CN110118840A - The measuring method of organic amine in a kind of atmosphere PM2.5 - Google Patents

The measuring method of organic amine in a kind of atmosphere PM2.5 Download PDF

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CN110118840A
CN110118840A CN201910494552.5A CN201910494552A CN110118840A CN 110118840 A CN110118840 A CN 110118840A CN 201910494552 A CN201910494552 A CN 201910494552A CN 110118840 A CN110118840 A CN 110118840A
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organic amine
standard
amine
bottle
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朱济奇
冯加良
毛文文
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University of Shanghai for Science and Technology
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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
    • G01N2030/042—Standards
    • G01N2030/045—Standards internal
    • 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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  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
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Abstract

The invention discloses a kind of measuring methods of organic amine in Atmospheric particulates, comprising steps of S1. standard solution is prepared；S2. sample pre-treatments；S3. derivatization；S4. extracting concentration；S5. quantification and qualification；The present invention establishes a kind of method for quickly, simply measuring amine substance in Atmospheric particulates.This method derivatization process is not necessarily to add other reagents as catalyst, stirring at normal temperature need to only can be completed under alkaline condition, time saving and easy to operate.Present invention optimizes temperature programs, and the qualitative and quota ion of 6 kinds of aromatic amines (methylamine, dimethylamine, ethamine, diethylamine, propylamine, butylamine) has been determined, and this method is applied to the measurement of amine substance in real atmosphere particulate matter, technical support is provided further to carry out the research of organic amine physical environment behavior in aerosol.

