CN108872440B - Method for measuring content of phenol in water - Google Patents
Method for measuring content of phenol in water Download PDFInfo
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- CN108872440B CN108872440B CN201810910542.0A CN201810910542A CN108872440B CN 108872440 B CN108872440 B CN 108872440B CN 201810910542 A CN201810910542 A CN 201810910542A CN 108872440 B CN108872440 B CN 108872440B
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- G—PHYSICS
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- 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
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid chromatography
Abstract
The invention discloses a method for measuring the content of phenol in water, which has the technical scheme key points that the method comprises the following steps: step 1: taking 10-50 mL of water sample to be detected, adding 5-20 g of sodium chloride into the pressure container, and adding 5-20 mL of organic solvent; step 2: heating the container in a muffle furnace, naturally cooling to room temperature, collecting the upper organic solvent, and concentrating by using a rotary evaporator; and step 3: purifying by a solid phase extraction column, and collecting effluent liquid and eluent; and 4, step 4: concentrating to near dryness by using a nitrogen blowing instrument, adding a solvent for redissolution, and filtering by using an organic filter membrane of 0.02-0.45 um; and 5: testing phenol by using a high performance liquid chromatograph, wherein the chromatographic column is a C8 or C18 liquid chromatographic column; setting the speed of a mobile phase to be 0.5-2 mL/min, setting the volume of a sample to be 20-100 uL, and setting the temperature of a chromatographic column to be 20-50 ℃; the analysis was performed using a fluorescence detector. The method for measuring the content of phenol in water can simply, quickly, accurately, qualitatively and quantitatively detect the content of phenol in a sample.
Description
[ technical field ] A method for producing a semiconductor device
The invention belongs to the technical field of food detection, and particularly relates to a method for measuring the content of phenol in water.
[ background of the invention ]
People have higher and higher requirements on food safety, and the limit of harmful substances in drinking water, surface water and agricultural irrigation water is stricter and stricter. Phenol is widely used as a raw material for plastics, a production resin, a bactericide, a preservative and an important raw material for pharmaceuticals. However, phenol belongs to toxic substances, has strong corrosive action on skin and mucosa, and can inhibit central nerve or damage liver and kidney functions; headache, dizziness, hypodynamia, blurred vision, pulmonary edema and the like caused by high-concentration steam inhalation; the patients who take the medicine by mistake burn the digestive tract, and burn pain occurs, the exhaled air has phenolic smell, vomitus or stool can carry blood, gastrointestinal perforation is possible, shock, pulmonary edema, liver or kidney damage can occur, and acute renal failure occurs; eye contact can cause burns. Phenol can contact natural water in the production process and the product waste process, the natural water is very easy to be polluted based on the property that the phenol is slightly soluble in water, the purification effect of domestic drinking water on the phenol by the methods of filtering, aerating and ozone is limited, and most of agricultural irrigation water is directly used without being purified. Phenol in water will enter the food chain to be enriched, and the health of human body is affected finally. At present, for drinking water, there are related test standards GB/T5750.4-2006 clause 9 for testing the content of phenol in water by using a spectrophotometry, and there is a section I of chapter II of the fourth chapter II of the Water and wastewater monitoring and analyzing method (fourth edition) supplementary edition published by the State environmental protection administration. However, the above method has the following disadvantages: the pretreatment method needs to distill a water sample, collect distillate, develop color of the distillate, or use an organic solvent to extract and concentrate the developed material after color development for testing, the process is complicated, the pH value of water needs to be considered, a variety of reagents need to be configured, the process is difficult to control, and when the colorimetric method is used for testing, the color of the reagent and the color of the water sample have serious interference on the test result.
[ summary of the invention ]
The invention provides a method for measuring the content of phenol in water, which can simply, rapidly, accurately, qualitatively and quantitatively detect the content of phenol in a sample, and has the advantages of short detection time, accurate test result and low cost.
The technical scheme of the invention is as follows:
a method for measuring the content of phenol in water comprises the following steps:
step 1: taking 10-50 mL of water sample to be detected, adding 5-20 g of sodium chloride into the pressure container, and adding 5-20 mL of organic solvent;
step 2: heating the container in a muffle furnace, naturally cooling to room temperature, collecting the upper organic solvent, and concentrating by using a rotary evaporator;
and step 3: purifying by a solid phase extraction column, and collecting effluent liquid and eluent;
and 4, step 4: concentrating to near dryness by using a nitrogen blowing instrument, adding a solvent for redissolution, and filtering by using an organic filter membrane of 0.02-0.45 um;
and 5: testing phenol by using a high performance liquid chromatograph, wherein the chromatographic column is a C8 or C18 liquid chromatographic column; setting the speed of a mobile phase to be 0.5-2 mL/min, setting the volume of a sample to be 20-100 uL, and setting the temperature of a chromatographic column to be 20-50 ℃; the analysis was performed using a fluorescence detector.
Preferably, the organic reagent in step 1 is one or more of methanol, acetone, dichloromethane, tetrahydrofuran, chloroform, ethyl acetate and ethanol.
Preferably, the container in the step 2 is placed in a muffle furnace, and is heated at 300-500 ℃ for 30-90 minutes.
Preferably, the liquid phase extraction column in step 2 uses one or a combination of C18, C8, silica gel column, graphite carbon black column, etc.
Preferably, the mobile phase is methanol or acetonitrile or a mixture of the two. Methanol or acetonitrile is selected as an extracting agent, so that the adsorbent has strong adsorbability on target compounds.
Preferably, the fluorescence detector has an excitation wavelength of 260-290 nm and an emission wavelength of 300-340 nm.
Compared with the prior art, the invention has the following advantages:
the invention discloses a method for measuring the content of phenol in water, which uses an organic solvent to form mixed steam with a water sample to be measured under the conditions of high temperature and high pressure, forms the mixed steam by water and an organic solution, and allows phenol to enter the organic solvent through mutual contact and exchange between the steam. The method is different from a liquid-liquid extraction method, does not need complicated extraction operation, avoids the harm caused by long-term contact of operators with an organic solvent, is also different from a distillation method, consumes a large amount of electric energy and cooling water, overcomes the problems of long time consumption, high cost, large organic solvent consumption and reduction of occupational harm to the operators in the prior detection, and also overcomes the technical problems that the detection cannot be carried out when the phenol content in a sample is low, the phenol content in the sample cannot be accurately reflected and the like;
the method for measuring the content of phenol in water extracts phenol in a sample by adopting a liquid-liquid extraction mode combining an organic reagent and vortex mixed extraction, has high and quick extraction effect, is fully and conveniently operated, uses a high performance liquid chromatograph fluorescence detector which has high selectivity and response value on phenol, carries out qualitative and quantitative detection on phenol, has strong anti-interference capability, can optimally separate phenol by selecting a proper chromatographic column and controlling a proper mobile phase to set proper flow and column temperature conditions so as to solve the technical problems that the detection consumes long time and has high cost at present, the detection cannot be carried out when the content of phenol in the sample is lower, the content of phenol in the sample cannot be accurately reflected, and the like.
[ description of the drawings ]
FIG. 1: blank chromatograms in chromatographic analysis;
FIG. 2: chromatogram of each standard solution after superposition in chromatographic analysis
FIG. 3: sample chromatograms of water samples in chromatographic analysis.
[ detailed description ] embodiments
The following is a detailed description of the present invention:
the method for measuring the phenol content in water according to the present invention will be described with reference to the following specific examples:
step 1: taking 25mL of water sample to be detected, adding 10g of sodium chloride and 10mL of methanol into a high-temperature and high-pressure resistant container;
step 2: placing the container into a high-temperature and high-pressure resistant container, placing the container into a muffle furnace, heating at 400 ℃ for 60 minutes, naturally cooling to room temperature, collecting the upper organic solvent, and concentrating to about 2mL by using a rotary evaporator
And step 3: activating C18 solid phase extraction column with methanol/water solution, adding concentrated solution, collecting eluate, eluting with dichloromethane/methanol solution, collecting eluate, and mixing with the eluate;
and 4, step 4: concentrating to near dryness by using a nitrogen blowing instrument, adding 1mL of methanol and water (volume ratio is 1:1) for redissolution, and passing through a 0.22um organic filter membrane;
and 5: a chromatographic column: c18 liquid chromatography column mobile phase: the volume ratio is 65: 35 methanol-water mixed solution, column flow: column temperature 0.8 ml/min: sample volume at 40 ℃: 50 μ l fluorescence detector wavelength: excitation wavelength 275nm, emission wavelength 313nm, and analysis was performed using a fluorescence detector.
The abscissa in the chromatogram represents retention time, the ordinate represents response intensity, Emissiom _1 is the chromatogram detected by the fluorescence detector, the blank liquid is subjected to high performance liquid chromatography determination according to the determination conditions, the total target peak area response value is plotted against the concentration, and fig. 1 is a blank chromatogram.
Phenol standard stock solution: accurately weighing 0.100g of phenol standard substance, placing in a beaker, dissolving with methanol, fixing the volume to the scale, shaking up, and preparing into standard stock solution with the concentration of 1000 mg/L. And (3) diluting the phenol standard stock solution step by using methanol to obtain a standard working solution with the concentration of 2.5,5,10,20 and 40 mu g/L, carrying out sample injection test in sequence from low concentration to high concentration, drawing a graph according to the peak area response value of the target object to the concentration, establishing a phenol standard working curve according to the test result and the theoretical concentration of the working solution, obtaining a graph 2 (chromatogram of each standard solution after overlapping), and obtaining a standard curve regression equation. The concentration of phenol is within the range of 2.5-40 mu g/L, the concentration (X) and the corresponding peak area value (Y) are in good linear relation, and the correlation coefficient is 0.998.
The resulting linear equation is: Y84242X 49312.
Note: the calculation result is calculated as follows:
in the formula:
w-content of phenol (mg/L) in water sample;
c-concentration of the solution on the computer (mg/L)
V1 — final volumetric volume (mL);
v-volume (mL) of water sample to be measured is transferred;
f-dilution factor
The test was conducted 10 times, and 0.1ml of a standard solution having a phenol content of 25. mu.g/L was added to the sample, and the results of recovery and accuracy are shown in Table 1.
Table 1: phenol recovery and precision test results
As can be seen from Table 1, the average recovery rates of the target compounds are all 80-120%, which shows that the determination method provided by the invention has high accuracy, and the average RSD of the sample test result is less than 10%, which shows that the determination method has good repeatability.
And (3) verification testing:
transferring 25mL of a water sample to be detected, adding 10g of sodium chloride and 10mL of methanol, installing the water sample into a vortex oscillator, carrying out vortex mixing extraction for 30min at the vortex extraction speed of 1000 rpm; collecting the upper organic solvent, adding 10mL methanol repeatedly, extracting once according to the above steps, combining the upper methanol, concentrating to about 2mL by using a rotary evaporator, taking a C18 solid phase extraction column, activating by using methanol/water solution, adding a concentrated solution, collecting an effluent, eluting by using a dichloromethane/methanol solution, collecting the eluate, combining the eluate into the effluent, concentrating to near dryness by using a nitrogen blowing instrument, adding 1mL methanol and water (volume ratio is 1:1) for redissolution, and measuring by using a 0.22um organic filter membrane through high performance liquid chromatography.
And (3) plotting the total target peak area response value to the concentration, establishing a sample chromatogram according to the measurement result of the solution of the test part to obtain a graph 3, substituting the result into the linear equation for calculation, and determining the result: the content of phenol in water was 0.1 ug/L.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (1)
1. A method for measuring the content of phenol in water is characterized by comprising the following steps:
step 1: taking 10-50 mL of water sample to be detected, adding 5-20 g of sodium chloride into the pressure container, and adding 5-20 mL of organic solvent; the organic reagent is methanol;
step 2: heating the container in a muffle furnace, naturally cooling to room temperature, collecting the upper organic solvent, and concentrating by using a rotary evaporator; the container is placed into a muffle furnace, and is heated at 300-500 ℃ for 30-90 minutes;
and step 3: purifying by a solid phase extraction column, and collecting effluent liquid and eluent; the extraction column uses C18;
and 4, step 4: concentrating to near dryness by using a nitrogen blowing instrument, adding a solvent for redissolution, and filtering by using an organic filter membrane of 0.22-0.45 um;
and 5: testing phenol by using a high performance liquid chromatograph, wherein the chromatographic column is a C18 liquid chromatographic column; the speed of the mobile phase is set to be 0.5-2 mL/min, and the volume ratio of the mobile phase is 65: 35, setting the sample injection volume to be 20-100 uL, and setting the column temperature of a chromatographic column to be 20-50 ℃; and (3) analyzing by using a fluorescence detector, wherein the fluorescence detector has an excitation wavelength of 260-290 nm and an emission wavelength of 300-340 nm.
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