CN108845053A - The method of six six six and DDT in ultrasonic extraction-Soil by Gas Chromatography - Google Patents
The method of six six six and DDT in ultrasonic extraction-Soil by Gas Chromatography Download PDFInfo
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- 239000002689 soil Substances 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000004817 gas chromatography Methods 0.000 title claims abstract description 12
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims abstract description 46
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000002035 hexane extract Substances 0.000 claims abstract description 18
- 239000000523 sample Substances 0.000 claims abstract description 16
- 239000012488 sample solution Substances 0.000 claims abstract description 9
- WBZKQQHYRPRKNJ-UHFFFAOYSA-L disulfite Chemical compound [O-]S(=O)S([O-])(=O)=O WBZKQQHYRPRKNJ-UHFFFAOYSA-L 0.000 claims abstract description 8
- 238000011010 flushing procedure Methods 0.000 claims abstract description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 16
- 238000013517 stratification Methods 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 8
- 238000000605 extraction Methods 0.000 claims description 7
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 6
- 239000011521 glass Substances 0.000 claims description 5
- 238000009835 boiling Methods 0.000 claims description 3
- 210000003298 dental enamel Anatomy 0.000 claims description 3
- 239000012153 distilled water Substances 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 3
- 239000012528 membrane Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- 230000018044 dehydration Effects 0.000 claims 1
- 238000006297 dehydration reaction Methods 0.000 claims 1
- 238000002137 ultrasound extraction Methods 0.000 abstract description 13
- 238000002203 pretreatment Methods 0.000 abstract description 8
- 239000000284 extract Substances 0.000 abstract description 7
- 238000001914 filtration Methods 0.000 abstract description 4
- 238000012545 processing Methods 0.000 abstract description 3
- 230000010355 oscillation Effects 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 28
- 238000011084 recovery Methods 0.000 description 11
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 10
- 239000003208 petroleum Substances 0.000 description 8
- 238000001514 detection method Methods 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 239000007789 gas Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000012086 standard solution Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000004677 Nylon Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- HWJHWSBFPPPIPD-UHFFFAOYSA-N ethoxyethane;propan-2-one Chemical compound CC(C)=O.CCOCC HWJHWSBFPPPIPD-UHFFFAOYSA-N 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 229920001778 nylon Polymers 0.000 description 2
- 238000011017 operating method Methods 0.000 description 2
- 239000003993 organochlorine pesticide Substances 0.000 description 2
- 239000000575 pesticide Substances 0.000 description 2
- 239000000447 pesticide residue Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 238000010561 standard procedure Methods 0.000 description 2
- 206010016825 Flushing Diseases 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 238000000944 Soxhlet extraction Methods 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- JLYXXMFPNIAWKQ-SHFUYGGZSA-N alpha-hexachlorocyclohexane Chemical compound Cl[C@H]1[C@H](Cl)[C@@H](Cl)[C@H](Cl)[C@H](Cl)[C@H]1Cl JLYXXMFPNIAWKQ-SHFUYGGZSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000005264 electron capture Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000012259 ether extract Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229940088597 hormone Drugs 0.000 description 1
- 239000005556 hormone Substances 0.000 description 1
- 238000007327 hydrogenolysis reaction Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000006210 lotion Substances 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/14—Preparation by elimination of some components
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/50—Conditioning of the sorbent material or stationary liquid
- G01N30/52—Physical parameters
- G01N30/54—Temperature
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/025—Gas chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Extraction Or Liquid Replacement (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses a kind of methods of six six six and DDT in ultrasonic extraction-Soil by Gas Chromatography, include the following steps：The pedotheque being prepared is weighed to be placed in a beaker, the mixed liquor of acetone and n-hexane is added, is put into ultrasonic machine and extracts, extracting solution is added in separatory funnel after filtering, and beaker, soil sample and filter device are rinsed, flushing liquor, which merges, to be added in separatory funnel, and metabisulfite solution is added, stands after oscillation, discard aqueous acetone solution, hexane extract is left, then hexane extract is purified and is concentrated to get sample solution to be measured is arrived；The concentration of six six six and DDT in gained sample solution to be measured is detected with gas chromatograph.This method extracts six six six, DDT in pedotheque using ultrasonic extraction, substantially reduces the pre-treatment time, is suitable for quick, relatively accurate processing high-volume pedotheque.
