CN115480016A - Liquid chromatography analysis and detection method of laurinol polyoxyethylene ether nonionic surfactant - Google Patents
Liquid chromatography analysis and detection method of laurinol polyoxyethylene ether nonionic surfactant Download PDFInfo
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- CN115480016A CN115480016A CN202211248222.6A CN202211248222A CN115480016A CN 115480016 A CN115480016 A CN 115480016A CN 202211248222 A CN202211248222 A CN 202211248222A CN 115480016 A CN115480016 A CN 115480016A
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- nonionic surfactant
- polyoxyethylene ether
- ether nonionic
- laurinol polyoxyethylene
- laurinol
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- 239000002736 nonionic surfactant Substances 0.000 title claims abstract description 42
- 229940051841 polyoxyethylene ether Drugs 0.000 title claims abstract description 40
- 229920000056 polyoxyethylene ether Polymers 0.000 title claims abstract description 40
- 238000001514 detection method Methods 0.000 title claims abstract description 13
- 238000004458 analytical method Methods 0.000 title claims abstract description 10
- 238000004811 liquid chromatography Methods 0.000 title claims abstract description 9
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical group CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims abstract description 48
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000010828 elution Methods 0.000 claims abstract description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims abstract description 4
- 238000001819 mass spectrum Methods 0.000 claims description 4
- 230000035945 sensitivity Effects 0.000 abstract description 2
- OOCCDEMITAIZTP-QPJJXVBHSA-N (E)-cinnamyl alcohol Chemical compound OC\C=C\C1=CC=CC=C1 OOCCDEMITAIZTP-QPJJXVBHSA-N 0.000 description 6
- OOCCDEMITAIZTP-UHFFFAOYSA-N allylic benzylic alcohol Natural products OCC=CC1=CC=CC=C1 OOCCDEMITAIZTP-UHFFFAOYSA-N 0.000 description 3
- LQZZUXJYWNFBMV-UHFFFAOYSA-N dodecan-1-ol Chemical compound CCCCCCCCCCCCO LQZZUXJYWNFBMV-UHFFFAOYSA-N 0.000 description 3
- SFNALCNOMXIBKG-UHFFFAOYSA-N ethylene glycol monododecyl ether Chemical compound CCCCCCCCCCCCOCCO SFNALCNOMXIBKG-UHFFFAOYSA-N 0.000 description 2
- -1 polyoxyethylene lauryl ether Polymers 0.000 description 2
- 229920000259 polyoxyethylene lauryl ether Polymers 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000003129 oil well Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/30—Control of physical parameters of the fluid carrier of temperature
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/32—Control of physical parameters of the fluid carrier of pressure or speed
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/34—Control of physical parameters of the fluid carrier of fluid composition, e.g. gradient
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/86—Signal analysis
- G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/30—Control of physical parameters of the fluid carrier of temperature
- G01N2030/3007—Control of physical parameters of the fluid carrier of temperature same temperature for whole column
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/32—Control of physical parameters of the fluid carrier of pressure or speed
- G01N2030/324—Control of physical parameters of the fluid carrier of pressure or speed speed, flow rate
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Abstract
The invention discloses a liquid chromatography analysis and detection method of a laurinol polyoxyethylene ether nonionic surfactant. Carrying out liquid chromatography analysis detection on the laurinol polyoxyethylene ether nonionic surfactant solution, determining the chromatographic peak area of the laurinol polyoxyethylene ether nonionic surfactant solution, and obtaining the concentration of the laurinol polyoxyethylene ether nonionic surfactant according to the linear relation between the concentration of the laurinol polyoxyethylene ether nonionic surfactant and the chromatographic peak area; chromatographic conditions are as follows: a hydroxyl column chromatographic column with the specification of 150mm multiplied by 4.6mm and 5 mu m; the mobile phase is acetonitrile and water, the flow rate is 1.0 mL/min, and the gradient elution is carried out: 0-3min: volume fraction of 25% acetonitrile and 75% water, 3-8min: volume fraction of 90% acetonitrile and 10% water, 8.01min: the volume fraction was 25% acetonitrile and 75% water. The method has the characteristics of accuracy, rapidness and sensitivity.
Description
Technical Field
The invention belongs to the field of analytical chemistry, and relates to a liquid chromatography analysis and detection method of a laurinol polyoxyethylene ether nonionic surfactant.
