CN109781490A - A kind of pre-treating method that Organochlorine Pesticides In Soil extracts - Google Patents
A kind of pre-treating method that Organochlorine Pesticides In Soil extracts Download PDFInfo
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- CN109781490A CN109781490A CN201910204382.2A CN201910204382A CN109781490A CN 109781490 A CN109781490 A CN 109781490A CN 201910204382 A CN201910204382 A CN 201910204382A CN 109781490 A CN109781490 A CN 109781490A
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Abstract
The invention discloses the pre-treating methods that a kind of Organochlorine Pesticides In Soil extracts, it is related in environmental testing the pre-treating method field of the measurement of organo-chlorine pesticide in soils and sediments, it is not high to solve treatment effeciency in the prior art, it needs in advance to handle soil, complex steps, problem not easy enough.Include the following steps: step 1: weighing soil in 250mL indigo plant lid bottle；Step 2: appropriate anhydrous sodium sulfate dehydration is added, adds 100mL soil extract agent；Step 3: the ultrasound 5min in ultrasonoscope；Step 4: 2h is shaken on 28 bit flipping vibrating machines；Step 5: K-D device is built；Step 6: filtering；Step 7: it is concentrated using K-D device；Step 8: it is settled to 1mL；Step 9: if being detected with ECD, solvent switch is n-hexane (or similar nonpolar solvent)；Step 10: concentrating instrument progress nitrogen is blown using 12 nitrogen and blows concentration；Step 11: being settled to 1mL, is transferred into 2mL sample injection bottle with disposable pasteur pipet.
Description
Technical field
The present invention relates to the pre-treating method of the measurement of organo-chlorine pesticide in soils and sediments in environmental testing necks
Domain, the pre-treating method that specially a kind of Organochlorine Pesticides In Soil extracts.
Background technique
The pre-treating method that organo-chlorine pesticide extracts in existing soils and sediments is predominantly following several: Soxhlet extraction
Method, microwave extraction method and acceleration fluids extraction, wherein Soxhlet extraction is cumbersome, takes a long time, and working efficiency is low, organic
Solvent usage is larger, nitrogen blow concentration gas consumption it is larger, thickening efficiency is lower, and rotary evaporation can only handle a sample, nothing every time
Method is carried out at batch, and there are the possibility of cross contamination；There is still a need for further centrifuge separations after extraction for microwave extraction method
Organic phase, thus the influence of human error is increased, instrument cost is higher, and higher to operator's operation level requirement, nitrogen blows dense
Contracting gas consumption is larger, and thickening efficiency is lower, and rotary evaporation can only handle a sample every time, can not carry out at batch, and exists
The possibility of cross contamination；Accelerate fluids extraction instrument cost higher, the sample of high concentration easily causes pipeline to pollute, to operator
It is higher to operate level requirement, misoperation will cause pipeline blockage, and nitrogen blows that concentration gas consumption is larger, and thickening efficiency is lower；Rotation
Evaporation can only handle a sample every time, can not carry out at batch, and there are the possibility of cross contamination.
Existing pre-treating method needs in advance to handle soil, method and step for the inefficient of processing
It is cumbersome, it is not easy enough；Therefore market in urgent need develops a kind of pre-treating method of Organochlorine Pesticides In Soil extraction to help people
It solves the problems, such as existing.
Summary of the invention
The purpose of the present invention is to provide the pre-treating methods that a kind of Organochlorine Pesticides In Soil extracts, to solve above-mentioned back
The treatment effeciency proposed in scape technology is not high, and needs in advance to handle soil, and method and step is cumbersome, and not easy enough asks
Topic.
To achieve the above object, the invention provides the following technical scheme: the preceding place that a kind of Organochlorine Pesticides In Soil extracts
Reason method, includes the following steps:
Step 1: soil is weighed in 250mL indigo plant lid bottle；
Step 2: appropriate anhydrous sodium sulfate dehydration is added, adds 100mL soil extract agent；
Step 3: the ultrasound 5min in ultrasonoscope；
Step 4: 2h is shaken on 28 bit flipping vibrating machines；
Step 5: K-D device is built；
Step 6: filtering；
Step 7: it is concentrated using K-D device；
Step 8: it is settled to 1mL；
Step 9: if being detected with ECD, solvent switch is n-hexane (or similar nonpolar solvent)；
Step 10: concentrating instrument progress nitrogen is blown using 12 nitrogen and blows concentration；
Step 11: being settled to 1mL, is transferred into 2mL sample injection bottle with disposable pasteur pipet.
Preferably, in the step 1, it is furnished with PTFE gasket in the bottle cap of 250mL indigo plant lid bottle.