Description
Technical field
The present invention relates to analysis of agricultural drugs technical fields, it particularly relates in a kind of soil six six six and DDT inspection
Survey method.
Background technique
Organo-chlorine pesticide is first generation pesticide, is a kind of synthetic environment hormone to constitute a serious threat to environment,
Middle six six six, DDT are using earliest, most widely used pesticide, and environmental pollution is also the most serious.Though six six six, DDT
It is so disabled, but since its property is stablized, residual quantity is high in the environment such as soil, water body, organism, atmosphere, it is difficult to drop
Solution, so being still widely present in the environment.According to existing data logging, the hydrogenolysis half of the main isomer α-HCH in six six six
Decline the phase be 26 years, hydrolysising half-life be 64 years, and it be in all isomers of six six six it is most unstable, degradation rate is most fast
It is a kind of.In addition, DDT degrades 95% then need 30 years in the natural environment.It can be seen that there is no the case where human intervention
Under, these pesticide residues of degrading only are gone by the strength of the Nature, the time for needing to pay is incomparable very long.The country is to soil
In six six six, DDT pesticide residue research it is fewer, each laboratory also stops the detection of six six six, DDT in soil
On using national standard method, such as the gas-chromatography of GB/T 14550-2003 soil quality six six six and DDT measurement
Method.Although national standard method is classical, measurement is accurate, pre-treatment soil needs to impregnate, Soxhlet extraction is 16 hours time-consuming, adds
Other pre-treatments, machine substantially needs 24 hours in detection, too time-consuming, unsuitable mass disposal soil sample.
Summary of the invention
For above-mentioned technical problem in the related technology, the present invention proposes a kind of ultrasonic extraction-gas chromatography measurement soil
The method of six six six and DDT in earth can overcome the above-mentioned deficiency of the prior art.
To realize the above-mentioned technical purpose, the technical proposal of the invention is realized in this way：
The method of six six six and DDT, includes the following steps in a kind of ultrasonic extraction-Soil by Gas Chromatography：
(1) room is handled before soil soil is poured on enamel pallet, crushed with hammer, stick, pick impurity and use quartering
Sample after dividing pressure broken, crosses 60 mesh nylon mesh, pedotheque is made；It weighs 10g pedotheque to be placed in a beaker, 2mL is added
Distilled water mixes well, and the mixed mark solution of 20 μ L is added as mark-on, shelves several minutes, and mixing for 100mL acetone and n-hexane is added
Liquid is closed, the beaker sealed membrane sealing of mixed liquor and soil equipped with acetone and n-hexane is prevented from volatilizing, is put into ultrasonic machine
It extracts 10-30 minutes, is separated sample and extracting solution with full glass sand core filter device after extraction, liquid separation leakage is added in extracting solution
In bucket, and 2-3 flushing, flushing liquor are carried out to beaker, soil sample and filter device with the mixed liquor of 10-15mL acetone and n-hexane
Merge in addition separatory funnel, addition 100mL metabisulfite solution, oscillation 1min, after stratification, it is water-soluble to discard lower layer's acetone
Liquid leaves hexane extract, and 1/10th concentrated sulfuric acid of hexane extract volume, shaking are added in separatory funnel
1min after stratification, discards sulfuric acid layer, is repeated several times according to above-mentioned steps, until two phase boundary of hexane extract being added
Stop when clear uniformly transparent in face；Then the sodium sulphate of its volume half is added into the hexane extract for discard sulfuric acid layer
Solution；Shaking 10-20 times, water layer is discarded after its stratification, is stopped when so repeating to hexane extract into neutrality, just oneself
Alkane extracting solution is dehydrated through the cartridge type funnel equipped with a small amount of anhydrous sodium sulfate again, is filtered in boiling flask, is concentrated with rotary evaporator
To 1mL to get arrive sample solution to be measured；
(2) with the concentration of six six six and DDT in gas chromatograph detecting step (1) gained sample solution to be measured：
Injector temperature：220℃；
Column temperature：It 150 DEG C of initial temperature, is kept for 2 minutes, is then raised to 270 DEG C with the speed of 6 DEG C/min and is kept for 25 points
Clock；
Detector temperature：300℃；
Flow：1.4mL/min.
