CN112129855A - Method for measuring chloroacetic acid concentration in air by gas chromatography and application thereof - Google Patents
Method for measuring chloroacetic acid concentration in air by gas chromatography and application thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of chemical component detection and analysis, and discloses a method for determining chloroacetic acid concentration in air by using a gas chromatography and application thereof. According to the method, under the detection means of a gas chromatography, chloroacetic acid is silanized by N, O-bis (trimethylsilane) trifluoroacetamide under certain conditions, so that the polarity of chloroacetic acid is greatly reduced, the problem of inaccurate quantification caused by strong polarity tailing of chloroacetic acid is solved, and the detection sensitivity of chloroacetic acid is greatly improved. The detection method has good linear relation in the concentration range of 0-162.6 mug/mL, the correlation coefficient is 0.9997, the detection limit is 0.8 mug/mL, and the lowest detection concentration is 0.05mg/m3Relative Standard Deviation (RSD) of 5 replicates was between 0.5% and 1.3% (based on 15L air collected), and blank spiking recovery was 98.6 to 101.2 percent. The method is sensitive, simple and accurate, and can be used for measuring chloroacetic acid in air of a workplace.
Description
Technical Field
The invention belongs to the technical field of chemical component detection and analysis, and particularly relates to a method for determining chloroacetic acid concentration in air by using a gas chromatography and application thereof.
Background
Chloroacetic acid is an intermediate of dye, medicine, pesticide and other industries, and has wide application prospect. At room temperature, chloroacetic acid is colorless or white crystal, has pungent odor and strong corrosivity, and can be absorbed by respiratory tract, digestive tract and skin to cause multiple organ damage. The Maximum Allowable Concentration (MAC) of chloroacetic acid in the air of a daily workplace is 2mg/m3。
In the method provided by the national standard at present, chloroacetic acid in air of a workplace is conventionally collected by a silica gel tube, desorbed by water and measured by a packed column-gas chromatography. The method recommended by the national standard is not very suitable for detecting chloroacetic acid because chloroacetic acid has strong polarity, has a serious phenomenon of tailing of chromatographic peaks and has low sensitivity on an FID (fast infrared detection) detector.
In order to reduce the polarity of chloroacetic acid, in the prior art, concentrated sulfuric acid-ethanol solution is used for derivatizing chloroacetic acid into ethyl chloroacetate, and then the ethyl chloroacetate is measured by gas chromatography, but the method has complicated steps, and concentrated sulfuric acid has certain danger.
Because the capillary column has better separation effect and higher column efficiency, and is applied more in daily work, the development of a sensitive, simple and accurate gas chromatography detection method is very necessary.
Disclosure of Invention
In order to solve the problems in the prior art, the invention aims to provide a method for measuring the concentration of chloroacetic acid in air by using gas chromatography and application thereof.
The technical scheme adopted by the invention is as follows: a method for measuring chloroacetic acid concentration in air by gas chromatography comprises the steps of collecting chloroacetic acid in air by a silica gel tube as a sample, drying, adding a desorbent, desorbing at room temperature, carrying out silanization reaction to obtain a silanized product, measuring the silanized product by the gas chromatography, and quantitatively calculating the chloroacetic acid concentration by an external standard method.
Preferably, the measuring method comprises the steps of:
(1) preparation of standard series of solutions: respectively weighing a chloroacetic acid pure product, placing the chloroacetic acid pure product in a silica gel tube, respectively adding standard stock solutions, balancing for 24 hours, drying, adding a desorbent, desorbing at room temperature, and carrying out a silanization reaction to obtain a standard series solution;
(2) detection of standard series solution and drawing of working curve: measuring the standard series solution obtained in the step (1) by adopting gas chromatography, drawing a working curve, and calculating to obtain a linear regression equation;
(3) sample collection and treatment: collecting chloroacetic acid in air by using a silica gel tube, drying, adding a desorbent, desorbing at room temperature and carrying out a silanization reaction;
(4) the measurement mode of the sample: measuring the product of the chloroacetic acid silanization reaction in the step (3) by using gas chromatography, and substituting the measurement result into a formula of a working curve linear regression equation to obtain the concentration of chloroacetic acid in the sample solution;
(5) and (3) calculating: and (5) substituting the chloroacetic acid concentration in the sample solution measured in the step (4) into a formula to calculate the concentration of chloroacetic acid in the air.
Preferably, the desorbent in step (1) comprises acetonitrile and N, O-bis (trimethylsilane) trifluoroacetamide;
the volume ratio of acetonitrile to N, O-bis (trimethylsilane) trifluoroacetamide in the desorbent is 2: 1.
Preferably, the preparation of the standard stock solution in the step (1) is as follows:
adding a small amount of acetonitrile into a 10mL volumetric flask, accurately weighing 108.40mg of chloroacetic acid, adding into the volumetric flask, and metering the volume to a scale by using the acetonitrile to obtain a standard stock solution with the concentration of 10.840 mg/mL;
preferably, the mass concentration of the standard series solution in the step (1) is in the range of 0-162.6 mug/mL.
Preferably, the determination conditions in the gas chromatography determination in the step (2) include:
DB-5 column (30m × 0.32mm × 0.25 μm);
column temperature: the initial temperature is 50 ℃, and the temperature is increased to 120 ℃ at the speed of 5 ℃/min;
the temperatures of the vaporization chamber and the detector are both 250 ℃, the split ratio is 10:1, and the carrier gas is N2The flow rate of the carrier gas is 2 mL/min;
the amount of sample was 1. mu.L.
Preferably, the linear regression equation of the working curve in the step (2) is calculated by drawing the working curve with the concentration of the standard series solution as an abscissa and the peak area of the chloroacetic acid silanization product as an ordinate.
Preferably, in the step (3), a silica gel tube is used for collecting chloroacetic acid in the air, a desorbent is added after drying, and the time period for carrying out the desorption reaction comprises 28-90 minutes, preferably 30 minutes;
preferably, in the step (3), the air sample is collected at a flow rate of 1L/min for no more than 15 min.
Preferably, in the step (3), chloroacetic acid in the air is collected by using a silicone tube, and when the sampled silicone tube is dried, the drying temperature is 60-120 ℃, preferably 70-100 ℃, and further preferably 90 ℃;
the drying time is 10 to 45 minutes, preferably 15 to 30 minutes, and more preferably 20 minutes.
Preferably, the concentration of chloroacetic acid in air in the step (5) is calculated by the formula
C＝(C1+C2)V/V0
In the formula: c-concentration of chloroacetic acid in air in milligrams per cubic meterRice (mg/m)3)；C1，C2-measuring the concentration of chloroacetic acid in the sample solution at the front and back sections of the sampling tube in micrograms per milliliter (. mu.g/mL); v-volume of stripping solution, milliliters (mL); v0Standard sample volume, liter (L).
Use of a method for determining the concentration of chloroacetic acid in air by gas chromatography, for determining the concentration of chloroacetic acid in air at a workplace using the determination method of any of claims 1 to 9.
The invention has the beneficial effects that:
the invention provides a method for measuring chloroacetic acid concentration in air by gas chromatography and application thereof. The detection method has good linear relation in the concentration range of 0-162.6 mug/mL, the correlation coefficient is 0.9997, the detection limit is 0.8 mug/mL, and the lowest detection concentration is 0.05mg/m3Relative Standard Deviation (RSD) of 5 parallel measurements (calculated by collecting 15L of air) is between 0.5% and 1.3%, and blank standard addition recovery rate is between 98.6% and 101.2%. The method is sensitive, simple and accurate, and can be used for measuring chloroacetic acid in air of a workplace.
Drawings
FIG. 1 is a schematic diagram of a working standard curve of one embodiment of an example of a method for measuring chloroacetic acid concentration in air by gas chromatography;
FIG. 2 is a chromatogram of a chloroacetic acid standard solution with a mass concentration of 75.9. mu.g/mL in air of a workplace determined by gas chromatography (peak time of chromatography 5.425min) of an example;
FIG. 3 shows a specific embodiment of the chromatogram of the chloroacetic acid sample in air measured by gas chromatography (peak time of chromatogram is 5.425 min).
Detailed Description
The present invention is further illustrated below with reference to specific examples. It will be appreciated by those skilled in the art that the following examples, which are set forth to illustrate the present invention, are intended to be part of the present invention, but not to be construed as limiting the scope of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. The examples were carried out under the conventional conditions, unless otherwise specified. The reagents used are all conventional products which are commercially available.
Example (b):
the range is as follows: the method is suitable for measuring the concentration of chloroacetic acid in the air by using the gas chromatography.
The principle is as follows: adopt the silicone tube to gather chloroacetic acid in the air, the silicone tube who has adopted the appearance is dry in the oven, adds acetonitrile: the N, O-bis (trimethylsilane) trifluoroacetamide mixed solution was desorbed and reacted at room temperature, and the silanized product was analyzed by gas chromatography and quantified by an external standard method.
Instruments and devices: a Gilair plus explosion-proof individual air sampler (0-2L/min) (Gilian corporation, USA) is used for collecting samples.
Preparation of standard stock solution: adding a small amount of acetonitrile into a 10mL volumetric flask, accurately weighing 108.40mg of chloroacetic acid, adding into the volumetric flask, and fixing the volume to the scale by using the acetonitrile to obtain a standard stock solution with the concentration of 10.840 mg/mL.
Standard series solution preparation: adding 0.0, 1.0, 3.0, 5.0, 7.0, 10.0 and 15.0 μ L standard stock solution into 7 silica gel tubes respectively containing chloroacetic acid pure product, and balancing for 24 hr. And (3) drying the silica gel tube added with the standard stock solution in an oven at 90 ℃ for 20min, adding 1mL of acetonitrile: n, O-bis (trimethylsilane) trifluoroacetamide (2:1, V/V) is desorbed at room temperature and reacted for 30min to obtain standard series solutions with concentrations of 0, 10.8, 32.5, 54.2, 75.9, 108.4 and 162.6. mu.g/mL.
Blank sample: and (4) opening the seals at the two ends of the solvent desorption type silicone tube at the sampling point, immediately closing the two ends, and storing, transporting and measuring the same. The blank sample is a means of quality control and mainly used for judging whether the experimental sample is polluted in the transportation and storage processes.
Collecting samples: and opening the seals at two ends of the solvent desorption type silicone tube at a working site, collecting air with the flow rate of 1L/min not more than 15min, and sealing the two ends of the silicone tube after sampling.
Sample treatment: drying the sampled silicone tube in an oven at 90 ℃ for 20min, then pouring the front-section silica gel and the rear-section silica gel into desorption bottles respectively, and adding 1.0mL of acetonitrile into each of the silica gel tubes: n, O-bis (trimethylsilane) trifluoroacetamide (2:1, V/V), desorbed at room temperature and reacted for 30 min.
Setting instrument parameters: a1310 gas chromatograph (Thermo corporation, USA) is used in the measurement process, and a hydrogen flame ionization detector is configured.
The instrument conditions were as follows: DB-5 column (30m × 0.32mm × 0.25 μm); column temperature: the initial temperature is 50 ℃, and the temperature is increased to 120 ℃ at the speed of 5 ℃/min; the temperatures of the vaporization chamber and the detector are both 250 ℃, the split ratio is 10:1, and the carrier gas is N2The flow rate of the carrier gas is 2 mL/min; the amount of sample was 1. mu.L.
And (3) determination of a sample: and respectively detecting the treated sample solutions by using gas chromatography, and substituting peak areas into a linear regression equation of a working curve to obtain the concentration of chloroacetic acid in the sample solutions.
The calculation formula of the concentration of chloroacetic acid in air is as follows:
C＝(C1+C2)V/V0
in the formula: c-concentration of chloroacetic acid in air, milligrams per cubic meter (mg/m)3)；C1，C2-measuring the concentration of chloroacetic acid in the sample solution at the front and back sections of the sampling tube in micrograms per milliliter (. mu.g/mL); v-volume of stripping solution, milliliters (mL); v0Standard sample volume, liter (L).
Methodology investigation: preparing 7 chloroacetic acid standard solutions with mass concentration within the range of 0-162.6 mu g/mL, drawing a working curve by taking the concentration of chloroacetic acid as an abscissa and the peak area of a chloroacetic acid silanization product as an ordinate, and calculating to obtain a linear regression equation with y being 0.0118x and a linear correlation coefficient r being 0.9997, which shows that the linear relation is good. 5.4ug chloroacetic acid was added to each of 11 blank silica gel tubes and measured according to the analytical procedure, and the peak area standard deviation (n 11) was divided by 3 times the sensitivity(i.e. the slope of the working curve) the corresponding concentration is calculated as the detection limit of the method, the detection limit of the chloroacetic acid is calculated to be 0.8 mu g/ml, and the lowest detection concentration is 0.05mg/m3(to collect 15L air gauge). 15 blank silicone tubes are divided into 3 groups, 5 groups are respectively added with 21.7 mu g, 65.0 mu g and 108.4 mu g chloroacetic acid, detection is carried out according to the analysis steps, and the blank labeling recovery rate and RSD (n is 5) are calculated, and the results are shown in table 1.
Table 1 accuracy and repeatability test results (n ═ 5)
| Average recovery of blank/. mu.g | Average percent recovery of blank/%) | RSD/％ |
| 21.4 | 98.6 | 0.5 |
| 65.8 | 101.2 | 0.5 |
| 109.3 | 100.8 | 1.3 |
As can be seen from Table 1, the average blank standard recovery rate is between 98.6% and 101.2%, and the RSD is between 0.5% and 1.3%, indicating that the method has good accuracy and repeatability.
FIG. 1 is a schematic diagram showing the operating curve of gas chromatography for measuring the chloroacetic acid concentration in air by gas chromatography.
As shown in FIG. 2, the chromatogram for measuring chloroacetic acid standard substance in workplace air by gas chromatography provided above shows that the peak time is 5.425 min.
The detection method provided by the invention is adopted to detect chloroacetic acid in the air of a certain post site at different time intervals, and the measurement data result is shown in the following table 2:
TABLE 2 concentration of chloroacetic acid in workplace air
| Representing a time period | Sampling site | Concentration in air (mg/m)3) |
| 8:00-10:00 | Reaction kettle | 0.31 |
| 12:00-14:00 | Reaction kettle | 0.19 |
| 14:00-16:00 | Reaction kettle | 0.42 |
As shown in FIG. 3, the chromatogram of the chloroacetic acid sample in air measured by the gas chromatography of the invention shows that the peak time is 5.425 min.
The invention provides a method for measuring chloroacetic acid concentration in air by gas chromatography and a method for measuring chloroacetic acid concentration in air by gas chromatographyIn the determination method, chloroacetic acid is silanized by N, O-bis (trimethylsilane) trifluoroacetamide under a certain condition, so that the polarity of chloroacetic acid is greatly reduced, the problem of inaccurate quantification caused by strong polarity tailing of chloroacetic acid is solved, and the detection sensitivity of chloroacetic acid is greatly improved. The detection method has good linear relation in the concentration range of 0-162.8 mug/mL, the correlation coefficient (r) is 0.9997, the detection limit is 0.8 mug/mL, and the lowest detection concentration is 0.05mg/m3Relative Standard Deviation (RSD) of 5 parallel measurements (calculated by collecting 15L of air) is between 0.5% and 1.3%, and blank standard addition recovery rate is between 98.6% and 101.2%. The method is sensitive, simple and accurate, and can be used for measuring chloroacetic acid in air of a workplace.
While particular embodiments of the present invention have been illustrated and described, it will be appreciated that the present invention is not limited to the above-described alternative embodiments, and that various other forms of product may be devised by anyone in light of the present invention. The foregoing detailed description should not be construed as limiting the scope of the invention, and those skilled in the art will understand that various modifications can be made to the technical solutions described in the foregoing embodiments, or some or all of the technical features can be equivalently replaced, without departing from the spirit and scope of the invention, and at the same time, such modifications or replacements do not cause the essence of the corresponding technical solutions to depart from the scope of the technical solutions of the embodiments of the invention; the scope of the invention should be determined with reference to the appended claims, and the description should be construed to interpret the claims.
Claims (10)
1. A method for measuring chloroacetic acid concentration in air by gas chromatography is characterized in that chloroacetic acid in air is collected by a silicone tube and used as a sample, a desorbent is added, desorption is carried out at room temperature, a silanization reaction is carried out to obtain a silanization product, the silanization product is measured by the gas chromatography, and the chloroacetic acid concentration is quantitatively calculated by an external standard method.
2. The method of claim 1, wherein the method comprises the steps of:
(1) preparation of standard series of solutions: respectively and accurately weighing the chloroacetic acid pure products, placing the chloroacetic acid pure products into a silica gel tube, respectively adding standard stock solutions, balancing for 24 hours, drying, adding a desorbent, desorbing at room temperature, and carrying out silanization reaction to obtain standard series solutions;
(2) detection of standard series solution and drawing of working curve: measuring the standard series solution obtained in the step (1) by adopting gas chromatography, drawing a working curve, and calculating to obtain a linear regression equation;
(3) sample collection and treatment: collecting chloroacetic acid in air by using a silica gel tube, drying, adding a desorbent, desorbing at room temperature and carrying out a silanization reaction;
(4) the measurement mode of the sample: measuring the product of the chloroacetic acid silanization reaction in the step (3) by using gas chromatography, and substituting the measurement result into a formula of a working curve linear regression equation to obtain the concentration of chloroacetic acid in the sample solution;
(5) and (3) calculating: and (5) substituting the chloroacetic acid concentration in the sample solution measured in the step (4) into a formula to calculate the concentration of chloroacetic acid in the air.
3. The method for measuring chloroacetic acid concentration in air by gas chromatography as claimed in claim 1, wherein said desorbent in step (1) comprises acetonitrile and N, O-bis (trimethylsilane) trifluoroacetamide;
the volume ratio of acetonitrile to N, O-bis (trimethylsilane) trifluoroacetamide in the desorbent is 2: 1.
4. The method for measuring the concentration of chloroacetic acid in air by gas chromatography as claimed in claim 1, wherein said standard stock solution in step (1) is prepared by:
adding a small amount of acetonitrile into a 10mL volumetric flask, accurately weighing 108.40mg of chloroacetic acid, adding into the volumetric flask, and metering the volume to a scale by using the acetonitrile to obtain a standard stock solution with the concentration of 10.840 mg/mL;
preferably, the mass concentration of the standard series solution in the step (1) is in the range of 0-162.6 mug/mL.
5. The method for measuring chloroacetic acid concentration in air by gas chromatography as set forth in claim 1, wherein the conditions for gas chromatography measurement in step (2) comprise:
DB-5 column (30m × 0.32mm × 0.25 μm);
column temperature: the initial temperature is 50 ℃, and the temperature is increased to 120 ℃ at the speed of 5 ℃/min;
the temperatures of the vaporization chamber and the detector are both 250 ℃, the split ratio is 10:1, and the carrier gas is N2The flow rate of the carrier gas is 2 mL/min;
the amount of sample was 1. mu.L.
6. The method for measuring chloroacetic acid concentration in air by gas chromatography as claimed in claim 1, wherein said working curve linear regression equation in step (2) is calculated by plotting the working curve with the concentration of the standard series solution as abscissa and the peak area of the chloroacetic acid silanization product as ordinate.
7. The method for measuring the concentration of chloroacetic acid in air by gas chromatography as claimed in claim 1, wherein in step (3), the chloroacetic acid in air is collected by silica gel tube, and after drying, the desorbent is added, and the desorption reaction is carried out for a period of time comprising 28-90 minutes, preferably 30 minutes;
preferably, in the step (3), the air sample is collected at a flow rate of 1L/min for no more than 15 min.
8. The method for measuring the concentration of chloroacetic acid in air by gas chromatography as claimed in claim 1, wherein in step (3), chloroacetic acid in air is collected by a silicone tube, and when the collected silicone tube is dried, the drying temperature is 60-120 ℃, preferably 70-100 ℃, and further preferably 90 ℃;
the drying time is 10 to 45 minutes, preferably 15 to 30 minutes, and more preferably 20 minutes.
9. The method for measuring the concentration of chloroacetic acid in air by gas chromatography as claimed in claim 1, wherein the formula for calculating the concentration of chloroacetic acid in air in step (5) is
C＝(C1+C2)V/V0
In the formula: c-concentration of chloroacetic acid in air, milligrams per cubic meter (mg/m)3)；C1，C2-measuring the concentration of chloroacetic acid in the sample solution at the front and back sections of the sampling tube in micrograms per milliliter (. mu.g/mL); v-volume of stripping solution, milliliters (mL); v0Standard sample volume, liter (L).
10. Use of a method for measuring the concentration of chloroacetic acid in air by gas chromatography, characterized in that the method of any of claims 1 to 9 is used for the measurement of chloroacetic acid concentration in air at a workplace.
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