Preferably, in the step 2, anhydrous sodium sulfate can adsorbable organic impurities through 400 DEG C of removals in calcination 4 hours
Solvent rinse is cooled down or uses afterwards, soil extract agent is acetone-methylene chloride extractant, and (gas-chromatography grade is higher by acetone
Rank) and methylene chloride (gas-chromatography grade or higher level) the ratio mixing of 1:1 or acetone-n-hexane extract by volume
Agent, by the ratio of acetone (gas-chromatography grade or higher level) and n-hexane (gas-chromatography grade or higher level) 1:1 by volume
Example mixing.
Preferably, in the step 4, vibrating machine revolving speed 30r/min ± 2r/min is overturn.
Preferably, in the step 5, K-D device reception pipe containing 10mL, 500mL liquid feeding flask, three ball Schneider columns and
Two ball Schneider columns, K-D device is using preceding needing with n-hexane rinse one time, when using acetone-methylene chloride soil extract agent,
With methylene chloride rinse, used after discarding waste liquid.
Preferably, in the step 6, a small amount of anhydrous sodium sulfate is added in glass fiber filter, liquid level is high in toppling process
Degree is no more than glass fiber filter height.
Preferably, in the step 8, three balls concentration on 5-8 carbonization silicone zeolite framves will first be added when concentration in sample
Column is concentrated in thermostat water bath, 85 DEG C of bath temperature, takes out when sample concentration is to 6-8mL, after being cooled to room temperature, dismantle plus
Liquid flask and three ball evaporating columns, change two ball evaporating columns, continue to be concentrated into 0.6-0.8mL or so.
Preferably, in the step 10, before nitrogen blows concentration, a certain amount of sample concentration liquid is taken, 10-20 times is added and measures just
Hexane (or similar nonpolar solvent).
Preferably, in the step 11,2mL sample injection bottle is furnished with the lid of PTFE dottle pin.
Compared with prior art, the beneficial effects of the present invention are:
1, the invention can carry out pre-treatment to batch soil sample simultaneously, be compared to microwave extraction method and accelerate fluids extraction, rotation
Turn the case where evaporation can only handle a sample every time, can not carry out at batch, treatment effeciency greatly improves；
2, the invention can batch processed sample, it is time-consuming shorter, it is easy to operate, it is relatively low to operator's level requirement, be easy to push away
Extensively；
3, the invention is without the use of expensive instrument, and low in cost, saving nitrogen does not easily cause cross contamination；
4, the dispersibility and uniformity of soil are preferable after invention ultrasound, do not have to grinding soil in advance, cause to the quality of soil
Loss, and preparation is few before processing, requires soil property lower；
5, the invention extraction step is completed in relatively closed space, and favorable reproducibility, the rate of recovery is up to 80% or more.
Detailed description of the invention
Fig. 1 is the work flow diagram for the pre-treating method that a kind of Organochlorine Pesticides In Soil of the invention extracts.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.
Referring to Fig. 1, a kind of embodiment provided by the invention: a kind of pre-treatment side that Organochlorine Pesticides In Soil extracts
Method includes the following steps:
Step 1: soil is weighed in 250mL indigo plant lid bottle；
Step 2: appropriate anhydrous sodium sulfate dehydration is added, adds 100mL soil extract agent；
Step 3: the ultrasound 5min in ultrasonoscope disperses the soil to agglomerate by water content height, and it is right in advance not need
Soil is ground, and the soil of any soil property can be handled；
Step 4: shaking 2h on 28 bit flipping vibrating machines, and shaking is uniform；
Step 5: building K-D device, if soil extract agent be acetone-n-hexane extractant, K-D device using preceding need use just oneself
It alkane rinse one time, when using acetone-methylene chloride soil extract agent, with methylene chloride rinse, is used after discarding waste liquid；
Step 6: filtering twice by glass fiber filter doubling, is put into glass funnel, by glass fiber filter in triangular shape
The inner surface of expansion fitting glass funnel；
Step 7: it is concentrated using K-D device；
Step 8: being settled to 1mL, is transferred into 2mL sample injection bottle with disposable pasteur pipet, 2mL sample injection bottle equipped with PTFE every
The lid of pad；
Step 9: if being detected with ECD, solvent switch is n-hexane (or similar nonpolar solvent)；
Step 10: concentrating instrument progress nitrogen is blown using 12 nitrogen and blows concentration；
Step 11: being settled to 1mL, is transferred into 2mL sample injection bottle with disposable pasteur pipet.
Further, in step 1, it is furnished with PTFE gasket in the bottle cap of 250mL indigo plant lid bottle.
Further, in step 2, anhydrous sodium sulfate through 400 DEG C of removals in calcination 4 hours can after adsorbable organic impurities it is cold
But or solvent rinse is used, soil extract agent is acetone-methylene chloride extractant, by acetone (gas-chromatography grade or higher level)
With methylene chloride (gas-chromatography grade or higher level) by volume 1:1 ratio mixing or acetone-n-hexane extractant, will
The ratio of acetone (gas-chromatography grade or higher level) and n-hexane (gas-chromatography grade or higher level) 1:1 by volume are mixed
It closes.
Further, in step 4, vibrating machine revolving speed 30r/min ± 2r/min is overturn.
Further, in step 5, K-D device reception pipe containing 10mL, 500mL liquid feeding flask, three ball Schneider columns and two balls
Schneider column, K-D device is using preceding needing to use n-hexane rinse one time, when using acetone-methylene chloride soil extract agent, with two
Chloromethanes rinse uses after discarding waste liquid.
Further, a small amount of anhydrous sodium sulfate is added in step 6, in glass fiber filter, anhydrous sodium sulfate burns through 400 DEG C
Solvent rinse can be cooled down or use after adsorbable organic impurities by burning removal in 4 hours, and liquid level is no more than glass in toppling process
Glass fibrous filter membrane height, avoids non-filter material from therefrom filtering out.
Further, in step 8, three ball evaporating columns on 5-8 carbonization silicone zeolite framves will first be added when concentration in sample, in
It is concentrated in thermostat water bath, 85 DEG C of bath temperature, is taken out when sample concentration is to 6-8mL, after being cooled to room temperature, liquid feeding flask of dismantling
With three ball evaporating columns, two ball evaporating columns are changed, continue to be concentrated into 0.6-0.8mL or so.
Further, in step 10, before nitrogen blows concentration, a certain amount of sample concentration liquid is taken, the 10-20 times of n-hexane measured is added
(or similar nonpolar solvent).
Further, in step 11,2mL sample injection bottle is furnished with the lid of PTFE dottle pin.
The measurement of six six six and DDT in bed mud (deposit), carries out pre-treatment with this method, can once handle simultaneously
28 samples.Since Water Content Tests in Soil Samples is higher, part soil sample can make after soil extract agent this method ultrasound is added at a shape
Soil sample particle relative distribution filters, the constant volume after K-D is concentrated, upper machine testing after two hours are vibrated in overturning.Use ECD
Detection, the rate of recovery of blank mark-on are able to reach 85%-105%, meet the requirement of standard HJ921-2017.It is examined with GCMS
When survey, the rate of recovery of blank mark-on and actual sample mark-on is 91%-111% and 82%-102%, meets standard HJ835-2017
Requirement.
Working principle: weighing a certain amount of soil sample in 250mL indigo plant lid bottle, and soil sample will stir evenly before claiming sample, then plus
Enter appropriate anhydrous sodium sulfate dehydration, 100mL soil extract agent is added with bottleneck pipettor, covers bottle cap, soil will be filled and mentioned
The blue lid bottle of agent is taken to be placed in ultrasonoscope, ultrasonic 5min disperses the soil of agglomeration youngster as far as possible, is then put in overturning vibrating machine
Upper shaking 2 hours, revolving speed 30r/min ± 2r/min, puts up the reception pipe and liquid feeding flask in K-D device, in glass funnel
In be put into the glass fiber filter rolled well, a small amount of anhydrous sodium sulfate is added in filter membrane for being dehydrated, a whole set of filter device is with just
It is stand-by that waste liquid is discarded after hexane (when using acetone-methylene chloride extractant, with methylene chloride rinse) rinse one time, by soil sample
Extracting solution slowly pours into glass funnel, and liquid level does not exceed filter membrane height during this, with 30mL n-hexane rinse
Blue lid bottle 3 times of soil sample are filled, rinse liquid is merged into K-D device, and 5 ~ 8 carbonization silicone zeolites are added after the completion of filtering in sample
Three ball evaporating columns, is concentrated in water-bath on frame, 85 DEG C of bath temperature, takes out, is cooled to room temperature when sample concentration is to 6 ~ 8mL
Afterwards, it dismantles liquid feeding flask and three ball evaporating columns, changes two ball evaporating columns, continue to be concentrated into 0.6 ~ 0.8mL or so, but can not be concentrated
To dry, final sample is settled to 1.0mL, be transferred to disposable pasteur pipet it is to be measured in 2mL sample introduction product, when using acetone-
It should be n-hexane (or similar non-pole by solvent switch if sample needs to be tested with ECD detector when methylene chloride extractant
Property solvent), take a certain amount of sample concentration liquid, the n-hexanes (or similar nonpolar solvent) of 10 ~ 20 times of amounts be added, using nitrogen
It blows concentration and is settled to 1mL.
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie
In the case where without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power
Benefit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent elements of the claims
Variation is included within the present invention.Any reference signs in the claims should not be construed as limiting the involved claims.
Claims (9)
1. the pre-treating method that a kind of Organochlorine Pesticides In Soil extracts, which comprises the steps of:
Step 1: soil is weighed in 250mL indigo plant lid bottle；
Step 2: appropriate anhydrous sodium sulfate dehydration is added, adds 100mL soil extract agent；
Step 3: the ultrasound 5min in ultrasonoscope；
Step 4: 2h is shaken on 28 bit flipping vibrating machines；
Step 5: K-D device is built；
Step 6: filtering；
Step 7: it is concentrated using K-D device；
Step 8: it is settled to 1mL；
Step 9: if being detected with ECD, solvent switch is n-hexane (or similar nonpolar solvent)；
Step 10: concentrating instrument progress nitrogen is blown using 12 nitrogen and blows concentration；
Step 11: being settled to 1mL, is transferred into 2mL sample injection bottle with disposable pasteur pipet.
2. the pre-treating method that a kind of Organochlorine Pesticides In Soil according to claim 1 extracts, it is characterised in that: described
In step 1, it is furnished with PTFE gasket in the bottle cap of 250mL indigo plant lid bottle.
3. the pre-treating method that a kind of Organochlorine Pesticides In Soil according to claim 1 extracts, it is characterised in that: described
In step 2, anhydrous sodium sulfate can be cooled down or be moistened using solvent after adsorbable organic impurities through 400 DEG C of removals in calcination 4 hours
It washes, soil extract agent is acetone-methylene chloride extractant, by acetone (gas-chromatography grade or higher level) and methylene chloride (gas
Phase chromatographic grade or higher level) by volume 1:1 ratio mixing or acetone-n-hexane extractant, by acetone (gas-chromatography
Grade or higher level) and n-hexane (gas-chromatography grade or higher level) by volume 1:1 ratio mix.
4. the pre-treating method that a kind of Organochlorine Pesticides In Soil according to claim 1 extracts, it is characterised in that: described
In step 4, vibrating machine revolving speed 30r/min ± 2r/min is overturn.
5. the pre-treating method that a kind of Organochlorine Pesticides In Soil according to claim 1 extracts, it is characterised in that: described
In step 5, K-D device reception pipe containing 10mL, 500mL liquid feeding flask, three ball Schneider columns and two ball Schneider columns, K-D device
It needs when using acetone-methylene chloride soil extract agent, with methylene chloride rinse, to be discarded with n-hexane rinse one time before use
It is used after waste liquid.
6. the pre-treating method that a kind of Organochlorine Pesticides In Soil according to claim 1 extracts, it is characterised in that: described
A small amount of anhydrous sodium sulfate is added in step 6, in glass fiber filter, liquid level is filtered no more than glass fibre in toppling process
Film height.
7. the pre-treating method that a kind of Organochlorine Pesticides In Soil according to claim 1 extracts, it is characterised in that: described
In step 8,5-8 carbonization silicone zeolites will first be added when concentration in sample, three ball evaporating columns on frame are dense in thermostat water bath
Contracting, is taken out when sample concentration is to 6-8mL by 85 DEG C of bath temperature, after being cooled to room temperature, dismantle liquid feeding flask and three ball evaporating columns,
Two ball evaporating columns are changed, continue to be concentrated into 0.6-0.8mL or so.
8. the pre-treating method that a kind of Organochlorine Pesticides In Soil according to claim 1 extracts, it is characterised in that: described
In step 10, before nitrogen blows concentration, a certain amount of sample concentration liquid is taken, the 10-20 times of n-hexane measured (or similar nonpolarity is added
Solvent).
9. the pre-treating method that a kind of Organochlorine Pesticides In Soil according to claim 1 extracts, it is characterised in that: described
In step 11,2mL sample injection bottle is furnished with the lid of PTFE dottle pin.
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| CN110865135A (en) * | 2019-10-30 | 2020-03-06 | 河南大学 | Method for measuring capacity of micro plastic for adsorbing soil organic chlorine pesticide |
| CN111257076A (en) * | 2020-02-24 | 2020-06-09 | 重庆中科检测技术服务有限公司 | Pretreatment method for extracting organochlorine pesticide in soil |
| CN112946141A (en) * | 2021-03-15 | 2021-06-11 | 上海国齐检测技术有限公司 | Method for detecting phosmet in soil |
| CN115979772A (en) * | 2022-12-16 | 2023-04-18 | 珠海汇华环境有限公司 | Pressurized fluid extraction device capable of being pretreated in soil and detection method |
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Application publication date: 20190521 |