CN110824058A - Method for detecting chlorinated dioxin - Google Patents
Method for detecting chlorinated dioxin Download PDFInfo
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention discloses a method for detecting chlorinated dioxin, and belongs to the technical field of dioxin detection. The dioxin detection method comprises the steps of extraction, purification, nitrogen blowing concentration and on-machine detection which are sequentially carried out, wherein the extraction comprises the following steps: s1: drying the adsorption material; s2: soaking the filter cylinder with hydrochloric acid to obtain the filter cylinder and hydrochloric acid treatment liquid; s3: washing the filter cylinder with water, adding methanol to obtain a first mixed solution, and drying the filter cylinder; s4: washing the smoke tube with water and methanol to obtain a second mixed solution, and pouring the second mixed solution into a Buchner funnel to obtain a third mixed solution and a glass fiber membrane; s5: drying the glass fiber membrane; s6: extracting the third mixed solution to obtain a first extract; s7: and mixing the condensed water, the first mixed solution and the first extraction liquid to obtain a fourth mixed solution, and performing oscillation extraction to obtain a second extraction liquid. According to the invention, the filter cartridge, the condensed water, the smoke tube and the adsorbing material are all treated, so that the target substance is fully extracted.
Description
Technical Field
The invention relates to the technical field of dioxin detection, in particular to a chlorinated dioxin detection method.
Background
Dioxin is a persistent organic pollutant with extremely strong carcinogenicity, biological enrichment and other hazards, and is a byproduct of combustion and various industrial production; it is very slow to decompose under the action of organism, is easily adsorbed by soil, is easily dissolved in fat, and is easily accumulated in human body, and has teratogenicity, carcinogenesis and mutagenicity as the most harm.
The fixed source waste gas sampling of dioxin is generally realized by a dioxin sampling gun, the waste gas is absorbed into the sampling gun and is absorbed in an absorption column, and then the waste gas is transferred to a laboratory to be extracted and purified, and finally the dioxin is tested on a computer. The sampling gun comprises an air inlet sampling nozzle, a smoke pipe, an adsorption pipe at the end part of the smoke pipe, a filter cartridge part, an adsorption column and a condenser.
In the extraction step, the target substance in the sampling gun is fully extracted as far as possible. In the prior art, for example, chinese patent No. CN104749287B discloses a method for determining brominated dioxins in an environmental sample, which refers to the following extraction steps: carrying out Soxhlet extraction on an environmental sample to be detected to obtain an extracting solution containing brominated dioxin; however, the specific steps of how to extract the target substance from the sampling gun are not mentioned, and whether the extraction is sufficient or not is very important for the detection accuracy, and the sufficient extraction can improve the detection accuracy.
Disclosure of Invention
The invention aims to provide a chlorodioxin detection method, which achieves the effects of fully extracting target substances from a sampling gun and improving the detection accuracy.
In order to achieve the first object, the invention provides the following technical scheme:
the technical purpose of the invention is realized by the following technical scheme:
a method for detecting chlorodioxin comprises the steps of extraction, purification, nitrogen blowing concentration and on-machine detection which are sequentially carried out, wherein the extraction comprises the following steps:
s1: drying the adsorption material in the adsorption column of the sampling gun;
s2: taking out the filter cylinder in the sampling gun, soaking the filter cylinder in hydrochloric acid until no bubbles are generated, and completely immersing the filter cylinder in the hydrochloric acid to obtain the filter cylinder and hydrochloric acid treatment solution;
s3: washing the filter cylinder with 20-30mL of water, washing the filter cylinder with 10-20mL of methanol, adding the water and methanol which wash the filter cylinder into the hydrochloric acid treatment solution to obtain a first mixed solution, and drying the washed filter cylinder;
s4: detaching the smoke tube, pouring 40-60mL of water and 18-25mL of methanol into the smoke tube along the inner wall of one end of the smoke tube, flushing the inner wall surface of the smoke tube, collecting a second mixed solution after flushing, pouring the second mixed solution into a Buchner funnel paved with a glass fiber membrane for suction filtration to obtain a third mixed solution and the glass fiber membrane;
s5: drying the glass fiber membrane;
s6: extracting the third mixed solution by using 190-215mL of dichloromethane to obtain a first extraction solution;
s7: mixing the condensed water, the first mixed solution and the first extract liquid in the condenser to obtain a fourth mixed solution, adding dichloromethane into the fourth mixed solution, performing oscillation extraction to obtain a second extract liquid, and dehydrating the second extract liquid through anhydrous sodium sulfate; the volume ratio of the fourth mixed solution to the dichloromethane is 1: 0.08-0.15;
s8: carrying out Soxhlet extraction on the dried adsorbing material, the filter cylinder and the glass fiber membrane for 16-24h by taking toluene as a solvent to obtain an extracting solution;
s9: mixing the extracting solution and the second extracting solution, concentrating to 0.05-1mL, adding n-hexane to a constant volume of 10mL to obtain a sample solution;
s1, S2 and S4 may be performed simultaneously, S5 and S6 may be performed simultaneously, and S7 and S8 may be performed simultaneously;
the purification comprises multilayer silica gel purification and activated carbon silica gel column purification, and the multilayer silica gel purification comprises the following steps:
d1: transferring the sample solution to a multilayer silica gel column, rinsing the sample solution container with 1-2mL of n-hexane for 1-3 times, and transferring the rinsed solution to the multilayer silica gel column;
d2: leaching the multilayer silica gel column by using 90mL of normal hexane to obtain a leaching solution consisting of the normal hexane and the sample solution, and concentrating the leaching solution to 1-2 mL;
d3: repeating D1-D2 until the color of the multiple layers of silica gel columns is not penetrated, and obtaining first purified liquid;
the activated carbon purification comprises the following steps:
x1: adding 20-30mL of normal hexane into the activated carbon silica gel column, and transferring the first purifying liquid to the activated carbon silica gel column;
x2: adding 20-30mL of n-hexane solution into the activated carbon silica gel column, adding 38-42mL of mixed eluent, and discarding the eluent, wherein the mixed eluent comprises dichloromethane and n-hexane in a volume ratio of 1: 3;
x3: and adding 60-80mL of toluene into the activated carbon silica gel column for elution, and collecting the eluate to obtain a second purified solution.
By adopting the technical scheme, the adsorption material of the sampling gun is treated in S1, so that the water content of the adsorption material is reduced; and S2-S3, sequentially performing hydrochloric acid soaking and water washing on the filter cartridge, wherein the hydrochloric acid soaking decomposes some carbides and peracids, and finally drying the filter cartridge to finish the treatment of the filter cartridge. S4-S6 washing the inner wall surface of the sampling gun, dissolving the target substance adhered to the inner wall surface of the sampling gun, collecting to obtain a second mixed solution, performing suction filtration to obtain a third mixed solution, and transferring the target substance in the third mixed solution into the extraction liquid through extraction of dichloromethane. The filtration speed can be increased by suction filtration, and the pretreatment time is shortened.
In S7-S8, the first mixed solution and the first extract obtained in the above-mentioned treatment process are mixed with condensed water of a condenser in a sampling gun, extraction is performed, and the target substance is transferred to the second extract. Although the chlorodioxin is insoluble in water, a trace amount of the chlorodioxin is dissolved in condensed water, and on the other hand, some dust particles are adsorbed in the condensation process, and the surfaces of the dust particles are also adhered with the chlorodioxin.
Since the cartridge, the adsorbent, and the glass fiber membrane are washed with the solution, the target substance remains in each member, and therefore, in step S9, the cartridge, the adsorbent, and the glass fiber membrane are subjected to soxhlet extraction, and the target substance is gradually dissolved in toluene by long-term purification, thereby sufficiently extracting the target substance.
More preferably: the extraction in step S7 is repeated 2-3 times.
By adopting the technical scheme, the target substance is fully extracted by multiple times of extraction.
More preferably: in step S7, the volume ratio of the fourth mixed solution to dichloromethane is 1: 0.1.
By adopting the technical scheme, according to experiments, good extraction effect can be obtained when the mixing volume of the fourth mixed solution and the dichloromethane is 1: 0.1.
More preferably: the drying temperature of the adsorbing material, the filter cartridge and the glass fiber membrane is 50-60 ℃, and the drying time is 7-8.5 h.
By adopting the technical scheme, the step is mainly used for drying methanol and part of water, and ensuring that the adsorption material, the filter cylinder and the glass fiber membrane are fully dried.
More preferably: the multilayer silica gel column is a hand-packed column and sequentially comprises quartz cotton, anhydrous sodium sulfate, activated silica gel, 2% potassium hydroxide silica gel, activated silica gel, 44% sulfuric acid silica gel, 22% sulfuric acid silica gel, activated silica gel, 10% silver nitrate silica gel and an anhydrous sodium sulfate layer from bottom to top.
By adopting the technical scheme, firstly, the multi-layer silica gel column is a hand-packed column, an experimenter can pack about 25 columns in 30 minutes, and can buy a packed silica gel column to buy the column and the adsorbing material of 5 hand-packed columns, so that in summary, the time cost is not high, the cost is low, and the cost of the multi-layer silica gel column purification step can be greatly reduced. On the other hand, the layer structure can achieve the best effect in purification, meanwhile, the purification device is matched with a hand-packed column for use, and the using amount and the thickness of each layer of adsorption and filtering material can be adjusted at will according to the estimated concentration condition of a sample, so that the purification device is very convenient and fast.
More preferably: in the step X1, the first purifying liquid container is rinsed with 1-2mL of n-hexane for 1-3 times, and the container rinsing liquid is transferred to an activated carbon silica gel column together.
By adopting the technical scheme, the container residue is reduced, the sufficiency of sample extraction is ensured, the detection accuracy is favorably ensured, and the result is closer to the true value.
More preferably: in the step X3, the activated carbon silica gel column is reversed, and then toluene is added for elution to obtain a second purified liquid.
By adopting the technical scheme, the adsorption capacity of the activated carbon on dioxin substances is stronger, and the activated carbon can be easily eluted from the activated carbon by toluene. When the column is not reversed, 200mL of toluene is probably consumed for elution, and after the column is reversed, 60-80mL of toluene is only consumed for elution, so that the toluene consumption is reduced, and the elution time is also saved; the material in the first purifying liquid is adsorbed by forward on the active carbon, adsorbs the space and blocks up very easily to and the surface of the part that the active carbon silica gel is close to first purifying liquid feed end also can adsorb the dioxin, causes the situation that the forward upper end is covered and blocks up, if carry out forward elution, it is saturated and can not play fine elution effect to adsorb the space to block up, and reverse elution can be fine with active carbon silica gel surface and adsorbed dioxin elute.
More preferably: in the step X3, the leaching speed of the toluene is 2.2-2.6 mL/min.
By adopting the technical scheme, reasonable leaching time can balance elution sufficiency and detection time.
In conclusion, the invention has the following beneficial effects:
1. the filter cartridge, the adsorption material, the condensed water and the sampling gun which are involved in the whole sampling are all processed, so that the sufficiency of sample extraction is ensured, the detection accuracy is favorably ensured, and the result is closer to the true value.
2. Through adopting the column of filling out with the hand, can greatly reduced the cost of multilayer silica gel column purification step, can be simultaneously according to the concentration condition of estimating of sample, the quantity and the thickness of every layer of absorption and filtering material all can be adjusted wantonly, and is very convenient, improves purifying effect.
3. By adopting the reverse-rotation activated carbon silica gel column and adding toluene for elution, the toluene consumption is reduced, the elution time is saved, and the purification efficiency is improved.
Detailed Description
Examples 1 to 5: a method for detecting chlorodioxin comprises the steps of extraction, purification, nitrogen blowing concentration and on-machine detection which are sequentially carried out, wherein the specific steps and parameters of the method are shown in Table 1 in the following embodiments 1 to 5.
The extraction comprises the following steps:
s1: putting the adsorption material in the adsorption column of the sampling gun into an oven for drying;
s2: taking out the filter cylinder in the sampling gun, and completely immersing the filter cylinder in 2mol/L hydrochloric acid until no bubbles are generated to obtain the filter cylinder and hydrochloric acid treatment solution;
s3: washing the filter cylinder with water, washing the filter cylinder with methanol, adding water and methanol which are washed from the filter cylinder into hydrochloric acid treatment solution to obtain first mixed solution, and drying the washed filter cylinder in an oven;
s4: removing the smoke tube, pouring water and methanol into the smoke tube along the inner wall of one end of the smoke tube, washing the inner wall surface of the smoke tube, collecting a second mixed solution after washing, pouring the second mixed solution into a Buchner funnel paved with a glass fiber membrane for suction filtration, and obtaining a third mixed solution and the glass fiber membrane after the suction filtration is finished;
s5: putting the glass fiber membrane into an oven for drying;
s6: extracting the third mixed solution by using dichloromethane to obtain a first extract;
s7: mixing the condensed water, the first mixed solution and the first extract liquid in the condenser to obtain a fourth mixed solution, adding dichloromethane into the fourth mixed solution, performing oscillation extraction to obtain a second extract liquid, and dehydrating the second extract liquid through anhydrous sodium sulfate;
s8: carrying out Soxhlet extraction on the dried adsorbing material, the filter cylinder and the glass fiber membrane by taking toluene as a solvent to obtain an extracting solution;
s9: mixing the extracting solution with the second extracting solution, concentrating in a rotary evaporator, adding n-hexane after concentration to constant volume of 10mL to obtain a sample solution;
s1, S2 and S4 may be performed simultaneously, S5 and S6 may be performed simultaneously, and S7 and S8 may be performed simultaneously;
the purification comprises multilayer silica gel purification and activated carbon column purification, and the multilayer silica gel purification comprises the following steps:
d1: transferring the sample solution to a multilayer silica gel column, rinsing the sample solution container with n-hexane, and transferring the rinsed solution to the multilayer silica gel column;
d2: leaching the multilayer silica gel column by using 90mL of normal hexane to obtain a leaching solution consisting of the normal hexane and the sample solution, and concentrating the leaching solution in a rotary evaporator;
d3: repeating D1-D2 until the color of the multiple layers of silica gel columns is not penetrated, and obtaining first purified liquid;
the activated carbon purification comprises the following steps:
x1: adding normal hexane into the activated carbon column, and transferring the first purifying liquid to the activated carbon column;
x2: adding a normal hexane solution into the activated carbon column, adding a mixed eluent, and discarding a desorption solution, wherein the mixed eluent consists of dichloromethane and normal hexane;
x3: adding toluene into the activated carbon column at a certain speed for elution, and collecting the eluate to obtain a second purified solution;
and (3) nitrogen blowing concentration: concentrating the second purifying solution to 0.5mL in a rotary evaporator, transferring to a KD tube, rinsing the second purifying solution container with 2mL of n-hexane for 3 times, transferring the rinsing solution to the KD tube, concentrating to 0.5mL in the rotary evaporator again, drying with nitrogen to obtain nitrogen blowing solution, adding dioxin sample injection internal standard, performing constant volume to 20 mu L with nonane, performing ultrasonic treatment in an ultrasonic oscillator for 20min to obtain a solution to be detected, transferring the solution to be detected in the KD tube to an inner lining tube of a sample injection vial, and performing on-machine analysis.
In examples 1 to 5, the silica gel column was composed of, from bottom to top, quartz wool, 1cm thick anhydrous sodium sulfate, 0.9g of activated silica gel, 5g of 2% potassium hydroxide silica gel, 0.9g of activated silica gel, 10g of 44% sulfuric acid silica gel, 5g of 22% sulfuric acid silica gel, 0.9g of activated silica gel, 3g of 10% silver nitrate silica gel, and 2cm thick anhydrous sodium sulfate layer. The activated carbon silica gel column was filled with 0.5g of activated carbon silica gel.
The activated carbon silica gel column of example 1-2 was filled with 0.5g of activated carbon silica gel, and the activated carbon silica gel column of example 3-5 was filled with quartz wool, 0.5g of activated carbon silica gel, and quartz wool from top to bottom.
TABLE 1 EXAMPLES 1-5 Steps drug use amounts and parameters (kg)
Example 6: a chlorodioxin detection method differs from example 2 in that the number of extractions in step S7 is 3, the number of rinses in step D1 is 3, and the number of rinses in step X1 is 3.
Example 7: a chlorodioxin detection method is different from the method in example 6 in that an activated carbon silica gel column is filled with quartz cotton, 0.5g of activated carbon silica gel and quartz cotton from top to bottom.
Example 8: a method for detecting chlorodioxin, which is different from that of example 7, in that step X3 is performed by inverting the column of activated carbon silica gel and then eluting with toluene.
Comparative example 1: a chlorodioxin detection method differs from example 1 in that the fourth mixed liquid in step S7 does not contain condensed water and does not flush the inner wall of the sampling gun.
Comparative example 2: a chlorodioxin detection method differs from example 1 in that in the extraction step, S1 to S8 are replaced with: and directly carrying out Soxhlet extraction on the filter cartridge and the adsorbing material to obtain an extracting solution.
Comparative example 3: a chlorodioxin detection method differs from example 1 in that a multi-layer silica gel purification step was performed using a multi-layer silica gel purification column in CN 104749287A.
Characterization experiment:
recovery and precision experiments
(1) Recovery evaluation of examples and comparative examples
Subject: the same batch of sampling guns which are used for sampling in the same field are respectively used for completing the detection by adopting examples 1-8 and comparative examples 1-3.
The experimental method comprises the following steps: the amount of internal standard added was 1000pg (5. mu.L, 200ng/mL) to provide recovery and precision data for examples 1-8 and comparative examples 1-3.
The experimental results are as follows: the recovery and precision test records of the examples are shown in Table 2, and the recovery and precision test records of the comparative examples are shown in Table 3.
TABLE 2 record of recovery and precision of the examples
TABLE 3 comparative example recovery and precision test results
And (3) data analysis: the overall recovery of comparative example 3 is best in comparative examples 1-3, and worst in comparative example 2; the recovery rate of some substances in the comparative example could not reach 60%, and it did not have good accuracy and reproducibility. The multilayer silica gel purification column in comparative example 3 did not achieve the purification effect in the examples, so the overall recovery rate was low; comparative example 1, in which the treatment of condensed water and the inner wall of the sampling gun was omitted, was inferior to comparative example 3, and comparative example 2, in which the part was directly subjected to soxhlet extraction, had a large content of impurities and many interfering substances, resulting in a low recovery rate.
(2) Recovery evaluation of single-example multiple parallel experiments
Subject: the same batch of sampling guns which are used for sampling in the same field are respectively adopted to finish the detection in embodiment 8.
The experimental method comprises the following steps: the amount of internal standard added was 1000pg (5. mu.L, 200ng/mL) to obtain the recovery and precision data of example 8.
The experimental results are as follows: the recovery and precision test records of example 5 are shown in Table 4.
TABLE 4 record of recovery and precision of the examples
And (3) data analysis: in the embodiment 8, RSD of a plurality of parallel experiments is not more than 15 percent, the precision requirement is met, the recovery rate range is 60-120 percent, the precision requirement is met, and the method has good accuracy and repeatability and can be used for detecting dioxin.
The above-mentioned embodiments are merely illustrative and not restrictive, and those skilled in the art can modify the embodiments without inventive contribution as required after reading this specification, but only fall within the scope of the claims of the present invention.
Claims (8)
1. The method for detecting the chlorinated dioxin is characterized by comprising the following steps of extraction, purification, nitrogen blowing concentration and on-machine detection in sequence, wherein the extraction comprises the following steps:
s1: drying the adsorption material in the adsorption column of the sampling gun;
s2: taking out the filter cylinder in the sampling gun, soaking the filter cylinder in hydrochloric acid until no bubbles are generated, and completely immersing the filter cylinder in the hydrochloric acid to obtain the filter cylinder and hydrochloric acid treatment solution;
s3: washing the filter cylinder with 20-30mL of water, washing the filter cylinder with 10-20mL of methanol, adding the water and methanol which wash the filter cylinder into the hydrochloric acid treatment solution to obtain a first mixed solution, and drying the washed filter cylinder;
s4: detaching the smoke tube, pouring 40-60mL of water and 18-25mL of methanol into the smoke tube along the inner wall of one end of the smoke tube, flushing the inner wall surface of the smoke tube, collecting a second mixed solution after flushing, pouring the second mixed solution into a Buchner funnel paved with a glass fiber membrane for suction filtration to obtain a third mixed solution and the glass fiber membrane;
s5: drying the glass fiber membrane;
s6: extracting the third mixed solution by using 190-215mL of dichloromethane to obtain a first extraction solution;
s7: mixing the condensed water, the first mixed solution and the first extract liquid in the condenser to obtain a fourth mixed solution, adding dichloromethane into the fourth mixed solution, performing oscillation extraction to obtain a second extract liquid, and dehydrating the second extract liquid through anhydrous sodium sulfate; the volume ratio of the fourth mixed solution to the dichloromethane is 1: 0.08-0.15;
s8: carrying out Soxhlet extraction on the dried adsorbing material, the filter cylinder and the glass fiber membrane for 16-24h by taking toluene as a solvent to obtain an extracting solution;
s9: mixing the extracting solution and the second extracting solution, concentrating to 0.05-1mL, adding n-hexane to a constant volume of 10mL to obtain a sample solution;
s1, S2 and S4 may be performed simultaneously, S5 and S6 may be performed simultaneously, and S7 and S8 may be performed simultaneously;
the purification comprises multilayer silica gel purification and activated carbon silica gel column purification, and the multilayer silica gel purification comprises the following steps:
d1: transferring the sample solution to a multilayer silica gel column, rinsing the sample solution container with 1-2mL of n-hexane for 1-3 times, and transferring the rinsed solution to the multilayer silica gel column;
d2: leaching the multilayer silica gel column by using 90mL of normal hexane to obtain a leaching solution consisting of the normal hexane and the sample solution, and concentrating the leaching solution to 1-2 mL;
d3: repeating D1-D2 until the color of the multiple layers of silica gel columns is not penetrated, and obtaining first purified liquid;
the activated carbon purification comprises the following steps:
x1: adding 20-30mL of normal hexane into the activated carbon silica gel column, and transferring the first purifying liquid to the activated carbon silica gel column;
x2: adding 20-30mL of n-hexane solution into the activated carbon silica gel column, adding 38-42mL of mixed eluent, and discarding the eluent, wherein the mixed eluent comprises dichloromethane and n-hexane in a volume ratio of 1: 3;
x3: and adding 60-80mL of toluene into the activated carbon silica gel column for elution, and collecting the eluate to obtain a second purified solution.
2. The method of detecting chlorodioxin in the form of chlorine in claim 1, wherein the extraction in step S7 is repeated 2 to 3 times.
3. The method for detecting chlorodioxin according to claim 1, wherein the volume ratio of the fourth mixed solution to dichloromethane in step S7 is 1: 0.1.
4. The method for detecting chlorodioxin according to claim 1, characterized in that the drying temperature of the adsorbing material, the filter cartridge and the glass fiber membrane is 50 to 60 ℃ and the drying time is 7 to 8.5 hours.
5. The method for detecting chlorodioxin according to claim 1, wherein the multi-layer silica gel column is a hand-packed column and is composed of layers of quartz wool, anhydrous sodium sulfate, activated silica gel, 2% potassium hydroxide silica gel, activated silica gel, 44% silica gel sulfate, 22% silica gel sulfate, activated silica gel, 10% silver nitrate silica gel and anhydrous sodium sulfate from bottom to top in sequence.
6. The method for detecting chlorodioxin according to claim 1, wherein in the step X1, the first purifying solution container is rinsed 1 to 3 times with 1 to 2mL of n-hexane, and the container rinsing solution is transferred to an activated carbon silica gel column together.
7. The method for detecting chlorodioxin according to claim 6, wherein in the step X3, the column of activated carbon silica gel is reversed, and toluene is added for elution to obtain a second purified liquid.
8. The method for detecting chlorodioxin in the chemical mechanical polishing technique of claim 7, wherein the elution rate of toluene in step X3 is 2.2 to 2.6 mL/min.
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