Method for analyzing and determining 4-nonyl phenol, bisphenol A and pentachlorophenol in water

Abstract

The invention discloses a method for analyzing and determining 4-nonylphenol, bisphenol A and pentachlorophenol in water, which comprises the following steps of: eluting impurities in a solid-phase extraction column by using a reagent, adding a water sample into the solid-phase extraction column, leaving a compound to be detected in a filler of the solid-phase extraction column, discarding water, eluting the compound to be detected in the filler by using an organic reagent, and detecting the content of 4-nonylphenol, bisphenol A and pentachlorophenol in the solid-phase extraction column. The method comprises the following steps of: adding 4-nonylphenol and bisphenol A into an organic solvent, concentrating, separating through liquid chromatography, detecting pentachlorophenol through an ultraviolet detector, detecting 4-nonylphenol and bisphenol A through a fluorescence detector, and determining nature and quantifying peak area through retention time of an ultraviolet spectrogram and a fluorescence spectrogram. The method overcomes the defect that three traditional compounds need to be independently analyzed and determined, is simple and convenient to operate and easy to implement, does not need expensive materials, can be used for obtaining reagent consumables in situ, saves the manpower and material resource cost, and improves the efficiency of analysis and determination operation.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of environmental detection, in particular to a method for analyzing and determining 4-nonyl phenol, bisphenol A and pentachlorophenol in water. BACKGROUND

[0002] Alkyl phenolic compounds, bisphenol A and pentachlorophenol are widely used in surfactants, rubber antioxidants, inks, lubricating oil additives and other fields. Such compounds have both hydrophilic and hydrophobic groups, can replace estrogen molecules to bind to receptors, and belong to endocrine disruptors. At present, 4-nonyl phenol, bisphenol A and pentachlorophenol in water each have a corresponding industry detection standard, but there is no method for simultaneously analyzing and determining the three compounds, which needs to be analyzed and determined separately, resulting in low work efficiency and high labor and material costs. SUMMARY

[0003] The technical problem to be solved by the present application is to provide a method for analyzing and determining 4-nonyl phenol, bisphenol A and pentachlorophenol in water, which overcomes the defects of traditional three compounds that need to be analyzed and determined separately, is simple to operate, easy to perform, does not require expensive materials, and saves labor and material costs, thereby improving the efficiency of analysis and determination work.

[0004] To solve the above technical problems, the method for analyzing and determining 4-nonyl phenol, bisphenol A and pentachlorophenol in water comprises the following steps: Step one, after washing the inner wall of the dichloromethane solid phase extraction column, discarding it, then sequentially using 15ml of n-hexane, dichloromethane, methanol and pure water to elute the solid phase extraction column; Step two, adding 200ml of water sample into the solid phase extraction column, then using 20ml of methanol aqueous solution with a volume ratio of 1:1 to leach the solid phase extraction column, and drying the liquid on the solid phase extraction column; Step three, sequentially using 2ml of methanol and 5ml of dichloromethane to elute the solid phase column, and collecting and concentrating the eluent to 1ml, and transferring to a liquid chromatograph for detection; Step four, the liquid chromatograph separates by liquid chromatography, detects pentachlorophenol by a ultraviolet detector, and detects 4-nonyl phenol and bisphenol A by a fluorescence detector, and qualitatively determines by the retention time of the ultraviolet spectrum and the fluorescence spectrum, and quantitatively determines by the peak area.

[0005] Further, the solid phase extraction column filler is polystyrene-divinylbenzene.

[0006] Further, the liquid chromatograph condition of the liquid chromatograph is that a C18 chromatographic column is used, a mobile phase A is 0.1% formic acid aqueous solution, a mobile phase B is 0.1% formic acid acetonitrile solution, a gradient condition is 0 min, 45% B, 15 min, 60% B, 35 min, 84% B, 40 min, 90% B, 41 min, 45% B, and 45 min, 45% B, a flow rate is 1.0 ml / min, a column temperature is 40 DEG C, a sample injection volume is 20 mu l, and a UV detector is 304 nm with a bandwidth of 4 nm, and a fluorescence detector is 227 nm in excitation wavelength and 315 nm in emission wavelength.

[0007] Since the method for analyzing and determining 4-nonyl phenol, bisphenol A and pentachlorophenol in water adopts the technical scheme, i.e., the method first elutes impurities in the solid phase extraction column with a reagent, adds a water sample into the solid phase extraction column, and leaves the to-be-tested compound in the filler of the solid phase extraction column, then elutes the to-be-tested compound in the filler with an organic reagent, concentrates, separates through liquid chromatography, detects pentachlorophenol through a UV detector, and detects 4-nonyl phenol and bisphenol A through a fluorescence detector, and qualitatively determines the retention time of the UV spectrum and the fluorescence spectrum and quantitatively determines the peak area. The method overcomes the defects of the traditional three compounds which need to be separately analyzed and determined, is simple to operate, is easy to implement, does not need expensive materials, can obtain the reagent and consumables on site, saves manpower and material resources, and improves the efficiency of the analysis and determination work. BRIEF DESCRIPTION OF DRAWINGS

[0008] The application will be further described in detail below in combination with the drawings and embodiments: Figure 1 The fluorescence spectrum of bisphenol A and 4-nonyl phenol in the method is shown in the figure; Figure 2 The UV spectrum of pentachlorophenol in the method is shown in the figure. DETAILED DESCRIPTION

