CN108241027A - The assay method of chlorobenzene compound in environmental water sample - Google Patents
The assay method of chlorobenzene compound in environmental water sample Download PDFInfo
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- CN108241027A CN108241027A CN201611218441.4A CN201611218441A CN108241027A CN 108241027 A CN108241027 A CN 108241027A CN 201611218441 A CN201611218441 A CN 201611218441A CN 108241027 A CN108241027 A CN 108241027A
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- G—PHYSICS
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- 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
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Abstract
The present invention provides a kind of assay method of chlorobenzene compound in environmental water sample; this method protects the Sample Pretreatment Technique of micro- Solid Phase Extraction to be used in conjunction with gas-chromatography with film; the extraction and analysis carried out to the trace CBs in environmental water sample; the technical issues of present analysis instrument is difficult to direct quantitative detection is efficiently solved, realizes the quantitative detection of chlorobenzene compound in environmental water sample.
Description
Technical field
The present invention relates to chlorobenzene compounds, and in particular to the assay method of chlorobenzene compound in a kind of environmental water sample.
Background technology
Chlorobenzene compound (CBs) be the widely applied industrial chemicals of the industries such as dyestuff, medicine, chemical industry, organic solvent or
Organic synthesis intermediate, smell is strong, and chemical property is stablized, and not easily passs through physics, chemistry or biological method and degrades, therefore
The residence time is long, accumulative big in environment.Research shows that the CBs contents in environment water are low (ng/L~μ g/L), but CBs into
Entering human body, easily accumulated in the abundant tissue of fat content, inhibit nerve center, serious poisoning is liver injury and kidney,
And there is carcinogenic, teratogenesis and mutagenicity mostly, therefore be included in priority acccess control by many countries including our countries
Pollutant.Therefore, it has great significance to the Accurate Determining of CBs contents in water body and being controlled.Since CBs contains in water body
Amount belongs to microgram, nanogram level, and current analytical instrument is not enough to directly detect the CBs of underwater trace, chlorine in development environment water sample
The method of benzene-like compounds Accurate Determining is very necessary.
At present, traditional liquid-liquid extraction (LLE) is most domestic and international common water sample pretreatment technology, is had as many
CBs standard methods in extraction environmental water sample as defined in the standard preprocess method of machine compound and Ministry of Environmental Protection；But
Its consumption of organic solvent is big, easily generates emulsion, and be easy to cause secondary pollution.Since the seventies, Solid Phase Extraction
(SPE) with its it is efficient, accurate the advantages that be developed rapidly；But this method takes, subsequent purification, concentration step are cumbersome,
Solid phase microextraction column is expensive, and cost is higher.In view of the requirement of Green Chemistry, reduces the use of organic solvent, makes equipment as far as possible
Micromation and analytical procedure simplicity reduce the analyzing and processing time, and the micromation of traditional technology is that the development of sample pre-treatments becomes
Gesture.
It is mutually to tie traditional SPE approach and hollow-fibre membrane protection SPME methods that film, which protects micro- Solid Phase Extraction (μ-SPE),
It closes, a kind of novel sample pretreating method pre-processed to environmental sample.This method is only with organic molten less than 100 μ l
Agent, it is smaller to organic solvent dependence, meet the theory of " Green Chemistry "；And have for severe experiment condition higher resistance to
It, can also be to macromolecular chaff interference contaminant filter, purification, so as to simplify sample pre-treatments step by property.By a few years
Development, which has been applied to aldehyde in environmental water sample, carbaminate pesticide, aromatic amine and PAHs in soil
(PAHs) and in the pretreatment of polybrominated diphenyl ethers.Limited solid extracting agent (C18, C8, C2 and carbon nanotube of commercialization) limit
The development of μ-SPE is made.
Invention content
The defects of in order to overcome the prior art, the object of the present invention is to provide chlorobenzene compounds in a kind of environmental water sample
Assay method, the extraction and analysis that this method carries out the trace CBs in environmental water sample, detection efficiency is high, favorable reproducibility.
