CN112730294A - Method for rapidly determining total phenol content in dilute phenol water - Google Patents
Method for rapidly determining total phenol content in dilute phenol water Download PDFInfo
- Publication number
- CN112730294A CN112730294A CN202110165887.XA CN202110165887A CN112730294A CN 112730294 A CN112730294 A CN 112730294A CN 202110165887 A CN202110165887 A CN 202110165887A CN 112730294 A CN112730294 A CN 112730294A
- Authority
- CN
- China
- Prior art keywords
- phenol
- dilute
- water
- solution
- sample
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 title claims abstract description 61
- KSSNXJHPEFVKHY-UHFFFAOYSA-N phenol;hydrate Chemical compound O.OC1=CC=CC=C1 KSSNXJHPEFVKHY-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 238000000034 method Methods 0.000 title claims abstract description 44
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 46
- 239000000523 sample Substances 0.000 claims abstract description 37
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910052794 bromium Inorganic materials 0.000 claims abstract description 21
- 239000000243 solution Substances 0.000 claims abstract description 18
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 16
- 239000012086 standard solution Substances 0.000 claims abstract description 15
- 239000012488 sample solution Substances 0.000 claims abstract description 12
- 239000002253 acid Substances 0.000 claims abstract description 11
- 238000007865 diluting Methods 0.000 claims abstract description 10
- 239000012085 test solution Substances 0.000 claims abstract description 9
- 230000031700 light absorption Effects 0.000 claims abstract description 8
- 238000004364 calculation method Methods 0.000 claims abstract description 6
- 230000001502 supplementing effect Effects 0.000 claims abstract description 6
- 238000000870 ultraviolet spectroscopy Methods 0.000 claims abstract description 6
- 238000010790 dilution Methods 0.000 claims description 12
- 239000012895 dilution Substances 0.000 claims description 12
- 238000002835 absorbance Methods 0.000 claims description 10
- 239000010453 quartz Substances 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- 238000012417 linear regression Methods 0.000 claims description 2
- 150000002989 phenols Chemical class 0.000 abstract description 6
- 230000035945 sensitivity Effects 0.000 abstract description 3
- 238000005259 measurement Methods 0.000 description 15
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 description 15
- 238000012360 testing method Methods 0.000 description 12
- 238000004448 titration Methods 0.000 description 9
- 238000004458 analytical method Methods 0.000 description 8
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 description 7
- 235000019345 sodium thiosulphate Nutrition 0.000 description 7
- 238000002798 spectrophotometry method Methods 0.000 description 6
- 230000006872 improvement Effects 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 239000012153 distilled water Substances 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 2
- 229920002472 Starch Polymers 0.000 description 2
- 238000003556 assay Methods 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 229910052740 iodine Inorganic materials 0.000 description 2
- 239000011630 iodine Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical compound [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 235000019698 starch Nutrition 0.000 description 2
- 239000008107 starch Substances 0.000 description 2
- BSWWXRFVMJHFBN-UHFFFAOYSA-N 2,4,6-tribromophenol Chemical compound OC1=C(Br)C=C(Br)C=C1Br BSWWXRFVMJHFBN-UHFFFAOYSA-N 0.000 description 1
- XWNSFEAWWGGSKJ-UHFFFAOYSA-N 4-acetyl-4-methylheptanedinitrile Chemical compound N#CCCC(C)(C(=O)C)CCC#N XWNSFEAWWGGSKJ-UHFFFAOYSA-N 0.000 description 1
- 239000004153 Potassium bromate Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000003034 coal gas Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000009615 deamination Effects 0.000 description 1
- 238000006481 deamination reaction Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 238000005375 photometry Methods 0.000 description 1
- 150000008442 polyphenolic compounds Chemical class 0.000 description 1
- 235000013824 polyphenols Nutrition 0.000 description 1
- 229940094037 potassium bromate Drugs 0.000 description 1
- 235000019396 potassium bromate Nutrition 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 239000011550 stock solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- 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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a method for rapidly determining the content of total phenols in dilute phenol water, which comprises the following steps: taking 2.5mL of dilute phenol water sample, titrating the total phenol amount in the dilute phenol water by a bromine quantity method, and taking the total phenol amount as the concentration of a standard solution; taking 2.5mL of dilute phenol water sample, adding 1-10 mL of 0.01-5 mol/L acid, diluting with water to a constant volume 100mL volumetric flask, respectively transferring different amounts into a colorimetric tube, respectively supplementing 0.005mol/L hydrochloric acid solution until the total amount of the solution is 10mL, shaking up to obtain each test solution, using a reagent blank as a reference, carrying out colorimetric determination on each test solution on an ultraviolet visible spectrophotometer to determine the light absorption value of each test solution at the determination wavelength of 275mm, drawing a standard curve and linearly regressing to obtain a calculation formula; the phenol content of the sample solution was measured according to the standard curve. The method can rapidly measure the total phenol content in the dilute phenol water within 10 minutes, and has higher sensitivity and accuracy.
