the solution was about 9, with the same conditions.
The standard curve fitting equation obtained in this embodiment is: a=0.00546c+0.01131, r=0.9997.
The absorbance of the sample of this example was 0.528;
the blank absorbance was 0.006.
The mass concentration of sodium acetate in the technical grade sodium acetate solution in the embodiment is calculated as follows:
[(0.528-0.006)-0.01131]/0.00546×3125＝292290.52mg/L。
the mass fraction of the product is as follows:
[(292290.52×10 -3 )/(1000+292290.52×10 -3 )]×100％＝22.6％。
the industrial sodium acetate solution sample in this example was measured by acid-base titration to determine that the mass fraction of sodium acetate was 22.4%.
The comparison of the results obtained by the method of the invention with the results obtained by the classical acid-base titration method is shown in the following table:
TABLE 1
As can be seen from the above table, the results obtained by the method are consistent with those obtained by the classical acid-base titration method, which shows that the method is accurate.
Comparative example 1
In this comparative example, compared with example 1, the pH value of the sample solution for measuring absorbance placed in the plug-ground glass cuvette was measured to be 6.7 without adding a stabilizer to both the standard solution and the sample solution to be measured; the rest conditions are 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 determined by an acid-base titration method, and the mass content of sodium acetate is 19.4%; the measurement result of the example 1 added with the stabilizer is consistent with the measurement result of the classical acid-base method, which is 19.2%; the measurement result of comparative example 1, in which the stabilizer was not added, was lower than 17.2%; as shown in table 2:
TABLE 2
The above 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 color changes made in the main design concept and spirit of the present invention are still consistent with the present invention, and all the technical problems to be solved are included in the scope of the present invention.
Claims (9)
1. The method for rapidly determining the sodium acetate content in the industrial sodium acetate solution is characterized by comprising the following steps of:
s1, drawing a standard curve: respectively measuring standard use solutions of sodium acetate with different concentrations, adding a stabilizing agent, and uniformly mixing to obtain standard solutions to be tested with different concentrations; measuring the absorbance at the characteristic absorption wavelength respectively; deionized water is used as a blank control, and absorbance is measured by the same method; the absorbance of the standard use solution of sodium acetate with different concentrations is subtracted from the absorbance of the blank control to obtain standard solution corrected absorbance, the standard solution concentration is taken as an abscissa, the standard solution corrected absorbance is taken as an ordinate, and a standard curve is drawn;
s2, taking an industrial sodium acetate solution sample, adding a stabilizer, and uniformly mixing to obtain a sample solution to be detected; measuring the absorbance of the sample solution to be measured at the characteristic absorption wavelength; deionized water is used as a blank control, and absorbance is measured by the same method; subtracting the blank control absorbance from the sample absorbance to obtain a sample corrected absorbance;
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 sodium acetate content in an industrial grade sodium acetate solution according to claim 1, wherein the stabilizer comprises one or more of potassium hydroxide, sodium hydroxide, potassium phosphate, sodium phosphate, tris, glycine, borax, boric acid, and hydrochloric acid.
3. A method for rapid determination of sodium acetate content in technical grade sodium acetate solution according to claim 2 wherein the stabilizer solution pH >7 and blank absorbance <0.100 at characteristic absorption wavelength.
4. The method for rapidly determining sodium acetate content in technical grade sodium acetate solution according to claim 1 wherein the characteristic absorption wavelength range is 190-210nm.
5. The method for rapidly determining sodium acetate content in an industrial grade sodium acetate solution according to claim 4, wherein the concentration of the standard curve is in the range of 0-100mg/L.
6. The method for rapidly determining sodium acetate content in industrial grade sodium acetate solution according to claim 5, wherein 0.5-5 mL of stabilizer is added into each 50mL of standard solution to be tested; preferably 1mL.
7. The method for rapidly determining sodium acetate content in industrial sodium acetate solution according to claim 6, wherein 0.5-5 mL of stabilizer is added into each 50mL of sample solution to be tested; preferably 1mL.
8. The method for rapidly determining sodium acetate content in an industrial sodium acetate solution according to claim 6, wherein in S2, a stabilizer is added after diluting the industrial sodium acetate solution sample.
9. The method for rapidly determining sodium acetate content in an industrial sodium acetate solution according to claim 7, wherein the concentration range of the standard curve is exceeded by the corrected absorbance of the sample obtained in S2, and the industrial sodium acetate solution sample is diluted and then determined.
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