Further, ultrasonic machine is put into equipped with acetone and the mixed liquor of n-hexane and the beaker of soil described in step (1)
The time of middle extraction is 20min.
Further, α-six six six in step (1) the mixed mark solution, β-six six six, γ-six six six, δ-six six six,
The concentration of p.p'-DDE, p.p'-DDD are that the concentration of 4 μ g/mL, o.p'-DDT, p.p'-DDT is 32 μ g/mL.
Further, acetone and n-hexane volume ratio are 1 in the mixed liquor of step (1) acetone and n-hexane:1.
Further, the concentration of metabisulfite solution described in step (1) is 20g/L.
Beneficial effects of the present invention：Six six six and DDT in ultrasonic extraction-Soil by Gas Chromatography of the invention
Method improve soil pre-treatment extracting method, using ultrasonic extraction extract pedotheque in six six six, DDT
Organo-chlorine pesticide extracts reagent and filtering cleaning method, to greatly shorten pre-treatment by the optimum experimental optimum extraction time
Time improves recovery of standard addition, is adapted to quick, relatively accurate processing high-volume pedotheque.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
Technical staff's every other embodiment obtained, shall fall within the protection scope of the present invention.
The instrument and device of use
Good fortune is stood GC9720 gas chromatograph (Ni electron capture detector), the residual dedicated elas-tic quartz capillary B column (30m* of KB agriculture
0.25mm*0.25 μm), KQ-50DE type numerical control supersonic instrument (Kunshan Ultrasonic Instruments Co., Ltd.), MTN-5800 nitrogen evaporator
(Tianjin Ao Tesaiensi Instrument Ltd.), RE-52AA rotary evaporator (Shanghai Yarong Biochemical Instrument Plant), full glass Soxhlet
Extractor, water-bath, full glass sand core filter device, 500ml separatory funnel.
The reagent and standard liquid of use, mixed mark solution
N-hexane, acetone (chromatographically pure)；
The concentrated sulfuric acid (excellent pure grade)；
Anhydrous sodium sulfate (excellent pure grade)：It is dried 4 hours at 450 DEG C；
Single standard solution：Concentration be α-six six six of 100 μ g/mL, β-six six six, γ-six six six, δ-six six six,
P.p'-DDE, o.p'-DDT, p.p'-DDD, p.p'-DDT standard solution (purchase detects institute from Ministry of Agriculture's environmental protection scientific research)；
Mixed mark solution：Using n-hexane as solvent, with α-six six six, β-six six six, γ-six six six, δ-six six six,
P.p'-DDE, o.p'-DDT, p.p'-DDD, p.p'-DDT standard solution prepare mixed mark solution, mix α-six six six, β-in mark solution
Six six six, γ-six six six, δ-six six six, p.p'-DDE, p.p'-DDD concentration be 4 μ g/mL, o.p'-DDT, p.p'-DDT
Concentration be 32 μ g/mL.
Comparative example
Precise 20.0g soil is placed in small beaker, adds distilled water 2mL, diatomite 4g, and the mixed mark solution of 40 μ L is added and makees
It for mark-on, mixes well, nondestructively moves into filtration paper cylinder, filtration paper cylinder is fitted into Soxhlet extractor by a piece of filter paper of upper cap, is used
30mL petroleum ether-acetone mixture (volume ratio 1:1) after impregnating soil sample 12 hours, add 100mL petroleum ether-acetone mixture
(volume ratio 1:1), the heating extraction 4h on 75-95 DEG C of thermostat water bath, reflux 4 times -6 times every time, after cooling, by extracting solution
It moves into separatory funnel, rinses extractor and flask in three times with 10mL petroleum ether, washing lotion is incorporated in separatory funnel, be added
100mL metabisulfite solution (concentration 20g/L) vibrates 1min, after stratification, discards lower layer's aqueous acetone solution, leaves petroleum
Ether extracting solution purifies petroleum ether extract, is concentrated according to purification method in national standard GB/T14550-2003, upper machine is surveyed
It is fixed.