Background
Lauryl alcohol polyoxyethylene ether is a nonionic surfactant with wide application, and is formed by combining lauryl alcohol and polyoxyethylene ether. In recent years, polyoxyethylene lauryl ether frequently appears in the field of tertiary oil recovery, so that a chromatographic detection method of a polyoxyethylene lauryl ether nonionic surfactant in an oil well produced liquid is needed to be established, and technical support is provided for smooth implementation of a tertiary oil recovery technology.
Disclosure of Invention
The invention provides an accurate, rapid and sensitive chromatographic analysis and detection method of a laurinol polyoxyethylene ether nonionic surfactant.
The liquid chromatography analysis and detection method of the laurinol polyoxyethylene ether nonionic surfactant comprises the following steps:
carrying out liquid chromatography analysis and detection on a sample to be detected of the laurinol polyoxyethylene ether nonionic surfactant under the following chromatographic conditions, determining the chromatographic peak area of a laurinol polyoxyethylene ether nonionic surfactant solution, and calculating the concentration of the laurinol polyoxyethylene ether nonionic surfactant according to the linear relation between the concentration of the laurinol polyoxyethylene ether nonionic surfactant and the chromatographic peak area;
chromatographic conditions are as follows: a hydroxyl column chromatographic column with the specification of 150mm multiplied by 4.6mm and 5 mu m; the mobile phase is acetonitrile and water, the flow rate is 1.0 mL/min, and the gradient elution is carried out: 0-3min: volume fraction of 25% acetonitrile and 75% water, 3-8min: volume fraction of 90% acetonitrile and 10% water, 8.01min: the volume fraction is 25% acetonitrile and 75% water, and one-time analysis is completed in 15 min; and detecting by adopting a mass spectrum detector in a positive mode.
The concentration of the cinnamyl alcohol polyoxyethylene ether nonionic surfactant is in the range of 20-200 mg/L, the linear relation between the concentration of the cinnamyl alcohol polyoxyethylene ether nonionic surfactant and the chromatographic peak area is Y = -419467.55 + 2638050X, the linear correlation coefficient R = 0.99995, wherein X is the concentration of the cinnamyl alcohol polyoxyethylene ether nonionic surfactant, the unit is mg/L, and Y is the chromatographic peak area.
The method for analyzing and detecting the laurinol polyoxyethylene ether nonionic surfactant has the characteristics of accuracy, rapidness, sensitivity and good repeatability.
Drawings
FIG. 1 is a chromatogram of 200 mg/L laurinol polyoxyethylene ether nonionic surfactant. It can be seen that the laureth nonionic surfactant peaked at around 5.0 min.
FIG. 2 is a mass spectrum corresponding to the chromatographic peak of 200 mg/L laurinol polyoxyethylene ether nonionic surfactant.
FIG. 3 is a linear relationship between the chromatographic peak area and the concentration of a laureth nonionic surfactant.
Detailed Description
For a better understanding of the present invention, reference is made to the following examples.
Examples
(1) Linear relation
Chromatographic conditions are as follows: the hydroxyl column is a chromatographic column (150 mm multiplied by 4.6mm,5 μm); the mobile phase is acetonitrile and water, the flow rate is 1.0 mL/min, and the gradient elution is carried out: 0-3min: volume fraction of 25% acetonitrile and 75% water, 3-8min: volume fraction of 90% acetonitrile and 10% water, 8.01min: volume fraction of 25% acetonitrile and 75% water; and detecting by adopting a mass spectrum detector in a positive mode.
Preparing series of lauryl alcohol polyoxyethylene ether nonionic surfactant aqueous solutions (10, 20, 50, 100, 200, 500 mg/L) with different concentrations.
Under the chromatographic conditions, 5 mu L of sample is injected, the laurinol polyoxyethylene ether nonionic surfactant peaks at 5.0 min, see fig. 1, the corresponding mass spectrogram is shown in fig. 2, the chromatographic peak areas of series of laurinol polyoxyethylene ether nonionic surfactants with different concentrations are measured, the linear relation between the chromatographic peak area and the concentration is established, see fig. 3, the linear relation between the concentration of the laurinol polyoxyethylene ether nonionic surfactant and the chromatographic peak area is Y = -419467.55 + 2638050X, the linear correlation coefficient R = 0.99995, wherein X is the concentration of the laurinol polyoxyethylene ether nonionic surfactant, the unit mg/L is, and Y is the chromatographic peak area.
(2) Detection limit
The chromatographic conditions are the same as those above, the concentration of the laurinol polyoxyethylene ether nonionic surfactant is continuously diluted, the chromatographic peak response intensity is measured, and the detection limit of the method can be determined to be as low as 2 mg/L.