Description

The measuring method of organic amine in a kind of atmosphere PM2.5
Technical field
The present invention relates to Atmospheric Chemistry analysis fields, and in particular to the measuring method of organic amine in a kind of atmosphere PM2.5.
Background technique
Organic amine pollutant is a subset of water soluble organic nitrogen (WSON), because its have influence new particle formed and The potentiality of cloud chemistry receive more and more attention in recent years.Organic amine is the alkaline gas being widely present in atmosphere, is had only Special acid neutralization capacity, but since the lower source of abundance is complicated and the atmosphere residence time compared with short-range missile causes its thermodynamics and kinetics The more difficult acquisition of matter.The low-molecular weight amines being primarily present in atmosphere vapour pressure with higher and high water solubility, Neng Gouying Ring the hygroscopicity of aerosol.Amine is by alkyl or aryl by replacing the hydrogen atom on amino molecule to generate, therefore amine has and ammonia The properties such as the same strong alkaline water dissolubility.Research finds that the content of amine in atmosphere is up to the 14-23% of ammonia, and gaseous state aliphatic amine is big It can be with acidic components (HCl, HNO in gas3, H2SO4) acyl group reaction quickly occurs, salt particle is formed, into particulate form.
New particle generates the main source of (NPF) as particulate in atmosphere, and it is flat may to significantly affect global radiation Weighing apparatus and climate change.Scientific research personnel is observed during NPF event containing a large amount of amine salt in nano particle (8-10nm), than hair Existing amine can significantly facilitate new particle to be formed.The process that acid-base reaction forms ammonium salt facilitates particulate form organic amine shape in atmosphere At: organic amine replaces ammonia from ammonium salt or neutralizes hydrosulphate, by the growth for participating in new particle at salt.
Just by the serious pollution of fine particle, partly cause is that its Fossil fuel consumption increases sharply and dioxy for China Change a large amount of discharges of sulphur and nitrogen oxides.Scientific research personnel confirms that a series of serious city haze events are by NPF and particle Sustainable growth caused by；In North China and Yangtze River Delta high pollution event, effect of the sulfate in NPF is obtained Pay attention to.However, as far as we know, there is not been reported for the feature of particle amine during NPF event.
Organic amine is prevalent in atmospheric environment, especially low molecular weight fatty amine, detection frequency in an atmosphere and Concentrations are higher.But it low molecular weight fatty amine high volatility, absorbs without ultraviolet and unstressed configuration, and polarity is strong, in an atmosphere Concentration is low, atmosphere substrate is complicated, therefore measure atmosphere PM2.5Middle organic amine is more difficult.Organic amine in measurement atmosphere at present Common method has liquid chromatography, liquid chromatography mass spectrometric method, gas chromatography, mass spectrometer and the chromatography of ions.Wherein, gas phase color The sensitivity of spectrometry and the chromatography of ions is lower, and more difficult is kept completely separate that molecular weight is low and the more similar organic amine of structure；Liquid Though the sensitivity with higher of phase mass spectrography, higher cost, easily residual and it is more demanding to operator；Liquid chromatography and Mass spectrometer is the current measurement more common method of atmosphere organic amine, but all needs to reduce target compound by derivative Polarity, the selectivity and sensitivity for improving target compound, and reported deriving method is often cumbersome, derives the time It is long, and poor reproducibility.
Summary of the invention
It is an object of the invention to overcome the above deficiencies in the existing technologies, and providing has in a kind of atmosphere PM2.5 The measuring method of machine amine.Realize under the conditions of derivative, it is sensitive, accurately batch measurement Atmospheric particulates in methylamine, dimethylamine, Six kinds of ethamine, diethylamine, propylamine and butylamine organic amines.
Technical solution used by the present invention solves the above problems is:
The measuring method of organic amine in a kind of atmosphere PM2.5, it is characterised in that: the following steps are included:
The preparation of step 1. standard solution: organic amine is mixed into standard liquid (methylamine, dimethylamine, ethamine, diethyl with ultrapure water Amine, propylamine, butylamine) be formulated as the mixing standard liquid of 100 μ g/ml (ppm) of 50ml, the mixed mark of 100ppm is diluted to 0.05,0.1,1, 2,5,10ppm；
