CN106053631A - Automatic dispersed liquid-liquid micro-extraction system and applications thereof - Google Patents
Automatic dispersed liquid-liquid micro-extraction system and applications thereof Download PDFInfo
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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
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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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
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/025—Gas chromatography
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
Abstract
The invention discloses an automatic dispersed liquid-liquid micro-extraction system, which comprises an injection pump, an 8-position electromagnetic rotary valve, a three-way valve, a mixer, and a control device. On the basis of the system, an automatic in-situ DLLME method is established, the DLLME method is used to extract PAEs in natural water and has the advantages of simpleness, miniaturization, and efficiency, and after extraction, the sample is analyzed by gas chromatography-mass spectrum (GC-MS). The test results show that the provided system can be used to in-situ extract PAEs from a ground water sample, the detection limit is low, moreover, the extraction time is short, the sample throughput is large, and the system can be used to process trace PAEs in natural water onsite automatically.
Description
Technical field
The present invention relates to a kind of full-automatic dispersion liquid-liquid current micro-extraction system, further relate to its O-phthalic in Environmental Water
Application in esters of gallic acid extracting substances.
Background technology
Phthalic acid ester (being commonly called as plasticiser, PAEs) can increase the plasticity of plastic, is widely used in industry
Produce and in goods.Owing to PAEs is more weak with the intermolecular forces of polymer, the PAEs in plastic is very easy to be released to
In food, beverage and natural water.There are some researches show, PAEs is a kind of environmental endocrine disruptors, can be to human body
Kidney, hormonal system, reproductive system and respiratory system cause serious harm.Therefore, PAEs is all classified as preferential dirt by various countries
Dye thing is strictly monitored and controlled.But PAEs concentration in environment water is the lowest, and aqueous samples is complicated, is often analyzing
Need sample is effectively separated enrichment before.
Dispersion liquid-liquid micro-extraction (DLLME) is a kind of simplification, milligram ammonia and high efficiency separation and concentration technology, and
It is successfully applied to the extraction of PAEs.In DLLME, the extractant of trace and appropriate dispersant, then it is rapidly injected
In sample, under the effect of dispersant, the extractant of trace disperses in the sample with the form of superfine microdroplet, forms dispersion
System.Under such dispersion, on the one hand add the contact area of extractant and sample, on the other hand decrease object
To the mass transfer distance of extractant, therefore extraction efficiency is greatly improved.After extraction, by centrifugal, extractant is deposited on test tube
Bottom or float over sample surfaces, Instrumental Analysis can be entered with microsyringe after pipetting.
At present, common dispersion liquid-liquid micro-extracting method includes multiple, such as ionic liquid-dispersive liquid-liquid microextraction, super
Sound wave aid dispersion liquid-liquid micro-extraction-organic drop solid-state that suspends, air aid dispersion liquid-liquid micro-extraction etc..But, at these
In method, it is all manual operation, complex operation, the longest, and detection limit is higher, and the original position being also unsuitable for sample is (the most existing
Field on field) process.
Therefore, it is necessary to set up a kind of simple, miniaturization, efficient full-automatic DLLME system in situ for Environmental Water
The extraction of PAEs in body.
Summary of the invention
For solving the problems referred to above, the invention provides a kind of full-automatic dispersion liquid-liquid current micro-extraction system, it includes injection
Pump, 8 electromagnetic rotating valves, three-way valve, blender and control device；
Described syringe pump, three-way valve are connected with control device with electromagnetic valve；
Described syringe pump is provided with syringe；
Described electromagnetic valve is provided with discharging opening, logical blender mouth, enters air scoop, water inlet, injection port, waste discharge mouth, enters point
Powder mouth and enter extractant mouth；
Described three-way valve includes liquid outlet (A), inlet (B) and commutation mouth (C)；
Wherein, the inlet (B) of described three-way valve is communicated by connecting tube with the discharging opening of electromagnetic valve, commutation mouth (C) with
The geat of syringe communicates；Logical blender mouth on described electromagnetic valve is communicated by connecting tube with blender.
Further, it is additionally provided with between described blender with logical blender mouth and mixes circle.
Further, described connecting tube is the polyfluortetraethylene pipe of 0.79mm internal diameter.
