CN110646360A - Method for measuring concentrations of bisphenol A, bisphenol S and bisphenol AF - Google Patents
Method for measuring concentrations of bisphenol A, bisphenol S and bisphenol AF Download PDFInfo
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- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 title claims abstract description 370
- ZFVMWEVVKGLCIJ-UHFFFAOYSA-N bisphenol AF Chemical compound C1=CC(O)=CC=C1C(C(F)(F)F)(C(F)(F)F)C1=CC=C(O)C=C1 ZFVMWEVVKGLCIJ-UHFFFAOYSA-N 0.000 title claims abstract description 193
- VPWNQTHUCYMVMZ-UHFFFAOYSA-N 4,4'-sulfonyldiphenol Chemical compound C1=CC(O)=CC=C1S(=O)(=O)C1=CC=C(O)C=C1 VPWNQTHUCYMVMZ-UHFFFAOYSA-N 0.000 title claims abstract description 155
- 238000000034 method Methods 0.000 title claims abstract description 45
- 239000012086 standard solution Substances 0.000 claims abstract description 173
- 238000010521 absorption reaction Methods 0.000 claims abstract description 109
- 238000000862 absorption spectrum Methods 0.000 claims abstract description 101
- 239000000243 solution Substances 0.000 claims abstract description 89
- 239000007864 aqueous solution Substances 0.000 claims description 29
- 239000011550 stock solution Substances 0.000 claims description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 238000002835 absorbance Methods 0.000 claims description 13
- 238000012545 processing Methods 0.000 claims description 12
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 10
- 238000005303 weighing Methods 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000009795 derivation Methods 0.000 claims description 4
- 238000010790 dilution Methods 0.000 claims description 3
- 239000012895 dilution Substances 0.000 claims description 3
- 238000001514 detection method Methods 0.000 abstract description 21
- 230000008569 process Effects 0.000 abstract description 13
- 238000004458 analytical method Methods 0.000 abstract description 4
- 238000005375 photometry Methods 0.000 abstract description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 12
- 238000011084 recovery Methods 0.000 description 11
- 229930185605 Bisphenol Natural products 0.000 description 10
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 7
- 239000004033 plastic Substances 0.000 description 6
- 229920003023 plastic Polymers 0.000 description 6
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 239000012634 fragment Substances 0.000 description 4
- 239000006228 supernatant Substances 0.000 description 3
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- -1 bisphenol compound Chemical class 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
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- 230000007613 environmental effect Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000000589 high-performance liquid chromatography-mass spectrometry Methods 0.000 description 2
- 229910052740 iodine Inorganic materials 0.000 description 2
- 239000011630 iodine Substances 0.000 description 2
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 2
- 235000019341 magnesium sulphate Nutrition 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000008213 purified water Substances 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 239000012224 working solution Substances 0.000 description 2
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000013375 chromatographic separation Methods 0.000 description 1
- 231100000049 endocrine disruptor Toxicity 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000001076 estrogenic effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000005003 food packaging material Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000002372 labelling Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- CFNHVUGPXZUTRR-UHFFFAOYSA-N n'-propylethane-1,2-diamine Chemical compound CCCNCCN CFNHVUGPXZUTRR-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000001632 sodium acetate Substances 0.000 description 1
- 235000017281 sodium acetate Nutrition 0.000 description 1
- 239000002904 solvent Substances 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
-
- 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
- G01N21/314—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry with comparison of measurements at specific and non-specific wavelengths
-
- 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
- G01N21/314—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry with comparison of measurements at specific and non-specific wavelengths
- G01N2021/3148—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry with comparison of measurements at specific and non-specific wavelengths using three or more wavelengths
Abstract
The invention provides a method for measuring the concentration of bisphenol A, bisphenol S and bisphenol AF, which relates to the technical field of analysis and detection and comprises the following steps: s1: respectively preparing bisphenol A standard solutions, bisphenol S standard solutions and bisphenol AF standard solutions with different concentrations; s2: respectively obtaining derivative ultraviolet absorption spectrograms of various standard solutions with different concentrations; s3: establishing a standard curve according to the concentration of each standard solution and the absorption spectrum derivative value of each solution at the zero wavelength; s4: and calculating the concentration of bisphenol A, the concentration of bisphenol S and the concentration of bisphenol AF in the sample to be detected according to the absorption spectrum derivative value of the solution to be detected at the zero wavelength and the standard curve. The derivative photometry is used for detection, a large instrument is not needed in the detection process, and the detection method is simple, convenient, low in price and environment-friendly.
Description
Technical Field
The invention relates to the technical field of analysis and detection, and particularly relates to a method for measuring the concentrations of bisphenol A, bisphenol S and bisphenol AF.
Background
Bisphenol a is a chemical widely used as a monomer for producing plastic polymers, is widely used as a plasticizer in plastics, and bisphenol S, bisphenol AF and the like are widely used in the production of food packaging materials, containers and the like as substitutes for bisphenol a. The bisphenol compounds have estrogen-like action and are potential hazards to human health and ecological environment as typical environmental endocrine disruptors. In recent years, exposure of baby bottles to the bisphenol A substance has attracted attention to bisphenol endocrine disrupters. Therefore, the method has important ecological environmental protection value for enhancing the detection of the bisphenol substances, and has important significance for establishing a simple, convenient, rapid and efficient detection method.
At present, chromatographic separation methods are adopted for simultaneously detecting bisphenol A, bisphenol S and bisphenol AF, required instruments are complex, and the detection process is not convenient enough.
Disclosure of Invention
The invention solves the problem that the detection process of the method for simultaneously detecting bisphenol A, bisphenol S and bisphenol AF is not convenient enough.
In order to solve the above problems, the present invention provides a method for measuring the concentrations of bisphenol a, bisphenol S, and bisphenol AF, comprising the steps of:
s1: respectively preparing bisphenol A standard solutions, bisphenol S standard solutions and bisphenol AF standard solutions with different concentrations;
s2: respectively obtaining derivative ultraviolet absorption spectrograms of the bisphenol A standard solution, the bisphenol S standard solution and the bisphenol AF standard solution with different concentrations;
s3: establishing a standard curve according to the concentration of the bisphenol A standard solution, the concentration of the bisphenol S standard solution, the concentration of the bisphenol AF standard solution and the absorption spectrum derivative value of each solution at a zero wavelength;
s4: and calculating the concentration of bisphenol A, the concentration of bisphenol S and the concentration of bisphenol AF in the sample to be detected according to the absorption spectrum derivative value of the solution to be detected at the zero wavelength and the standard curve.