Step 2. sample pre-treatments: interception 15cm2Sampling membrane pipettes certain Milli-Q water, ice in 30ml ultrasound bottle Water bath sonicator extracts 30min, is repeated 3 times, and control Milli-Q water inventory is 20ml, obtains sample solution, meanwhile, take same batch Blank quartz filter and sample carry out pre-treatment simultaneously, obtain blank sample solution；
Step 3. derivatization: it takes 1ml standard liquid in 30ml ultrasound bottle respectively, 9ml ultrapure water, 800 μ l 10mol/ is added LNaOH solution, the 20 deuterated standard specimens of μ l20ppm (dimethylamine-d6), 300 μ l derivatization reagents (benzene sulfonyl chloride, BSC) seal room temperature Lower magnetic agitation 30min；The same standard liquid of sample solution；
Step 4. stirring terminates, and 800 μ l 10mol/LNaOH solution are added in continuation in ultrasonic bottle, seals, in 80 DEG C of items Magnetic agitation 30min under part；
Step 5. reaction terminates, and ultrasonic bottle is placed in ice water and is slowly cooled to room temperature, is adjusted to pH=with 36.5%HCl 5.5；
Step 6. extracts organic phase (3 times) with 3ml methylene chloride, and organic phase is collected in chicken heart bottle, 3mL is used 0.05mol/l Na2CO3Solution washs organic phase, uses anhydrous Na2SO4It is dry, subsequent rotary evaporation to about 1mL；
Concentrate is transferred in 4ml sample injection bottle by step 7., in soft N2It flows down to be blown to and closely do, add 20 μ l 50ppm internal standards (hexamethylbenzene), n-hexane hydrocarbon are settled to 500 μ l, and 2 μ l is then taken to carry out GC-MS analysis,
Step 8. instrument condition: sample analysis instrument is Agilent gas chromatograph-mass spectrometer (GC-MS) (6890/ 5975, GC/MS), chromatographic column is DB-5MS column (30m × 0.25mm × 0.25 μm), and carrier gas is high-purity He, injector temperature 290 DEG C, gas-matter transmission line temperature: 290 DEG C；Splitless injecting samples, flow: 1.56mL/min；2 μ L of sample volume, temperature program: prerun 5min, 80 DEG C of initial temperature (1min), 5 DEG C/min → 180 DEG C, 10 DEG C/min → 240 DEG C, 25 DEG C/min → 290 DEG C (10min), 230 DEG C of ion source temperature, mass spectrum mass scan range m/z:50-450, EI ion source, 70eV, full scan mode,
Step 9. qualitative analysis: when the reservation of the retention time of target compound and organic amine standard solution in sample solution Time error then contains organic amine in judgement sample within 5%, and when fragment ion is consistent；
Step 10. quantitative analysis: when the mixed standard solution for being continuously 1 μ g/ml into nine concentration, target compound is obtained Retention time and the relative standard deviation of peak area be respectively less than 5%；The standard curve of each target compound has good Linearly, and when the rate of recovery of sample mark-on is within the scope of 80-120%, then it is assumed that the measuring method is suitable for PM2.5In it is organic The measurement of amine.
Compared with prior art, the present invention having the following advantages that and effect:
(1) present invention establishes a kind of method for quickly, simply measuring amine substance in Atmospheric particulates, and this method is derivative Change process stirring at normal temperature need to only can be completed, time saving and operation under alkaline condition without adding other reagents as catalyst Simply.
(2) present invention optimizes temperature programs, and 6 kinds of aromatic amines (methylamine, MA have been determined；Dimethylamine, DMA；Ethamine, EA；Two Ethamine, DEA；Propylamine, PA；Butylamine, BA) qualitative and quota ion, and by this method be applied to real atmosphere particulate matter in amine The measurement of substance provides technical support further to carry out the research of organic amine physical environment behavior in aerosol.
Detailed description of the invention
Fig. 1 is measurement of embodiment of the present invention atmosphere PM2.5Determine the general flow chart of method in the side of middle organic amine；
Fig. 2 is six kinds of organic amine standard specimen working curve diagrams in the embodiment of the present invention；
Fig. 3 is that organic amine derives schematic diagram in the embodiment of the present invention；
Fig. 4 is the chromatogram of organic amine mixed standard solution in the embodiment of the present invention；
Fig. 5 is the chromatogram of atmospheric aerosol samples in the embodiment of the present invention.
Specific embodiment
The present invention is described in further detail with reference to the accompanying drawing and by embodiment, and following embodiment is to this hair Bright explanation and the invention is not limited to following embodiments.
Referring to Fig. 1, the measuring method of trace organic amine in a kind of Atmospheric particulates of the present embodiment the present embodiment, including it is following
Step:
A. the preparation of standard solution；With ultrapure water by organic amine mix standard liquid (methylamine, dimethylamine, ethamine, diethylamine, third Amine, butylamine) be formulated as the mixing standard liquid of 100 μ g/ml (ppm) of 50ml, the mixed mark of 100ppm is diluted to 0.05,0.1,1,2,5, 10ppm；
B. sample pre-treatments；Intercept 15cm2Sampling membrane pipettes certain Milli-Q water, ice-water bath in 30ml ultrasound bottle Ultrasonic extraction 30min, is repeated 3 times, and control Milli-Q water inventory is 20ml, obtains sample solution.It is dry to verify possible local It disturbs and artificial pollution, takes that the blank quartz filter of same batch carries out pre-treatment as blank sample and sample simultaneously and upper machine is surveyed Examination.Through analyzing, all target compounds are not detected in blank film and blank solvent, show the entire reality including sampling Process is tested all not by local interference and artificially-contaminated influence；
C. derivatization；It takes 1ml standard liquid in 30ml ultrasound bottle respectively, 9ml ultrapure water is added, 800 μ l 10mol/LNaOH are molten Liquid, the 20 deuterated standard specimens of μ l20ppm (dimethylamine-d6), 300 μ l derivatization reagents (benzene sulfonyl chloride, BSC) seal magnetic force under room temperature and stir Mix 30min；The same standard liquid of sample solution；
D. stirring terminates, and 800 μ l 10mol/LNaOH solution are added in continuation in ultrasonic bottle, seals, under the conditions of 80 DEG C Magnetic agitation 30min；
E. reaction terminates, and ultrasonic bottle is placed in ice water and is slowly cooled to room temperature, is adjusted to pH=5.5 with 36.5%HCl；
F. organic phase (3 times) are extracted with 3ml methylene chloride, organic phase is collected in chicken heart bottle.With 3mL 0.05mol/ lNa2CO3Solution washs organic phase, uses anhydrous Na2SO4It is dry, subsequent rotary evaporation to about 1mL；
G. concentrate is transferred in 4ml sample injection bottle, in soft N2It flows down to be blown to and closely do, add 20 μ l 50ppm internal standards (six Methylbenzene), n-hexane hydrocarbon is settled to 500 μ l, and 2 μ l is then taken to carry out GC-MS analysis.
H. instrument condition: sample analysis instrument is Agilent gas chromatograph-mass spectrometer (GC-MS) (6890/5975, GC/ ), MS chromatographic column be DB-5MS column (30m × 0.25mm × 0.25 μm), carrier gas be high-purity He, 290 DEG C of injector temperature, gas-matter Transmission line temperature: 290 DEG C；Splitless injecting samples, flow: 1.56mL/min；2 μ L of sample volume.Temperature program: prerun 5min, just 80 DEG C of beginning temperature (1min), 5 DEG C/min → 180 DEG C, 10 DEG C/min → 240 DEG C, 25 DEG C/min → 290 DEG C (10min).Ion source 230 DEG C of temperature, mass spectrum mass scan range m/z:50-450, EI ion source, 70eV, full scan mode.
I. qualitative analysis: when the retention time of the retention time of target compound and organic amine standard solution in sample solution Error then contains organic amine in judgement sample within 5%, and when fragment ion is consistent；
J. quantitative analysis: when the mixed standard solution for being continuously 1 μ g/ml into nine concentration, the guarantor of target compound is obtained The relative standard deviation of time and peak area is stayed to be respectively less than 5%；The standard curve of each target compound have it is good linear, And when the rate of recovery of sample mark-on is within the scope of 80-120%, then it is assumed that the measuring method is suitable for PM2.5The survey of middle organic amine It is fixed.
According to the response of organic amine standard sample and internal standard mellitene that concentration gradient is 0.05,0.1,1,2,5,10ppm Obtain standard curve.If linear good, this standard specimen can be used to draw working curve (for quantitative), by Fig. 2, it is known that six kinds organic Amine standard specimen is linearly good, demonstrates the reliability of method.The measurement of organic amine is as shown in Figure 4 and Figure 5, and Fig. 4 is 5ppm organic amine The chromatographic curve of mixed standard solution, Fig. 5 are atmosphere PM2.5The chromatographic curve of organic amine in sample, number respectively represents on curve Each organic amine target compound: 1. mellitenes；2. dimethylamine-d6；3. dimethylamine；4. methylamine；5. ethamine；6. diethylamine；7. third Amine；8. butylamine；It can be seen that the measuring method of offer of the invention is smaller relative to standard deviation, it can Accurate Determining Atmospheric particulates Middle organic amine content.
Above content is only illustrations made for the present invention described in this specification.Technology belonging to the present invention The technical staff in field can make various modifications or additions to the described embodiments or by a similar method Substitution, content without departing from description of the invention or beyond the scope defined by this claim should belong to this The protection scope of invention.

Claims (1)

1. the measuring method of organic amine in a kind of atmosphere PM2.5, it is characterised in that: the following steps are included:
The preparation of step 1. standard solution: with ultrapure water by organic amine mix standard liquid (methylamine, dimethylamine, ethamine, diethylamine, third Amine, butylamine) be formulated as the mixing standard liquid of 100 μ g/ml (ppm) of 50ml, the mixed mark of 100ppm is diluted to 0.05,0.1,1,2,5, 10ppm；
Step 2. sample pre-treatments: interception 15cm2Sampling membrane pipettes certain Milli-Q water, ice-water bath in 30ml ultrasound bottle Ultrasonic extraction 30min, is repeated 3 times, and control Milli-Q water inventory is 20ml, obtains sample solution, meanwhile, take the sky of same batch Crystobalite filter membrane and sample carry out pre-treatment simultaneously, obtain blank sample solution；
Step 3. derivatization: it takes 1ml standard liquid in 30ml ultrasound bottle respectively, 9ml ultrapure water is added, 800 μ l 10mol/LNaOH are molten Liquid, the 20 deuterated standard specimens of μ l20ppm (dimethylamine-d6), 300 μ l derivatization reagents (benzene sulfonyl chloride, BSC) seal magnetic force under room temperature and stir Mix 30min；The same standard liquid of sample solution；
Step 4. stirring terminates, and 800 μ l 10mol/L NaOH solutions are added in continuation in ultrasonic bottle, seals, under the conditions of 80 DEG C Magnetic agitation 30min；
Step 5. reaction terminates, and ultrasonic bottle is placed in ice water and is slowly cooled to room temperature, is adjusted to pH=5.5 with 36.5%HCl；
Step 6. extracts organic phase (3 times) with 3ml methylene chloride, organic phase is collected in chicken heart bottle, with 3mL 0.05mol/l Na2CO3Solution washs organic phase, uses anhydrous Na2SO4It is dry, subsequent rotary evaporation to about 1mL；
Concentrate is transferred in 4ml sample injection bottle by step 7., in soft N2It flows down to be blown to and closely do, add 20 μ l 50ppm internal standard (pregnancy Base benzene), n-hexane hydrocarbon is settled to 500 μ l, and then take 2 μ l to carry out GC-MS analysis,
Step 8. instrument condition: sample analysis instrument is Agilent gas chromatograph-mass spectrometer (GC-MS) (6890/5975, GC/ ), MS chromatographic column be DB-5MS column (30m × 0.25mm × 0.25 μm), carrier gas be high-purity He, 290 DEG C of injector temperature, gas-matter Transmission line temperature: 290 DEG C；Splitless injecting samples, flow: 1.56mL/min；2 μ L of sample volume, temperature program: prerun 5min, just 80 DEG C of beginning temperature (1min), 5 DEG C/min → 180 DEG C, 10 DEG C/min → 240 DEG C, 25 DEG C/min → 290 DEG C (10min), ion source 230 DEG C of temperature, mass spectrum mass scan range m/z:50-450, EI ion source, 70eV, full scan mode,
Step 9. qualitative analysis: when the retention time of the retention time of target compound and organic amine standard solution in sample solution Error then contains organic amine in judgement sample within 5%, and when fragment ion is consistent；
Step 10. quantitative analysis: when the mixed standard solution for being continuously 1 μ g/ml into nine concentration, the guarantor of target compound is obtained The relative standard deviation of time and peak area is stayed to be respectively less than 5%；The standard curve of each target compound have it is good linear, And when the rate of recovery of sample mark-on is within the scope of 80-120%, then it is assumed that the measuring method is suitable for PM2.5The survey of middle organic amine It is fixed.
CN201910494552.5A 2019-06-10 2019-06-10 The measuring method of organic amine in a kind of atmosphere PM2.5 Withdrawn CN110118840A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113009038A (en) * 2021-03-09 2021-06-22 广东工业大学 Analysis method for simultaneously collecting and detecting gas-phase and particle-phase organic amine in atmospheric environment
CN115078589A (en) * 2022-07-15 2022-09-20 贵州省烟草科学研究院 Chromatographic analysis method for amine additive in biodegradable mulch film

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113009038A (en) * 2021-03-09 2021-06-22 广东工业大学 Analysis method for simultaneously collecting and detecting gas-phase and particle-phase organic amine in atmospheric environment
CN115078589A (en) * 2022-07-15 2022-09-20 贵州省烟草科学研究院 Chromatographic analysis method for amine additive in biodegradable mulch film
CN115078589B (en) * 2022-07-15 2023-11-21 贵州省烟草科学研究院 Chromatographic analysis method for amine additives in biodegradable mulch film

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Application publication date: 20190813