CN115144496A - Method for detecting acrylamide content in water based on gas chromatograph - Google Patents
Method for detecting acrylamide content in water based on gas chromatograph Download PDFInfo
- Publication number
- CN115144496A CN115144496A CN202210768701.4A CN202210768701A CN115144496A CN 115144496 A CN115144496 A CN 115144496A CN 202210768701 A CN202210768701 A CN 202210768701A CN 115144496 A CN115144496 A CN 115144496A
- Authority
- CN
- China
- Prior art keywords
- acrylamide
- detected
- sample
- water
- gas chromatograph
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 72
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 title claims abstract description 67
- 238000000034 method Methods 0.000 title claims abstract description 33
- 239000012535 impurity Substances 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 10
- 239000007789 gas Substances 0.000 claims description 34
- 238000000605 extraction Methods 0.000 claims description 15
- 238000001514 detection method Methods 0.000 claims description 13
- 239000012528 membrane Substances 0.000 claims description 8
- 230000008016 vaporization Effects 0.000 claims description 8
- 239000012159 carrier gas Substances 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000006228 supernatant Substances 0.000 claims description 4
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 3
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 3
- 235000011152 sodium sulphate Nutrition 0.000 claims description 3
- 150000003926 acrylamides Chemical class 0.000 claims description 2
- 238000004458 analytical method Methods 0.000 abstract description 6
- 238000005259 measurement Methods 0.000 abstract description 6
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 239000000306 component Substances 0.000 description 12
- 239000007788 liquid Substances 0.000 description 7
- 239000012071 phase Substances 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 230000005526 G1 to G0 transition Effects 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical compound [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000012086 standard solution Substances 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- FIRSEDASHWXORN-UHFFFAOYSA-N 3,3-dibromoprop-2-enamide Chemical compound BrC(=CC(=O)N)Br FIRSEDASHWXORN-UHFFFAOYSA-N 0.000 description 1
- XWNSFEAWWGGSKJ-UHFFFAOYSA-N 4-acetyl-4-methylheptanedinitrile Chemical compound N#CCCC(C)(C(=O)C)CCC#N XWNSFEAWWGGSKJ-UHFFFAOYSA-N 0.000 description 1
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 1
- 206010067125 Liver injury Diseases 0.000 description 1
- 239000004153 Potassium bromate Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000013375 chromatographic separation Methods 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 239000000701 coagulant Substances 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000001212 derivatisation Methods 0.000 description 1
- 239000004205 dimethyl polysiloxane Substances 0.000 description 1
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 1
- 239000003651 drinking water Substances 0.000 description 1
- 235000020188 drinking water Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 239000005350 fused silica glass Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 231100000753 hepatic injury Toxicity 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 description 1
- 230000009965 odorless effect Effects 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 229920002401 polyacrylamide Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229940094037 potassium bromate Drugs 0.000 description 1
- 235000019396 potassium bromate Nutrition 0.000 description 1
- QJWFJOSRSZOLKK-UHFFFAOYSA-N prop-2-enamide Chemical compound NC(=O)C=C.NC(=O)C=C QJWFJOSRSZOLKK-UHFFFAOYSA-N 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 description 1
- 235000019345 sodium thiosulphate Nutrition 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
Images
Classifications
-
- 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
-
- 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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- 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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/12—Preparation by evaporation
-
- 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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
-
- 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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/067—Preparation by reaction, e.g. derivatising the sample
-
- 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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/12—Preparation by evaporation
- G01N2030/126—Preparation by evaporation evaporating sample
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention relates to the field of measurement and analysis, in particular to a method for detecting the content of acrylamide in water based on a gas chromatograph, which comprises the steps of treating impurities in the water to obtain a water body to be detected; converting acrylamide in a water body to be detected into an acrylamide brominated derivative and extracting to obtain an extract; drying the extract to obtain a sample to be detected; and detecting the sample to be detected by adopting a gas chromatograph to obtain the content of the sample to be detected. Through the steps, impurities which are convenient to separate in water can be separated firstly, so that the data processing amount during analysis in the later period can be reduced, then, acrylamide brominated derivatives are generated through reaction to further extract acrylamide, so that the impurities in the acrylamide brominated derivatives are further reduced, and finally, a gas chromatograph is adopted to accurately measure the acrylamide in a sample to be measured, so that the measurement precision can be improved.
Description
Technical Field
The invention relates to the field of measurement and analysis, in particular to a method for detecting acrylamide content in water based on a gas chromatograph.
