CN113552267A - Method for simultaneously measuring aniline, nitrobenzene and polycyclic aromatic hydrocarbon in soil - Google Patents
Method for simultaneously measuring aniline, nitrobenzene and polycyclic aromatic hydrocarbon in soil Download PDFInfo
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Abstract
The invention relates to a method for simultaneously measuring aniline, nitrobenzene and polycyclic aromatic hydrocarbon in soil, which comprises the steps of soil sample preparation, standard solution preparation, working curve drawing and sample result measurement, and is characterized in that the measuring method comprises the following steps: extracting the soil sample in an accelerated solvent extractor, adding 100-: extracting with dichloromethane solvent, concentrating the extractive solution to 1mL, adding internal standard, filtering with 0.22 μm filter head, loading on the machine, and measuring with gas chromatography mass spectrometer to calculate the content of the substance to be measured in soil. The method simplifies the complex means that aniline, nitrobenzene and polycyclic aromatic hydrocarbon are pretreated for three times and respectively measured in the procedures of the existing method, simplifies the operation steps, reduces the experiment cost, improves the recovery rate of the target, makes up the defects of the current standard, and is easy to popularize and use in the actual pollution investigation.
Description
Technical Field
The invention relates to a method for simultaneously measuring aniline, nitrobenzene and polycyclic aromatic hydrocarbon in soil.
Background
The soil is a material foundation for sustainable development of economic society, and the soil environment quality is established in China with the relationship of health and beauty of people. The state pays more and more attention to the soil environment condition, soil detection plays a role that other subjects cannot replace in soil pollution attack and soil environment evaluation, high-quality detection data provide basic data for scientifically formulating ecological environment governance policies, and development of a test method is an important way for improving data reliability.
Aniline is easy to volatilize, and after entering a water body, the molecular structure is very stable, so that persistent environmental pollution is easy to cause, and the aniline has high toxicity, and can cause poisoning only in a small amount. Mainly causes hemoglobinemia, hemolytic anemia and liver and kidney damage; nitrobenzene is widely used in production of pesticides, dyes, explosives, rubber and other chemical products, belongs to a high-toxicity pollutant, and can invade human body through respiratory tract, digestive tract and skin. Because the nitrobenzene has a stable structure and is difficult to degrade, the nitrobenzene causes persistent pollution to soil; polycyclic aromatic hydrocarbons PAHs are environmental chemical carcinogens, and the main harm parts to human bodies are respiratory tracts and skins. People are in polycyclic aromatic hydrocarbon polluted environment for a long time, can cause acute or chronic injury, and have more and more serious threats to human health.
Aniline, nitrobenzene and polycyclic aromatic hydrocarbon belong to semi-volatile organic matters in basic items in soil environmental quality construction land soil pollution risk control standards (GB 36600-2018) and are pollutants with high investigation and detection rate of polluted sites, but the existing detection methods for three substances have certain limitations, aniline substances can be subjected to quantitative analysis by liquid chromatography-triple quadrupole mass spectrometry, but the operation steps are complicated, the extraction efficiency is low, and the instrument cost is high; nitrobenzene and polycyclic aromatic hydrocarbons can be determined by gas chromatography-mass spectrometry, but need to be treated separately, and are not suitable for popularization and use. At present, a universal method for simultaneously measuring the three substances is lacked, so that the detection efficiency of soil pollution is limited. The pressurized fluid extraction technology has the obvious advantages of solvent saving, rapidness, high recovery rate, high automation degree and the like. The accelerated solvent extraction method provides favorable conditions for improving the accuracy, precision and practicability of analysis of semi-volatile organic compounds in soil. The gas chromatography-mass spectrometry can realize accurate qualitative and quantitative detection of semi-volatile organic compounds simultaneously by selecting a proper sample pretreatment method and a proper quantitative means. The accelerated solvent extraction instrument and the gas combination instrument are common instruments in an environment detection laboratory, and the application combines the advantages of the two methods and has wide popularization and application prospects.
Disclosure of Invention
A method for simultaneously measuring aniline, nitrobenzene and polycyclic aromatic hydrocarbon in soil solves the technical problems of simplifying analysis operation steps, improving the recovery rate of target objects and improving the detection efficiency.
In order to solve the technical problems, the invention adopts the following technical scheme:
a method for simultaneously measuring aniline, nitrobenzene and polycyclic aromatic hydrocarbon in soil comprises the steps of soil sample preparation, standard solution preparation, working curve drawing and sample result measurement, and comprises the following steps: weighing 10 g of freeze-dried soil sample, adding ammonia water into the sample to adjust the pH value to 10-12, and extracting by using an extraction solvent to obtain an extract liquor; concentrating the extract to 1mL to obtain a concentrated solution, adding 6 SVOC internal standard solutions into the concentrated solution, filtering by using a 0.22-micrometer organic filter head to obtain a filtrate, namely the solution to be detected, and detecting by using a gas chromatography mass spectrometer to calculate the content of the substance to be detected in the soil.
The freeze-dried soil sample is prepared according to the following steps: and (3) putting the sample on an enamel plate and a stainless steel plate, removing foreign matters, uniformly stirring, putting into a vacuum freeze dryer for drying and dehydrating for 15-24h, drying, grinding through a sieve with the aperture of 0.25mm, and processing into particles with the diameter of 240-260 mu m to obtain the freeze-dried soil sample.
The extraction conditions are that the temperature is 100 ℃, the extraction pressure is 105 bar, and the extraction solvent is a mixed solvent of acetone and dichloromethane in a volume ratio of 1: 1;
the ratio of the volume of extraction solvent (mL) to the mass of soil (g) is 7: 1;
the foreign matter is one or more of branches, leaves and stones.
The adding amount of the ammonia water is that every 10 g of soil sample is added with 500 mul of ammonia water of 100-; the concentration of the ammonia water is 25-28 wt%;
and concentrating by using a parallel concentrator under the conditions of 30 ℃ of temperature and 300 mbar of pressure to 0.8-1.2 mL, adding 5 mL of n-hexane for phase exchange, and concentrating again to 1 mL.
The organic filter head is a nylon 6 filter head.
The extraction concentrated solution is light-colored or colorless transparent liquid, if the extraction concentrated solution is dark-colored opaque or viscous liquid, the measurement is carried out after dilution, and the dilution step is as follows: and (3) taking 20-200 mu l of concentrated solution, supplementing 800-980 mu l of n-hexane to enable the total volume of the concentrated solution and the n-hexane to be 1mL, and supplementing 1-10 mu l of 6 SVOC internal standard solutions to enable the internal standard concentration to be 10 mu g/mL.
The 6 SVOC internal standard solutions added into the concentrated solution are acenaphthene-d 10, chrysene- d 12, 1, 4-dichlorobenzene-d 4, naphthalene-d 8, perylene-d 12 and phenanthrene-d 10 according to the mass ratio of 1: 1: 1: 1: 1: 1; the concentration of 6 SVOC internal standard solutions in the solution to be detected is 10 mug/mL.
The gas chromatography and mass spectrum conditions of the gas chromatography-mass spectrometer are as follows:
a chromatographic column: DB-5MS chromatographic column with length of 30m, inner diameter of 0.25mm and film thickness of 0.25 μm;
sample inlet temperature: 280 ℃, sample injection mode: no flow diversion; sample introduction amount: 1.0 mul, the main flow is 1.0 mL/min;
temperature programming process: starting to maintain at 35 deg.C for 2 min, heating to 150 deg.C at 15 deg.C/min, maintaining for 5 min, heating to 290 deg.C at 10 deg.C/min, and maintaining for 9.0 min;
the mass spectrum conditions of the gas chromatography mass spectrometer are as follows:
an ion source: an electron impact source (EI);
the ion source temperature is 230 ℃;
ionization energy is 70 eV;
the interface temperature is 280 ℃;
the temperature of the four-level bar is 150 ℃;
the mass scanning range is 35 amu-450 amu;
the solvent delay time is 4-5 min;
the data acquisition mode is a full Scan (Scan) mode.
The standard solution preparation is carried out according to the following steps:
1) standard stock solutions: transferring 0.1 mL of 2000 mg/L64 mixed standard solutions and 0.2 mL of 1000 mg/L aniline standard solutions into a 1mL volumetric flask, and performing constant volume by using dichloromethane to obtain a standard stock solution;
2) standard use solutions: sucking the standard stock solution in the step 1), adding the standard stock solution into a volumetric flask, adding 10 mu l of 6 SVOC internal standard solutions into the volumetric flask, and performing constant volume by adopting dichloromethane to obtain a standard use solution;
the concentration of 6 SVOC internal standards in the standard use solution is 10 mug/mL;
the 64 mixed standard execution standards are HJ834 and 2017.
The concentrations of the standard use solutions are 1 mg/L, 2 mg/L, 5 mg/L, 10 mg/L and 20 mg/L respectively;
the concentrations in the standard use solution are the respective concentrations of aniline, nitrobenzene and polycyclic aromatic hydrocarbon.
Drawing the working curve according to the following steps:
a) sequentially enabling standard use solutions to enter a gas chromatography mass spectrometer through a sample injector in sequence from low concentration to high concentration, separating different target substances by using programmed heating, and determining quantitative ion response values of aniline, nitrobenzene and polycyclic aromatic hydrocarbon in each standard use solution;
b) taking the concentration of the target compound as a horizontal coordinate, taking the product of the ratio of the quantitative ion response value of the target compound and the internal standard compound and the mass concentration of the internal standard compound as a vertical coordinate, and drawing a calibration curve;
the sample result determination is carried out according to the following steps:
and (3) feeding the liquid to be detected into a gas chromatography mass spectrometer through a sample injector for analysis to obtain peak areas of quantitative ions of different compounds, and substituting an internal standard method into a working curve to calculate the contents of aniline, nitrobenzene and polycyclic aromatic hydrocarbon in the soil sample.
The invention has the following beneficial technical effects:
1. compared with the prior art, the method has the advantages that 100-500 mu l of ammonia water is added during extraction, the pH value of the soil is adjusted to 10-12, the recovery rate of extraction can be improved, the stability of aniline in the whole extraction process is facilitated, and the accuracy of experimental data is improved.
2. The method adopts the 0.22 mu m filter head for filtration and then is used for detection on the computer after concentration, simplifies the operation steps, improves the analysis efficiency, reduces the labor cost and is beneficial to the detection of a large batch of samples in a laboratory compared with the steps of three batches of purification treatment required by other methods.
3. The method adopts the gas chromatography-mass spectrometer to measure the semi-volatile organic compounds in the extraction liquid, has the advantages of small interference, equivalent detection limit, good reproducibility, high accuracy and the like compared with a liquid chromatography-triple quadrupole mass spectrometry method and a gas chromatography method, simultaneously optimizes the temperature rise rate of the gas chromatography-mass spectrometer, realizes the simultaneous, rapid and accurate measurement of aniline, nitrobenzene and polycyclic aromatic hydrocarbon (except 2-chlorophenol) which are basic items of the semi-volatile organic compounds in GB3660, and greatly improves the analysis efficiency.
Drawings
FIG. 1 is a standard graph of aniline and nitrobenzene in accordance with the present invention;
FIG. 2 is a standard graph of naphthalene and benzo (a) anthracene according to the invention;
FIG. 3 is a standard graph of chrysene and benzo (b) fluoranthene of the present invention;
FIG. 4 is a standard graph of benzo [ k ] fluoranthene and benzo [ a ] pyrene of the present invention;
FIG. 5 is a graph of a standard plot of indeno [1.2.3-c, d ] pyrene and dibenzo [ a.h ] anthracene according to the present invention;
FIG. 6 is a total ion flow chart of aniline, nitrobenzene and polycyclic aromatic hydrocarbon according to the present invention.
Detailed Description
The present invention is further illustrated by the following specific examples.
Example 1
1. Sample preparation
1) Sample lyophilization
Placing the sample on an enamel plate or a stainless steel plate, removing foreign matters such as branches, leaves, stones and the like, uniformly mixing, placing in a vacuum freeze dryer for drying and dehydrating for 15-24h, drying, grinding through a sieve with the aperture of 0.25mm, and homogenizing to obtain particles with the diameter of about 250 mu m.
2) Sample extraction
Weighing 10.00g of sample, placing the sample into an extraction tank, adding 200 mul of ammonia water to adjust the pH to be more than 10, placing the sample into an accelerated solvent extraction instrument, and selecting an extraction solvent as acetone with the volume ratio of 1: dichloromethane, temperature 100 ℃ and pressure 105 bar were set. The extraction is circulated for 2 times, and the extract is collected.
3) Concentrating
Placing the extractive solution on a parallel concentration instrument, and setting the concentration condition at 30 deg.C in water bath and 300 mbar in concentration pressure. Concentrating to about 1mL, adding 5 mL n-hexane for phase exchange, and concentrating again to 1mL concentrated solution.
4) Filtration
After 10 μ L of 6 SVOC internal standards (acenaphthene-d 10, chrysene- d 12, 1, 4-dichlorobenzene-d 4, naphthalene-d 8, perylene-d 12 and phenanthrene-d 10) are added into the concentrated solution, the concentration of the internal standards is 10 μ g/mL. Then transferring the solution to a 1mL glass needle tube and passing through a 0.22 mu m nylon 6 filter head to obtain the solution to be detected.
2. Drawing a standard curve
(1) Preparation of Mixed Standard solution
1) Standard stock solutions: transferring 0.1 mL of 2000 mg/L64 mixed standard (HJ 834-2017) standard solutions and 0.2 mL of 1000 mg/L aniline standard solutions into a 1mL volumetric flask, and performing constant volume by using dichloromethane to obtain a standard stock solution, wherein the 64SVOC internal standard comprises compounds such as nitrobenzene, polycyclic aromatic hydrocarbon and the like;
2) standard use solutions: sucking the standard stock solutions with different volumes in the step 1) into a 1mL volumetric flask, adding 10 mu l of 6 SVOC internal standard solutions into the volumetric flask, and finally performing constant volume by adopting dichloromethane to obtain a series of standard use solutions with different concentrations;
the concentration of 6 SVOC internal standards in the standard use solution was 10. mu.g/mL. The concentrations of the standard use solutions (aniline, nitrobenzene and polycyclic aromatic hydrocarbons) were 1 mg/L, 2 mg/L, 5 mg/L, 10 mg/L and 20 mg/L, respectively.
(2) Drawing a standard curve
a) Sequentially feeding standard use solutions of aniline, nitrobenzene and polycyclic aromatic hydrocarbon with different concentrations into a gas chromatography mass spectrometer from low concentration to high concentration through a sample injector for analysis, separating different target substances by using a programmed temperature rise method, and determining quantitative ion response values of the aniline, the nitrobenzene and the polycyclic aromatic hydrocarbon in each mixed standard solution;
b) and (3) taking the concentration of the target compound as an abscissa, and taking the product of the ratio of the quantitative ion response value of the target compound to the internal standard compound and the mass concentration of the internal standard compound as an ordinate to draw a calibration curve.
Setting the gas chromatography conditions of the gas chromatography mass spectrometer as follows:
a chromatographic column: DB-5MS chromatographic column with length of 30m, inner diameter of 0.25mm and film thickness of 0.25 μm;
sample inlet temperature: 280 ℃, sample injection mode: no flow diversion; sample introduction amount: 1.0. mu.l, main flow 1.0 mL/min
Temperature programming process: holding at 35 deg.C for 2 min, heating to 150 deg.C at 15 deg.C/min for 5 min, and heating at 10 deg.C/min
To 290 deg.C, maintain for 9.0 min.
The mass spectrum conditions of the gas chromatography mass spectrometer are as follows:
an ion source: an electron impact source (EI);
the ion source temperature is 230 ℃;
ionization energy is 70 eV;
the interface temperature is 280 ℃;
the temperature of the four-level bar is 150 ℃;
the mass scanning range is 35 amu-450 amu;
the solvent delay time is 4-5 min;
the data acquisition mode is a full Scan (Scan) mode.
(3) Determination of soil samples
And (3) feeding the prepared sample solution to be detected into a gas chromatography mass spectrometer through a sample injector for simultaneous analysis to obtain peak areas of quantitative ions of different compounds, and substituting an internal standard method into a working curve to calculate the contents of aniline, nitrobenzene and polycyclic aromatic hydrocarbon in the soil sample.
The recovery rates of three types of compounds are calculated by measuring the contents of aniline, nitrobenzene and polycyclic aromatic hydrocarbon in the soil samples of the added standard sample 1, the sample 2 and the sample 3, the recovery rate ranges from 47.3% to 82.6%, and the test requirements of HJ834-2017 are met.
As can be seen from Table 1, the pH value is adjusted to 10-12, the stability of the aniline can be obviously improved, the recovery rate of a detection sample is 47.3-82.6%, the detection result is more accurate, and the problem of low aniline recovery rate exists when the pH =8, the detection result is not accurate, and the detection result is inaccurate when the pH value is adjusted to 10-82.7.
Claims (13)
1. A method for simultaneously measuring aniline, nitrobenzene and polycyclic aromatic hydrocarbon in soil comprises the steps of soil sample preparation, standard solution preparation, working curve drawing and sample result measurement, and is characterized by comprising the following steps: weighing 10 g of freeze-dried soil sample, adding ammonia water into the sample to adjust the pH value to 10-12, and extracting by using an extraction solvent to obtain an extract liquor; concentrating the extract to 1mL to obtain a concentrated solution, adding 6 SVOC internal standard solutions into the concentrated solution, filtering by using a 0.22-micrometer organic filter head to obtain a filtrate, namely the solution to be detected, and detecting by using a gas chromatography mass spectrometer to calculate the content of the substance to be detected in the soil.
2. The method for simultaneously measuring the aniline, the nitrobenzene and the polycyclic aromatic hydrocarbon in the soil according to claim 1, wherein the freeze-drying soil sample is carried out according to the following steps: and (3) putting the sample on an enamel plate and a stainless steel plate, removing foreign matters, uniformly stirring, putting into a vacuum freeze dryer for drying and dehydrating for 15-24h, drying, grinding through a sieve with the aperture of 0.25mm, and processing into particles with the diameter of 240-260 mu m to obtain the freeze-dried soil sample.
3. The method for simultaneously measuring the aniline, the nitrobenzene and the polycyclic aromatic hydrocarbon in the soil according to claim 1, wherein the extraction conditions are that the temperature is 100 ℃, the extraction pressure is 105 bar, and the extraction solvent is a mixed solvent of acetone and dichloromethane in a volume ratio of 1: 1;
the ratio of the volume of extraction solvent (mL) to the mass of soil (g) is 7: 1;
the foreign matter is one or more of branches, leaves and stones.
4. The method for simultaneously measuring aniline, nitrobenzene and polycyclic aromatic hydrocarbon in soil as claimed in claim 1, wherein the amount of ammonia added is 500 μ l of ammonia per 10 g of soil sample; the concentration of the ammonia water is 25-28 wt%.
5. The method for simultaneously measuring the aniline, the nitrobenzene and the polycyclic aromatic hydrocarbon in the soil according to claim 1, wherein a parallel concentrator is adopted for concentration, the concentration condition is that the temperature is 30 ℃, the pressure is 300 mbar, after the concentration is carried out to 0.8-1.2 mL, 5 mL of n-hexane is added for phase change, and the concentration is carried out again to 1 mL.
6. The method for simultaneously measuring the aniline, the nitrobenzene and the polycyclic aromatic hydrocarbon in the soil according to claim 1, wherein the organic filter head is a nylon 6 filter head.
7. The method for simultaneously measuring the aniline, the nitrobenzene and the polycyclic aromatic hydrocarbon in the soil as claimed in claim 1, wherein the extraction concentrate is a light-colored or colorless transparent liquid, and is measured after being diluted if the extraction concentrate is a dark-colored opaque or viscous liquid, and the dilution step comprises the following steps: and (3) taking 20-200 mu l of concentrated solution, supplementing 800-980 mu l of n-hexane to enable the total volume of the concentrated solution and the n-hexane to be 1mL, and supplementing 1-10 mu l of 6 SVOC internal standard solutions to enable the internal standard concentration to be 10 mu g/mL.
8. The method for simultaneously measuring the aniline, the nitrobenzene and the polycyclic aromatic hydrocarbon in the soil as claimed in claim 1, wherein the 6 SVOC internal standard solutions added into the concentrated solution are acenaphthene-d 10, chrysene-d 12, 1, 4-dichlorobenzene-d 4, naphthalene-d 8, perylene-d 12 and phenanthrene-d 10 according to the mass ratio of 1: 1: 1: 1: 1: 1; the concentration of 6 SVOC internal standard solutions in the solution to be detected is 10 mug/mL.
9. The method for simultaneously measuring the aniline, the nitrobenzene and the polycyclic aromatic hydrocarbon in the soil according to claim 1, wherein the gas chromatography mass spectrometer has the following gas chromatography and mass spectrum conditions:
a chromatographic column: DB-5MS chromatographic column with length of 30m, inner diameter of 0.25mm and film thickness of 0.25 μm;
sample inlet temperature: 280 ℃, sample injection mode: no flow diversion; sample introduction amount: 1.0 mul, the main flow is 1.0 mL/min;
temperature programming process: starting to maintain at 35 deg.C for 2 min, heating to 150 deg.C at 15 deg.C/min, maintaining for 5 min, heating to 290 deg.C at 10 deg.C/min, and maintaining for 9.0 min;
the mass spectrum conditions of the gas chromatography mass spectrometer are as follows:
an ion source: an electron impact source (EI);
the ion source temperature is 230 ℃;
ionization energy is 70 eV;
the interface temperature is 280 ℃;
the temperature of the four-level bar is 150 ℃;
the mass scanning range is 35 amu-450 amu;
the solvent delay time is 4-5 min;
the data acquisition mode is a full Scan (Scan) mode.
10. The method for simultaneously measuring the aniline, the nitrobenzene and the polycyclic aromatic hydrocarbon in the soil according to claim 1, wherein the standard solution preparation is carried out according to the following steps:
1) standard stock solutions: transferring 0.1 mL of 2000 mg/L64 mixed standard solutions and 0.2 mL of 1000 mg/L aniline standard solutions into a 1mL volumetric flask, and performing constant volume by using dichloromethane to obtain a standard stock solution;
2) standard use solutions: sucking the standard stock solution in the step 1), adding the standard stock solution into a volumetric flask, adding 10 mu l of 6 SVOC internal standard solutions into the volumetric flask, and performing constant volume by adopting dichloromethane to obtain a standard use solution;
the concentration of 6 SVOC internal standards in the standard use solution is 10 mug/mL;
the 64 mixed standard execution standards are HJ 834-2017.
11. The method for simultaneously measuring the aniline, the nitrobenzene and the polycyclic aromatic hydrocarbon in the soil according to claim 10, wherein the standard use solution concentration is 1 mg/L, 2 mg/L, 5 mg/L, 10 mg/L and 20 mg/L respectively;
the concentrations in the standard use solution are the respective concentrations of aniline, nitrobenzene and polycyclic aromatic hydrocarbon.
12. The method for simultaneously measuring the aniline, the nitrobenzene and the polycyclic aromatic hydrocarbon in the soil according to claim 11, wherein the working curve is drawn according to the following steps:
a) sequentially enabling standard use solutions to enter a gas chromatography mass spectrometer through a sample injector in sequence from low concentration to high concentration, separating different target substances by using programmed heating, and determining quantitative ion response values of aniline, nitrobenzene and polycyclic aromatic hydrocarbon in each standard use solution;
b) and drawing a working curve by taking the concentration of the target compound as an abscissa and taking the product of the ratio of the quantitative ion response value of the target compound to the internal standard compound and the mass concentration of the internal standard compound as an ordinate.
13. The method for simultaneously measuring the aniline, the nitrobenzene and the polycyclic aromatic hydrocarbon in the soil according to claim 1, wherein the sample result measurement is carried out according to the following steps:
and (3) feeding the liquid to be detected into a gas chromatography mass spectrometer through a sample injector for analysis to obtain peak areas of quantitative ions of different compounds, and substituting an internal standard method into a working curve to calculate the contents of aniline, nitrobenzene and polycyclic aromatic hydrocarbon in the soil sample.
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Application publication date: 20211026 |