[0009] The method for analyzing and determining 4-nonyl phenol, bisphenol A and pentachlorophenol in water includes the following steps: Step one, after the inner wall of the solid phase extraction column is rinsed with dichloromethane, 15 ml of n-hexane, 15 ml of dichloromethane, 15 ml of methanol and 15 ml of pure water are sequentially used to elute the solid phase extraction column; Step two, 200 ml of a water sample is added into the solid phase extraction column, 20 ml of a methanol aqueous solution with a volume ratio of 1:1 is used to rinse the solid phase extraction column, and the liquid on the solid phase extraction column is dried; Step three, 2 ml of methanol and 5 ml of dichloromethane are sequentially used to elute the solid phase column, the eluent is collected and concentrated to 1 ml, and then transferred to a liquid chromatograph for detection; Step four, as Figure 1 and Figure 2As shown, the liquid chromatograph separates by liquid chromatography, and the pentachlorophenol is detected by the ultraviolet detector, and the 4-nonylphenol and bisphenol A are detected by the fluorescence detector, and the retention time of the ultraviolet spectrum and the fluorescence spectrum is respectively used for qualitative analysis, and the peak area is used for quantitative analysis.

[0010] The retention time of the ultraviolet spectrum and the fluorescence spectrum can be used for preparing the single compound standard solution of bisphenol A, 4-nonylphenol and pentachlorophenol, and the single compound standard solution is analyzed on the instrument one by one according to the instrument analysis method, the fluorescence detector spectrum is used for bisphenol A and 4-nonylphenol, and the ultraviolet detector spectrum is used for pentachlorophenol, the retention time of the single compound standard solution is determined as the retention time of the corresponding target compound, and the retention time is used as the qualitative basis.

[0011] The peak area quantitative analysis is accurate, the standard series with a certain concentration is prepared, and the standard series is analyzed on the instrument; the standard curve is drawn according to the relationship between the instrument response (peak area) of the target compound and the concentration, the actual sample is quantitatively analyzed by using the standard curve, and the actual sample concentration is obtained by conversion according to the constant volume (1 ml of the concentrated eluent in step three) and the sampling volume (200 ml of the water sample in step two).

[0012] Preferably, the solid-phase extraction column filler is polystyrene-divinylbenzene.

[0013] Preferably, the liquid chromatograph has the following liquid chromatography conditions: a C18 chromatographic column; a mobile phase A of 0.1% formic acid aqueous solution and a mobile phase B of 0.1% formic acid acetonitrile solution; a gradient condition of 0 min, 45% B, 15 min, 60% B, 35 min, 84% B, 40 min, 90% B, 41 min, 45% B, 45 min, 45% B; a flow rate of 1.0 ml / min; a column temperature of 40°C; an injection volume of 20 µl; an ultraviolet detector of 304 nm with a bandwidth of 4 nm; and a fluorescence detector with an excitation wavelength of 227 nm and an emission wavelength of 315 nm.

[0014] The method can simultaneously analyze and determine the 4-nonylphenol, bisphenol A and pentachlorophenol in water, is simple and easy to perform, does not involve expensive test materials and reagent consumables in the analysis and determination process, and can be locally sourced without the need for special procurement, thereby effectively saving manpower and material costs, greatly improving the efficiency of the analysis and determination operation, and meeting the requirements of the analysis and determination.

Claims

1. A method for the determination of 4-nonylphenol, bisphenol A and pentachlorophenol in water, characterized in that The method comprises the following steps: Step one: rinse the inner wall of the solid phase extraction column with dichloromethane, then discard, and then elute the solid phase extraction column with 15 ml of n-hexane, 15 ml of dichloromethane, 15 ml of methanol and 15 ml of pure water in sequence; Step two: add 200 ml of water sample into the solid phase extraction column, then elute the solid phase extraction column with 20 ml of methanol water solution with a volume ratio of 1:1, and dry the liquid on the solid phase extraction column; Step three: elute the solid phase column with 2 ml of methanol and 5 ml of dichloromethane in sequence, collect and concentrate the eluent to 1 ml, and then transfer to a liquid chromatograph for detection; Step four: the liquid chromatograph separates by liquid chromatography, detects pentachlorophenol by a UV detector, and detects 4-nonylphenol and bisphenol A by a fluorescence detector, and the qualitative analysis is performed by the retention time of the UV spectrum and the fluorescence spectrum, and the quantitative analysis is performed by the peak area.

2. The method for the determination of 4-nonylphenol, bisphenol A and pentachlorophenol in water according to claim 1, characterized in that: The solid phase extraction column filler is polystyrene-divinylbenzene.

3. The method for the determination of 4-nonylphenol, bisphenol A and pentachlorophenol in water according to claim 1 or 2, characterized in that: The liquid chromatograph has the following liquid chromatography conditions: a C18 chromatographic column, a mobile phase A of 0.1% formic acid aqueous solution, a mobile phase B of 0.1% formic acid acetonitrile solution, a gradient condition of 0 min, 45% B, 15 min, 60% B, 35 min, 84% B, 40 min, 90% B, 41 min, 45% B, 45 min, 45% B, a flow rate of 1.0 ml / min, a column temperature of 40 DEG C, a sample injection volume of 20 µl, a UV detector of 304 nm with a bandwidth of 4 nm, and a fluorescence detector with an excitation wavelength of 227 nm and an emission wavelength of 315 nm.

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