Background
Acrylamide (Acrylamide) with a molecular weight of 71.08, is colorless transparent flaky crystal, odorless, and toxic. Dissolving in water and ethanol, and slightly dissolving in benzene and toluene. Easy sublimation and easy polymerization. The solid is stable at room temperature and polymerizes violently when molten. Prepared by hydrolyzing acrylonitrile with sulfuric acid or with a metal catalyst. It is extremely toxic, and when inhaled by steam or absorbed through skin, it can cause poisoning, produce nerve center disturbance and liver injury, corrode skin, and irritate eyes.
The residual acrylamide in drinking water is derived from the use of polyacrylamide as a high molecular coagulant aid in water treatment processes, and WHO regulates that the residual concentration thereof should not exceed 0.5 mug/L.
The existing detection method is complex in operation and low in accuracy.
Disclosure of Invention
The invention aims to provide a method for detecting the content of acrylamide in water based on a gas chromatograph, which aims to remove impurities in a detected water body as much as possible and improve the speed and the precision of later-stage gas detection.
In order to achieve the aim, the invention provides a method for detecting the content of acrylamide in water based on a gas chromatograph, which comprises the steps of treating impurities in water to obtain a water body to be detected;
converting acrylamide in a water body to be detected into an acrylamide brominated derivative and extracting to obtain an extract;
drying the extract to obtain a sample to be detected;
detecting a sample to be detected by adopting a gas chromatograph, and obtaining the content of the sample to be detected.
The method comprises the following specific steps of treating impurities in water to obtain a water body to be detected:
obtaining a set amount of water containing acrylamide;
putting water into a centrifuge for centrifugal treatment;
and taking the supernatant and filtering again to obtain the water body to be detected.
Wherein the time of the centrifugal treatment is 3-5 min, and the rotating speed is 6000-8000 r/min.
The method comprises the following steps of (1) converting acrylamide in a water body to be detected into an acrylamide brominated derivative and extracting the acrylamide brominated derivative to obtain an extract:
converting acrylamide in a water body to be detected into an acrylamide brominated derivative;
adjusting the pH value to 2.1-2.6, and then adding sodium sulfate;
and (3) extracting the brominated derivative of the acrylamide by using an extraction membrane.
Wherein the extraction time of extracting the brominated derivatives of the acrylamide by adopting the extraction membrane is 60-75 min, and the extraction temperature is 55-68 ℃.
The method for drying the extract to obtain the sample to be detected comprises the following specific steps:
heating the extract;
and grinding the heated extract to obtain a sample to be detected.
The method comprises the following steps of detecting a sample to be detected by adopting a gas chromatograph, and obtaining the content of the sample to be detected:
vaporizing the sample to be tested in a vaporizing chamber, and then carrying the vaporized sample into a chromatographic column through carrier gas;
separating each component in the sample to be detected in the chromatographic column, and enabling the components to flow into the chromatographic column and enter a detector;
the detector identifies the sample flowing out of the column to obtain detection data;
obtaining a chromatogram based on the detection data;
and combining the chromatogram with the standard curve to obtain the content of the sample to be detected.
The invention discloses a method for detecting acrylamide content in water based on a gas chromatograph, which comprises the following steps: processing impurities in water to obtain a water body to be detected; converting acrylamide in a water body to be detected into an acrylamide brominated derivative, and extracting to obtain an extract; drying the extract to obtain a sample to be detected; and detecting the sample to be detected by adopting a gas chromatograph to obtain the content of the sample to be detected. Through the steps, impurities which are convenient to separate in water can be separated firstly, so that the data processing amount during analysis in the later period can be reduced, then, acrylamide brominated derivatives are generated through reaction to further extract acrylamide, so that the impurities in the acrylamide brominated derivatives are further reduced, and finally, a gas chromatograph is adopted to accurately measure the acrylamide in a sample to be measured, so that the measurement precision can be improved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a flow chart of a method for detecting the content of acrylamide in water based on a gas chromatograph according to the invention.
FIG. 2 is a flow chart of the method for treating impurities in water to obtain a water body to be measured.
Fig. 3 is a flow chart of the present invention for converting acrylamide in a water body to be tested into an acrylamide brominated derivative and extracting the same to obtain an extract.
FIG. 4 is a flow chart of the present invention for drying the extract to obtain a sample to be tested.
Fig. 5 is a flow chart of detecting a sample to be detected by using a gas chromatograph to obtain the content of the sample to be detected according to the present invention.
FIG. 6 is a flow chart for preparing the standard curve of the present invention.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the accompanying drawings are illustrative and intended to explain the present invention and should not be construed as limiting the present invention.