The object of the present invention is achieved like this：
The assay method of chlorobenzene compound in a kind of environmental water sample is walked including sample pre-treatments and gas chromatographic detection
Suddenly, it is characterised in that：The sample pre-treatments are micro- Solid Phase Extraction material bag to be protected to be placed in the extraction glass containing sample water sample film
Vial will be extracted in glass bottle, after sealing with whirlpool instrument with the rotating speed elution operation 1-7min of 2000~4000rpm, it then will material
Bag is removed and placed in the gas chromatographic sample introduction bottle containing interpolation pipe, is added in organic solvent ultrasound and is eluted 3~20min, formation
Eluent is gas chromatographic detection sample；The organic solvent is acetonitrile, ethyl acetate, methanol, one kind in n-hexane or several
Kind combination.
An embodiment according to the present invention, above-mentioned chlorobenzene compound be selected from 1,3- dichloro-benzenes (1,3-DCB), Isosorbide-5-Nitrae-
Dichloro-benzenes (1,4-DCB), 1,2,4- trichloro-benzenes (1,2,4-TCB), 1,2,4,5, one kind in-tetrachlorobenzene (1,2,4,5-TeCB)
Or several combinations.
An embodiment according to the present invention, above-mentioned film protect micro- Solid Phase Extraction material bag solid to be added in polypropylene screen bag
Body adsorbent, drying are made；The solid absorbent is NZIF-8, C18 or C8.
An embodiment according to the present invention, above-mentioned solid absorbent NZIF are nano zeolite imidazate skeleton structure material
Material.
An embodiment according to the present invention, above-mentioned solid absorbent NZIF-8 are made by following steps：
Zinc nitrate hexahydrate and 2-methylimidazole are dissolved with methanol and mixing under agitation, 0.5~2h of room temperature reaction,
Muddy solution is obtained, precipitation is collected by centrifugation, methanol washing is subsequently placed in baking oven and had both been obtained in 70~90 DEG C of drying.
An embodiment according to the present invention, above-mentioned sample pre-treatments are to be placed in the polypropylene screen bag equipped with NZIF-8
In extraction vial containing sample water sample, extraction vial is washed with whirlpool instrument with the rotating speed of 2000~4000rpm after sealing
Material bag, is then removed and placed in the gas chromatographic sample introduction bottle containing interpolation pipe by de- operation 4-6min, adds in organic solvent and surpasses
Sound elutes 3~20min, and the eluent of formation is gas chromatographic detection sample；The organic solvent is acetonitrile, ethyl acetate, first
The combination of one or more of alcohol, n-hexane.
An embodiment according to the present invention, above-mentioned sample pre-treatments are to be placed in the polypropylene screen bag equipped with NZIF-8
In extraction vial containing sample water sample, extraction vial is washed with whirlpool instrument with the rotating speed of 2000~4000rpm after sealing
Material bag, is then removed and placed in the gas chromatographic sample introduction bottle containing interpolation pipe by de- operation 4-6min, adds in organic solvent and surpasses
Sound elutes 5~10min, and the eluent of formation is gas chromatographic detection sample；The organic solvent is acetonitrile, ethyl acetate, first
The combination of one or more of alcohol, n-hexane.
An embodiment according to the present invention, above-mentioned sample pre-treatments are to be placed in the polypropylene screen bag equipped with NZIF-8
Vial will be extracted in extraction vial containing sample water sample, after sealing, and 4- is run with the rotating speed of 3000rpm with whirlpool instrument
Then material bag is removed and placed in the gas chromatographic sample introduction bottle containing interpolation pipe by 6min, and addition n-hexane ultrasound elution 5~
10min, the eluent of formation is gas chromatographic detection sample.