Present invention also offers a kind of phthalate extracting substances method in Environmental Water, described phthalic acid
Ester includes any one in dibutyl phthalate, dimethyl phthalate and dioctyl phthalate or many
Kind, it uses weighs aforesaid full-automatic dispersion liquid-liquid current micro-extraction system, comprises the following steps:
(1) syringe and pipeline are cleaned:
Making inlet (B) and commutation mouth (C) communicate, syringe sucks ultra-pure water from water inlet, then by waste discharge mouth 5 row
Go out；
(2) extractant and the mixing of dispersant:
Syringe is first from entering dispersant mouth suction dispersant and sucking extractant from entering extractant mouth, then inhales from entering air scoop
Enter air, then discharge it into formation mixed liquor in blender, then by this mixed liquor inhalation syringe；
Wherein, the order sucking dispersant and suction extractant can be optional.
(3) sample injects:
Syringe sucks testing sample from injection port, mixes with the mixed liquor of step (3), forms dispersion；
(4) extraction and the collection of object:
After stratification goes out organic facies, make liquid outlet (A) and commutation mouth (C) communicate, discharge organic facies from liquid outlet (A),
Collect stand-by；
(5) waste liquid is discharged:
Make liquid outlet (B) and commutation mouth (C) communicate, remaining sample is discharged by waste discharge mouth.
Further, in step (2), described extractant is selected from toluene or dimethylbenzene, and dispersant is selected from acetone, acetonitrile or first
Alcohol；Preferably extractant is toluene, and dispersant is acetonitrile.
Further, in step (2), the dispersant of described suction and extractant volume ratio are 20:1.
Further, in step (3), the suction speed of described suction sample is 125mL/min.
Further, in step (4), the time of described stratification is 60 seconds.
Further, described Environmental Water is surface water.
Further, described phthalate material includes dibutyl phthalate, dimethyl phthalate
With any one or more in dioctyl phthalate.
Therefore, the invention provides a kind of full-automatic dispersion liquid-liquid current micro-extraction system, on the basis of this system, set up
A kind of simple, miniaturization, the efficient full-automatic extraction of PAEs in natural water of DLLME method in situ, extracted
After finishing, sample is analyzed through gas chromatography mass spectrometer (GC-MS).
The present invention optimizes the key parameter of method the most further, such as extractant and the kind of dispersant and consumption, sample
Product injection rate, extraction time, sample pH value, salt effect and matrix effect etc..Finally, the inventive method is used for reagent ground
The situ extracting of PAEs in table water sample, has relatively low detection limit, and extraction time is short, and sample throughput is big, it is adaptable to
The on-the-spot full automatic treatment of trace PAEs in natural water.
Obviously, according to the foregoing of the present invention, according to ordinary technical knowledge and the customary means of this area, without departing from
Under the present invention above-mentioned basic fundamental thought premise, it is also possible to make the amendment of other various ways, replace or change.
The detailed description of the invention of form by the following examples, remakes the most specifically the foregoing of the present invention
Bright.But this should not being interpreted as, the scope of the above-mentioned theme of the present invention is only limitted to Examples below.All based on foregoing of the present invention
The technology realized belongs to the scope of the present invention.
Accompanying drawing explanation
Fig. 1 is present system structural representation.
Fig. 2 is the optimum decision system structural representation employed in the embodiment of the present invention 1, and electromagnetic valve is provided with discharging port A, leads to
Blender mouth 1, enter air scoop 2, water inlet 3, injection port 4, waste discharge mouth 5, enter dispersant mouth 7 and enter extractant mouth 8；SP be complete from
Dynamic syringe pump；MPV is one 8 electromagnetic rotating valves (MPV)；V is dedicated three-way selector valve.
Fig. 3 is full-automatic DLLME effect of extracting schematic diagram: (a) rinse；(b) extractant and the mixing of dispersant；(c) sample
Product inject, and dispersion is formed；(d) stratification；The collection of (e) organic facies.
Fig. 4 is different extractant and full-automatic DLLME effect of extracting is affected by dispersant.Wherein 1 toluene-acetone 2 toluene-
Acetonitrile 3 methylbenzene methanol l；4 dimethylbenzene acetone；5 dimethylbenzene-acetonitrile 6 dimethylbenzene-methanol；7 normal hexane-acetone；8 hexamethylene-the third
Ketone；9 isobutyltrimethylmethane .s-acetone. experiment condition: sample volume 5mL；Sample injection rate 150ml/min；Extraction time 2min；Do not increase
Add ionic strength；Sample mark-on 5.0ng；N=3.