Referring to fig. 1 to 6, the present invention provides a method for detecting acrylamide content in water based on a gas chromatograph, including:
s101, treating impurities in water to obtain a water body to be detected;
the method comprises the following specific steps:
s201, acquiring a set amount of water containing acrylamide;
the water source to be tested is taken and can be laboratory water or domestic water.
S202, putting water into a centrifuge for centrifugal treatment;
the centrifugal treatment time is 3-5 min, and the rotating speed is 6000-8000 r/min.
The water-insoluble impurities in the water can be separated by layers through the treatment of a centrifugal machine, so that the interference in the subsequent gas phase measurement can be reduced.
S203, taking the supernatant and filtering again to obtain the water body to be detected.
The supernatant liquid, which may contain some less dense objects, may be filtered again using the filtering device to further reduce impurities in the water.
S102, converting acrylamide in a water body to be detected into an acrylamide brominated derivative and extracting to obtain an extract;
the method comprises the following specific steps:
s301, converting acrylamide in a water body to be detected into an acrylamide brominated derivative;
adding potassium bromide and potassium bromate into a water body to be detected, uniformly mixing, standing for 30min at 4 ℃, adding 0.3ml of sodium thiosulfate with the concentration of 1mol/L to quench the derivatization process, and converting acrylamide in the water body into dibromoacrylamide.
S302, after the pH value is adjusted to 2.1-2.6, adding sodium sulfate;
s303, extracting the brominated derivative of acrylamide by using an extraction membrane.
The extraction time is 60-75 min, and the extraction temperature is 55-68 ℃. The extraction membrane can be treated with CAR/PDMS extraction membrane.
S103, drying the extract to obtain a sample to be detected;
the method comprises the following specific steps:
s401, heating the extract;
separating the extract from the extraction membrane, and heating at 130-169 deg.C to evaporate water.
S402, grinding the heated extract to obtain a sample to be detected.
The extract can avoid bonding after grinding, thereby being more convenient when a gas chromatograph is used for detection.
And S104, detecting the sample to be detected by adopting a gas chromatograph to obtain the content of the sample to be detected.
The gas chromatograph is an instrument for qualitatively and quantitatively analyzing a multi-component complex mixture by utilizing a chromatographic separation technology and a detection technology. The gas chromatograph generally comprises a gas path system, a sample introduction system, a separation system (chromatographic column system), a detection and temperature control system, and a recording system, wherein the separation system is the heart part of the chromatograph. The function of the method is to separate each component in the sample. The separation system consists of a column chamber, a chromatographic column and a temperature control component. Wherein the chromatographic column is a core component of the chromatograph. There are two main types of chromatography columns: packed columns and capillary columns (open columns). Column materials include metal, glass, fused quartz, polytetrafluoro, and the like. The separation effect of a chromatographic column is related to a plurality of factors such as the length, the diameter and the column shape of the column, the preparation technology of the selected stationary phase and column packing, the operation condition and the like. The detector is a device for converting the concentration or mass (content) of each component separated by the chromatographic column into an electrical signal (such as voltage, current, etc.) that can be easily measured, and performing signal processing, and is the eye of the chromatograph. The device is generally composed of a detection element, an amplifier and a digital-to-analog converter. The components separated by the chromatographic column enter a detector in sequence, are converted into corresponding electric signals according to the change of the concentration or the quality of the components along with time, and are recorded and displayed after being amplified to draw a chromatogram. The quality of the performance of the detector directly influences the accuracy of the final analysis result of the chromatographic instrument. The method comprises the following specific steps:
s501, vaporizing a sample to be detected in a vaporizing chamber, and then carrying the vaporized sample into a chromatographic column through carrier gas;
introducing gas into a vaporization chamber, wherein the chromatographic column is a polar capillary chromatographic column, and the chromatographic conditions are as follows: selecting a stainless steel FFAP column with the length of 2.5m and the inner diameter of 3 mm; column temperature: the temperature of the vaporizing chamber and the detection chamber are both 240 ℃, the flow rate of the carrier gas is 60mL/min, and the sample injection amount is 2 mu L.
S502, separating each component in a sample to be detected in a chromatographic column, and enabling the components to flow into the chromatographic column and enter a detector;
due to the difference of distribution or adsorption coefficient between the mobile phase (gas phase) and the stationary phase (liquid phase or solid phase) of each component in the sample in the chromatographic column, under the flushing of the carrier gas, each component is repeatedly distributed between the two phases to be separated in the column.
S503, identifying the sample flowing out of the column by the detector to obtain detection data;
s504, obtaining a chromatogram based on the detection data;
and S505, combining the chromatogram and the standard curve to obtain the content of the sample to be detected.
The preparation steps of the standard curve are as follows:
s601 is prepared from 0.1 mu g/mL acrylamide standard solution with the concentration of 0.01 gradient liquid of 0.03, 0.05, 0.07 and 0.09 mu g/mL;
and respectively adding corresponding diluted pure water into the standard solution to respectively obtain gradient solutions with corresponding configured concentrations.
S602, brominating each gradient liquid respectively, and extracting and drying the gradient liquids;
the gradient liquid was treated in the same manner as described above.
S603, measuring the processed gradient liquid through a gas chromatograph;
the gradient liquid was measured in the same manner as described above.
And S604, plotting the acrylamide content to the peak area and drawing a standard curve.
The content of the acrylamide can be conveniently measured by comparing with a standard curve, so that the content of the acrylamide in the water with a set amount can be obtained.
The invention discloses a method for detecting acrylamide content in water based on a gas chromatograph, which comprises the following steps: processing impurities in water to obtain a water body to be detected; converting acrylamide in a water body to be detected into an acrylamide brominated derivative and extracting to obtain an extract; drying the extract to obtain a sample to be detected; and detecting the sample to be detected by adopting a gas chromatograph to obtain the content of the sample to be detected. Through the steps, impurities which are convenient to separate in water can be separated firstly, so that the data processing amount during analysis in the later period can be reduced, then, acrylamide brominated derivatives are generated through reaction to further extract acrylamide, so that the impurities in the acrylamide brominated derivatives are further reduced, and finally, a gas chromatograph is adopted to accurately measure the acrylamide in a sample to be measured, so that the measurement precision can be improved.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (7)
1. A method for detecting the content of acrylamide in water based on a gas chromatograph is characterized in that,
the method comprises the following steps: processing impurities in water to obtain a water body to be detected;
converting acrylamide in a water body to be detected into an acrylamide brominated derivative and extracting to obtain an extract;
drying the extract to obtain a sample to be detected;
and detecting the sample to be detected by adopting a gas chromatograph to obtain the content of the sample to be detected.
2. The method for detecting the acrylamide content in water based on gas chromatograph as claimed in claim 1,
the method comprises the following specific steps of treating impurities in water to obtain a water body to be detected:
obtaining a set amount of water containing acrylamide;
putting water into a centrifuge for centrifugal treatment;
and taking the supernatant and filtering again to obtain the water body to be detected.
3. The method for detecting the acrylamide content in water based on gas chromatograph as claimed in claim 2,
the time of the centrifugal treatment is 3-5 min, and the rotating speed is 6000-8000 r/min.
4. The method for detecting the acrylamide content in water based on gas chromatograph as claimed in claim 1,
the method comprises the following specific steps of converting acrylamide in a water body to be detected into an acrylamide brominated derivative and extracting the acrylamide brominated derivative to obtain an extract:
converting acrylamide in a water body to be detected into an acrylamide brominated derivative;
adjusting the pH value to 2.1-2.6, and then adding sodium sulfate;
and (3) extracting the brominated derivative of the acrylamide by using an extraction membrane.
5. The method of claim 4, wherein the content of acrylamide in water is detected by gas chromatograph,
the extraction time of the extraction of the brominated acrylamide derivative by adopting the extraction membrane is 60-75 min, and the extraction temperature is 55-68 ℃.
6. The method for detecting the acrylamide content in water based on gas chromatograph as claimed in claim 1,
the specific steps of drying the extract to obtain a sample to be tested are as follows:
heating the extract;
and grinding the heated extract to obtain a sample to be detected.
7. The method for detecting the acrylamide content in water based on gas chromatograph as claimed in claim 1,
the method comprises the following specific steps of detecting a sample to be detected by adopting a gas chromatograph to obtain the content of the sample to be detected:
vaporizing the sample to be detected in a vaporizing chamber, and then carrying the vaporized sample into a chromatographic column through carrier gas;
separating each component in the sample to be detected in the chromatographic column, and the chromatographic column is flowed in parallel and enters a detector;
the detector identifies the sample flowing out of the column to obtain detection data;
obtaining a chromatogram based on the detection data;
and combining the chromatogram map and the standard curve to obtain the content of the sample to be detected.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210768701.4A CN115144496A (en) | 2022-06-30 | 2022-06-30 | Method for detecting acrylamide content in water based on gas chromatograph |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210768701.4A CN115144496A (en) | 2022-06-30 | 2022-06-30 | Method for detecting acrylamide content in water based on gas chromatograph |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115144496A true CN115144496A (en) | 2022-10-04 |
Family
ID=83411139
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210768701.4A Pending CN115144496A (en) | 2022-06-30 | 2022-06-30 | Method for detecting acrylamide content in water based on gas chromatograph |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115144496A (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107356683A (en) * | 2017-05-22 | 2017-11-17 | 安徽宏远职业卫生技术服务有限公司 | A kind of method of acrylamide in Air of Workplace by Gas Chromatography |
| CN107884482A (en) * | 2017-09-18 | 2018-04-06 | 同济大学 | The detection method of acrylamide in a kind of water |
-
2022
- 2022-06-30 CN CN202210768701.4A patent/CN115144496A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107356683A (en) * | 2017-05-22 | 2017-11-17 | 安徽宏远职业卫生技术服务有限公司 | A kind of method of acrylamide in Air of Workplace by Gas Chromatography |
| CN107884482A (en) * | 2017-09-18 | 2018-04-06 | 同济大学 | The detection method of acrylamide in a kind of water |
Non-Patent Citations (4)
| Title |
|---|
| 李丽萍: "气相色谱法测定水中丙烯酰胺的方法改进", 广东化工, vol. 37, no. 6, pages 63 - 64 * |
| 王慧 等: "分析化合综合实验教程", 30 November 2021, 黑龙江科学技术出版社, pages: 143 * |
| 董丽华 等: "溴化衍生-液液萃取-气相色谱法检测水中的丙烯酰胺", 分析仪器, no. 4, pages 31 - 34 * |
| 虞精明 等: "水中微量丙烯酰胺的检测方法", 中国卫生检验杂志, vol. 26, no. 16, pages 2425 - 2428 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Mei et al. | Determination of trace bisphenol A in complex samples using selective molecularly imprinted solid-phase extraction coupled with capillary electrophoresis | |
| WO2021022876A1 (en) | Method for determining halogenated acid content in chloral hydrate or preparation thereof | |
| Edlund | Determination of opiates in biological samples by glass capillary gas chromatography with electron-capture detection | |
| Liu et al. | Elimination of matrix effects for headspace solid-phase microextraction of important volatile compounds in red wine using a novel coating | |
| CN107389811B (en) | Method for measuring diisopropyl naphthalene in cigarette tipping paper | |
| CN104820056A (en) | Method for measuring tert-butyl hydrazine hydrochloride by use of pre-column derivatization-high performance liquid chromatography | |
| CN110849980A (en) | Method for detecting content of enantiomer in isopropyl L-alanine | |
| CN106053659A (en) | Method for measuring ratio of nicotine carbon, hydrogen and nitrogen stable isotopes in tobacco | |
| Du et al. | Determination of taurine in human tear fluid by capillary electrophoresis with indirect amperometric detection based on electrogenerated bromine | |
| CN106645477B (en) | A kind of remaining method of detection florfenicol amine and application | |
| Faraji et al. | β-cyclodextrin-bonded silica particles as novel sorbent for stir bar sorptive extraction of phenolic compounds | |
| CN115144496A (en) | Method for detecting acrylamide content in water based on gas chromatograph | |
| CN115656398A (en) | Detection method of 4-chloro-3-hydroxybutyronitrile | |
| Chen et al. | Double salting-out effect assisted heat-shrinkable tubing liquid phase microextraction followed by high performance liquid chromatography for determination of flavonoids in human plasma | |
| Oefner et al. | Isotachophoretic separation of organic acids in biological fluids | |
| CN112255341A (en) | Method for detecting benzene series in water by negative pressure headspace gas chromatography | |
| CN102721781B (en) | A kind of quick mensuration lactic acid bacteria fermentation product organic acid kind and the method for yield | |
| CN111398494A (en) | Nicotine optical isomer separation and determination method based on reversed-phase two-dimensional liquid chromatography | |
| CN104931325B (en) | The extracting method of incretion interferent | |
| CN115452967B (en) | Method for detecting content of organic acid and solvent in tobacco essence | |
| Xu et al. | Separation and determination of cinchona alkaloids by ligand-exchange capillary electrophoresis using a Cu (II)–l-lysine complex as selector | |
| Casselman et al. | A rapid, sensitive, gas-liquid chromatographic method for the analysis of bis (2-chloroethyl) sulfide collected from air in hydrocarbon solvents | |
| Kesner et al. | [62] Separation of citric acid cycle and related compounds by partition column chromatography | |
| Du et al. | Rapid determination of geosmin and 2-MIB in water by headspace solid phase microextraction gas chromatography-mass spectrometry | |
| CN218298148U (en) | Detection device and detection system for content of organic acid and solvent in tobacco essence |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |