CN113607832B - Method for measuring fatty acid methyl ester in biodiesel wastewater by novel solid-phase microextraction technology - Google Patents
Method for measuring fatty acid methyl ester in biodiesel wastewater by novel solid-phase microextraction technology Download PDFInfo
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- 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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- 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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- 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
- G01N30/04—Preparation or injection of sample to be analysed
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- G01N2030/062—Preparation extracting sample from raw material
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
Abstract
The invention discloses a method for determining fatty acid methyl ester in biodiesel wastewater by a hollow fiber membrane solid-phase microextraction technology, which adopts the hollow fiber membrane solid-phase microextraction technology and a direct sample injection mode of a micro sample collector to realize qualitative and quantitative analysis of fatty acid methyl ester in biodiesel wastewater; the hollow fiber membrane solid-phase microextraction is a pretreatment technology with few extraction steps, low cost and small organic solvent consumption, and the micro-sample collector is used as a hollow fiber membrane direct sample injection device, so that the defects of dilution of a target object in traditional elution sample injection and high sample injection price by using a cracker are overcome, the sensitivity of an analysis method is improved, and the method is a novel analysis technology with simplicity, convenience and low cost.
Description
Technical Field
The invention relates to a method for determining fatty acid methyl ester in biodiesel wastewater by a novel solid-phase microextraction technology, in particular to a method for determining fatty acid methyl ester in wastewater by combining solid-phase microextraction of a hollow fiber membrane with direct sample injection of a micro sample collector.
Background
Biodiesel is composed of various Fatty Acid Methyl Esters (FAMEs), produced mainly by transesterification of vegetable oils or animal fats. The problem of environmental pollution is becoming serious when biodiesel is processed, and organic wastewater discharged in production can pollute river water and destroy water source. Therefore, in order to meet the wastewater discharge standard, digestion treatment is required for wastewater. In order to monitor the change of fatty acid methyl esters in the wastewater treatment process, a method needs to be established to detect and analyze the content of fatty acid methyl esters in the wastewater before and after the treatment. On the other hand, biodiesel must be purified to the maximum extent before it is marketed to meet its product standards, and the common purification method is water washing. However, water washing inevitably results in the retention of FAMEs in the wastewater, which means a loss of industrial profits. In order to monitor the content of FAMEs in wastewater, it is necessary to design a method for enriching and detecting trace FAMEs in wastewater.
Conventional enrichment extraction pretreatment methods include liquid-liquid extraction, solid-phase extraction and solid-phase microextraction, however, both of the former two conventional methods have the disadvantage of using a large amount of organic solvents and long operation time. The solid phase microextraction is an environment-friendly pretreatment method integrating sampling, extraction and concentration, and has low organic solvent consumption, and the method is gradually popularized and applied due to the unique advantages. However, commercial solid-phase microextraction devices are expensive and easy to break, and repeated use easily causes sample residues, which cause cross contamination and affect the sensitivity of detection.
As a novel sample pretreatment technology, the hollow fiber membrane microextraction technology has the advantages of simple device, low cost, low organic solvent consumption and the like. At present, two sample injection modes are available after the extraction of the hollow fiber membrane is completed, namely elution sample injection and cracker sample injection. The elution sample injection method can cause dilution of the target object due to the elution step of the organic solvent, so that the sensitivity of the method is reduced, and the detection limit is improved; the direct sample feeding mode of the cracker overcomes the defects of elution sample feeding, but the price of the cracker is high, so that the promotion and the use of the cracker are limited. The invention aims to overcome the defects of the method by combining a hollow fiber membrane solid-phase microextraction technology with a direct sample injection mode of a micro sample collector, and realizes the determination of fatty acid methyl ester in biodiesel wastewater.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention provides a novel hollow fiber membrane solid-phase microextraction technology for qualitatively and quantitatively analyzing fatty acid methyl ester in biodiesel wastewater.
The technical scheme of the invention is as follows:
a method for determining fatty acid methyl ester in biodiesel wastewater by using a hollow fiber membrane solid-phase microextraction technology, which comprises the following steps:
(1) Sample pretreatment
Taking a water sample, adding NaCl and methanol as solutions to be detected, placing the solutions to be detected into a headspace bottle, placing a hollow fiber membrane, extracting for 40min at a temperature of 40 ℃ and a stirring speed of 500rpm, taking out the hollow fiber membrane, and removing surface moisture (on filter paper) for later use;
the concentration of NaCl in the solution to be detected is 0.20mol/L;
the volume ratio of the water sample to the methanol is 1:1, a step of;
the hollow fiber membrane is a polypropylene membrane, the outer diameter of the membrane is 300 mu m, the inner diameter of the membrane is 260 mu m, and the aperture of the membrane is 20-200 nm, and the hollow fiber membrane can be obtained commercially by a conventional way; before use, cutting into small sections with the length of 1cm, soaking in ethanol for 20min, and drying in a 50 ℃ oven for 30min for later use;
(2) Sample introduction detection
Sleeving the hollow fiber membrane prepared in the step (1) on a needle core of a micro-sample collector and withdrawing the micro-sample collector into a needle cylinder under the action of a push rod, then pricking the micro-sample collector into a sample inlet of a gas chromatograph, pushing the push rod out, enabling the needle core and the hollow fiber membrane to be exposed to the temperature of the sample inlet of 270 ℃ for analysis for 2min, withdrawing the needle core and the glassy hollow fiber membrane into the needle cylinder after the analysis is completed, withdrawing the micro-sample collector, and pressing a START button of an instrument to perform GC/MS separation analysis;
the micro sample collector includes: the needle core can go in and out of the needle cylinder under the push-pull action of the push rod; the inner diameter of the needle cylinder is 400 mu m, and the maximum diameter of the needle core is as follows: 300 μm;
GC/MS instrument conditions:
instrument: GCMS-QP2010SE gas chromatograph-mass spectrometer; sample inlet temperature: 270 ℃; chromatographic column: TG-1MS capillary chromatographic column (30 m X0.25 mm i.d.X0.25 μm,100% polydimethylsiloxane); temperature programming conditions: heating to 190 ℃ at 20 ℃ per minute at the initial 80 ℃, maintaining for 15min, heating to 270 ℃ at 20 ℃ per minute, and maintaining for 5min; split ratio: 10:1, a step of; the carrier gas is high-purity helium, and the column flow rate is as follows: 1mL/min; ion source: EI; ion source temperature: 230 ℃; transmission line temperature: 270 ℃; electron energy 70eV; scanning mode: full scanning; scanning period: 0.5s; scanning range: m/z:50-600amu;
(3) Establishing a standard curve
Preparing standard substances of methyl palmitate, methyl linoleate, methyl oleate and methyl stearate, preparing standard curve working solutions with serial concentrations by taking deionized water and methanol as solvents, preprocessing the standard curve working solutions according to the method of the step (1) (namely, replacing a water sample in the step (1) with the standard curve working solution), detecting according to the method of the step (2), obtaining a gas chromatograph and a mass spectrogram of the standard substances, and drawing a standard curve by taking the concentration of the standard substances in the standard curve working solution as an abscissa and the peak area of the standard substances in the gas chromatograph as an ordinate;
the concentration range of each standard substance in the standard curve working solution is 10-2000 mug/L;
(4) Detection result of fatty acid methyl ester in sample
Comparing the spectrogram obtained by the sample detection in the step (2) with the spectrogram of the standard substance obtained in the step (3) to obtain a qualitative result of fatty acid methyl ester contained in an actual water sample;
substituting the peak area of the fatty acid methyl ester compound in the spectrogram obtained by the sample detection in the step (2) into the standard curve established in the step (3), and calculating to obtain the content of the fatty acid methyl ester compound in the actual water sample.
Compared with the prior art, the invention has the main advantages that:
the hollow fiber membrane solid-phase microextraction is a pretreatment technology with few extraction steps, low cost and small organic solvent consumption, and the micro-sample collector is used as a hollow fiber membrane direct sample injection device, so that the defects of dilution of a target object in traditional elution sample injection and high sample injection price by using a cracker are overcome, the sensitivity of an analysis method is improved, and the method is a novel analysis technology with simplicity, convenience and low cost.
Drawings
Fig. 1: a schematic of a micro sample collector.
Fig. 2: and a micro-sample collector loaded hollow fiber membrane direct sample injection flow schematic diagram.
Fig. 3: total ion flow diagram of fatty acid methyl ester standard; a, extracting (1 mg/L) by a hollow fiber membrane; b was not extracted (100 mg/L).
Fig. 4: extracting a total ion flow diagram by using a hollow fiber membrane in an actual wastewater sample; a is sample number 1; b is sample number 2; c is sample No. 3.
Detailed Description
The present invention is further described below by way of specific examples, but the scope of the present invention is not limited thereto.
Example 1 selection of extraction time
The longer the extraction time is, the more favorable the target substance enters the membrane, and the increase of the extraction time after reaching the equilibrium has little influence on the increase of the extraction efficiency. If the extraction time is extended after equilibration, this will lead to membrane instability and thus to a reduction in extraction efficiency. Extraction efficiencies at 10, 20, 30, 40, 50min were examined, respectively, and other experimental conditions were: the extraction temperature was 40℃and the stirring rate was 500rpm. The results show that the extraction efficiency of the target substances is obviously improved with the increase of time. When the fatty acid methyl ester compound reaches extraction equilibrium for about 40min, the time is continuously increased, the extraction efficiency is reduced instead, and the continuous extension of the extraction time after the equilibrium leads to instability of the membrane, thereby reducing the extraction efficiency. Thus, an extraction time of 40min was chosen.
Example 2 selection of extraction temperature
Increasing the temperature may facilitate the ingress of the target from the water sample into the fibrous membrane. However, thermodynamically, the adsorption equilibrium is an exothermic process, and the adsorption coefficient decreases with increasing temperature, resulting in a decrease in extraction efficiency. In the invention, the extraction efficiency at the extraction temperature of 20, 30, 40 and 50 ℃ is respectively examined, and other experimental conditions are as follows: the extraction time was 40min and the stirring rate was 500rpm. The results showed that the extraction efficiency was highest at 40 ℃, so the extraction temperature of 40 ℃ was selected.
Example 3 selection of stirring speed
The stirring speed is increased, so that the mass transfer process can be improved, the speed of a target object entering the membrane is increased, the extraction efficiency is improved, but the structure of the membrane is damaged by too fast stirring, and the extraction efficiency is reduced. Extraction efficiencies at stirring speeds of 200, 300, 400, 500, 600rpm were examined, respectively, with other experimental conditions: the temperature was 40℃and the extraction time was 40min. The results showed that the extraction efficiency was highest at 500rpm, so the stirring rate was 500rpm.
EXAMPLE 4 selection of salt concentration
The influence of the salt effect on the extraction is bidirectional, on one hand, the addition of the salt can increase the ionic strength of the solution, reduce the solubility of the to-be-detected object and further increase the extraction efficiency, and on the other hand, the electrostatic effect can inhibit the extraction of the organic matters. The influence of NaCl concentration 0.05,0.10,0.15 and 0.20,0.25mol/L in the sample solution on the extraction efficiency was examined, and the other conditions were: the extraction temperature was 40℃and the stirring rate was 500rpm, the extraction time was 40min. The results showed that the extraction efficiency was highest when the concentration of NaCl was 0.20mol/L of fatty acid methyl ester compound, and therefore, the concentration of NaCl was selected to be 0.20mol/L.
Example 5 investigation of methodology
(1) Instrument and reagent
Gas chromatography-mass spectrometry (SHMADZU GCMS-QP2010 SE). Methyl palmitate, methyl linoleate, methyl oleate, methyl stearate standards.
(2) Experimental method
(2-1) the hollow fiber membrane was cut into small pieces of 1cm in length before use, and immersed in ethanol for 20 minutes, after which the hollow fiber membrane was dried in an oven at 50℃for 30 minutes.
And preparing a wastewater sample No. 1-3, wherein No. 1 is untreated, and No. 2 and No. 3 are digested.
Taking a No. 1-3 wastewater sample (wherein the No. 1 wastewater sample is pre-treatment wastewater, diluting the wastewater sample by deionized water for 25 times before extraction), respectively adding NaCl and an equal volume of methanol as a solution to be detected, enabling the concentration of the NaCl in the solution to be detected to be 0.20mol/L, taking 4mL of the solution to be detected, placing the solution into a headspace bottle, placing the headspace bottle into a stirring magnet, placing the stirring magnet on a magnetic stirrer, then taking a hollow fiber membrane of 1.0cm, placing the hollow fiber membrane into the headspace bottle, starting the magnetic stirrer, extracting the hollow fiber membrane at the stirring speed of 500rpm for 40min at 40 ℃, taking out the hollow fiber membrane, placing the hollow fiber membrane on filter paper, and removing surface moisture for later use;
(2-2) sample introduction
Sleeving the hollow fiber membrane after the extraction in the step (2-1) on the needle core of the micro-sample collector, then withdrawing the needle core of the micro-sample collector into the needle cylinder through the push rod, pricking the micro-sample collector into a sample inlet of the gas chromatograph, pushing the push rod out, enabling the needle core and the hollow fiber membrane to be exposed to the temperature of the sample inlet of 270 ℃ for analysis for 2min, withdrawing the needle core and the glassy hollow fiber membrane into the needle cylinder, withdrawing the micro-sample collector, pressing an instrument START button, and performing GC/MS separation analysis;
GC/MS instrument conditions:
instrument: GCMS-QP2010SE gas chromatograph-mass spectrometer; sample inlet temperature: 270 ℃; chromatographic column: TG-1MS capillary chromatographic column (30 m X0.25 mm i.d.X0.25 μm,100% polydimethylsiloxane); temperature programming conditions: heating to 190 ℃ at 20 ℃ per minute at the initial 80 ℃, maintaining for 15min, heating to 270 ℃ at 20 ℃ per minute, and maintaining for 5min; split ratio: 10:1, a step of; the carrier gas is high-purity helium, and the column flow rate is as follows: 1mL/min; ion source: EI; ion source temperature: 230 ℃; transmission line temperature: 270 ℃; electron energy 70eV; scanning mode: full scanning; scanning period: 0.5s; scanning range: m/z:50-600amu;
(2-3) establishing a Standard Curve
Preparing a mixed standard stock solution by taking methyl palmitate, methyl linoleate, methyl oleate and methyl stearate as standard substances, preparing the mixed standard stock solution by taking methanol as a solvent, diluting the obtained mixed standard stock solution by a mixed solution with the volume ratio of deionized water to methanol of 1:1 to obtain a standard curve working solution, preprocessing the obtained standard curve working solution according to the preprocessing method in the step (2-1) (namely, replacing water in the step (2-1) with the standard curve working solution), then feeding the target substances into an instrument in a sample feeding mode in the step (2-2), carrying out gas chromatography under the detection condition in the step (2-2), obtaining a standard substance spectrogram, and drawing a standard curve by taking the concentration of the standard substance in the standard curve working solution as an abscissa and the area of the standard substance in the spectrogram as an ordinate.
The concentration range of each standard substance in the standard curve working solution is 10-2000 mug/L;
(2-4) commercial SPME comparison
Taking 1mg/L standard solution, wherein the concentration of NaCl is 0.20mol/L, immersing a commercial extraction head into the solution, extracting for 40min at the temperature of 40 ℃ and the stirring speed of 500rpm, taking out, slightly wiping surface water with filter paper, and then entering an instrument for analysis to obtain the peak area of each fatty acid methyl ester; taking 1 mu L of 100mg/L fatty acid methyl ester standard methanol solution, injecting the solution into a gasometer to obtain the peak areas of each fatty acid methyl ester, and comparing the peak areas to obtain the enrichment multiplying power of various commercial extraction heads.
The commercial extraction heads included PDMS (100 μm), PDMS/DVB (65 μm), CAR/PDMS (75 μm).
(3) Results and discussion
The linearity, detection limit, quantitative limit and other parameters of the method are examined, and the results are shown in Table 1. As can be seen from Table 1, the test object has good linearity in the range of 10-2000 mug/L, r is more than 0.9990, and the daily precision of 4 target objects under the conditions of low concentration, medium concentration and high concentration is examined, RSD is less than 12.9%, and the results are shown in Table 2 in detail. Therefore, the method is considered to have good accuracy and can be used for measuring fatty acid methyl ester compounds in the wastewater sample.
Table 1: linear, fold enrichment, detection limit and quantitative limit results for 4 fatty acid methyl esters
Table 2: results of daytime and daytime precision of 4 fatty acid methyl esters
The content of 4 fatty acid methyl esters in the 3 wastewater samples is measured respectively, and a standard adding recovery rate experiment is carried out on the No. 2 wastewater sample. FIG. 4 is a solid phase microextraction total ion flow diagram of a hollow fiber membrane of an actual sample, the content of fatty acid methyl ester in a wastewater sample is quantified by a standard curve method, RSD is less than 14.8%, the results are shown in Table 3, and the standard recovery rate is shown in Table 4.
Table 3: determination results of 4 fatty acid methyl esters in actual wastewater sample
Table 4: standard recovery rate of 4 fatty acid methyl esters in waste water sample 2
Three commercial SPME (PDMS (100 μm), PDMS/DVB (65 μm), CAR/PDMS (75 μm)) extraction heads were used to explore the enrichment ratio of fatty acid methyl esters and compare with the enrichment ratio of hollow fiber membranes in the present invention, and the results show that the enrichment ratio of hollow fiber membranes is superior to PDMS, PDMS/DVB, but slightly lower than CAR/PDMS, and the results are shown in Table 5.
Table 5: commercial SPME extraction head and hollow fiber membrane extraction enrichment ratio comparison result
Claims (4)
1. The method for determining fatty acid methyl ester in biodiesel wastewater by using a hollow fiber membrane solid-phase microextraction technology is characterized by comprising the following steps of:
(1) Sample pretreatment
Taking a water sample, adding NaCl and methanol as solutions to be detected, placing the solutions to be detected into a headspace bottle, placing a hollow fiber membrane, extracting for 40min at a temperature of 40 ℃ and a stirring speed of 500rpm, taking out the hollow fiber membrane, and removing surface moisture for later use;
the hollow fiber membrane is a polypropylene membrane, the outer diameter of the membrane is 300 mu m, the inner diameter of the membrane is 260 mu m, and the aperture of the membrane is 20-200 nm;
(2) Sample introduction detection
Sleeving the hollow fiber membrane prepared in the step (1) on a needle core of a micro-sample collector and withdrawing the micro-sample collector into a needle cylinder under the action of a push rod, then pricking the micro-sample collector into a sample inlet of a gas chromatograph, pushing the push rod out, enabling the needle core and the hollow fiber membrane to be exposed to the temperature of the sample inlet of 270 ℃ for analysis for 2min, withdrawing the needle core and the glassy hollow fiber membrane into the needle cylinder after the analysis is completed, withdrawing the micro-sample collector, and pressing a START button of an instrument to perform GC/MS separation analysis;
the micro sample collector includes: the needle core can go in and out of the needle cylinder under the push-pull action of the push rod; the inner diameter of the needle cylinder is 400 mu m, and the maximum diameter of the needle core is as follows: 300 μm;
GC/MS instrument conditions:
instrument: GCMS-QP2010SE gas chromatograph-mass spectrometer; sample inlet temperature: 270 ℃; chromatographic column: TG-1MS capillary chromatographic column; temperature programming conditions: heating to 190 ℃ at 20 ℃ per minute at the initial 80 ℃, maintaining for 15min, heating to 270 ℃ at 20 ℃ per minute, and maintaining for 5min; split ratio: 10:1, a step of; the carrier gas is high-purity helium, and the column flow rate is as follows: 1mL/min; ion source: EI; ion source temperature: 230 ℃; transmission line temperature: 270 ℃; electron energy 70eV; scanning mode: full scanning; scanning period: 0.5s; scanning range: m/z:50-600amu;
(3) Establishing a standard curve
Preparing standard curve working solutions with serial concentrations by taking standard substances of methyl palmitate, methyl linoleate, methyl oleate and methyl stearate as solvents, preprocessing the standard curve working solutions according to the method of the step (1), detecting according to the method of the step (2) to obtain a standard substance gas chromatograph and a mass spectrogram, taking the concentration of the standard substance in the standard curve working solutions as an abscissa, the peak area of the standard substance in the gas chromatograph as an ordinate, and drawing a standard curve;
(4) Detection result of fatty acid methyl ester in sample
Comparing the spectrogram obtained by the sample detection in the step (2) with the spectrogram of the standard substance obtained in the step (3) to obtain a qualitative result of fatty acid methyl ester contained in an actual water sample;
substituting the peak area of the fatty acid methyl ester compound in the spectrogram obtained by the sample detection in the step (2) into the standard curve established in the step (3), and calculating to obtain the content of the fatty acid methyl ester compound in the actual water sample.
2. The method for determining fatty acid methyl ester in biodiesel wastewater by using a hollow fiber membrane solid-phase microextraction technology as claimed in claim 1, wherein in the step (1), the concentration of NaCl in the solution to be tested is 0.20mol/L.
3. The method for determining fatty acid methyl ester in biodiesel wastewater by using a hollow fiber membrane solid phase microextraction technology as claimed in claim 1, wherein in the step (1), the volume ratio of the water sample to the methanol is 1:1.
4. the method for determining fatty acid methyl ester in biodiesel wastewater by using a hollow fiber membrane solid-phase microextraction technology as set forth in claim 1, wherein in the step (3), the concentration of each standard substance in the standard curve working solution ranges from 10 to 2000 μg/L.
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| CN101496958B (en) * | 2009-01-14 | 2011-03-16 | 南开大学 | Solid phase micro-extraction device and method for preparing fibre extraction head thereof |
| JP5293959B2 (en) * | 2009-04-02 | 2013-09-18 | ユニチカ株式会社 | Hollow fiber membrane and method for producing the same |
| CN102749396B (en) * | 2012-07-17 | 2013-10-23 | 陕西科技大学 | Method for detecting fatty acid content by gas chromatography-mass spectrometry (GC-MS) |
| US10324012B2 (en) * | 2015-08-20 | 2019-06-18 | King Fahd University Of Petroleum And Minerals | Method for detecting and quantifying haloether contamination in aqueous samples by flow assisted electro-enhanced solid-phase microextraction |
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| CN110736801B (en) * | 2019-12-02 | 2020-12-04 | 山东农业大学 | Method for measuring fatty acid in rice by using gas chromatography-mass spectrometry |
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