(3) Determination of concentration of laurinol polyoxyethylene ether nonionic surfactant
The chromatographic conditions are the same as the above, a sample of the laurinol polyoxyethylene ether nonionic surfactant with the concentration of 50 mg/L is injected, the chromatographic peak area is determined to be 125036157, the concentration is calculated to be 47.56 mg/L according to the linear relation Y = -419467.55 + 2638050X, and the measurement is accurate.
(4) Repeatability
Under the same chromatographic conditions, 50 mg/L laurinol polyoxyethylene ether nonionic surfactant is injected on the first day, the third day and the fifth day respectively, and the area of chromatographic peaks is determined, as shown in Table 1, and the repeatability of data is examined. The chromatographic peak areas are 125036157, 139267561 and 136372254 respectively through determination, and the relative standard deviation is 5.63% through calculation and is small, so that the repeatability of data is good.
Claims (2)
1. A liquid chromatography analysis and detection method of laurinol polyoxyethylene ether nonionic surfactant comprises the following steps:
carrying out liquid chromatography analysis and detection on a sample to be detected of the laurinol polyoxyethylene ether nonionic surfactant under the following chromatographic conditions, determining the chromatographic peak area of a laurinol polyoxyethylene ether nonionic surfactant solution, and calculating the concentration of the laurinol polyoxyethylene ether nonionic surfactant according to the linear relation between the concentration of the laurinol polyoxyethylene ether nonionic surfactant and the chromatographic peak area;
chromatographic conditions are as follows: a hydroxyl column chromatographic column with the specification of 150mm multiplied by 4.6mm and 5 mu m; the mobile phase is acetonitrile and water, the flow rate is 1.0 mL/min, and the gradient elution is carried out: 0-3min: volume fraction of 25% acetonitrile and 75% water, 3-8min: volume fraction of 90% acetonitrile and 10% water, 8.01min: volume fraction of 25% acetonitrile and 75% water; and detecting by adopting a positive mode of a mass spectrum detector.
2. The method for detecting laurinol polyoxyethylene ether nonionic surfactant according to claim 1, wherein: the concentration of the laurinol polyoxyethylene ether nonionic surfactant is in the range of 20-200 mg/L, the linear relation between the concentration of the laurinol polyoxyethylene ether nonionic surfactant and the chromatographic peak area is Y = -419467.55 + 2638050X, the linear correlation coefficient R = 0.99995, wherein X is the concentration of the laurinol polyoxyethylene ether nonionic surfactant, the unit is mg/L, and Y is the chromatographic peak area.
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN105067739A (en) * | 2015-07-28 | 2015-11-18 | 中国检验检疫科学研究院 | Laurinol polyoxyethylene ether fully two-dimensional separation analysis method |
CN106404978A (en) * | 2016-11-11 | 2017-02-15 | 中国日用化学工业研究院 | Liquid chromatography analysis method of fatty alcohol polyoxyethylene ether composition distribution |
CN111307963A (en) * | 2019-12-11 | 2020-06-19 | 文水县是大高分子材料有限公司 | Chromatographic detection method of nonionic surfactant |
CN112439395A (en) * | 2020-11-18 | 2021-03-05 | 中国科学院兰州化学物理研究所 | Preparation method of liquid chromatographic column for analyzing and detecting surface polymerization agent in oil well produced liquid |
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- 2022-10-12 CN CN202211248222.6A patent/CN115480016A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN105067739A (en) * | 2015-07-28 | 2015-11-18 | 中国检验检疫科学研究院 | Laurinol polyoxyethylene ether fully two-dimensional separation analysis method |
CN106404978A (en) * | 2016-11-11 | 2017-02-15 | 中国日用化学工业研究院 | Liquid chromatography analysis method of fatty alcohol polyoxyethylene ether composition distribution |
CN111307963A (en) * | 2019-12-11 | 2020-06-19 | 文水县是大高分子材料有限公司 | Chromatographic detection method of nonionic surfactant |
CN112439395A (en) * | 2020-11-18 | 2021-03-05 | 中国科学院兰州化学物理研究所 | Preparation method of liquid chromatographic column for analyzing and detecting surface polymerization agent in oil well produced liquid |
Non-Patent Citations (4)
Title |
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PINO, V等: "Determination of polycyclic aromatic hydrocarbons in seawater by high-performance liquid chromatography with fluorescence detection following micelle-mediated preconcentration", 《JOURNAL OF CHROMATOGRAPHY A》, vol. 949, no. 1, 8 March 2002 (2002-03-08), pages 291 - 299, XP004339472, DOI: 10.1016/S0021-9673(01)01589-8 * |
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