Description
Technical Field
The invention relates to the technical field of chemical analysis, in particular to a method for rapidly determining the content of total phenols in dilute phenol water.
Background
The crude gas generated by the crushed coal pressure gasification furnace is subjected to gas-water separation, deacidification and deamination, and then phenol extraction is carried out, and the water at the outlet of the phenol extraction tower is diluted phenol water. The main assay analysis index is total phenol content, which is the embodiment of phenol extraction efficiency and is also the main index of whether the phenol can enter a biochemical treatment system.
The total phenols in the coal gas water are a general term of compounds which can have hydroxyl (-OH) substituent groups in a benzene ring structure. Including monophenols and polyphenols, depending primarily on the number of hydroxyl groups present in the phenol. The total phenol content reflects whether the phenol content in the process discharge water exceeds the standard or not.
The measurement is carried out by taking a certain amount of sample, adding acid, adding bromine standard solution, reacting for 1 h in dark, adding potassium iodide solution, reacting for 10 min in dark, and titrating with sodium thiosulfate standard solution. Sampling, adding reagent, reacting, adding reagent, re-reacting, finally titrating, calculating and reporting data. The whole process generally needs 2.5-3 hours, which is greatly lagged behind the process adjustment, and especially in the driving stage, the analysis frequency is 1 time/2 hours, which can not meet the production requirement.
The measurement of phenol in water by ultraviolet spectrophotometry has been reported. For example, in the article "determination of phenol in wastewater by ultraviolet spectrophotometry", quantitative determination is carried out by using the ultraviolet absorption characteristics of a phenol aqueous solution and selecting a wavelength of 215nm as an absorption wavelength, and satisfactory results are obtained. In the text of ultraviolet spectrophotometry for the total phenol content in water, the wavelength of 235nm is selected for measurement, the recovery rate is 99-102%, and the result is accurate. The ultraviolet difference spectrophotometry for measuring the content of volatile phenol in water is also used for measuring by selecting the wavelength of 235nm, and when the sample contains para-phenol, a more accurate analysis result can be obtained.
The method for measuring the phenol content in the water by using the ultraviolet spectrophotometry has the characteristics of high accuracy, simplicity, rapidness and the like; however, the total phenols determined by the UV method described in the literature are determined under alkaline or neutral conditions using phenol as a standard solution, and the wavelengths selected are 215mm and 235mm as the determination wavelengths. However, the types of phenols in the dilute phenol water are more than twenty, the result of measuring the total phenol by using the ultraviolet method and the result of measuring the total phenol by using the bromine amount method only by using phenol as a standard solution are extremely inconsistent, and the method is not applied to the alternative application of measuring the total phenol by using the bromine amount method in the dilute phenol water.
Disclosure of Invention
In view of this, the present invention provides a method for rapidly determining the total phenol content in dilute phenol water, which can rapidly determine the total phenol content in dilute phenol water and has high sensitivity and accuracy.