An embodiment according to the present invention, the assay method of chlorobenzene compound in a kind of environmental water sample, including sample
Product pre-treatment and gas-chromatography detecting step, it is characterised in that：The sample pre-treatments is will be equipped with the polypropylene screen of NZIF-8
Bag is placed in the extraction vial containing sample water sample, and vial will be extracted after sealing and is transported with whirlpool instrument with the rotating speed of 3000rpm
Row 5min takes out the μ-SPE material bags in vial and is wiped to suck residual moisture with lint-free paper；The solid absorbent
For NZIF-8 for zinc nitrate hexahydrate and 2-methylimidazole are dissolved with methanol, 0.5~2h of room temperature reaction obtains muddy solution, from
The heart collects precipitation, and methanol washing is subsequently placed in baking oven and is made in 70~90 DEG C of drying；Finally μ-SPE material bags be put into containing
In the gas chromatographic sample introduction bottle of interpolation pipe, n-hexane ultrasound elution 5min is added in, the eluent of formation is gas chromatographic detection sample
Product；The testing conditions are gas chromatography-mass spectrum condition：Chromatographic column:DB-5MS capillary chromatographic columns, column length 30m, internal diameter
0.25mm；Carrier gas：Hydrogen；Flow velocity：1.8ml/min；220 DEG C of injector temperature；240 DEG C of detector temperature；Column temperature：Initial temperature 40
DEG C, 2min is stopped, 8 DEG C per minute are raised to 220 DEG C, finally stop 4min at 220 DEG C.
Advantageous effect
The present invention provides a kind of assay method of chlorobenzene compound in environmental water sample, and this method protects micro- solid phase to extract with film
The Sample Pretreatment Technique taken is used in conjunction with gas-chromatography, to extraction and analysis that the trace CBs in environmental water sample is carried out, effectively solves
Present analysis instrument of having determined is difficult to the technical issues of direct quantitative detection, realizes quantifying for chlorobenzene compound in environmental water sample
Detection.
A kind of VA- μ-SPE the present invention provides novel NZIFs are organic to the trace in environmental water sample with reference to GC-MS
The detection method of pollutant CBs.Under the auxiliary of vortex instrument, μ-SPE optimum extraction times only need 5min, and this method is effective
Reduce the extraction time of AA- μ-SPE (usually>30min).The present invention achieves wider, the preferable range of linearity of the degree of correlation
And the excellent performance of NZIF-8 is applied in μ-SPE by relatively low LODs, this method, completes the absorption to CBs in water sample
Work is extracted, applies for it and lays a good foundation in the organic pollutant monitoring direction of environmental water sample, it is effective to expand
Applications of the ZIFs in sample pre-treatments.
It is vortexed the present invention provides film protection nano zeolite imidazate frame structure material 8 (NZIF-8) and assists micro- solid phase extraction
The Sample Pretreatment Technique of (VA- μ-SPE) is taken, and the extraction carried out to the trace CBs in environmental water sample is used in conjunction with gas-chromatography
And analysis.By the control of a series of conditions such as eluant, eluent, extraction time, ultrasonic elution time, the detection limit model of CBs is realized
It encloses for 0.002~0.008ng/ml, in linearly ranging from 0.1-50ng/ml, the coefficient of determination (r2) it is all higher than 0.991.Experiment
The result shows that the present invention carries out 5 parallel determinations in the CBs samples of a concentration of 5ng/ml, relative standard deviation (RSD%) is equal
Less than 8.4%；Simultaneously to four kinds of CBs in actual water sample, relative recovery is 87.9%~111.1%.
Description of the drawings
Fig. 1 eluant, eluents are to the influence figure of chlorobenzene compound effect of extracting in water sample；
Fig. 2 whirlpool times are to the influence figure of chlorobenzene compound effect of extracting in water sample；
Fig. 3 ultrasounds elution time is to the influence figure of chlorobenzene compound effect of extracting in water sample；
Fig. 4 VA- μ-SPE and comparison of the AA- μ-SPE extraction process to water sample CBs extraction efficiencies；
Influence of Fig. 5 solid extracting agents to CBs extraction efficiencies in water sample.
Specific embodiment
In order to make the purpose of the present invention and technical solution clearer, the preferred embodiment of the present invention is carried out below detailed
Description.To illustrate that：Following embodiment is served only for that the present invention is further detailed, and it is not intended that this hair
The limitation of bright protection domain.Those skilled in the art's the above according to the present invention make some it is nonessential improvement and
Adjustment all belongs to the scope of protection of the present invention.Instrument of the present invention, raw material and reagent are commercial product.Wherein, reagent：1,
3- dichloro-benzenes (1,3-DCB), Isosorbide-5-Nitrae-dichloro-benzenes (Isosorbide-5-Nitrae-DCB), 1,2,4- trichloro-benzenes (1,2,4-TCB), 1,2,4,5 ,-tetrachlorobenzene
(1,2,4,5-TeCB) is purchased from Sigma-Aldrich companies.Unless otherwise noted, reagent is that analysis is pure used by this experiment
Or higher level, water are distilled water.
Embodiment 1
The preparation of NZIF-8
Zinc nitrate hexahydrate (1.467,4.94mmol) and 2-methylimidazole (3.245g, 39.52mmol) are dissolved in respectively
In the methanol of 100ml, under agitation, zinc nitrate hexahydrate solution is quickly added in 2-methylimidazole methanol solution.
After reaction 1 hour, muddy solution is obtained, precipitation is collected by centrifugation.Obtained product is washed with methanol, is finally placed in baking oven
It is dried at 80 DEG C.
The preparation of μ-SPE material bags
Polypropylene screen is used as to prepare μ-SPE material bags.The preparation process of μ-SPE material bags is as follows：By polypropylene screen ruler
It is very little to cut out to 1.4cm × 0.8cm, both sides are sealed long side doubling, and with plastic packaging machine, add in 5mg's in the side of opening
NZIF-8 as solid absorbent, post heat-seal opening.It prepares the μ-SPE material bags completed and is placed in methanol and be cleaned by ultrasonic 5min,
To remove pollution that may be present in preparation process, taking-up is placed in baking oven to dry and be sealed to be treated in Brown Glass Brown glass bottles and jars only
With.
VA-μ-SPE
μ-SPE material bags and 10ml mark-on water samples are put into togerther in the extraction vial of 15ml and are sealed first.Then
Extraction vial is placed on whirlpool instrument runs 5min with the rotating speed of 3000rpm, takes out μ-SPE material bags in vial and with lint-free
Paper wipes to suck residual moisture.Finally μ-SPE material bags are put into the gas chromatographic sample introduction bottle containing 300 μ l interpolation pipes, are added
Enter 80 μ l eluant, eluents and carry out ultrasound elution 5min, take out the μ-SPE material bags cleaning reuse in sample injection bottle, and the eluant, eluent of 1 μ l
It is injected into gas chromatograph and carries out quantitative analysis (every group parallel determination 3 times).
AA-μ-SPE
10ml mark-ons water sample, magneton and μ-SPE material bags are added in 15ml extraction flasks.Extraction flask is placed in magnetic stirring apparatus
It is extracted.After stirring, the μ-SPE material bags of extraction flask are taken out, are wiped to suck residual moisture with lint-free paper.Elution and
The process of analysis such as above-mentioned steps
VA-μ-SPE。
The detection of gas-chromatography
Gas chromatography-mass spectrum condition：Chromatographic column:DB-5MS capillary chromatographic columns, column length 30m, internal diameter 0.25mm.Carrier gas：
High-purity hydrogen；Flow velocity：1.8ml/min；220 DEG C of injector temperature；240 DEG C of detector temperature.Column temperature：40 DEG C of initial temperature stops
2min, 8 DEG C per minute are raised to 220 DEG C, finally stop 4min at 220 DEG C.
With reference to above-described embodiment 1, the investigation to some important factor in order in embodiment
(1) influence of eluant, eluent
In the factor for influencing extraction efficiency in research, the 5ng/ml during mass concentration of CBs constituent parts.It is in whirlpool instrument rotating speed
Under conditions of 3000rpm, extraction time 2min, elution time are 5min, investigation ethyl acetate, methanol and n-hexane, which are used as, to be washed
The elution effect of de- agent.As shown in Figure 1, when it is eluant, eluent to use n-hexane, the peak area of each CBs is maximum.So just oneself
Alkane is selected as the eluant, eluent of the experiment.
(2) influence of extraction time
For μ-SPE processes, mass transport process of the analyte from water sample to sorbing material is that the dynamic of a Time-Dependent is put down
Weighing apparatus process rather than a limit extractive process, so extraction time is also to influence one important factor of extraction efficiency.In whirlpool
Under conditions of whirlpool instrument rotating speed is 3000rpm, elution time 5min, eluant, eluent are n-hexane, extraction time has been investigated as 1-
Effect of extracting during 7min.From Figure 2 it can be seen that in 1-5min, the peak area of each CBs is increased over time and is gradually increased, in 5-
The peak area of 7min, CBs have the tendency that slightly decreasing, this is because a small amount of solution occurs after optimum extraction time for object
Analysis.In order to reach best effect of extracting, 5min is selected as optimum extraction time.
(3) influence of ultrasonic elution time
Similar with considering for extraction time, target molecule object is eluted from NZIF-8 to be also required to certain time and reaches de-
Attached dynamic equilibrium.Under conditions of whirlpool instrument rotating speed is 3000rpm, extraction time 5min, eluant, eluent are n-hexane, respectively
Investigated under different ultrasonic elution times (5,10,15,20min) each CBs elution profile.As seen from Figure 3, ultrasound elution 5min
Afterwards, the peak area response of CBs reaches maximum value, and extension at any time is only slightly fluctuated.The μ-SPE material bags of elution again
Be put into eluant, eluent ultrasound elution 5min, occur without apparent CBs peaks, illustrate after ultrasonic 5min, CBs substantially from
NZIF-8 is all eluted.
(4) comparison of VA- μ-SPE and AA- μ-SPE extraction results
AA- μ-SPE are the extraction process of traditional μ-SPE.As shown in figure 4, when extraction time is 5min, VA- μ-
The extraction of SPE approach performs clearly better than the AA- μ-SPE of AA- μ-SPE or even slightly above 30min.This result demonstrates VA-
μ-SPE are a kind of new and effective μ-SPE approaches, can effectively reduce the extraction time of traditional μ-SPE.
(5) influence of the solid extracting agent to extraction efficiency
The solid extracting agent C18 and C8 of commercialization are common μ-SPE solid extracting agents.It is being n-hexane in eluant, eluent,
Extraction time is 5min, under conditions of elution time is 5min, has investigated the effect of extracting of NZIF-8, C18, C8.It can from Fig. 5
See, the effect of extracting of NZIF-8 is substantially better than commercialization adsorbent C18 and C8.
(6) methodological study
In order to verify the reliability of trace CBs methods in the VA- μ-SPE water samples of NZIF-8, investigated respectively in eluant, eluent
For n-hexane, extraction time 5min, under conditions of elution time is 5min, the range of linearity of each CBs, is marked detection limit relatively
Quasi- deviation and repetitive rate (table 1).There is table 1 as it can be seen that in linearly ranging from 0.1-50ng/ml, the coefficient of determination (r2) be all higher than
0.991.Spiked levels are that the peak area relative standard deviation (RSD%) of the CBs5 parallel determination of 5ng/ml is below
8.4%.LODs define be signal-to-noise ratio be equal to 3 when mass concentration, be 0.002-0.008ng/ml, these results be better than EPA in
8121 methods (Y.He, Y.Wang, H.K.Lee, J.Chromatogr.A 874 (2000) 149), with headspace solid-phase microextraction
As a result quite.
The range of linearity of 1 method of table and regression equation, related coefficient, detection limit and standard deviation
(7) practicability of detection method is investigated
In order to evaluate the practicability of this method, the water sample for acquiring Yunnan Province Kunming Economic Development Zone river is detected.
The water sample of acquisition into filtering, does not carry out VA- μ-SPE directly, does not detect object, illustrate the river not by CBs
Pollution or content are less than the LODs of the detection method.In order to investigate the matrix effect of this method, the mark-on in actual water sample
Quantitative, addition is respectively 0.5 and 5ng/ml.For relative recovery between 87.9%-111.1%, RSD% is below 9.3%,
With preferable reproducibility.These results illustrate that this method has good application in actual water sample.
2 actual water sample mark-on of table (0.5ng/ml and 5ng/ml) testing result
Inventor extracts NZIF-8 (ZIF-8 and ZIF-4) applied to μ-SPE the organic micro-pollutant of environmental water sample,
Its effect of extracting is substantially better than the material (C18 and C8) of commercialization.The present invention is by NZIF-8 first Applications to CBs in μ-SPE
Extraction in, extract auxiliary μ-SPE (VA- μ-SPE) by being vortexed, the effective extraction time for reducing micro-extraction process, relatively
For the extraction time 30min of traditional μ-SPE (magnetic agitation assists (AA- μ-SPE)), effect greatly promotes.
Novel NZIFs provided by the invention combines GC-MS to the organic dirt of trace in environmental water sample by VA- μ-SPE
Contaminate the detection method of object CBs.Under the auxiliary of vortex instrument, μ-SPE optimum extraction times only need 5min, are effectively reduced
The extraction time of AA- μ-SPE is (usually>30min), and the wider, the preferable range of linearity (0.5-50mg/ of the degree of correlation is achieved
) and relatively low LODs (0.002-0.008ng/ml) ml.ZIFs is a kind of novel and multifunctional porous material, and this method will
The excellent performance of NZIF-8 is applied in μ-SPE, completes and works the sorption extraction of CBs in water sample, is applied for it in environment
The organic pollutant monitoring direction of water sample is laid a good foundation, and has effectively expanded applications of the ZIFs in sample pre-treatments.
Claims (8)
1. the assay method of chlorobenzene compound in a kind of environmental water sample, including sample pre-treatments and gas-chromatography detecting step,
It is characterized in that：The sample pre-treatments are micro- Solid Phase Extraction material bag to be protected to be placed in the extraction vial containing sample water sample film
In, vial will be extracted after sealing with whirlpool instrument with the rotating speed elution operation 1-7min of 2000~4000rpm, then takes material bag
Go out and be put into the gas chromatographic sample introduction bottle containing interpolation pipe, add in organic solvent ultrasound and elute 5~20min, the elution of formation
Liquid is gas chromatographic detection sample；The organic solvent is one or more of acetonitrile, ethyl acetate, methanol, n-hexane group
It closes.
2. the method as described in claim 1, it is characterised in that：The chlorobenzene compound is selected from 1,3- dichloro-benzenes（1,3-
DCB）, Isosorbide-5-Nitrae-dichloro-benzenes（1,4-DCB）, 1,2,4- trichloro-benzenes（1,2,4-TCB）, 1,2,4,5 ,-tetrachlorobenzene（1,2,4,5-
TeCB）One or more of combination.
3. method as claimed in claim 1 or 2, it is characterised in that：It is polypropylene screen that the film, which protects micro- Solid Phase Extraction material bag,
Solid absorbent is added in bag, drying is made；The solid absorbent is NZIF-8, C18 or C8.
4. method as claimed in claim 3, it is characterised in that：The solid absorbent NZIF-8 is made by following steps：
Zinc nitrate hexahydrate and 2-methylimidazole with methanol are dissolved, react at room temperature 0.5~2h, obtains muddy solution, centrifugation is received
Collection precipitation, methanol washing are subsequently placed in baking oven and had both been obtained in 70~90 °C of drying.
5. such as claim 1,2 or 4 any one of them methods, it is characterised in that：The sample pre-treatments is will be equipped with
The polypropylene screen bag of NZIF-8 is placed in the extraction vial containing sample water sample, after sealing will extraction vial with whirlpool instrument with
2000~4000rpm rotating speed elution operation 4-6min, then by material bag be removed and placed in the gas-chromatography containing interpolation pipe into
In sample bottle, add in organic solvent ultrasound and elute 3~20min, the eluent of formation is gas chromatographic detection sample；It is described organic molten
Agent is the combination of one or more of acetonitrile, ethyl acetate, methanol, n-hexane.
6. method as claimed in claim 3, it is characterised in that：The sample pre-treatments is will be equipped with the polypropylene screen of NZIF-8
Bag is placed in the extraction vial containing sample water sample, and vial will be extracted after sealing with whirlpool instrument with 2000~4000rpm's
Material bag, is then removed and placed in the gas chromatographic sample introduction bottle containing interpolation pipe, adds in organic by rotating speed elution operation 4-6min
Solvent supersonic elutes 5~10min, and the eluent of formation is gas chromatographic detection sample；The organic solvent is acetonitrile, acetic acid second
The combination of one or more of ester, methanol, n-hexane.
7. such as claim 1,2 or 4 any one of them methods, it is characterised in that：The sample pre-treatments is will be equipped with
The polypropylene screen bag of NZIF-8 is placed in the extraction vial containing sample water sample, after sealing will extraction vial with whirlpool instrument with
Material bag, is then removed and placed in the gas chromatographic sample introduction bottle containing interpolation pipe, adds in by the rotating speed operation 4-6min of 3000rpm
N-hexane ultrasound elutes 5~10min, and the eluent of formation is gas chromatographic detection sample.
8. the assay method of chlorobenzene compound in a kind of environmental water sample, including sample pre-treatments and gas-chromatography detecting step,
It is characterized in that：The sample pre-treatments are that the polypropylene screen bag equipped with NZIF-8 is placed in the extraction glass containing sample water sample
Vial will be extracted in bottle, after sealing, 5min is run with the rotating speed of 3000rpm with whirlpool instrument, take out the μ-SPE material in vial
Bag simultaneously is wiped to suck residual moisture with lint-free paper；The solid absorbent NZIF-8 is by zinc nitrate hexahydrate and 2-methylimidazole
It is dissolved with methanol, reacts at room temperature 0.5~2h, obtain muddy solution, precipitation is collected by centrifugation, methanol washing is subsequently placed in baking oven
In 70~90 °C drying be made；Finally μ-SPE material bags are put into the gas chromatographic sample introduction bottle containing interpolation pipe, add in just oneself
Alkane ultrasound elutes 5min, and the eluent of formation is gas chromatographic detection sample；The testing conditions are gas chromatography-mass spectrum item
Part：Chromatographic column:DB-5MS capillary chromatographic columns, column length 30m, internal diameter 0.25mm；Carrier gas：Hydrogen；Flow velocity：1.8ml/min；Sample introduction
220 °C of temperature of mouth；240 °C of detector temperature；Column temperature：40 °C of initial temperature stops 2min, and 8 °C per minute are raised to 220 °C, finally exist
220 °C of stop 4min.
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| CN109613155A (en) * | 2018-11-29 | 2019-04-12 | 同济大学 | A kind of detection method of armaticity nitrogenous disinfection byproducts |
| CN111796040A (en) * | 2020-07-14 | 2020-10-20 | 南京海关工业产品检测中心 | Method for separating isomeride chlorobenzene and toluene chloride by adopting gas chromatography-mass spectrometry |
| CN116754348A (en) * | 2023-06-06 | 2023-09-15 | 华北理工大学 | ZIF-8-90 material-based effervescent tablet, preparation method and application thereof |
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| CN116754348B (en) * | 2023-06-06 | 2024-03-08 | 华北理工大学 | ZIF-8-90 material-based effervescent tablet, preparation method and application thereof |
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