The derivative photometry is used for detection, a large instrument is not needed in the detection process, and the detection method is simple, convenient, low in price and environment-friendly.
Optionally, the step S1 includes:
s1-1: respectively weighing bisphenol A, bisphenol S and bisphenol AF, respectively adding absolute ethyl alcohol and water, dissolving and fixing the volume to obtain a bisphenol A stock solution, a bisphenol S stock solution and a bisphenol AF stock solution;
s1-2: and respectively adding water into the bisphenol A stock solution, the bisphenol S stock solution and the bisphenol AF stock solution for dilution, and preparing bisphenol A aqueous solution, bisphenol S aqueous solution and bisphenol AF aqueous solution with different concentrations.
Optionally, the step S1 further includes:
s1-3: respectively adding ammonia solutions into the bisphenol A aqueous solution, the bisphenol S aqueous solution and the bisphenol AF aqueous solution with different concentrations to obtain the bisphenol A standard solution, the bisphenol S standard solution and the bisphenol AF standard solution with different concentrations.
Optionally, step S2 includes:
s2-1: respectively measuring the absorbances of the bisphenol A standard solution, the bisphenol S standard solution and the bisphenol AF standard solution with different concentrations to obtain ultraviolet absorption spectrograms of the bisphenol A standard solution, the bisphenol S standard solution and the bisphenol AF standard solution with different concentrations;
s2-2: and respectively carrying out derivation data processing on the ultraviolet absorption spectrograms to obtain first derivative ultraviolet absorption spectrograms and third derivative ultraviolet absorption spectrograms of the bisphenol A standard solution, the bisphenol S standard solution and the bisphenol AF standard solution with different concentrations.
Optionally, step S3 includes:
s3-1: establishing a first standard curve equation of the bisphenol A according to the concentration of the bisphenol A standard solution and the first derivative value of the absorption spectrum of the bisphenol A standard solution with different concentrations at a first zero wavelength through a first derivative ultraviolet absorption spectrogram of the bisphenol A standard solution;
s3-2: establishing a second standard curve equation of the bisphenol A according to the concentration of the bisphenol A standard solution and the first derivative value of the absorption spectrum of the bisphenol A standard solution with different concentrations at a second zero wavelength through the first derivative ultraviolet absorption spectrogram of the bisphenol A standard solution;
s3-3: establishing a bisphenol AF (AF) first standard curve equation according to the concentration of the bisphenol AF standard solution and the absorption spectrum first derivative value of the bisphenol AF standard solution with different concentrations at the first zero wavelength through a first derivative ultraviolet absorption spectrogram of the bisphenol AF standard solution;
s3-4: establishing a bisphenol S standard curve equation according to the concentration of the bisphenol S standard solution and the first derivative value of the absorption spectrum of the bisphenol S standard solution with different concentrations at the second zero wavelength through the first derivative ultraviolet absorption spectrogram of the bisphenol S standard solution;
s3-5: and establishing a second standard curve equation of the bisphenol AF according to the concentration of the bisphenol AF standard solution and the absorption spectrum third-order derivative values of the bisphenol AF standard solution with different concentrations at a third zero wavelength through a third-order derivative ultraviolet absorption spectrogram of the bisphenol AF standard solution.
Optionally, the first zero wavelength is 263 nm; the second zero wavelength is 272 nm; the third zero wavelength is 245 nm.
Optionally, the bisphenol A first standard curve equation is CA-2548.6B + 0.4691; the second standard curve equation of the bisphenol A is CA5138D + 0.5375; wherein C isAIs the concentration of bisphenol A, and the unit is mg/mL; b is the first derivative value of the absorption spectrum of the bisphenol A standard solution at the first zero wavelength; d is the first derivative value of the absorption spectrum of the bisphenol A standard solution at the second zero wavelength.
Optionally, the bisphenol AF first standard curve equation is
CAF＝-391.49A-0.2822；
The second standard curve equation of the bisphenol AF is CAF-12165E-0.4491; wherein C isAFIs the concentration of bisphenol AF in mg/mL; a is the first derivative value of the absorption spectrum of the bisphenol AF standard solution at a first zero wavelength; and E is the third derivative value of the absorption spectrum of the bisphenol AF standard solution at the third zero wavelength.
Optionally, the bisphenol S standard curve equation is CS395.73C + 0.6785; wherein C isSIs the concentration of bisphenol S, and the unit is mg/mL;c is the first derivative value of the absorption spectrum of the bisphenol S standard solution at the second zero wavelength.
Optionally, step S4 includes:
s4-1: measuring the absorbance of the solution to be measured to obtain an ultraviolet absorption spectrogram of the solution to be measured;
s4-2: performing derivative data processing on the ultraviolet absorption spectrogram of the solution to be detected to obtain a first derivative ultraviolet absorption spectrogram and a third derivative ultraviolet absorption spectrogram of the solution to be detected;
s4-3: calculating the concentration of the bisphenol AF in the solution to be detected according to the third derivative ultraviolet absorption spectrogram and the bisphenol AF second standard curve equation;
s4-4: calculating the concentration of the bisphenol A in the solution to be detected according to the concentration of the bisphenol AF in the solution to be detected, the first derivative ultraviolet absorption spectrogram, the second standard curve equation of the bisphenol AF and the first standard curve equation of the bisphenol A;
s4-5: and calculating the concentration of the bisphenol S in the solution to be detected according to the concentration of the bisphenol A in the solution to be detected, the first derivative ultraviolet absorption spectrogram, the second standard curve equation of the bisphenol A and the standard curve equation of the bisphenol S.
Compared with the prior art, the method for measuring the concentrations of bisphenol A, bisphenol S and bisphenol AF provided by the invention has the following advantages:
according to the method for measuring the concentrations of the bisphenol A, the bisphenol S and the bisphenol AF, provided by the invention, the ultraviolet absorption spectrogram and the derivative ultraviolet absorption spectrogram of standard solutions of the bisphenol A, the bisphenol S and the bisphenol AF are researched, and a standard curve is established by using a derivative photometry according to the concentration of the bisphenol A, the concentration of the bisphenol S, the concentration of the bisphenol AF and the absorption spectrum derivative value at the zero wavelength respectively, so that the concentration of the bisphenol A, the concentration of the bisphenol S and the concentration of the bisphenol AF in the solution can be simultaneously calculated according to the absorption spectrum derivative value of the solution to be measured at the zero wavelength, a large instrument is not needed in the detection process, and the detection method is simple, convenient, low in price and green and environment-friendly.