In order to achieve the purpose of the invention, the technical scheme is as follows:
a method for rapidly determining the total phenol content in dilute phenol water comprises the following steps:
a) preparation of standard solution: taking 2.5mL of dilute phenol water sample, titrating total phenol in the dilute phenol water by a bromine quantity method to obtain the total phenol quantity, and taking the total phenol quantity as the concentration of a standard solution;
b) and (3) preparing a standard curve: taking 2.5mL of dilute phenol water sample, adding 1-10 mL of 0.01-5 mol/L acid, diluting with water to a constant volume 100mL volumetric flask, respectively transferring 0mL, 1.0mL, 2.0mL, 4.0mL, 6.0mL, 8.0mL and 10.0mL into a colorimetric tube, respectively supplementing 0.005mol/L hydrochloric acid solution 10.0mL, 9.0mL, 8.0mL, 6.0mL, 4.0mL, 2.0mL and 0mL, shaking uniformly to obtain each test solution, using a reagent blank as a reference, using a 10mm quartz cuvette, carrying out colorimetric determination on each test solution on an ultraviolet visible spectrophotometer, using the measured total phenol content as a concentration reference, dividing a value of a dilution multiple into a horizontal coordinate, drawing a standard curve at a determination wavelength of 275mm by using a vertical coordinate, and obtaining a linear regression calculation formula as follows:
C＝nKA (1)
in the formula:
c, total phenol concentration (mg/L) in the dilute phenol water to be detected;
n-dilution multiple;
k-is the inverse of the slope of the standard curve;
a-absorbance;
c) and (3) sample determination: taking 2.5mL of dilute phenol water sample, adding 1-10 mL of 0.01-5 mol/L acid, diluting with water and fixing the volume to a 100mL volumetric flask to obtain a sample solution, taking a reagent blank as a reference, adopting a 10mm quartz cuvette, carrying out colorimetric determination on the sample solution on an ultraviolet visible spectrophotometer to determine the light absorption value of the sample solution with the determination wavelength of 275mm, and determining the phenol content in the sample solution according to the standard curve obtained in the step b).
As a further improvement of the method, the dilution multiple of the dilute phenol water sample is 10-100 times.
As a further improvement of the method, the dilution multiple of the dilute phenol water sample is 25-50 times.
As a further improvement of the invention, the acid is one of hydrochloric acid, sulfuric acid and phosphoric acid.
As a further improvement of the invention, the acid is hydrochloric acid, the addition amount of the hydrochloric acid is 5mL, and the concentration of the hydrochloric acid is 0.1-0.5 mol/L.
The invention has the beneficial effects that: compared with the prior art, the invention provides a simple and rapid determination method, which can rapidly determine the total phenol content in the dilute phenol water within 10 minutes, guide the production operation in time and avoid that the dilute phenol water cannot enter a biochemical treatment system in time due to data lag. Compared with the bromine quantity method, the method has the advantages of time-saving and labor-saving operation, extremely high goodness of fit between the measurement result and the measurement result of the bromine quantity method, and saving a large amount of valuable reagents such as potassium bromate, potassium bromide, potassium iodide and the like. The method is simple to operate, and has high sensitivity and accuracy, so that the method has a wide application prospect.
Detailed Description
The following examples are intended to further illustrate the present invention and should not be construed as limiting the scope of the invention, and other insubstantial modifications and adaptations of the invention by those skilled in the art based on the teachings herein are intended to be covered thereby.
In the examples, the reagents used are analytically pure or more than analytically pure, and the water is distilled water or deionized water. In the following examples, reagents and instruments were commercially available and were operated according to the instructions unless otherwise specified.
A method for rapidly determining the total phenol content in dilute phenol water comprises the following steps:
a) preparation of standard solution: taking 2.5mL of a dilute phenol water sample with a dilution multiple of 25-50 times, titrating total phenol in the dilute phenol water by a bromine quantity method to obtain the amount of the total phenol, and taking the amount of the total phenol as the concentration of a standard solution;
b) and (3) preparing a standard curve: taking 2.5mL of dilute phenol water sample, adding 5mL of 0.1mol/L hydrochloric acid, diluting with water to a constant volume of 100mL volumetric flask, transferring 0mL, 1.0mL, 2.0mL, 4.0mL, 6.0mL, 8.0mL and 10.0mL into a colorimetric tube respectively, then respectively supplementing 10.0mL, 9.0mL, 8.0mL, 6.0mL, 4.0mL, 2.0mL and 0mL of hydrochloric acid solution 0.005mol/L, shaking uniformly to obtain each test solution, using a reagent blank as a reference, using a 10mm quartz cuvette, carrying out colorimetric determination on each test solution on a UV-visible spectrophotometer to obtain an absorbance value of 275mm in the determination wavelength, using the measured total phenol content as a concentration reference, dividing a value of a dilution multiple as a horizontal coordinate, drawing a standard curve at the determination wavelength of 275mm by using the absorbance value as a vertical coordinate, and linearly obtaining a regression formula:
C＝nKA (1)
in the formula:
c, total phenol concentration (mg/L) in the dilute phenol water to be detected;
n-dilution multiple;
k-is the inverse of the slope of the standard curve;
a-absorbance;
c) and (3) sample determination: taking 2.5mL of dilute phenol water sample, adding 5mL of 0.1 hydrochloric acid, diluting with water and fixing the volume to a 100mL volumetric flask to obtain a sample solution, taking a reagent blank as a reference, adopting a 10mm quartz cuvette, carrying out colorimetric determination on the sample solution on an ultraviolet visible spectrophotometer to obtain a light absorption value with a determination wavelength of 275mm, and determining the phenol content in the sample solution according to the standard curve obtained in the step b).
Measurement by bromine amount method
(1) The principle is as follows: under the acidic condition, adding excessive bromine into a sample, reacting the bromine with phenol to generate tribromophenol, reacting the residual unreacted bromine with potassium iodide to release free iodine, titrating with a sodium thiosulfate standard solution, and calculating the total phenol content according to the consumption. The main reaction is as follows:
Br2+2I-→I2+2Br- (3)
I2+2Na2S2O3→Na2S4O6+2NaI (4)
(2) reagent
a. Distilled or deionized water;
b. bromine standard titration solution: c (KBr-KBrO)3)＝0.1000mol/L。
c. Sodium thiosulfate standard titration solution: c (Na)2S2O3)＝0.1000mol/L。
d. Sulfuric acid solution: 1+1.
e. Potassium iodide solution: 10 percent.
f. Starch indicator fluid: 5 g/L.
(3) Analytical procedure
A proper amount of sample is taken and put into a 250mL iodine flask, 10mL (1+1) sulfuric acid solution is added, the iodine flask is slowly shaken, 25mL of bromine standard solution is added, and a water seal is covered. The mixture was left in dark for 1 hour. Then adding 10mL of 10% potassium iodide solution, sealing the cap with water, keeping the mixture in the dark for 10 minutes, titrating the mixture by using 0.1mol/L sodium thiosulfate standard titration solution, adding 1mL of starch indicator when the mixture is dripped to be light yellow, continuously titrating the mixture until the blue color fades, and recording the consumption volume. A blank test was carried out according to the above procedure using the same volume of distilled water instead of the sample.
(4) Calculation of results
The total phenol content in the sample (in terms of phenol) is expressed in g/L as follows:
in the formula: c-concentration of sodium thiosulfate standard titration solution, mol/L;
V0-blank test consumes volume of sodium thiosulfate standard solution, mL;
V1sample titration consumed sodium thiosulfate standard solution volume, mL;
v-sample volume, mL;
15.68-phenol (1/6C)6H5OH) molar mass, g/mol.
Second, ultraviolet photometry
(1) Principle of method
In an acid medium, phenols have a strong absorption peak at 275nm, and are measured by an ultraviolet spectrophotometry.
Taking 2.5mL of dilute phenol water sample, adding 5mL of 0.1mol/L hydrochloric acid, diluting to a constant volume to 100mL of volumetric flask, respectively transferring 0mL, 1.0mL, 2.0mL, 4.0mL, 6.0mL, 8.0mL and 10.0mL into a colorimetric tube, respectively supplementing 0.005mol/L hydrochloric acid solution of 10.0mL, 9.0mL, 8.0mL, 6.0mL, 4.0mL, 2.0mL and 0mL, shaking uniformly, measuring the light absorption value in a quartz cuvette with a reagent blank as a reference at 275nm and 10mm within 30 min.
And (3) determining the concentration of the total phenol content in the obtained diluted phenol water by a bromine amount method to be the concentration of the standard stock solution, taking the concentration of the diluted solution as an abscissa and the light absorption value as an ordinate, making a standard curve and linearly regressing to obtain a calculation formula.
(2) Determination of samples
Taking 2.5mL of dilute phenol water sample, adding 5mL0.1mol/L hydrochloric acid, diluting to a constant volume of 100mL volumetric flask, taking a reagent blank as a reference, and measuring the light absorption value in a 275nm and 10mm quartz cuvette.
(3) Calculation of analysis results
The phenol content of the dilute phenol water is calculated according to the following formula:
C＝nKA (1)
in the formula:
c, total phenol concentration (mg/L) in the dilute phenol water to be detected;
n-dilution multiple;
k-is the inverse of the slope of the standard curve;
a-absorbance;
third, test results
The sample assay and control results are shown in table 1:
TABLE 1 sample measurement and control results
As can be seen from Table 1, the error between the ultraviolet method measurement result and the bromine quantity method measurement result is basically within 5 percent, and the coincidence degree of the two results is high. Can meet the requirement of control analysis in the middle of production.