Embodiment 1
(1) sample pre-treatments：
Room is handled before soil soil is poured on enamel pallet, be crushed with hammer, stick, pick impurity and taken with quartering point
Sample after crushing crosses 60 mesh nylon mesh, pedotheque is made.It weighs 10g pedotheque to be placed in a beaker, 2mL distillation is added
Water mixes well, be added the mixed mark solution of 20 μ L (α-six six six in mixed mark solution, β-six six six, γ-six six six, δ-six six six,
The concentration of p.p'-DDE, p.p'-DDD are that the concentration of 4 μ g/mL, o.p'-DDT, p.p'-DDT is 32 μ g/mL) as plus
Mark, is shelved several minutes, and the mixed liquor (volume ratio 1 of 100mL acetone and n-hexane is added:It 1), will be equipped with acetone and n-hexane
The sealing of the beaker sealed membrane of mixed liquor and soil prevents from volatilizing, and is put into ultrasonic machine and extracts 20 minutes, with full glass after extraction
Sand core filter device separates sample and extracting solution, and extracting solution is added in separatory funnel, and mixed with 15mL acetone and n-hexane
Close liquid (volume ratio 1:1) 3 flushings are carried out to beaker, soil sample and filter device, flushing liquor, which merges, to be added in separatory funnel, is added
Enter 100mL metabisulfite solution (concentration 20g/L), vibrate 1min, after stratification, discards lower layer's aqueous acetone solution, leave just
/ 10th concentrated sulfuric acid (excellent pure grade) of hexane extract volume, shaking is added in hexane extracting solution in separatory funnel
1min after stratification, discards sulfuric acid layer, is repeated several times according to above-mentioned steps, until two phase boundary of hexane extract being added
Stop when clear uniformly transparent in face.Then the sulphur of its volume half or so is added into the hexane extract for discard sulfuric acid layer
Acid sodium solution (concentration 20g/L).Shaking more than ten times, water layer is discarded after its stratification.It so repeats to n-hexane to extract
Stop when liquid is at neutrality, hexane extract is dehydrated through the cartridge type funnel equipped with a small amount of anhydrous sodium sulfate again, is filtered into the flat burning of 250mL
In bottle, 1mL is concentrated into rotary evaporator to get sample solution to be measured is arrived (according to purification side in national standard GB/T14550-2003
Method purifies hexane extract, is concentrated) to get arrive sample solution to be measured.
(2) with the concentration of six six six and DDT in gas chromatograph detecting step (1) gained sample solution to be measured：
Injector temperature：220℃；
Column temperature：It 150 DEG C of initial temperature, is kept for 2 minutes, is then raised to 270 DEG C with the speed of 6 DEG C/min and is kept for 25 points
Clock；
Detector temperature：300℃；
Flow：1.4mL/min.
Embodiment 2
The ultrasonic extraction time is 10min, remaining operating procedure is the same as embodiment 1.
Embodiment 3
The ultrasonic extraction time is 30min, remaining operating procedure is the same as embodiment 1.
Embodiment 4
The recovery of standard addition of comparing embodiment 1-3, the results are shown in Table 1：
The rate of recovery of the different ultrasonic extraction times of table 1 compares
Seen from table 1, the recovery of standard addition of each detection project of ultrasonic extraction 20min is apparently higher than ultrasonic extraction 10min's
Recovery of standard addition, but ultrasonic extraction 30min recovery of standard addition is without significant change.Therefore 20 minutes are the best ultrasonic extraction time.
Embodiment 5
The recovery of standard addition for comparing comparative example Yu embodiment 1, the results are shown in Table 2：
Table 2 extracts the comparison of recovery of standard addition using ultrasonic extraction and Soxhlet extractor
It is returned as can be seen from Table 2, identical soil sample detects resulting mark-on with improved pre-treating method (ultrasonic extraction)
Yield and traditional national standard Soxhlet extractor extraction method detect resulting recovery of standard addition and all meet to soil recovery of standard addition
The requirement of 70%-130%, and data are close.But ultrasonic extraction pretreatment process is utilized to save 15 than traditional national standard pretreatment process
The processing sample time of hour, substantially reduces sample detection time, improves detection efficiency, and improved pre-treating method
Petroleum ether in extracting solution is become into n-hexane, compensates for the petroleum ether disadvantage volatile, explosive since low boiling point heats, not only
Laboratory safety coefficient, and the not volatile small toxicity of n-hexane are improved, the body harm of experiment testing staff will be dropped to
It is minimum.