Drawings
FIG. 1 is a diagram showing ultraviolet absorption spectra of bisphenol A, bisphenol S and bisphenol AF according to the present invention;
FIG. 2 is a first derivative ultraviolet absorption spectrum of bisphenol A, bisphenol S and bisphenol AF in accordance with the present invention;
FIG. 3 is a third derivative ultraviolet absorption spectrum of bisphenol A, bisphenol S and bisphenol AF in accordance with the present invention.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below.
In order to solve the problem that the existing method for simultaneously measuring bisphenol A, bisphenol S and bisphenol AF is not convenient enough in the detection process, the invention provides a method for measuring the concentrations of bisphenol A, bisphenol S and bisphenol AF, which comprises the following steps:
s1: respectively preparing bisphenol A standard solutions, bisphenol S standard solutions and bisphenol AF standard solutions with different concentrations;
s2: respectively obtaining derivative ultraviolet absorption spectrograms of bisphenol A standard solution, bisphenol S standard solution and bisphenol AF standard solution with different concentrations;
s3: establishing a standard curve according to the concentration of the bisphenol A standard solution, the concentration of the bisphenol S standard solution, the concentration of the bisphenol AF standard solution and the absorption spectrum derivative value of each solution at the zero wavelength;
s4: and calculating the concentration of bisphenol A, the concentration of bisphenol S and the concentration of bisphenol AF in the sample to be detected according to the absorption spectrum derivative value of the solution to be detected at the zero wavelength and the standard curve.
The zero wavelength refers to the wavelength which can be used for simultaneously calculating the concentrations of bisphenol A, bisphenol S and bisphenol AF according to the characteristics of the ultraviolet absorption spectrogram and the derivative spectrogram of each standard solution.
By respectively preparing a series of bisphenol A standard solutions with different concentrations, a series of bisphenol S standard solutions with different concentrations and a series of bisphenol AF standard solutions with different concentrations, further respectively obtaining derivative ultraviolet absorption spectrograms of the bisphenol A standard solutions with different concentrations, derivative ultraviolet absorption spectrograms of the bisphenol S standard solutions with different concentrations and derivative ultraviolet absorption spectrograms of the bisphenol AF standard solutions with different concentrations, selecting a zero wavelength, respectively establishing a bisphenol A standard curve for the concentration of the bisphenol A standard solution and the absorption spectrum derivative value of the bisphenol A standard solution at the zero wavelength, establishing a bisphenol S standard curve for the concentration of the bisphenol S standard solution and the absorption spectrum derivative value of the bisphenol S standard solution at the zero wavelength, establishing a bisphenol AF standard curve for the concentration of the bisphenol AF standard solution and the absorption spectrum derivative value of the bisphenol AF standard solution at the zero wavelength; and then obtaining an absorption derivative spectrogram of the solution to be detected, obtaining an absorption spectrum derivative value of the solution to be detected at a zero wavelength according to the absorption derivative spectrogram of the solution to be detected, and combining the absorption spectrum derivative value of the solution to be detected at the zero wavelength with the standard curve respectively to obtain the concentration of the bisphenol A, the concentration of the bisphenol S and the concentration of the bisphenol AF.
According to the method for measuring the concentrations of the bisphenol A, the bisphenol S and the bisphenol AF, provided by the invention, the ultraviolet absorption spectrogram and the derivative ultraviolet absorption spectrogram of standard solutions of the bisphenol A, the bisphenol S and the bisphenol AF are researched, and a standard curve is established by using a derivative photometry according to the concentration of the bisphenol A, the concentration of the bisphenol S, the concentration of the bisphenol AF and the absorption spectrum derivative value at the zero wavelength respectively, so that the concentration of the bisphenol A, the concentration of the bisphenol S and the concentration of the bisphenol AF in the solution can be simultaneously calculated according to the absorption spectrum derivative value of the solution to be measured at the zero wavelength, a large instrument is not needed in the detection process, and the detection method is simple, convenient, low in price and green and environment-friendly.
Specifically, the process of preparing the standard solution in step S1 includes:
s1-1: respectively weighing bisphenol A, bisphenol S and bisphenol AF, respectively adding absolute ethyl alcohol and water, dissolving and fixing the volume to obtain a bisphenol A stock solution, a bisphenol S stock solution and a bisphenol AF stock solution;
s1-2: and respectively taking a certain amount of the bisphenol A stock solution, the bisphenol S stock solution and the bisphenol AF stock solution, adding water for dilution, and preparing bisphenol A aqueous solution, bisphenol S aqueous solution and bisphenol AF aqueous solution with different concentrations.
In order to improve the detection accuracy, the water in the invention specifically refers to secondary deionized water; a series of bisphenol A aqueous solutions with different concentrations, a series of bisphenol S aqueous solutions with different concentrations and a series of bisphenol AF aqueous solutions with different concentrations are prepared respectively, and the aqueous solutions with different concentrations are used as standard solutions to establish a standard curve so as to respectively search the relationship between the concentration of bisphenol A and the absorption spectrum derivative value at the zero-point wavelength, the relationship between the concentration of bisphenol S and the absorption spectrum derivative value at the zero-point wavelength and the relationship between the concentration of bisphenol AF and the absorption spectrum derivative value at the zero-point wavelength.
Because the maximum absorption wavelength of bisphenol A, bisphenol S and bisphenol AF in the ammonia solution is red-shifted, the absorbance signal is obviously increased compared with the absorbance signal under the same concentration condition in the aqueous solution, the absorbance performance is stable, and in order to improve the sensitivity of detecting the bisphenol substances by a photometric method, the step S1 in the invention also comprises the following steps:
s1-3: and respectively adding ammonia solutions into bisphenol A aqueous solutions, bisphenol S aqueous solutions and bisphenol AF aqueous solutions with different concentrations to obtain bisphenol A standard solutions, bisphenol S standard solutions and bisphenol AF standard solutions with different concentrations.
Namely, by adding the ammonia solution and taking the bisphenol A ammonia solution, the bisphenol S ammonia solution and the bisphenol AF ammonia solution with different concentrations as standard solutions, the relation between the concentration of the bisphenol A and the absorption spectrum derivative value at the zero point wavelength, the relation between the concentration of the bisphenol S and the absorption spectrum derivative value at the zero point wavelength and the relation between the concentration of the bisphenol AF and the absorption spectrum derivative value at the zero point wavelength are respectively searched, the operation process is simple, and the sensitivity is high.
Specifically, the step S2 of obtaining the derivative ultraviolet absorption spectrogram of each standard solution includes:
s2-1: respectively measuring the absorbances of the bisphenol A standard solution, the bisphenol S standard solution and the bisphenol AF standard solution with different concentrations to obtain ultraviolet absorption spectrograms of the bisphenol A standard solution, the bisphenol S standard solution and the bisphenol AF standard solution with different concentrations;
s2-2: and respectively carrying out derivation data processing on the ultraviolet absorption spectrograms to obtain first-order derivative ultraviolet absorption spectrograms and third-order derivative ultraviolet absorption spectrograms of the bisphenol A standard solution, the bisphenol S standard solution and the bisphenol AF standard solution with different concentrations.
In the step S2-1, an ultraviolet spectrophotometer is used for measuring the absorbance of each standard solution, and the scanning range of the ultraviolet spectrophotometer is 200-340 nm; referring to FIG. 1, 1 is a diagram of an ultraviolet absorption spectrum of bisphenol AF, 2 is a diagram of an ultraviolet absorption spectrum of bisphenol S, and 3 is a diagram of an ultraviolet absorption spectrum of bisphenol A; as can be seen from fig. 1, there is an overlap in the absorption peaks of the three bisphenols; in order to facilitate the simultaneous determination of the concentrations of bisphenol a, bisphenol S and bisphenol AF, derivative data processing is further performed on the ultraviolet absorption spectrograms of the three bisphenols, first derivative is firstly performed to obtain a first derivative ultraviolet absorption spectrogram, which is shown in fig. 2, wherein 1 is the first derivative ultraviolet absorption spectrogram of bisphenol AF, 2 is the first derivative ultraviolet absorption spectrogram of bisphenol S, and 3 is the first derivative ultraviolet absorption spectrogram of bisphenol a; as can be seen from FIG. 2, the first derivative of the absorption spectrum of bisphenol S at point a (263nm) was 0, and therefore the sum of the bisphenol A concentration and the bisphenol AF concentration was measured at this wavelength; at point b (272nm), the first derivative of the absorption spectrum of bisphenol AF is 0, at which the sum of the bisphenol S concentration and bisphenol A concentration can be determined; and further carrying out two derivative data processing on the first derivative absorption spectrograms of the three bisphenols to obtain third derivative absorption spectrograms of the three bisphenols, wherein the third derivative absorption spectrograms of the absorption spectrums of the bisphenol S and the bisphenol A are equal to zero at a point c (245nm) shown in figure 3, and the concentration of the bisphenol AF can be measured at the point c, so that the concentrations of the bisphenol A, the bisphenol S and the bisphenol AF can be measured by combining and processing the data of the three points.
According to the above analysis, the present invention preferably selects three zero points, i.e., point a, point b, and point c, as zero point wavelengths, and defines point a as a first zero point wavelength, point b as a second zero point wavelength, and point c as a third zero point wavelength, i.e., the first zero point wavelength is 263 nm; the second zero wavelength is 272 nm; the third zero wavelength is 245 nm; and then respectively establishing a standard curve according to absorption spectrum derivative values of the bisphenol a standard solution, the bisphenol S standard solution and the bisphenol AF standard solution with different concentrations at the first zero point wavelength, the second zero point wavelength and the third zero point wavelength, specifically, the step S3 of establishing the standard curve includes:
s3-1: establishing a first standard curve equation of the bisphenol A according to the concentration of the bisphenol A standard solution and the first derivative value of the absorption spectrum of the bisphenol A standard solution with different concentrations at a first zero wavelength through a first derivative ultraviolet absorption spectrogram of the bisphenol A standard solution;
s3-2: establishing a second standard curve equation of the bisphenol A according to the concentration of the bisphenol A standard solution and the first derivative value of the absorption spectrum of the bisphenol A standard solution with different concentrations at a second zero wavelength through a first derivative ultraviolet absorption spectrogram of the bisphenol A standard solution;
s3-3: establishing a first standard curve equation of the bisphenol AF according to the concentration of the bisphenol AF standard solution and the first derivative value of the absorption spectrum of the bisphenol AF standard solution with different concentrations at a first zero wavelength through a first derivative ultraviolet absorption spectrogram of the bisphenol AF standard solution;
s3-4: establishing a bisphenol S standard curve equation according to the concentration of the bisphenol S standard solution and the first derivative value of the absorption spectrum of the bisphenol S standard solution with different concentrations at the second zero wavelength through the first derivative ultraviolet absorption spectrogram of the bisphenol S standard solution;
s3-5: and establishing a second standard curve equation of the bisphenol AF according to the concentration of the bisphenol AF standard solution and the three-order derivative value of the absorption spectrum of the bisphenol AF standard solution with different concentrations at the third zero wavelength through a three-order derivative ultraviolet absorption spectrogram of the bisphenol AF standard solution.
Wherein the established bisphenol A first standard curve equation is an equation related to the concentration of bisphenol A and the first derivative value of the absorption spectrum of the bisphenol A solution at the first zero wavelength; the established bisphenol A second standard curve equation is an equation related to the concentration of the bisphenol A and the first derivative value of the absorption spectrum of the bisphenol A solution at the second zero wavelength; the established bisphenol AF first standard curve equation is an equation related to the concentration of bisphenol AF and the first derivative value of the absorption spectrum of the bisphenol AF solution at the first zero wavelength; the established bisphenol AF second standard curve equation is an equation related to the concentration of the bisphenol AF and the absorption spectrum third-order derivative value of the bisphenol AF solution at the third zero wavelength; the established bisphenol S standard curve equation is an equation related to the concentration of bisphenol S and the first derivative value of the absorption spectrum of the bisphenol S solution at the second zero wavelength.
Specifically, the first standard curve equation of bisphenol A is CA-2548.6B + 0.4691; the second standard curve equation of bisphenol A is CA5138D + 0.5375; wherein C isAIs the concentration of bisphenol A, and the unit is mg/mL; b is the first derivative value of the absorption spectrum of the bisphenol A standard solution at the first zero wavelength; d is the first derivative value of the absorption spectrum of the bisphenol A standard solution at the second zero wavelength.
The first standard curve equation of bisphenol AF is CAF-391.49 a-0.2822; the second standard curve equation of bisphenol AF is CAF-12165E-0.4491; wherein C isAFIs the concentration of bisphenol AF in mg/mL; a is the first derivative value of the absorption spectrum of the bisphenol AF standard solution at the first zero wavelength; and E is the third derivative value of the absorption spectrum of the bisphenol AF standard solution at the third zero wavelength.
The standard curve equation of bisphenol S is CS395.73C + 0.6785; wherein C isSIs the concentration of bisphenol S, and the unit is mg/mL; c is the first derivative value of the absorption spectrum of the bisphenol S standard solution at the second zero wavelength.
Therefore, at the first zero wavelength, the second zero wavelength and the third zero wavelength, the concentrations of the bisphenol A, the bisphenol S and the bisphenol AF are in a linear relation with corresponding absorption spectrum derivative values, and the linear ranges of the bisphenol A, the bisphenol S and the bisphenol AF are respectively 3.6-14.4 mg/L, 1.8-6.6 mg/L and 1.8-8.4 mg/L, namely, the bisphenol A with the concentration range of 3.6-14.4 mg/L, the bisphenol S with the concentration range of 1.8-6.6 mg/L and the bisphenol AF with the concentration range of 1.8-8.4 mg/L can be accurately measured by using the measuring method provided by the invention.
Standard koji created by the above methodIn the linear equation, the correlation coefficient R of the first standard curve equation of bisphenol A20.9799, correlation coefficient R of bisphenol A second standard curve equation20.9978, correlation coefficient R of first standard curve equation of bisphenol AF20.9971, correlation coefficient R of bisphenol AF second standard curve equation20.9976, correlation coefficient R of standard curve equation of bisphenol S20.9741, it can be seen that the five standard curve equations established have good linear relationship, thereby ensuring high accuracy of the results measured by the standard curve equations.
Calculating the concentration of bisphenol A, the concentration of bisphenol S and the concentration of bisphenol AF in the sample to be detected by the standard curve equation comprises the following steps:
s4-1: measuring the absorbance of the solution to be measured to obtain an ultraviolet absorption spectrogram of the solution to be measured;
s4-2: carrying out derivative data processing on the ultraviolet absorption spectrogram of the solution to be detected to obtain a first derivative ultraviolet absorption spectrogram and a third derivative ultraviolet absorption spectrogram of the solution to be detected;
s4-3: calculating the concentration of bisphenol AF in the solution to be detected according to the third derivative ultraviolet absorption spectrogram and a bisphenol AF second standard curve equation;
s4-4: calculating the concentration of bisphenol A in the solution to be detected according to the concentration of bisphenol AF in the solution to be detected and the first derivative ultraviolet absorption spectrogram;
s4-5: and calculating the concentration of the bisphenol S in the solution to be detected according to the concentration of the bisphenol A in the solution to be detected and the ultraviolet absorption spectrogram of the first derivative.
From the above analysis, the three-order derivative values of the absorption spectra of the bisphenol S and the bisphenol a at the third zero wavelength are both equal to zero, so that the three-order derivative value of the absorption spectrum at the third zero wavelength in the ultraviolet absorption spectrogram of the solution to be detected is the three-order derivative value of the absorption spectrum of the bisphenol AF, namely E in the second standard curve equation of the bisphenol AF; substituting the value into a second standard curve equation of the bisphenol AF, and solving to obtain the concentration of the bisphenol AF in the solution to be detected.
Substituting the concentration of the bisphenol AF obtained by the solution into a first standard curve equation of the bisphenol AF to obtain an A value in the first standard curve equation of the bisphenol AF, namely a first derivative value of an absorption spectrum of the bisphenol AF in the solution to be detected at a first zero wavelength in a first derivative ultraviolet absorption spectrogram; because the first derivative value of the absorption spectrum of the bisphenol S at the first zero wavelength in the first derivative ultraviolet absorption spectrogram is 0, the first derivative value of the absorption spectrum at the first zero wavelength in the first derivative ultraviolet absorption spectrogram of the solution to be detected is the sum of the first derivative value of the absorption spectrum of the bisphenol AF at the position and the first derivative value of the absorption spectrum of the bisphenol A at the position, namely the sum of A and B; subtracting the first derivative value of the absorption spectrum of the bisphenol AF at the first zero wavelength in the first derivative ultraviolet absorption spectrogram of the solution to be detected, namely the value A, from the first derivative value of the absorption spectrum of the bisphenol AF at the first zero wavelength in the first derivative ultraviolet absorption spectrogram to obtain a value B, namely the first derivative value of the absorption spectrum of the bisphenol A at the first zero wavelength in the first derivative ultraviolet absorption spectrogram of the solution to be detected; and substituting the value B into a first standard curve equation of the bisphenol A, and solving to obtain the concentration of the bisphenol A in the solution to be detected.
The concentration of the bisphenol A is substituted into a second standard curve equation of the bisphenol A, and a D value, namely a first derivative value of an absorption spectrum of the bisphenol A in the solution to be detected at a second zero wavelength in a first derivative ultraviolet absorption spectrogram, is obtained by solving; because the first derivative value of the absorption spectrum of the bisphenol AF at the second zero wavelength in the first derivative ultraviolet absorption spectrogram is 0, the first derivative value of the absorption spectrum at the second zero wavelength in the first derivative ultraviolet absorption spectrogram of the solution to be detected is the sum of the first derivative value of the absorption spectrum of the bisphenol A at the position and the first derivative value of the absorption spectrum of the bisphenol S at the position, namely the sum of D and C; subtracting the first derivative value of the absorption spectrum of the bisphenol A at the second zero wavelength in the first derivative ultraviolet absorption spectrogram of the solution to be detected, namely the D value, from the first derivative value of the absorption spectrum of the bisphenol A at the second zero wavelength in the first derivative ultraviolet absorption spectrogram to obtain a C value, namely the first derivative value of the absorption spectrum of the bisphenol S in the solution to be detected at the second zero wavelength in the first derivative ultraviolet absorption spectrogram; and substituting the C value into a bisphenol S standard curve equation, and solving to obtain the concentration of the bisphenol S in the solution to be detected.
According to the method for measuring the concentrations of the bisphenol A, the bisphenol S and the bisphenol AF, the concentration of the bisphenol A, the concentration of the bisphenol S and the concentration of the bisphenol AF in the solution to be measured are obtained through calculation according to the standard curve equation of the concentration of the bisphenol A, the concentration of the bisphenol S and the absorption spectrum derivative value at the zero wavelength respectively established and the corresponding derivative ultraviolet absorption spectrogram of the solution to be measured, so that the concentrations of the bisphenol A, the bisphenol S and the bisphenol AF in the solution to be measured are measured simultaneously, the measuring process is convenient and fast, no organic reagent is added in the measuring process, and the method is green and environment-friendly.
Example one
This example provides a method for measuring the concentration of bisphenol a, bisphenol S, and bisphenol AF, comprising the steps of:
s1-1: accurately weighing 3.0mg of bisphenol A in a small beaker, adding 0.50mL of absolute ethyl alcohol and a small amount of secondary deionized water, ultrasonically dissolving, transferring to a 25.0mL volumetric flask, and carrying out constant volume to obtain a bisphenol A stock solution with the concentration of 0.12 mg/mL;
accurately weighing 3.0mg of bisphenol S in a small beaker, adding 0.50mL of absolute ethyl alcohol and a small amount of secondary deionized water, ultrasonically dissolving, transferring to a 25.0mL volumetric flask, and carrying out constant volume to obtain a bisphenol S stock solution with the concentration of 0.12 mg/mL;
accurately weighing 3.0mg of bisphenol AF in a small beaker, adding 0.50mL of absolute ethyl alcohol and a small amount of secondary deionized water, ultrasonically dissolving, transferring to a 25.0mL volumetric flask, and carrying out constant volume to obtain a bisphenol AF stock solution with the concentration of 0.12 mg/mL;
s1-2: respectively adding secondary deionized water into the bisphenol A stock solution, the bisphenol S stock solution and the bisphenol AF stock solution to prepare bisphenol A aqueous solution, bisphenol S aqueous solution and bisphenol AF aqueous solution with different concentrations;
s1-3: respectively adding a certain amount of 0.88mg/mL ammonia water into bisphenol A aqueous solution, bisphenol S aqueous solution and bisphenol AF aqueous solution with different concentrations to ensure that the concentration of the ammonia water in each solution is 264mg/L, thus obtaining bisphenol A standard solution, bisphenol S standard solution and bisphenol AF standard solution with different concentrations;
s2-1: respectively measuring the absorbances of the bisphenol A standard solution, the bisphenol S standard solution and the bisphenol AF standard solution with different concentrations to obtain ultraviolet absorption spectrograms of the bisphenol A standard solution, the bisphenol S standard solution and the bisphenol AF standard solution with different concentrations;
s2-2: respectively carrying out derivation data processing on the ultraviolet absorption spectrograms to obtain first-order derivative ultraviolet absorption spectrograms and third-order derivative ultraviolet absorption spectrograms of bisphenol A standard solutions, bisphenol S standard solutions and bisphenol AF standard solutions with different concentrations;
s3-1: establishing a first standard curve equation of bisphenol A, C, according to the concentration of the bisphenol A standard solution and the first derivative value of the absorption spectrum of the bisphenol A standard solution with different concentrations at a first zero wavelength through a first derivative ultraviolet absorption spectrogram of the bisphenol A standard solutionA＝-2548.6B+0.4691；
S3-2: establishing a second standard curve equation of bisphenol A, C, according to the concentration of the bisphenol A standard solution and the first derivative value of the absorption spectrum of the bisphenol A standard solution with different concentrations at a second zero wavelength by a first derivative ultraviolet absorption spectrogram of the bisphenol A standard solutionA＝5138D+0.5375；
S3-3: establishing a first standard curve equation, C, of bisphenol AF according to the concentration of the bisphenol AF standard solution and the first derivative value of the absorption spectrum of the bisphenol AF standard solution with different concentrations at a first zero wavelength through a first derivative ultraviolet absorption spectrogram of the bisphenol AF standard solutionAF＝-391.49A-0.2822；
S3-4: establishing a bisphenol S standard curve equation C according to the concentration of the bisphenol S standard solution and the first derivative value of the absorption spectrum of the bisphenol S standard solution with different concentrations at the second zero wavelength through the first derivative ultraviolet absorption spectrogram of the bisphenol S standard solutionS＝395.73C+0.6785；
S3-5: establishing a second standard curve equation of bisphenol AF (alpha-hydroxy bisphenol) C according to the concentration of the bisphenol AF standard solution and the absorption spectrum third-order derivative value of the bisphenol AF standard solution with different concentrations at a third zero wavelength through a third-order derivative ultraviolet absorption spectrogram of the bisphenol AF standard solutionAF＝-12165E-0.4491；
S4-1: accurately weighing 10.0mg of plastic bottle, cutting the plastic bottle into 0.5cmx0.5cm fragments, weighing 1.000g of the fragments into an iodine measuring bottle, adding 50.0mL of secondary purified water, placing the obtained product into a water bath kettle, heating at the constant temperature of 70 ℃ for 90min, cooling to room temperature, taking a certain amount of solution as a solution to be measured, and measuring the absorbance of the solution to be measured to obtain an ultraviolet absorption spectrogram of the solution to be measured;
s4-2: carrying out derivative data processing on the ultraviolet absorption spectrogram of the solution to be detected to obtain a first derivative ultraviolet absorption spectrogram and a third derivative ultraviolet absorption spectrogram of the solution to be detected;
s4-3: the third derivative value of the absorption spectrum at the third zero wavelength in the ultraviolet absorption spectrogram is-4.49061 × 10-4Substituting the value into a second standard curve equation of the bisphenol AF, and calculating the concentration of the bisphenol AF in the solution to be detected to be 5.01 mg/L;
s4-4: calculating the concentration of bisphenol A in the solution to be detected to be 10.03mg/L according to the concentration of bisphenol AF in the solution to be detected of 5.01mg/L, a first standard curve equation of bisphenol AF, and a first derivative value-0.01727 of an absorption spectrum at the first zero wavelength in a first derivative ultraviolet absorption spectrogram;
s4-5: and calculating the concentration of the bisphenol S in the solution to be detected to be 3.84mg/L according to the concentration of the bisphenol A in the solution to be detected of 10.03mg/L, a second standard curve equation of the bisphenol A, and a first derivative value of 0.0103 of the absorption spectrum at the second zero wavelength in the first derivative ultraviolet absorption spectrogram.
The sample to be tested is measured in parallel for three times by the steps, and the result consistency is good; the recovery rate of bisphenol AF in the sample is 104.4-112%, the recovery rate of bisphenol S is 88.5-91.4%, and the recovery rate of bisphenol A is 103.6-108.4%. Meets the requirements.
Example two
Unlike the first embodiment, the steps S4-1 to S4-5 and the data in the present embodiment are as follows:
s4-1: accurately weighing 10.0mg of plastic bottle, cutting the plastic bottle into 0.5cmx0.5cm fragments, weighing 1.000g of the fragments into an iodine measuring bottle, adding 50.0mL of secondary purified water, placing the obtained product into a water bath kettle, heating at the constant temperature of 70 ℃ for 90min, cooling to room temperature, taking a certain amount of solution as a solution to be measured, and measuring the absorbance of the solution to be measured to obtain an ultraviolet absorption spectrogram of the solution to be measured;
s4-2: carrying out derivative data processing on the ultraviolet absorption spectrogram of the solution to be detected to obtain a first derivative ultraviolet absorption spectrogram and a third derivative ultraviolet absorption spectrogram of the solution to be detected;
s4-3: third derivative the value of the third derivative of the absorption spectrum at the third zero wavelength in the ultraviolet absorption spectrum is-3.692 x10-5Substituting the value into a second standard curve equation of the bisphenol AF to calculate the concentration of the bisphenol AF in the solution to be measured to be 0;
s4-4: calculating the concentration of bisphenol A in the solution to be detected to be 1.49mg/L according to the concentration of bisphenol AF in the solution to be detected, a first standard curve equation of bisphenol AF and a first derivative value of-0.00040 of an absorption spectrum at the first zero wavelength in a first derivative ultraviolet absorption spectrogram;
s4-5: and calculating the concentration of the bisphenol S in the solution to be detected to be 0 according to the concentration of the bisphenol A in the solution to be detected of 1.49mg/L, a second standard curve equation of the bisphenol A, and a first derivative value-0.001715 of the absorption spectrum at the second zero wavelength in the first derivative ultraviolet absorption spectrogram.
Performing a labeling recovery experiment on the sample to be detected by the steps; the recovery rate of bisphenol AF in the sample is 104.4-112%, the recovery rate of bisphenol S is 88.5-91.4%, and the recovery rate of bisphenol A is 103.6-108.4%. Meets the requirements.
Comparative example 1
Placing a sample to be detected in a colorimetric tube with a plug, adding an extraction solvent, magnesium sulfate and sodium acetate, carrying out vortex and standing, taking supernatant, transferring the supernatant to another colorimetric tube, adding magnesium sulfate, N-propyl ethylenediamine and C18 for purification, carrying out vortex and standing, taking supernatant, blowing nitrogen to be nearly dry, redissolving by methanol and water, carrying out vortex and filtration, and taking a filtered liquid sample to be detected and analyzed on HPLC-MS/MS;
respectively placing a plurality of bisphenol compound standard substances into volumetric flasks, adding methanol for dissolving, and fixing the volume to prepare a single-standard stock solution; mixing the single standard stock solutions of the bisphenol compounds with the same volume, adding methanol and water to dilute the single standard stock solutions into an intermediate solution, adding methanol and water to dilute the intermediate solution to prepare a mixed standard working solution with various concentrations, and injecting the mixed standard working solution into an HPLC-MS/MS to perform measurement to obtain standard curves of various bisphenol compounds;
and calculating the concentration of the bisphenol compound in the sample to be detected according to the standard curve of the detection data obtained in the sample treatment and detection processes.
The recovery rate of the bisphenol AF in the sample to be detected measured by the method provided by the comparative example is 94.8-103%, the recovery rate of the bisphenol S is 92.0-101.3%, and the recovery rate of the bisphenol A is 95.1-101.4%.
Therefore, the method for measuring the concentrations of the bisphenol A, the bisphenol S and the bisphenol AF has higher recovery rates of the bisphenol A, the bisphenol S and the bisphenol AF, simultaneously, a large instrument is not needed in the detection process, and the operation method is simple, convenient and quick; no organic reagent is needed to be added, no secondary pollution is caused to the environment, and the method is green and environment-friendly.
Although the present disclosure has been described above, the scope of the present disclosure is not limited thereto. Those skilled in the art can make various changes and modifications without departing from the spirit and scope of the present disclosure, and such changes and modifications will fall within the scope of the present invention.
Claims (10)
1. A method for measuring the concentration of bisphenol A, bisphenol S and bisphenol AF is characterized by comprising the following steps:
s1: respectively preparing bisphenol A standard solutions, bisphenol S standard solutions and bisphenol AF standard solutions with different concentrations;
s2: respectively obtaining derivative ultraviolet absorption spectrograms of the bisphenol A standard solution, the bisphenol S standard solution and the bisphenol AF standard solution with different concentrations;
s3: establishing a standard curve according to the concentration of the bisphenol A standard solution, the concentration of the bisphenol S standard solution, the concentration of the bisphenol AF standard solution and the absorption spectrum derivative value of each solution at a zero wavelength;
s4: and calculating the concentration of bisphenol A, the concentration of bisphenol S and the concentration of bisphenol AF in the sample to be detected according to the absorption spectrum derivative value of the solution to be detected at the zero wavelength and the standard curve.
2. The method for measuring the concentration of bisphenol a, bisphenol S, or bisphenol AF according to claim 1, wherein step S1 comprises:
s1-1: respectively weighing bisphenol A, bisphenol S and bisphenol AF, respectively adding absolute ethyl alcohol and water, dissolving and fixing the volume to obtain a bisphenol A stock solution, a bisphenol S stock solution and a bisphenol AF stock solution;
s1-2: and respectively adding water into the bisphenol A stock solution, the bisphenol S stock solution and the bisphenol AF stock solution for dilution, and preparing bisphenol A aqueous solution, bisphenol S aqueous solution and bisphenol AF aqueous solution with different concentrations.