Fourth, result analysis
(1) And (3) wavelength test:
1mL of dilute phenol water sample is put into a 100mL volumetric flask, 5mL of hydrochloric acid (0.1moL/L) is added, the solution is diluted to a scale mark and shaken up, and a wavelength experiment is carried out, wherein the wavelength experiment data are shown in Table 2.
TABLE 2 wavelength test data sheet
The experimental data of wavelength in Table 2 show that the absorption maximum is 275 nm.
(2) Acidity test
1mL of a dilute phenol aqueous sample was taken out and put in a 100mL volumetric flask, 1mL, 2mL, 3mL, 4mL, 5mL, and 10mL of 0.1moL/L hydrochloric acid was added thereto, and the volume was adjusted to the marked line with demineralized water, and the measured absorbance was as shown in Table 3.
Table 3 acidity test data table
| Volume (mL) | 1 | 2 | 3 | 4 | 5 | 10 |
| Absorbance value | 0.410 | 0.418 | 0.414 | 0.416 | 0.411 | 0.419 |
From the data, it can be seen that, when 0.1moL/L hydrochloric acid of 1mL to 10mL is added, the absorbance has no obvious change, and in order to better eliminate the background color, the addition amount of the hydrochloric acid in the experiment is determined to be 5 mL.
(3) Stability test
The same sample was subjected to the test for different times, and the results are shown in Table 4.
Table 4 time test table
| 1mL | 2mL | 4mL | 6mL | 8mL | 10mL | |
| 1min | 0.070 | 0.142 | 0.285 | 0.430 | 0.565 | 0.702 |
| 10min | 0.072 | 0.142 | 0.281 | 0.429 | 0.565 | 0.701 |
| 15min | 0.075 | 0.142 | 0.283 | 0.430 | 0.567 | 0.703 |
| 20min | 0.074 | 0.145 | 0.285 | 0.434 | 0.570 | 0.708 |
| 30min | 0.073 | 0.143 | 0.284 | 0.428 | 0.565 | 0.700 |
From the above data, the absorbance values of this experiment were stable for 30 min.
(4) Reproducibility test
The same sample was measured three times in succession, and the results are shown in Table 5.
TABLE 5 reproducibility test data sheet
| 1mL | 2mL | 4mL | 6mL | 8mL | 10mL | |
| 1 | 0.063 | 0.115 | 0.226 | 0.332 | 0.441 | 0.549 |
| 2 | 0.065 | 0.111 | 0.221 | 0.330 | 0.442 | 0.547 |
| 3 | 0.065 | 0.115 | 0.225 | 0.330 | 0.437 | 0.546 |
And the same sample is tested for three times to obtain the sample with good measurement repeatability when different volumes are taken.
(5) Linear test
Taking 2.5mL of dilute phenol water sample, adding 5mL of 0.1mol/L hydrochloric acid, diluting to a constant volume of 100mL, respectively transferring 0mL, 1.0mL, 2.0mL, 4.0mL, 6.0mL, 8.0mL and 10.0mL into a colorimetric tube, respectively supplementing 10.0mL, 9.0mL, 8.0mL, 6.0mL, 4.0mL, 2.0mL and 0mL of hydrochloric acid solution with 0.005mol/L, shaking uniformly, measuring the light absorption value in a quartz cuvette with the thickness of 275nm and 10mm by taking a reagent blank as a reference within 30 minutes. The measurement data are shown in tables 6 to 9.
Example 1: diluted phenol water (91)#2020.12.21 titration by bromine method: 572mg/L)
Table 6 measurement data of example 1
Example 2: diluted phenol water (92)#2020.12.21 titration by bromine method:623mg/L)
TABLE 7 measurement data of example 2
Example 3: diluted phenol water (92)#2020.12.21 titration by bromine method: 591mg/L)
Table 8 measurement data of example 3
Example 4: diluted phenol water (92)#2020.12.20 titration by bromine method: 633mg/L)
TABLE 9 measurement data of example 4
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (5)
1. A method for rapidly determining the total phenol content in dilute phenol water is characterized by comprising the following steps:
a) preparation of standard solution: taking 2.5mL of dilute phenol water sample, titrating total phenol in the dilute phenol water by a bromine quantity method to obtain the total phenol quantity, and taking the total phenol quantity as the concentration of a standard solution;
b) and (3) preparing a standard curve: taking 2.5mL of dilute phenol water sample, adding 1-10 mL of 0.01-5 mol/L acid, diluting with water to a constant volume 100mL volumetric flask, respectively transferring 0mL, 1.0mL, 2.0mL, 4.0mL, 6.0mL, 8.0mL and 10.0mL into a colorimetric tube, respectively supplementing 0.005mol/L hydrochloric acid solution 10.0mL, 9.0mL, 8.0mL, 6.0mL, 4.0mL, 2.0mL and 0mL, shaking uniformly to obtain each test solution, using a reagent blank as a reference, using a 10mm quartz cuvette, carrying out colorimetric determination on each test solution on an ultraviolet visible spectrophotometer, using the measured total phenol content as a concentration reference, dividing a value of a dilution multiple into a horizontal coordinate, drawing a standard curve at a determination wavelength of 275mm by using a vertical coordinate, and obtaining a linear regression calculation formula as follows:
C＝nKA (1)
in the formula:
c, total phenol concentration (mg/L) in the dilute phenol water to be detected;
n-dilution multiple;
k-is the inverse of the slope of the standard curve;
a-absorbance;
c) and (3) sample determination: taking 2.5mL of dilute phenol water sample, adding 1-10 mL of 0.01-5 mol/L acid, diluting with water and fixing the volume to a 100mL volumetric flask to obtain a sample solution, taking a reagent blank as a reference, adopting a 10mm quartz cuvette, carrying out colorimetric determination on the sample solution on an ultraviolet visible spectrophotometer to determine the light absorption value of the sample solution with the determination wavelength of 275mm, and determining the phenol content in the sample solution according to the standard curve obtained in the step b).
2. The method for rapidly determining the total phenol content in the dilute phenol water according to claim 1, wherein the dilution factor of the dilute phenol water sample is 10-100 times.
3. The method for rapidly determining the total phenol content in the dilute phenol water according to claim 2, wherein the dilution factor of the dilute phenol water sample is 25-50 times.
4. The method for rapidly determining the total phenol content in the dilute phenol water as claimed in claim 1, wherein the acid is one of hydrochloric acid, sulfuric acid and phosphoric acid.
5. The method for rapidly determining the total phenol content in dilute phenol water as claimed in claim 4, wherein the acid is hydrochloric acid, the addition amount of the hydrochloric acid is 5mL, and the concentration of the hydrochloric acid is 0.1 mol/L-0.5 mol/L.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110165887.XA CN112730294A (en) | 2021-02-06 | 2021-02-06 | Method for rapidly determining total phenol content in dilute phenol water |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110165887.XA CN112730294A (en) | 2021-02-06 | 2021-02-06 | Method for rapidly determining total phenol content in dilute phenol water |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112730294A true CN112730294A (en) | 2021-04-30 |
Family
ID=75596133
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110165887.XA Pending CN112730294A (en) | 2021-02-06 | 2021-02-06 | Method for rapidly determining total phenol content in dilute phenol water |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112730294A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114813603A (en) * | 2022-03-09 | 2022-07-29 | 南京林业大学 | Method for rapidly representing halogenation conversion rate of phenolic hydroxyl compounds without standard substance |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1057817A1 (en) * | 1982-05-21 | 1983-11-30 | Уральский Научно-Исследовательский Институт Комплексного Использования И Охраны Водных Ресурсов | Method of quantitative determination of phenols in natural waters |
| US4913821A (en) * | 1989-04-27 | 1990-04-03 | The Dow Chemical Company | Method for the determination of phenols in water |
| SU1578604A1 (en) * | 1988-07-18 | 1990-07-15 | Всесоюзный научно-исследовательский институт углеводородного сырья | Method of determining phenol |
| RU2533322C1 (en) * | 2013-07-12 | 2014-11-20 | Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Омский государственный университет им. Ф.М. Достоевского" | Method of determining total content of phenoles in waters |
| CN104374728A (en) * | 2014-09-29 | 2015-02-25 | 陕西华陆化工环保有限公司 | Method for detecting volatile phenol content of water |
| CN105021608A (en) * | 2015-08-20 | 2015-11-04 | 昆明理工大学 | Kit for detecting total polyphenol content in beverage, preparation method of kit and method for detecting total polyphenol content in beverage using kit |
| CN109444065A (en) * | 2018-12-21 | 2019-03-08 | 天津利海石化有限公司 | The measuring method of phenol content in by-product concentrated hydrochloric acid |
-
2021
- 2021-02-06 CN CN202110165887.XA patent/CN112730294A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1057817A1 (en) * | 1982-05-21 | 1983-11-30 | Уральский Научно-Исследовательский Институт Комплексного Использования И Охраны Водных Ресурсов | Method of quantitative determination of phenols in natural waters |
| SU1578604A1 (en) * | 1988-07-18 | 1990-07-15 | Всесоюзный научно-исследовательский институт углеводородного сырья | Method of determining phenol |
| US4913821A (en) * | 1989-04-27 | 1990-04-03 | The Dow Chemical Company | Method for the determination of phenols in water |
| RU2533322C1 (en) * | 2013-07-12 | 2014-11-20 | Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Омский государственный университет им. Ф.М. Достоевского" | Method of determining total content of phenoles in waters |
| CN104374728A (en) * | 2014-09-29 | 2015-02-25 | 陕西华陆化工环保有限公司 | Method for detecting volatile phenol content of water |
| CN105021608A (en) * | 2015-08-20 | 2015-11-04 | 昆明理工大学 | Kit for detecting total polyphenol content in beverage, preparation method of kit and method for detecting total polyphenol content in beverage using kit |
| CN109444065A (en) * | 2018-12-21 | 2019-03-08 | 天津利海石化有限公司 | The measuring method of phenol content in by-product concentrated hydrochloric acid |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114813603A (en) * | 2022-03-09 | 2022-07-29 | 南京林业大学 | Method for rapidly representing halogenation conversion rate of phenolic hydroxyl compounds without standard substance |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103163127A (en) | Method for detecting trivalent arsenic by protoheme horseradish peroxidase catalytic colorimetry | |
| CN112730294A (en) | Method for rapidly determining total phenol content in dilute phenol water | |
| CN101576501A (en) | Method for determining volatile phenol in water | |
| CN108680541A (en) | A kind of fluorescence molybdenum oxide quantum dot measurement determination of trace uranium（Ⅵ）Method | |
| CN103293114A (en) | Visual colorimetry for determination of phosphates | |
| Hanker et al. | Fluorometric and colorimetric estimation of cyanide and sulfide by demasking reactions of palladium chelates | |
| CN102221530A (en) | Method for automatically analyzing sulfide in water sample | |
| CN112179858A (en) | Water quality detection method based on turbidity compensation technology | |
| CN110132949A (en) | The method for measuring cement plant flue gas the escaping of ammonia | |
| CN111912800B (en) | Method for detecting low-concentration ammonia nitrogen in drinking water | |
| CN112255225A (en) | Method for testing COD (chemical oxygen demand) of organic matters in iron-containing waste hydrochloric acid | |
| CN109374608B (en) | Method for detecting amine collecting agent by spectrophotometry | |
| CN110441243A (en) | It is a kind of based on film enrichment and UV-vis DRS spectrum underwater trace copper ion quantitative analysis method | |
| CN118032742A (en) | Method for detecting chloride content in industrial potassium nitrate by ICP-OES | |
| He et al. | Precise and sensitive determination of nitrite by coulometric backtitration under flow conditions | |
| KR20240016488A (en) | A Low concentration hydrogen peroxide detection kit and the low concentration hydrogen peroxide detection method using the same | |
| CN111948165B (en) | Method for detecting hypochlorite ions of construction material based on optical probe | |
| CN110749574B (en) | Method for measuring perfluorooctane sulfonate by dual-wavelength resonance Rayleigh scattering method and application | |
| CN110501293B (en) | Ethanol detection method and kit | |
| CN103018184A (en) | Method for measuring trace amount of bromate in water | |
| RU2817516C1 (en) | Method of determining barium ions in formation water | |
| CN113567367B (en) | Method for rapidly detecting manganese content in water | |
| US11022557B2 (en) | Test kit for detecting arsenic | |
| CN113484260A (en) | Method for measuring fluoride in water by spectrophotometry | |
| CN117907315A (en) | Phosphate radical detection reagent, detection kit and detection method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |