CN112630337A - Method for cooperatively detecting polychlorinated biphenyl and polybrominated diphenyl ether in soil - Google Patents
Method for cooperatively detecting polychlorinated biphenyl and polybrominated diphenyl ether in soil Download PDFInfo
- Publication number
- CN112630337A CN112630337A CN202011495396.3A CN202011495396A CN112630337A CN 112630337 A CN112630337 A CN 112630337A CN 202011495396 A CN202011495396 A CN 202011495396A CN 112630337 A CN112630337 A CN 112630337A
- Authority
- CN
- China
- Prior art keywords
- temperature
- polychlorinated biphenyl
- polybrominated diphenyl
- extraction
- soil
- 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
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
- G01N30/86—Signal analysis
- G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
-
- 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
Abstract
The invention discloses a method for cooperatively detecting polychlorinated biphenyl and polybrominated diphenyl ethers in soil, which comprises the following steps of: s1, weighing a soil sample, putting the soil sample into an extraction tank, and adding polychlorinated biphenyl into the extraction tank13Method for extracting internal standard and polybrominated diphenyl ether by using C isotope13C isotope extraction internal standard, carrying out multiple times of circulating extraction under the conditions of fixed pressure and static extraction temperature, and concentrating to obtain concentrated extract liquor; s2, transferring the concentrated extract into a composite chromatographic column, synchronously purifying polychlorinated biphenyl and polybrominated diphenyl ether with different eluents to obtain eluent containing the polychlorinated biphenyl and the polybrominated diphenyl ether, and respectively adding the polychlorinated biphenyl after concentration13Internal C isotope sample injection label, polybrominated diphenyl ether13C isotope sample injection internal standard; s3, adopting high-resolution gas chromatography-high-resolution mass spectrometryAdding polychlorinated biphenyl into instrument pair13Internal C isotope sample injection label, polybrominated diphenyl ether13And C, carrying out qualitative analysis and quantitative detection on the concentrated eluent of the isotope injection internal standard.
Description
Technical Field
The invention relates to the field of environmental monitoring, in particular to a method for cooperatively detecting polychlorinated biphenyl and polybrominated diphenyl ether in soil.
Background
Polychlorinated biphenyls (PCBs) are chlorinated aromatic compounds of 209 homologs in which hydrogen atoms at different positions on the biphenyl are replaced with chlorine atoms. Polybrominated diphenyl ethers (PBDEs) are the brominated aromatic compounds of 209 homologs in which hydrogen atoms at different positions on the diphenyl ether are replaced by bromine atoms. The stockholm convention on persistent organic pollutants places polychlorinated biphenyls and polybrominated diphenyl ethers as the first subjects to ban or restrict use. The two kinds of organic matters have the characteristics of semi-volatility, long-distance migration, high toxicity, biological accumulation and the like, are easily and widely existed in soil, sediment, atmosphere and other environments, and are easily accumulated in organisms through a food chain, so that potential harm is generated to the organisms. Therefore, the two kinds of substances are more and more attracting wide attention at home and abroad.
Polychlorinated biphenyl is widely applied to the fields of plastic processing, electric power industry, printing, chemical industry and the like due to the characteristics of thermal stability, low conductivity, incombustibility and the like. Polybrominated diphenyl ethers are also widely used in circuit board, paint and other industries due to their flame retardant properties. These two substances are easy to enter various environments through leakage, incineration or improper disposal. Soil is one of the most important accumulation sites, and polychlorinated biphenyl and polybrominated diphenyl ether are easy to enter soil through migration and transformation, so that the soil is polluted. The soil pollution prevention and treatment law issued by China clearly stipulates that investigation on different types of soil pollution conditions is enhanced and important monitoring is implemented. Therefore, it is of great significance to enhance the monitoring of polychlorinated biphenyls and polybrominated diphenyl ethers in soil.
At present, China has already provided gas chromatography for measuring polychlorinated biphenyl of soils and sediments (HJ922-2017), gas chromatography-mass spectrometry for measuring polychlorinated biphenyl of soils and sediments (HJ743-2015) and the like. The standard method of polychlorinated biphenyl is also promulgated abroad. For polybrominated diphenyl ethers, the research field is mainly focused at present, and a unified standard is not yet provided. Although the existing detection method can meet most monitoring requirements, the problems that the soil environment is complex, the matrix effect is strong, and polychlorinated biphenyl and polybrominated diphenyl ether belong to trace level (ppb level), the anti-interference capability of a detection instrument is weak, the detection result is inaccurate and the like are caused, and a new detection method needs to be developed urgently. The outline of ecological environment monitoring planning (2020 + 2035) published by the ecological environment department is explicitly proposed, the innovation of environmental sample pretreatment technology and instrument analysis technology is enhanced, and efficient environment-friendly monitoring technology and method are established. Therefore, the method for rapidly extracting, synchronously purifying and accurately detecting the polychlorinated biphenyl and the polybrominated diphenyl ether in the soil is developed, and the further supplement of the existing standard method can be realized.
Disclosure of Invention
The invention aims to solve the problems and provides an accurate and reliable method for cooperatively detecting polychlorinated biphenyl and polybrominated diphenyl ether in soil.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a method for cooperatively detecting polychlorinated biphenyl and polybrominated diphenyl ethers in soil comprises the following steps:
s1, weighing a soil sample, putting the soil sample into an extraction tank, and respectively adding polychlorinated biphenyl into the extraction tank13Method for extracting internal standard and polybrominated diphenyl ether by using C isotope13C isotope extraction internal standard, carrying out multiple times of circulating extraction under the conditions of fixed pressure and static extraction temperature, and concentrating to obtain concentrated extract liquor;
s2, transferring the concentrated extract into a composite chromatographic column, synchronously purifying polychlorinated biphenyl and polybrominated diphenyl ether by different eluents to obtain eluent containing the polychlorinated biphenyl and the polybrominated diphenyl ether, concentrating the eluent, and respectively adding the polychlorinated biphenyl13Internal C isotope sample injection label, polybrominated diphenyl ether13C isotope sample injection internal standard;
s3 method for adding polychlorinated biphenyl by adopting high-resolution gas chromatography-high-resolution mass spectrometer13Internal C isotope sample injection label, polybrominated diphenyl ether13And C, carrying out qualitative analysis and quantitative detection on the concentrated eluent of the isotope injection internal standard.
Further, the concrete steps of loading the soil sample into the extraction cell in the step S1 are as follows:
s11, embedding filter paper at the bottom of a 40mL extraction tank, and adding quartz sand with the height of 1 cm;
s12, weighing 20g of soil sample, putting the soil sample into an extraction cell, and adding polychlorinated biphenyl into the extraction cell respectively13Method for extracting internal standard and polybrominated diphenyl ether by using C isotope13C isotope extraction internal standard;
and S13, adding quartz sand with the height of 1cm at the upper part of the extraction tank, and embedding filter paper at the upper end of the quartz sand again.
Further, when the extraction is performed in the step S1, the extraction pressure is 1.2MPa, and the extraction temperature is 120 ℃; the single static extraction time is 10 min/time, and the cycle time is 3 times; the extraction solvent was toluene.
Further, the composite chromatographic column in step S2 comprises, from bottom to top: glass wool, quartz sand 1cm in height, magnesium florisil 1g, basic alumina 3g, basic silica gel 4g, neutral silica gel 3g, acidic silica gel 40g, quartz sand 1cm in height.
Further, the alkaline silica gel is prepared by mixing 1mol/L sodium hydroxide solution and neutral silica gel, wherein the mass ratio of the 1mol/L sodium hydroxide solution to the neutral silica gel is 33: 67; the acidic silica gel is prepared by mixing concentrated sulfuric acid and neutral silica gel, wherein the mass ratio of the concentrated sulfuric acid to the neutral silica gel is 2: 3.
Further, the specific steps of synchronously purifying polychlorinated biphenyl and polybrominated diphenyl ether in the step S2 are as follows:
s21, transferring the concentrated extract into a composite chromatographic column, eluting with 120mL of normal hexane and 25mL of mixed solvent of normal hexane and dichloromethane respectively, and collecting the eluent;
s22, placing the collected eluent into a flat-bottomed flask for rotary evaporation concentration operation, and concentrating the eluent to 30 uL.
Further, in the mixed solvent of n-hexane and dichloromethane, the volume ratio of n-hexane to dichloromethane is 95: 5.
Further, when the high-resolution gas chromatography-high-resolution mass spectrometer is used to detect polychlorinated biphenyl in the concentrated eluate in step S3, the high-resolution gas chromatography parameters are as follows: the temperature of a sample inlet is 280 ℃, the temperature of a transmission line is 280 ℃, the flow rate of carrier gas is 1.0mL/min, the sample injection amount is 1uL, and the sample injection is not divided; the chromatographic column is DB-5MS, and the temperature-raising program of the chromatographic column is as follows: the initial temperature is 90 ℃, the temperature is kept for 2min, the temperature is increased to 220 ℃ at the speed of 13 ℃/min, and the temperature is kept for 7 min; then raising the temperature to 260 ℃ at a speed of 1.4 ℃/min; finally, raising the temperature to 310 ℃ at a speed of 4 ℃/min;
the high resolution mass spectrum parameters are as follows: the ion source temperature is 280 ℃, the electron energy is 45eV, and the resolution is more than 10000.
Further, when the high-resolution gas chromatography-high-resolution mass spectrometer is used to detect the polybrominated diphenyl ethers in the concentrated eluate in step S3, the high-resolution gas chromatography parameters are as follows: the temperature of a sample inlet is 280 ℃, the temperature of a transmission line is 280 ℃, the flow rate of carrier gas is 1.0mL/min, the sample injection amount is 1uL, and the sample injection is not divided; the chromatographic column is DB-5MS, and the temperature-raising program of the chromatographic column is as follows: the initial temperature is 90 ℃, the temperature is kept for 2min, the temperature is increased to 180 ℃ at the speed of 15 ℃/min, and the temperature is kept for 2 min; then raising the temperature to 240 ℃ at a speed of 5 ℃/min, and keeping the temperature at 3 ℃; finally, raising the temperature to 310 ℃ at a speed of 3 ℃/min;
the high resolution mass spectrum parameters are as follows: the ion source temperature is 300 ℃, the electron energy is 35eV, and the resolution is more than 10000.
Compared with the prior art, the invention has the advantages and positive effects that:
the invention provides a method for quickly extracting a solvent, synchronously purifying and accurately detecting polychlorinated biphenyl and polybrominated diphenyl ethers in soil, which has the advantages of quickness, accuracy, strong anti-interference capability and the like, can simultaneously realize quick pretreatment and accurate qualitative and quantitative detection of the polychlorinated biphenyl and the polybrominated diphenyl ethers in a soil sample, and can be widely applied to laboratories engaged in trace organic pollutant detection.
On the other hand, on the basis of overcoming the problems of time consumption, material consumption, weak anti-interference capability and the like in the sample extraction and purification process in the prior art, the method for synchronously purifying polychlorinated biphenyl and polybrominated diphenyl ether by using the composite chromatographic column is further developed and researched, and meanwhile, the parameters of the instrument detection method are further optimized, so that the aims of quickly extracting, accurately qualitatively analyzing and quantitatively detecting the polychlorinated biphenyl and the polybrominated diphenyl ether are fulfilled, and convenience is brought to the detection work of trace organic pollutants in the field of environmental monitoring.
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, and 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 these drawings without creative efforts.
FIG. 1 is a schematic structural diagram of a multi-layer composite chromatographic column for synchronously purifying polychlorinated biphenyl and polybrominated diphenyl ether;
FIG. 2 is a total ion flow diagram of polychlorinated biphenyl measured by high resolution gas chromatography-high resolution mass spectrometry;
FIG. 3 is a total ion flow diagram of polybrominated diphenyl ethers measured by high resolution gas chromatography-high resolution mass spectrometry.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived from the embodiments of the present invention by a person skilled in the art without any creative effort, should be included in the protection scope of the present invention.
As shown in fig. 1, fig. 2 and fig. 3, the present embodiment discloses a method for cooperatively detecting polychlorinated biphenyl and polybrominated diphenyl ethers in soil, which comprises the following steps:
1. a rapid solvent extraction step of a soil sample: accurately weighed 20g of soil sample is put into a 40mL extraction cell and then polychlorinated biphenyl is added respectively13Method for extracting internal standard and polybrominated diphenyl ethers by using C isotope13C isotope extraction internal standard, under the condition of specific pressure and static extraction temperature, using toluene as extractant to continuously make circular extraction; concentrating to obtain concentrated extract;
1.1, the concrete steps of filling a soil sample into an extraction tank are as follows:
embedding filter paper at the bottom of a 40mL extraction tank, adding quartz sand with the thickness of about 1cm, then loading 20g of accurately weighed dry soil into the extraction tank, and respectively adding polychlorinated biphenyl and polybrominated diphenyl ether13C isotope extraction internal standard, finally adding quartz sand and filter paper with the thickness of about 1cm into the upper part of the extraction tank in sequence, and installing and fixing the extraction tank.
1.2, the specific parameters of the rapid solvent extraction are as follows:
the static extraction pressure and temperature are respectively 1.2MPa and 120 ℃; the single static extraction time and the cycle times are respectively 10 min/time and 3 times;
2. synchronous purification of soil samples: adding the concentrated extract into a composite chromatographic column, synchronously purifying polychlorinated biphenyl and polybrominated diphenyl ethers by respectively using normal hexane and a mixed solvent of the normal hexane and dichloromethane as an eluent, concentrating the eluent, and adding the polychlorinated biphenyl13Internal C isotope sample injection standard and polybrominated diphenyl ether13C isotope sample injection internal standard;
2.1, the filling steps of the composite chromatographic column are as follows:
as shown in fig. 1, the composition of the composite chromatography column (from bottom to top): glass wool, 1cm of quartz sand, 1g of florisil magnesium silicate, 3g of alkaline alumina, 4g of alkaline silica gel (mass ratio, 1mol/L sodium hydroxide solution: neutral silica gel: 33:67), 3g of neutral silica gel, 40g of acidic silica gel (mass ratio, concentrated sulfuric acid: neutral silica gel: 2:3), and 1cm of quartz sand.
2.2, the synchronous purification of the soil sample comprises the following steps:
transferring the concentrated extract into a composite chromatographic column, eluting with 120mL of n-hexane, and collecting the eluate; then eluting with 25mL of a mixed solvent of n-hexane and dichloromethane (volume ratio, V, 95:5), and collecting eluent; collecting the two parts of eluate in the same flat-bottom flask, performing rotary evaporation concentration, concentrating to about 30uL by blowing nitrogen, and adding polychlorinated biphenyl13Internal C isotope sample injection standard and polybrominated diphenyl ether13C isotope sample injection internal standard;
3. detection and analysis steps of the soil sample: and (3) respectively carrying out qualitative analysis and quantitative detection on the polychlorinated biphenyl and the polybrominated diphenyl ether under certain conditions by adopting high-resolution gas chromatography-high-resolution mass spectrometry.
3.1, the high resolution gas chromatography parameters of the polychlorinated biphenyl are as follows: the temperature of the sample inlet is 280 ℃, the temperature of the transmission line is 280 ℃, the flow rate of the carrier gas is 1.0mL/min, the sample injection amount is 1uL, and the sample injection is not divided. The chromatographic column is DB-5MS (60m multiplied by 0.25mm multiplied by 0.25um), and the temperature program of the column is as follows: the initial temperature is 90 ℃, the temperature is kept for 2min, the temperature is increased to 220 ℃ at the speed of 13 ℃/min, and the temperature is kept for 7 min; then raising the temperature to 260 ℃ at a speed of 1.4 ℃/min; finally, the temperature is increased to 310 ℃ at a speed of 4 ℃/min.
The parameters of the high-resolution mass spectrum of the polychlorinated biphenyl are as follows: the ion source temperature is 280 ℃, the electron energy is 45eV, and the resolution is more than 10000.
3.2, the gas chromatography parameters of the polybrominated diphenyl ethers are as follows: the temperature of the sample inlet is 280 ℃, the temperature of the transmission line is 280 ℃, the flow rate of the carrier gas is 1.0mL/min, the sample injection amount is 1uL, and the sample injection is not divided. The chromatographic column is DB-5MS (20m multiplied by 0.25mm multiplied by 0.1um), and the temperature program of the column is as follows: the initial temperature is 90 ℃, the temperature is kept for 2min, the temperature is increased to 180 ℃ at the speed of 15 ℃/min, and the temperature is kept for 2 min; then raising the temperature to 240 ℃ at a speed of 5 ℃/min, and keeping the temperature at 3 ℃; finally, raising the temperature to 310 ℃ at a speed of 3 ℃/min;
the parameters of the high-resolution mass spectrum of the polybrominated diphenyl ether are as follows: the ion source temperature is 300 ℃, the electron energy is 35eV, and the resolution is more than 10000.
Method for adding polychlorinated biphenyl into 7 soil samples of concrete implementation examples by applying technical method of the invention13Method for extracting internal standard and polybrominated diphenyl ethers by using C isotope13C isotope extraction internal standard, high resolution gas chromatography-high resolution mass spectrometry is adopted for determination, and the optimal determination result of the extraction internal standard is shown in tables 1 and 2. Wherein, table 1 is the result of quantitative detection of the extraction internal standard of the polychlorinated biphenyl in the soil sample, and table 2 is the result of detection of the extraction internal standard of the polybrominated diphenyl ether in the soil sample.
TABLE 1 recovery of polychlorinated biphenyl extraction internal standard in soil
TABLE 2 recovery of inner polybrominated diphenyl ether extraction in soil
| Recovery Range (%) | Average recovery (%) | Standard deviation of | |
| 13C-BDE-28 | 77-90 | 81.9 | 4.5 |
| 13C-BDE-47 | 73-94 | 85.1 | 7.1 |
| 13C-BB-153 | 60-90 | 81.0 | 10.0 |
| 13C-BDE-154 | 63-99 | 86.3 | 12.6 |
| 13C-BDE-153 | 67-101 | 89.1 | 13.3 |
| 13C-BDE-183 | 91-114 | 104.7 | 7.3 |
| 13C-BDE-207 | 61-110 | 95.9 | 15.4 |
The measurement results of the specific embodiment show that the polychlorinated biphenyl is13Average recovery rate of C isotope internal standard is above 60%, and that of polybrominated diphenyl ether13The average recovery rate of the C isotope extraction internal standard is more than 81 percent. Therefore, the technical method can be applied to qualitative and quantitative detection of polychlorinated biphenyl and polybrominated diphenyl ethers in soil samples.
The invention provides a method for cooperatively detecting polychlorinated biphenyl and polybrominated diphenyl ethers in soil, which has the advantages of rapidness, accuracy, strong anti-interference capability and the like, can simultaneously realize the rapid pretreatment and accurate qualitative and quantitative detection of the polychlorinated biphenyl and the polybrominated diphenyl ethers in soil samples, and can be widely applied to laboratories engaged in the detection of trace organic pollutants.
On the other hand, on the basis of overcoming the problems of time consumption, material consumption, weak anti-interference capability and the like in the sample extraction and purification process in the prior art, the method for synchronously purifying polychlorinated biphenyl and polybrominated diphenyl ether by using the composite chromatographic column is further developed and researched, and meanwhile, the parameters of the instrument detection method are further optimized, so that the aims of quickly extracting, accurately qualitatively analyzing and quantitatively detecting the polychlorinated biphenyl and the polybrominated diphenyl ether are fulfilled, and convenience is brought to the detection work of trace organic pollutants in the field of environmental monitoring.
Claims (9)
1. A method for cooperatively detecting polychlorinated biphenyl and polybrominated diphenyl ethers in soil is characterized by comprising the following steps: the method comprises the following steps:
s1, weighing a soil sample, putting the soil sample into an extraction tank, and respectively adding polychlorinated biphenyl into the extraction tank13Method for extracting internal standard and polybrominated diphenyl ether by using C isotope13C isotope extraction internal standard, carrying out multiple times of circulating extraction under the conditions of fixed pressure and static extraction temperature, and concentrating to obtain concentrated extract liquor;
s2, transferring the concentrated extract into a composite chromatographic column, synchronously purifying polychlorinated biphenyl and polybrominated diphenyl ether by different eluents to obtain eluent containing the polychlorinated biphenyl and the polybrominated diphenyl ether, concentrating the eluent, and respectively adding the polychlorinated biphenyl13Internal C isotope sample injection label, polybrominated diphenyl ether13C isotope sample injection internal standard;
s3 method for adding polychlorinated biphenyl by adopting high-resolution gas chromatography-high-resolution mass spectrometer13Internal C isotope sample injection label, polybrominated diphenyl ether13And C, carrying out qualitative analysis and quantitative detection on the concentrated eluent of the isotope injection internal standard.
2. The method for the cooperative detection of polychlorinated biphenyl and polybrominated diphenyl ethers in soil according to claim 1, which comprises the following steps: the concrete steps of loading the soil sample into the extraction cell in the step S1 are as follows:
s11, embedding filter paper at the bottom of a 40mL extraction tank, and adding quartz sand with the height of 1 cm;
s12, weighing 20g of soil sample, putting the soil sample into an extraction cell, and adding polychlorinated biphenyl into the extraction cell respectively13Method for extracting internal standard and polybrominated diphenyl ether by using C isotope13C isotope extraction internal standard;
and S13, adding quartz sand with the height of 1cm at the upper part of the extraction tank, and embedding filter paper at the upper end of the quartz sand again.
3. The method for the cooperative detection of polychlorinated biphenyl and polybrominated diphenyl ethers in soil as set forth in claim 2, which comprises the steps of: when the extraction is carried out in the step S1, the extraction pressure is 1.2MPa, and the extraction temperature is 120 ℃; the single static extraction time is 10 min/time, and the cycle time is 3 times; the extraction solvent was toluene.
4. The method for the cooperative detection of polychlorinated biphenyl and polybrominated diphenyl ethers in soil as set forth in claim 3, which comprises the steps of: the composite chromatographic column in the step S2 comprises the following components from bottom to top: glass wool, quartz sand 1cm in height, magnesium florisil 1g, basic alumina 3g, basic silica gel 4g, neutral silica gel 3g, acidic silica gel 40g, quartz sand 1cm in height.
5. The method for the cooperative detection of polychlorinated biphenyl and polybrominated diphenyl ethers in soil according to claim 4, wherein the method comprises the following steps: the alkaline silica gel is prepared by mixing 1mol/L sodium hydroxide solution and neutral silica gel, wherein the mass ratio of the 1mol/L sodium hydroxide solution to the neutral silica gel is 33: 67; the acidic silica gel is prepared by mixing concentrated sulfuric acid and neutral silica gel, wherein the mass ratio of the concentrated sulfuric acid to the neutral silica gel is 2: 3.
6. The method for the cooperative detection of polychlorinated biphenyl and polybrominated diphenyl ethers in soil according to claim 5, wherein: the specific steps of synchronously purifying polychlorinated biphenyl and polybrominated diphenyl ether in the step S2 are as follows:
s21, transferring the concentrated extract into a composite chromatographic column, eluting with 120mL of normal hexane and 25mL of mixed solvent of normal hexane and dichloromethane respectively, and collecting the eluent;
s22, placing the collected eluent into a flat-bottomed flask for rotary evaporation concentration operation, and concentrating the eluent to 30 uL.
7. The method for the cooperative detection of polychlorinated biphenyl and polybrominated diphenyl ethers in soil according to claim 6, which comprises the following steps: in the mixed solvent of the normal hexane and the dichloromethane, the volume ratio of the normal hexane to the dichloromethane is 95: 5.
8. The method for the cooperative detection of polychlorinated biphenyl and polybrominated diphenyl ethers in soil according to claim 7, which comprises the following steps: when the high-resolution gas chromatography-high-resolution mass spectrometer is used for detecting polychlorinated biphenyl in the concentrated eluent in the step S3, the high-resolution gas chromatography parameters are as follows: the temperature of a sample inlet is 280 ℃, the temperature of a transmission line is 280 ℃, the flow rate of carrier gas is 1.0mL/min, the sample injection amount is 1uL, and the sample injection is not divided; the chromatographic column is DB-5MS, and the temperature-raising program of the chromatographic column is as follows: the initial temperature is 90 ℃, the temperature is kept for 2min, the temperature is increased to 220 ℃ at the speed of 13 ℃/min, and the temperature is kept for 7 min; then raising the temperature to 260 ℃ at a speed of 1.4 ℃/min; finally, raising the temperature to 310 ℃ at a speed of 4 ℃/min;
the high resolution mass spectrum parameters are as follows: the ion source temperature is 280 ℃, the electron energy is 45eV, and the resolution is more than 10000.
9. The method for the cooperative detection of polychlorinated biphenyl and polybrominated diphenyl ethers in soil according to claim 8, wherein: when the high-resolution gas chromatography-high-resolution mass spectrometer is used for detecting the polybrominated diphenyl ethers in the concentrated eluent in the step S3, the high-resolution gas chromatography parameters are as follows: the temperature of a sample inlet is 280 ℃, the temperature of a transmission line is 280 ℃, the flow rate of carrier gas is 1.0mL/min, the sample injection amount is 1uL, and the sample injection is not divided; the chromatographic column is DB-5MS, and the temperature-raising program of the chromatographic column is as follows: the initial temperature is 90 ℃, the temperature is kept for 2min, the temperature is increased to 180 ℃ at the speed of 15 ℃/min, and the temperature is kept for 2 min; then raising the temperature to 240 ℃ at a speed of 5 ℃/min, and keeping the temperature at 3 ℃; finally, raising the temperature to 310 ℃ at a speed of 3 ℃/min;
the high resolution mass spectrum parameters are as follows: the ion source temperature is 300 ℃, the electron energy is 35eV, and the resolution is more than 10000.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011495396.3A CN112630337A (en) | 2020-12-17 | 2020-12-17 | Method for cooperatively detecting polychlorinated biphenyl and polybrominated diphenyl ether in soil |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011495396.3A CN112630337A (en) | 2020-12-17 | 2020-12-17 | Method for cooperatively detecting polychlorinated biphenyl and polybrominated diphenyl ether in soil |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112630337A true CN112630337A (en) | 2021-04-09 |
Family
ID=75316381
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011495396.3A Pending CN112630337A (en) | 2020-12-17 | 2020-12-17 | Method for cooperatively detecting polychlorinated biphenyl and polybrominated diphenyl ether in soil |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112630337A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113933408A (en) * | 2021-09-09 | 2022-01-14 | 国家粮食和物资储备局科学研究院 | Analysis method of polybrominated diphenyl ethers in grains |
| CN113945650A (en) * | 2021-09-09 | 2022-01-18 | 国家粮食和物资储备局科学研究院 | Method for simultaneously analyzing persistent organic pollutants in grains |
| CN114814008A (en) * | 2022-04-06 | 2022-07-29 | 大连理工大学 | Method for synchronously extracting and purifying organic pollutants in soil and sediments |
| CN115963213A (en) * | 2023-02-08 | 2023-04-14 | 生态环境部华南环境科学研究所(生态环境部生态环境应急研究所) | Method for purifying and separating dioxin, polychlorinated biphenyl and polybrominated diphenyl ether in environmental medium |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102109505A (en) * | 2009-12-23 | 2011-06-29 | 中国科学院生态环境研究中心 | Pretreatment method for purifying extract liquor |
| CN102539548A (en) * | 2011-12-02 | 2012-07-04 | 环境保护部华南环境科学研究所 | Method and device for purifying dioxin substance in environmental matrix extracting solution by using one-stage method |
| CN103235062A (en) * | 2013-04-19 | 2013-08-07 | 华东理工大学 | Detecting method for multiple kinds of poly brominated diphenyl ethers in aquatic product |
| CN104237436A (en) * | 2014-09-03 | 2014-12-24 | 上海大学 | Qualitative screening method of semi-volatile halogenated organic pollutants in sediments |
| US20150132245A1 (en) * | 2012-04-26 | 2015-05-14 | Niva | Method for detoxification or measurement of at least one compound or at least one fluid in a host body |
| CN108535081A (en) * | 2018-05-11 | 2018-09-14 | 广东产品质量监督检验研究院（国家质量技术监督局广州电气安全检验所、广东省试验认证研究院、华安实验室） | Persistence organic pollutant purification system and its processing method in environment solid dielectric |
| CN208140456U (en) * | 2018-05-11 | 2018-11-23 | 广东产品质量监督检验研究院（国家质量技术监督局广州电气安全检验所、广东省试验认证研究院、华安实验室） | Persistence organic pollutant purification system in environment solid dielectric |
| WO2020128069A1 (en) * | 2018-12-20 | 2020-06-25 | Skillcell | Biodegradable biochemical sensor for determining the presence and/or the level of pesticides or endocrine disruptors: method and composition |
-
2020
- 2020-12-17 CN CN202011495396.3A patent/CN112630337A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102109505A (en) * | 2009-12-23 | 2011-06-29 | 中国科学院生态环境研究中心 | Pretreatment method for purifying extract liquor |
| CN102539548A (en) * | 2011-12-02 | 2012-07-04 | 环境保护部华南环境科学研究所 | Method and device for purifying dioxin substance in environmental matrix extracting solution by using one-stage method |
| US20150132245A1 (en) * | 2012-04-26 | 2015-05-14 | Niva | Method for detoxification or measurement of at least one compound or at least one fluid in a host body |
| CN103235062A (en) * | 2013-04-19 | 2013-08-07 | 华东理工大学 | Detecting method for multiple kinds of poly brominated diphenyl ethers in aquatic product |
| CN104237436A (en) * | 2014-09-03 | 2014-12-24 | 上海大学 | Qualitative screening method of semi-volatile halogenated organic pollutants in sediments |
| CN108535081A (en) * | 2018-05-11 | 2018-09-14 | 广东产品质量监督检验研究院（国家质量技术监督局广州电气安全检验所、广东省试验认证研究院、华安实验室） | Persistence organic pollutant purification system and its processing method in environment solid dielectric |
| CN208140456U (en) * | 2018-05-11 | 2018-11-23 | 广东产品质量监督检验研究院（国家质量技术监督局广州电气安全检验所、广东省试验认证研究院、华安实验室） | Persistence organic pollutant purification system in environment solid dielectric |
| WO2020128069A1 (en) * | 2018-12-20 | 2020-06-25 | Skillcell | Biodegradable biochemical sensor for determining the presence and/or the level of pesticides or endocrine disruptors: method and composition |
Non-Patent Citations (4)
| Title |
|---|
| 史双昕 等: "苏州、无锡和南通道路灰尘中的多溴联苯醚和多氯联苯", 《环境科学》 * |
| 李晓敏 等: "大流量采样高分辨气相色谱/高分辨质谱法测定大气中的多氯联苯和多溴联苯醚", 《色谱》 * |
| 韩善龙 等: "不同水源灌溉的农田表层土壤中多氯联苯和多溴联苯醚的浓度分布特征", 《环境化学》 * |
| 马召辉 等: "太湖沉积物中多溴联苯醚和类二英多氯联苯的水平垂直分布", 《环境科学》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113933408A (en) * | 2021-09-09 | 2022-01-14 | 国家粮食和物资储备局科学研究院 | Analysis method of polybrominated diphenyl ethers in grains |
| CN113945650A (en) * | 2021-09-09 | 2022-01-18 | 国家粮食和物资储备局科学研究院 | Method for simultaneously analyzing persistent organic pollutants in grains |
| CN114814008A (en) * | 2022-04-06 | 2022-07-29 | 大连理工大学 | Method for synchronously extracting and purifying organic pollutants in soil and sediments |
| CN115963213A (en) * | 2023-02-08 | 2023-04-14 | 生态环境部华南环境科学研究所(生态环境部生态环境应急研究所) | Method for purifying and separating dioxin, polychlorinated biphenyl and polybrominated diphenyl ether in environmental medium |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN112630337A (en) | Method for cooperatively detecting polychlorinated biphenyl and polybrominated diphenyl ether in soil | |
| CN105044236B (en) | Dispersive solid-phase extraction gas chromatography method for polychlorinated biphenyls in soil and sediment | |
| Ulrich | Speciation of antimony (III), antimony (V) and trimethylstiboxide by ion chromatography with inductively coupled plasma atomic emission spectrometric and mass spectrometric detection | |
| Ali et al. | Advances in arsenic speciation techniques | |
| McEvoy et al. | Accumulation of linear alkylbenzenesulphonate surfactants in sewage sludges | |
| CN108680656A (en) | A method of polybrominated biphenyls ether content in sludge composting sample is detected using accelerated solvent extraction in-line purification method | |
| CN109856285A (en) | Method that is a kind of while detecting multiclass persistent organism in water body | |
| Zhang et al. | Spatial distribution of polycyclic aromatic hydrocarbons from Lake Taihu, China | |
| Kodamatani et al. | Selective determination method for measurement of methylmercury and ethylmercury in soil/sediment samples using high-performance liquid chromatography–chemiluminescence detection coupled with simple extraction technique | |
| De la Torre et al. | Concentrations and sources of an emerging pollutant, decabromodiphenylethane (DBDPE), in sewage sludge for land application | |
| CN112362772A (en) | Method for detecting residual organic solvent in soil | |
| CN112666295A (en) | Method for extracting, cooperatively separating and detecting polychlorinated biphenyl and dioxin in soil | |
| Yang et al. | Determination of 4-tert-octylphenol in surface water samples of Jinan in China by solid phase extraction coupled with GC-MS | |
| CN108362786A (en) | The Accelerate solvent extraction analysis method of N,N-dimethylformamide in a kind of soil | |
| Zhang et al. | Enantioselective separation and determination of single nonylphenol isomers | |
| CN106053681A (en) | Pretreatment method for ambient air or exhaust gas sample and determination method for dioxin | |
| CN112630323A (en) | Method for detecting 46 semi-volatile organic compounds in underground water | |
| Wang et al. | Phthalate esters in sediments from Guanting Reservoir and the Yongding River, Beijing, People's Republic of China. | |
| CN111044647A (en) | Sample pretreatment and quantitative analysis method for detecting linear alkylbenzene in water body | |
| Greene et al. | Colorimetric detection of uranium (VI) on building surfaces after enrichment by solid phase extraction | |
| CN107727706B (en) | Preparation method and application of alumina hydrate bacterial cellulose carbon composite material | |
| Börjesson et al. | New method for determination of fecal sterols in urine using non-chlorinated solvents | |
| CN103293247A (en) | Quantitative determination method for naphthalene and anthracene in sediments on river channel with compound pollution | |
| CN106950301B (en) | Determination method of dioxin in sediment and rapid pretreatment method of sediment | |
| CN205280680U (en) | Survey system of trace alkyl mercury |
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 |