The present invention by a large amount of pedotheques carry out mark-on reclaims test (α-six six six, β-six six six, γ-six six six,
δ-six six six, P.P '-DDE, P.P '-DDD spiked levels are that 8 μ g/kg, P.P '-DDT O.P '-DDT spiked levels are 64 μ g/
Kg) analysis and summary obtains, carries out soil pre-treatment, each detection project standard relative deviation RSD using ultrasonic extracting method
0.92%-9.8%, recovery of standard addition 70.2%-129.4%, meets test requirements document.
In conclusion being dripped in the way of ultrasonic extraction to containing six six six, drop by means of above-mentioned technical proposal of the invention
The soil samples of tears carries out pre-treatment, not only substantially reduces time for sample pretreatment, improves conventional efficient, and with n-hexane generation
For petroleum ether as extracting solution, the safety of experimentation is not only increased, also reduces the body harm to testing staff, and
It is proved by largely detecting test, this improved method is able to satisfy the demand of high-volume Soil K+adsorption.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (5)
1. a kind of method of six six six and DDT in ultrasonic extraction-Soil by Gas Chromatography, which is characterized in that including such as
Lower step：
（1）Soil is poured on enamel pallet, is crushed, the sample after picking impurity and dividing pressure broken with quartering, 60 mesh Buddhist nuns are crossed
Dragon sieve, is made pedotheque；It weighs 10g pedotheque to be placed in a beaker, 2mL distilled water is added, mixes well, it is mixed that 20 μ L are added
Solution is marked as mark-on, is shelved several minutes, the mixed liquor of 100mL acetone and n-hexane is added, acetone and n-hexane will be housed
The beaker of mixed liquor and soil is sealed with sealed membrane, is put into ultrasonic machine and is extracted 10-30 minutes, with full glass sand core mistake after extraction
It filters device to separate sample and extracting solution, extracting solution is added in separatory funnel, and with the mixing of 10-15mL acetone and n-hexane
Liquid carries out 2-3 flushing to beaker, pedotheque and filter device, and flushing liquor, which merges, to be added in separatory funnel, and 100 mL are added
Metabisulfite solution vibrates 1 min, after stratification, discards lower layer's aqueous acetone solution, leaves hexane extract, leaks in liquid separation
/ 10th concentrated sulfuric acid of hexane extract volume is added in bucket, shakes 1min, after stratification, discards sulfuric acid layer, presses
It is repeated several times according to above-mentioned steps, until the hexane extract two-phase interface being added stops when clear uniformly transparent；Then to abandoning
It goes in the hexane extract of sulfuric acid layer that the metabisulfite solution of its volume half is added；Shaking 10-20 times, to its stratification
After discard water layer, stop when so repeating to hexane extract into neutrality, hexane extract pass through be equipped with a small amount of anhydrous sodium sulfate
The dehydration of cartridge type funnel, filter in boiling flask, be concentrated into 1mL with rotary evaporator to get to sample solution to be measured；
（2）With gas chromatograph detecting step（1）The concentration of six six six and DDT in gained sample solution to be measured：
Injector temperature：220℃；
Column temperature：It 150 DEG C of initial temperature, is kept for 2 minutes, is then raised to 270 DEG C with the speed of 6 DEG C/min and is kept for 25 minutes；
Detector temperature：300℃；
Flow：1.4mL/min.
2. the method for six six six and DDT in ultrasonic extraction-Soil by Gas Chromatography according to claim 1,
It is characterized in that, step（1）Described in be put into equipped with acetone and the mixed liquor of n-hexane and the beaker of soil and to be extracted in ultrasonic machine
Time is 20min.
3. the method for six six six and DDT in ultrasonic extraction-Soil by Gas Chromatography according to claim 1,
It is characterized in that, step（1）α-six six six in the mixed mark solution, β-six six six, γ-six six six, δ-six six six, p.p'-DDE,
The concentration of p.p'-DDD is that the concentration of 4 μ g/mL, o.p'-DDT, p.p'-DDT is 32 μ g/mL.
4. the method for six six six and DDT in ultrasonic extraction-Soil by Gas Chromatography according to claim 1,
It is characterized in that, step（1）Acetone and n-hexane volume ratio are 1 in the mixed liquor of the acetone and n-hexane:1.
5. the method for six six six and DDT in ultrasonic extraction-Soil by Gas Chromatography according to claim 1,
It is characterized in that, step（1）Described in metabisulfite solution concentration be 20g/L.
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