Fig. 5 is that extractant and dispersant volume are to DLLME influential effect.
Fig. 6 is full-automatic DLLME-GC-MS chromatogram. (a) sample mark-on 5.0ng；B () is mark-on sample.
Detailed description of the invention
Reagent and material:
The PAEs standard reserving solution of 1g/L, including dibutyl phthalate (DBP), dimethyl phthalate (DMP),
Dioctyl phthalate (DNOP) is purchased from Germany Merck；PAEs standard working solution is diluted by standard reserving solution ultra-pure water
Obtain.
Chromatographically pure normal hexane, toluene, dimethylbenzene, isobutyltrimethylmethane., hexamethylene, and analytically pure sodium chloride, hydrochloric acid, hydrogen-oxygen
Change sodium purchased from Chengdu Ke Long Reagent Company.
Chromatographically pure methanol, acetonitrile, acetone are purchased from U.S. Tedia.
For avoiding PAEs to pollute, first all glass drying ovens need to soak 6h in acetone, then dry 4h at 140 DEG C.
The system and method for embodiment 1 present invention
(1) system of the present invention
Full-automatic DLLME system schematic used by the present embodiment is as shown in Figure 2.This full-automatic DLLME system is by one
The full-automatic injecting pump (SP) of 9600 steps and one 8 electromagnetic rotating valves (MPV) are constituted.All connecting tubes are by 0.79mm internal diameter
Politef (PTFE) pipe is constituted.The syringe of dedicated three-way selector valve (V) and 1 10mL is provided on SP.MPV is used for sample
The transfer of product, extractant, dispersant, high purity water, air, waste liquid and other reagent and switching.Mixing pit (MC) is by 5mL's
Barrel syringe is constituted, for dispersant and the mixing of extractant.Whole system (except notebook computer) is by an AC adapter
It is powered with one group of lithium battery, and runs under 24V DC.Whole system is light and handy, portable, and weight is only 2.6kg and (includes electricity
Source).
Sample after extraction is combined 5975 type mass spectrographs by 7890 type gas chromatograies of Agilent company of the U.S. to be carried out
Quantitative analysis.Chromatographic column: HP-5MS (5%phenyl, 95%methylpolysiloxane, 30m × 0.25mm id × 0.25 μ
M) capillary column；Helium (> 99.999%) make carrier gas, flow 1.0mL/min.Injector temperature: 250 DEG C；Sample introduction pattern: regardless of
Stream.Column temperature program is as follows: 60 DEG C, keeps 1min, with 20 DEG C of min-1It is warming up to 220 DEG C, keeps 1min, with 5 DEG C of min-1Heat up
To 280 DEG C, keep 4min.Mass detector uses Salbutamol Selected Ion Monitoring pattern (SIM).Solvent delay 6min.Sweep time and
Monitoring ion is as follows: DMP, 6.0min, m/z 163,77,135；DBP,10.0min,m/z149,223,205；DNOP,
18.0min,149,279,167。
(2) sample and DLLME system operation programs
Natural water sample picks up from clear water river (Chengdu, China).After sample collecting, it is introduced directly into complete after crossing 0.22 μm filter membrane
Automatically DLLME system processes.
Electromagnetic valve is provided with discharging port A, logical blender mouth 1, enters air scoop 2, water inlet 3, injection port 4, waste discharge mouth 5, enters
Dispersant mouth 7 and enter extractant mouth 8.
DLLME working procedure:
(1) clean syringe pump and pipeline: SP sucks 10mL ultra-pure water (, No. 3 positions, V is in b position for MPV), then by waste liquid
Send (, No. 5 positions, V is in b position for MPV), the most reciprocal 3 times.
(2) extractant and the mixing of dispersant: SP suck 1mL dispersant (, No. 7 positions, V is in b position for MPV), 50 μ L successively
Extractant (, No. 8 positions, V is in b position for MPV) and 2mL air (, No. 2 positions, V is in b position for MPV), discharge it into the most again
In MC (, No. 1 position, V is in b position for MPV), for more effectively making dispersant and extractant mixing, the most reciprocal 2 times of this step, and
During the mixed liquor of dispersant and extractant sucks SP the most at last.
(3) sample injects: 5mL sample is quickly sucked in SP with the speed of 125mL/min, and (, No. 4 positions, V is at b for MPV
Number position), it is consequently formed dispersion.
(4) extraction and the collection of object: after forming dispersion, stands, and target substance is quickly at sample and extractant
Between reach balance, after 60s, organic facies floats on sample top layer, and switching V (a position) slowly promotes SP, 60 μ L min-1, by organic
It is collected in mutually in sample bottle, preserves to be measured.
(5) discharge waste liquid: switching MPV and V (, No. 5 positions, V is in b position for MPV), remaining sample is sent by waste liquid.
The effect of whole extraction process is as shown in Figure 3.
The craft screening of embodiment 2 the inventive method
1 extractant and the impact of dispersant
Compare variety classes extractant (normal hexane, toluene, dimethylbenzene, isobutyltrimethylmethane., hexamethylene) and dispersant (acetonitrile,
Acetone, methanol) impact on effect of extracting.
Sample volume 5mL；Sample injection rate 150ml/min；Extraction time 2min；Do not increase ionic strength；Sample adds
Mark 5.0ng；N=3；The ratio of all extractants and dispersant is 1:19, and cumulative volume is 1mL.Result is as shown in Figure 4.Result
Show, when toluene is as extractant, when acetonitrile is as dispersant, best results.
2 extractants and the impact of dispersant volume
The study tour extractant of different volumes (50to 150 μ L) and dispersant (0.25to 1.25mL) are to extraction effect
The impact of fruit, result is as shown in Figure 5.
Result shows, in 3, plasticiser variation tendency is similar, when 50 μ L extractants and 1mL dispersant are used for DLLME system
Time, extracting and enriching multiple is the highest, and effect of extracting is best.Wherein, enrichment times increases along with the minimizing of the amount of extractant, but
When extractant volume is less than 50 μ L, organic facies becomes unstable and is difficult to collect.It addition, enrichment times is along with the amount of dispersant
Increase and increase, but when the amount of dispersant is more than 1mL, declining occurs in enrichment times,
Therefore, 50 μ L extractants and 1mL dispersant selected be optimal.
The impact on effect of extracting of the 3 sample suction velocities
In the methods of the invention, sample is quickly sucked into SP, and with extractant/dispersant, formed dispersion.
Inventor have studied different sample and sucks speed (30to 150mL min-1) to this DLLME influential effect.
Result shows, increases to 125mL min along with sample sucks speed from 30-1, recovery of extraction and enrichment times increase
Add, when sample sucks speed more than 125mL min-1Time, effect of extracting is unaffected.The pump speed of two-forty can affect it and use the longevity
Life, therefore the inventive method selects 125mL min-1Sample suck speed be optimal.
The impact of 4 extraction times
In the methods of the invention, extraction time be defined as sample be inhaled into formation dispersion and proceed by sample receive
This time interval between collection.Have studied different extraction time (30,45,60,90,120,180,240and 300s) to extraction
Take the impact of effect.
Research shows, when extraction time is less than 30s, it is impossible to realize two-phase laminated flow, and recovery of extraction and enrichment times with
The increase of extraction time and increase.But, after extraction time is more than 60s, effect of extracting is without significant change.Therefore, the extraction of 60s
The time of taking is considered optimal.
5 salt effects and the impact of sample pH value
Have studied the impact on effect of extracting of the different sample pH value (2 to 11).Utilize 0.1M HCl and NaOH to regulate sample
pH.Result shows, along with the change of sample pH value, effect of extracting is without significant change.Therefore, extraction process is without regulating sample pH value.
In liquid-phase extraction, it will usually add salt and improve sample ions intensity, thus improve effect of extracting.Therefore, grind
Study carefully the impact having investigated different ionic strength to effect of extracting, add the NaCl (0to 5%, m/v) of variable concentrations in the sample,
Result shows, the sample extraction response rate and enrichment times reduce along with the increase of salinity.
Therefore, in the methods of the invention without adding salt.
6 method performance parameters
Fig. 6 is under optimal conditions, utilizes the chromatogram of the PAEs that the inventive method obtains.The main performance of the inventive method
Parameter, including detection limit, the range of linearity, correlation coefficient, enrichment times, the response rate and repeatability etc., is shown in Table 1.Full-automatic DLLME
The extraction of method single sample is spaced apart 170s, and sample throughput is 21h-1。
The full-automatic DLLME-GC/MS methods analyst performance parameter of PAEs in table 1 natural water
A:n=3；B: sample mark-on 1.0ng PAEs；C: sample mark-on 5.0ng PAEs；D: sample mark-on 10ng PAEs.
The inventive method is compared with other non-automated DLLME methods, the results are shown in Table 2.
The contrast of the non-full-automatic DLLME method of table 2 the inventive method and other PAEs
aIonic liquid-dispersive liquid-liquid microextractionb1-octyl group-3-Methylimidazole. hexafluorophosphatecUltrasonic assistant dispersion liquid
Liquid micro-extraction-suspend organic drop solid statedThe dispersion of extractant is realized by 8 air injections
[1]Pérez-Outeiral J.,Millán E.,Garcia-Arrona R.,Determination of
phthalates in food simulants and liquid samples using ultrasound-assisted
dispersive liquid-liquid microextraction followed by solidification of
floating organic drop.Food Control,2016,62,171-177.
[2]Mousa A.,Basheer C.,Al-Arfaj A.R.,Determination of phthalate
esters in bottled water using dispersive liquid-liquid microextraction
coupled with GC-MS.J.Sep.Sci.2013,36,2003-2009.
[3]Chen S.,Zhong Y.,Cheng S.,Qian T.,Sun H.,Development of an ionic
liquid-based dispersive liquid-liquid micro-extraction method for the
determination of phthalate esters in water samples.J.Sep.Sci.2011,34,1503-
1507.
[4]Farajzadeh M.A.,Mogaddam M.R.A.,Air-assisted liquid-liquid
microextraction method as a novel microextraction technique；Application in
extraction and preconcentration of phthalate esters in aqueous sample
followed by gas chromatography-flame ionization detection.Anal.Chim.Acta
2012,728,31-38.
[5]Farahani H.,Norouzi P.,Dinarvand R.,Ganjali M.R.,Development of
dispersive liquid-liquid microextraction combined with gas chromatography-
mass spectrometry as a simple,rapid and highly sensitive method for the
determination of phthalate esters in water samples.J.Chromatogr.A 2007,1172,
105-112
Comparing compared with these methods existing, the inventive method has relatively low detection limit, and, the inventive method extracts
Taking the time short, sample throughput is big, it is adaptable to the on-the-spot full automatic treatment of trace PAEs in natural water.
7 actual sample analyses
Utilize the inventive method that the PAEs in 6 samples of clear water river section (Chengdu, China) is processed and divided
Analysis, the results are shown in Table 3.
PAEs result in the full-automatic DLLME extractive analysis actual sample in situ of table 3
aN=3bSample mark-on 5.0ng PAEscDo not detect
Result shows, has all detected the DBP of variable concentrations in all samples.Additionally, the recovery testu of variable concentrations
Effect is satisfactory, shows that the inventive method is accurate, capacity of resisting disturbance strong, without matrix effect.
In sum, the invention provides a kind of full-automatic dispersion liquid-liquid current micro-extraction system, on the basis of this system,
Establish a kind of simple, miniaturization, efficient full-automatic DLLME method extraction of PAEs in natural water in situ, extraction
After taking, sample is analyzed through gas chromatography mass spectrometer (GC-MS).
The present invention optimizes the key parameter of method the most further, such as extractant and the kind of dispersant and consumption, sample
Product injection rate, extraction time, sample pH value, salt effect and matrix effect etc..Finally, the inventive method is used for reagent ground
The situ extracting of PAEs in table water sample, has relatively low detection limit, and extraction time is short, and sample throughput is big, it is adaptable to
The on-the-spot full automatic treatment of trace PAEs in natural water.
Claims (10)
1. a full-automatic dispersion liquid-liquid current micro-extraction system, it is characterised in that: it include syringe pump, 8 electromagnetic rotating valves, three
Logical valve, blender and control device；
Described syringe pump, three-way valve are connected with control device with electromagnetic valve；
Described syringe pump is provided with syringe；
Described electromagnetic valve is provided with discharging opening, logical blender mouth, enters air scoop, water inlet, injection port, waste discharge mouth, enters dispersant
Mouthful and enter extractant mouth；
Described three-way valve includes liquid outlet (A), inlet (B) and commutation mouth (C)；
Wherein, the inlet (B) of described three-way valve is communicated by connecting tube with the discharging opening of electromagnetic valve, commutation mouth (C) and injection
The geat of device communicates；Logical blender mouth on described electromagnetic valve is communicated by connecting tube with blender.
System the most according to claim 1, it is characterised in that: it is additionally provided with between described blender with logical blender mouth and mixes
Circle.
System the most according to claim 1 and 2, it is characterised in that: described connecting tube is the polytetrafluoroethyl-ne of 0.79mm internal diameter
Alkene pipe.
4. the phthalate extracting substances method in an Environmental Water, it is characterised in that: described phthalate
Material includes any one or more in dibutyl phthalate, dimethyl phthalate and dioctyl phthalate,
It uses the full-automatic dispersion liquid-liquid current micro-extraction system described in any one of claim 1-3, comprises the following steps:
(1) syringe and pipeline are cleaned:
Making inlet (B) and commutation mouth (C) communicate, syringe sucks ultra-pure water from water inlet, is then discharged by waste discharge mouth；
(2) extractant and the mixing of dispersant:
Syringe is first from entering dispersant mouth suction dispersant and sucking extractant from entering extractant mouth, then sucks sky from entering air scoop
Gas, then discharge it into formation mixed liquor in blender, then by this mixed liquor inhalation syringe；
(3) sample injects:
Syringe sucks testing sample from injection port, mixes with the mixed liquor of step (3), forms dispersion；
(4) extraction and the collection of object:
After stratification goes out organic facies, make liquid outlet (A) and commutation mouth (C) communicate, discharge organic facies from liquid outlet (A), collect
Stand-by；
(5) waste liquid is discharged:
Make liquid outlet (B) and commutation mouth (C) communicate, remaining sample is discharged by waste discharge mouth.
Method the most according to claim 4, it is characterised in that: in step (2), described extractant is selected from toluene or diformazan
Benzene, dispersant is selected from acetone, acetonitrile or methanol；Preferably extractant is toluene, and dispersant is acetonitrile.
Method the most according to claim 5, it is characterised in that: in step (2), the dispersant of described suction and extractant body
Long-pending ratio is 20:1.
Method the most according to claim 4, it is characterised in that: in step (3), the suction speed of described suction sample is
125mL/min。
Method the most according to claim 4, it is characterised in that: in step (4), the time of described stratification is 60 seconds.
Extracting method the most according to claim 9, it is characterised in that: described Environmental Water is surface water.
Extracting method the most according to claim 8 or claim 9, it is characterised in that: described phthalate material includes neighbour
Any one or more in phthalic acid dibutyl ester, dimethyl phthalate and dioctyl phthalate.
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| CN106802328A (en) * | 2017-01-18 | 2017-06-06 | 电子科技大学 | A kind of full-automatic dispersive liquid-liquid microextraction method of mercury shape material in ambient water |
| CN106802328B (en) * | 2017-01-18 | 2019-12-13 | 电子科技大学 | Full-automatic dispersion liquid-liquid micro-extraction method for mercury form substances in environmental water |
| CN107782724A (en) * | 2017-12-04 | 2018-03-09 | 深圳市朗诚科技股份有限公司 | A kind of nutritive salt in-situ analyzer and nutrient concentrations analysis method |
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| CN108872106A (en) * | 2018-06-26 | 2018-11-23 | 电子科技大学 | A kind of method of trace sulphite in measurement water body |
| CN114113282A (en) * | 2021-11-18 | 2022-03-01 | 中国检验检疫科学研究院 | Small portable mass spectrum on-site rapid detection method for harmful dyes in textiles |
| CN114113282B (en) * | 2021-11-18 | 2023-12-22 | 中国检验检疫科学研究院 | Small portable mass spectrum on-site rapid detection method for harmful dye in textile |
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