3. The method for measuring the concentrations of bisphenol a, bisphenol S, and bisphenol AF according to claim 2, wherein step S1 further comprises:
s1-3: respectively adding ammonia solutions into the bisphenol A aqueous solution, the bisphenol S aqueous solution and the bisphenol AF aqueous solution with different concentrations to obtain the bisphenol A standard solution, the bisphenol S standard solution and the bisphenol AF standard solution with different concentrations.
4. The method for measuring the concentration of bisphenol A, bisphenol S, or bisphenol AF as claimed in any one of claims 1 to 3, wherein step S2 includes:
s2-1: respectively measuring the absorbances of the bisphenol A standard solution, the bisphenol S standard solution and the bisphenol AF standard solution with different concentrations to obtain ultraviolet absorption spectrograms of the bisphenol A standard solution, the bisphenol S standard solution and the bisphenol AF standard solution with different concentrations;
s2-2: and respectively carrying out derivation data processing on the ultraviolet absorption spectrograms to obtain first derivative ultraviolet absorption spectrograms and third derivative ultraviolet absorption spectrograms of the bisphenol A standard solution, the bisphenol S standard solution and the bisphenol AF standard solution with different concentrations.
5. The method of claim 4, wherein step S3 comprises:
s3-1: establishing a first standard curve equation of the bisphenol A according to the first derivative ultraviolet absorption spectrogram of the bisphenol A standard solution and the first derivative values of the absorption spectra of the bisphenol A standard solutions with different concentrations at a first zero wavelength;
s3-2: establishing a second standard curve equation of the bisphenol A according to the first derivative ultraviolet absorption spectrogram of the bisphenol A standard solution and the first derivative values of the absorption spectra of the bisphenol A standard solutions with different concentrations at a second zero wavelength;
s3-3: establishing a bisphenol AF first standard curve equation according to the first derivative ultraviolet absorption spectrogram of the bisphenol AF standard solution and the first derivative values of the absorption spectra of the bisphenol AF standard solution at the first zero wavelength in different concentrations;
s3-4: establishing a bisphenol S standard curve equation according to the first derivative ultraviolet absorption spectrogram of the bisphenol S standard solution and the first derivative values of the absorption spectra of the bisphenol S standard solutions with different concentrations at the second zero wavelength;
s3-5: and establishing a second standard curve equation of the bisphenol AF according to the third derivative ultraviolet absorption spectrogram of the bisphenol AF standard solution and the absorption spectrum third derivative values of the bisphenol AF standard solution with different concentrations at a third zero wavelength.
6. The method of claim 5, wherein the first zero wavelength is 263 nm; the second zero wavelength is 272 nm; the third zero wavelength is 245 nm.
7. The method of claim 6, wherein the first standard curve equation of bisphenol A is CA-2548.6B + 0.4691; the second standard curve equation of the bisphenol A is CA＝5138D+05375; wherein C isAIs the concentration of bisphenol A, and the unit is mg/mL; b is the first derivative value of the absorption spectrum of the bisphenol A standard solution at the first zero wavelength; d is the first derivative value of the absorption spectrum of the bisphenol A standard solution at the second zero wavelength.
8. The method of claim 7, wherein the first standard curve equation of bisphenol AF is as follows
CAF＝-391.49A-0.2822；
The second standard curve equation of the bisphenol AF is CAF-12165E-0.4491; wherein C isAFIs the concentration of bisphenol AF in mg/mL; a is the first derivative value of the absorption spectrum of the bisphenol AF standard solution at a first zero wavelength; and E is the third derivative value of the absorption spectrum of the bisphenol AF standard solution at the third zero wavelength.
9. The method of claim 8, wherein the standard curve equation of bisphenol S is CS395.73C + 0.6785; wherein C isSIs the concentration of bisphenol S, and the unit is mg/mL; c is the first derivative value of the absorption spectrum of the bisphenol S standard solution at the second zero wavelength.
10. The method of claim 9, wherein step S4 comprises:
s4-1: measuring the absorbance of the solution to be measured to obtain an ultraviolet absorption spectrogram of the solution to be measured;
s4-2: performing derivative data processing on the ultraviolet absorption spectrogram of the solution to be detected to obtain a first derivative ultraviolet absorption spectrogram and a third derivative ultraviolet absorption spectrogram of the solution to be detected;
s4-3: calculating the concentration of the bisphenol AF in the solution to be detected according to the third derivative ultraviolet absorption spectrogram and the bisphenol AF second standard curve equation;
s4-4: calculating the concentration of the bisphenol A in the solution to be detected according to the concentration of the bisphenol AF in the solution to be detected, the first derivative ultraviolet absorption spectrogram, the second standard curve equation of the bisphenol AF and the first standard curve equation of the bisphenol A;
s4-5: and calculating the concentration of the bisphenol S in the solution to be detected according to the concentration of the bisphenol A in the solution to be detected, the first derivative ultraviolet absorption spectrogram, the second standard curve equation of the bisphenol A and the standard curve equation of the bisphenol S.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112557576A (en) * | 2020-12-04 | 2021-03-26 | 陕西省石油化工研究设计院 | Method for measuring content of calcium and magnesium ions in industrial circulating water |
| CN113533292A (en) * | 2021-08-24 | 2021-10-22 | 常州工学院 | Fluorescent detection method for content of bisphenol S |
| CN114295902A (en) * | 2021-12-30 | 2022-04-08 | 陕西科技大学 | Method for measuring surface charge density of lignin fiber |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112557576A (en) * | 2020-12-04 | 2021-03-26 | 陕西省石油化工研究设计院 | Method for measuring content of calcium and magnesium ions in industrial circulating water |
| CN113533292A (en) * | 2021-08-24 | 2021-10-22 | 常州工学院 | Fluorescent detection method for content of bisphenol S |
| CN113533292B (en) * | 2021-08-24 | 2024-04-26 | 常州工学院 | Fluorescence detection method for bisphenol S content |
| CN114295902A (en) * | 2021-12-30 | 2022-04-08 | 陕西科技大学 | Method for measuring surface charge density of lignin fiber |
| CN114295902B (en) * | 2021-12-30 | 2024-03-08 | 陕西科技大学 | Method for measuring surface charge density of lignin fiber |
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