CN108760925A - Humic-like substance separation method and its content assaying method in a kind of Atmospheric particulates - Google Patents
Humic-like substance separation method and its content assaying method in a kind of Atmospheric particulates Download PDFInfo
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Abstract
The present invention provides a kind of methods of humic-like substance (Humic-like substance, HULIS) and its carbon component (HULIS-C) in detection Atmospheric particulates.After HULIS component ultrasonic cryogenics in particulate matter are dissolved into ultra-pure water by this method, it is added in the solid-phase extraction column of pre-balance and activation after absorbing and filter, a small amount of pure water is added into column and removes the substance not adsorbed, elution is added to go out HULIS components into column again, last nitrogen drying, pure water constant volume measures the concentration of HULIS-C and HULIS using the total organic carbon analyzer of combustion oxidation non-dispersion infrared absorption process and the high performance liquid chromatograph with evaporative light scattering detector.
Description
Technical field
The present invention relates to the specific organic component detection methods of Atmospheric particulates, and in particular in a kind of detection Atmospheric particulates
The method of humic-like substance and its carbon component.
Background technology
Water Soluble Organic Carbon (Water-Soluble Organic Carbon, WSOC) is the important set in atmospheric aerosol
At part, complicated component is mainly made of acid and neutral polar organic matter.The sources WSOC mainly have burning etc. primary next
Source and the secondary source generated through photochemical reaction with atmospheric substance, WSOC can increase the hygroscopicity of particulate matter, and be easy to and carefully
Little particle combines and forms the nuclei of condensation, plays an important role to the formation of gray haze.Compound structure containing some macromoleculars in WSOC
At important component because the component have physicochemical characteristics similar with humic acid and fulvic acid (as it is water-soluble, acid,
Polarity etc.), so being referred to as humic-like substance (Humic-like substances, HULIS), carbon content is known as HULIS-C.
Studies have found that HULIS-C accounts for the 40-60% or so of WSOC mass.HULIS is mainly derived from biomass combustion, vehicle exhaust
And the isoprene and terpene compound of plant discharging pass through the secondary generation of heterogeneous reaction.HULIS is strong water-soluble due to it
Property and surface-active, play an important role, including light absorptive, hygroscopicity, cloud condense into nuclearity and to gas in Atmospheric processes
Wait the influence with radiation balance.The source of HULIS and the influence to air in air are obtained, first has to accurately detect that it contains
Amount.HULIS includes abundant functional group, it is difficult to directly measure the concentration of each substance in HULIS by certain method.
The country not yet promulgates the quantitative detecting method in relation to humic-like substance compound in Atmospheric particulates at present, only there are two
Patent is related to HULIS.First, Changzhou University discloses a kind of being detected containing carbon ratio for water-soluble humic-like substance aerosol (HULIS)
Method determines carbon component (the publication No. CN in HULIS using the hot light carbon reflectometer (OC/EC analyzers) of Sunset companies
106093259 A)；Another is exactly that China Environmental Science Research Institute discloses a kind of analysis different molecular weight humic-like substance function
The method (publication No. CN104458997 A) of group's composition.The invention discloses humic-like substance in a kind of detection Atmospheric particulates and
The method of its carbon component, after the HULIS components in particulate matter are extracted by Solid Phase Extraction, using total organic carbon analyzer to air
HULIS-C is analyzed in particulate matter, and evaporative light-scattering instrument is detected HULIS concentration.
To sum up, the separation and detection method about humic-like substance in Atmospheric particulates and its method of carbon component domestic at present
There is not been reported.The announcement of the method can be used for analyzing the analysis of HULIS and HULIS-C in not homologous Atmospheric particulates, be
Atmosphere pollution detection and source analysis lay the foundation.
Invention content
The present invention solves the deficiency of the existing existing detection technique of Atmospheric particulates feature organic component, provides a kind of inspection
Survey the method for humic-like substance and its carbon component in Atmospheric particulates.
The present invention provides a kind of detection method of humic-like substance in Atmospheric particulates, and this method comprises the steps of：
(1) sample collection：Use band PM2.5The big flow of cutter or middle traffic sampling device acquire Atmospheric particulates, take receipts
The filter membrane of collection Atmospheric particulates is set in pure water, ultrasonic extraction, and extracting solution filtering, constant volume obtains sample lysate；
(2) Solid Phase Extraction：By sample lysate obtained by step (1), it is adjusted with acid pH=2, preactivated and balance is added
Solid-phase extraction column in extract, first plus pure water eluted, eluent discards, then is eluted with eluant, eluent, collect eluent；
(3) prepared by sample solution：Eluent obtained by step (2) is subjected to liquid nitrogen drying, being settled to brown with pure water holds
In measuring bottle, -20 DEG C of preservations obtain sample solution；
(4) Specification Curve of Increasing：Matched with pure water and is set to 0, the SRFA standard solution of 1,5,10,25,75 μ g/mL, with efficient liquid
Phase chromatographic tandem evaporative light-scattering instrument is measured, and draws the relationship between signal-concentration, and standard curve is made；
(5) chromatographic condition：Chromatographic column is C18Column, mobile phase are acetonitrile-water 20-80, flow velocity 0.6mL/min, sample introduction body
Product is 60 μ L；ELSD setup parameters are as follows：Use N2As carrier gas, flow velocity 1.5L/min, 80-90 DEG C of drift tube temperature, GAIN
It is set as 6；The sample solution prepared to step (3) with high performance liquid chromatography cascade evaporation light scattering apparatus is detected, according to
SRFA standard curves are quantified, and the concentration of humic-like substance is measured.
Filter membrane described in preferred step (1) of the present invention is quartz fibre filter membrane, filter membrane using being preceding put into Muffle furnace,
5h is toasted at 450 DEG C, is removed organic principle, is sealed in constant temperature and humidity drying case after being put with aluminum foil sealing；Described is super
The time of sound extraction is 45-60min；The method of extracting solution filtering is：With the syringe filter filtering in 0.45 μm of aperture, move
Except suspension and insoluble particulate matter.
The hydrochloric acid that acid described in preferred step (2) of the present invention is 2mol/L.
Solid Phase Extraction described in preferred step (2) of the present invention is lived as reverse phase hydrophilic lipophilicity column, non-polar hydrophobic C18
Any one in column or nonionic macroreticular resin.
Preferably step (2) of the present invention is：By sample lysate obtained by step (1), it is adjusted with acid pH=2, is added advance
It is extracted in the reverse phase hydrophilic lipophilicity solid-phase extraction column of activation and balance, first plus pure water is eluted, and eluent discards, then uses body
Product is than being 2% ammonium hydroxide methanol solution.
Preferably step (2) of the present invention is：By sample lysate obtained by step (1), it is adjusted with acid pH=2, is added advance
The non-polar hydrophobic C of activation and balance18It is extracted in solid-phase extraction column, first plus pure water is eluted, and eluent discards, then uses first
Alcohol elutes, and collects eluent.
Preferably step (2) of the present invention is：By sample lysate obtained by step (1), it is adjusted with acid pH=2, is added advance
It is extracted in the nonionic macroreticular resin solid-phase extraction column of activation and balance, first plus pure water is eluted, and eluent discards, then uses
Volume ratio is 6:4 methanol-water solution is eluted, and eluent is collected.
The present invention also provides the detection method of carbon content in humic-like substance in a kind of Atmospheric particulates, this method is：It presses
According to humic-like substance detection method the step of (1) to (3) prepare sample solution, be detected class humic with the analyzer of TOC-L
Carbon content in matter.The parameter that the analyzer of the TOC-L is detected carbon content in humic-like substance is：Shimadzu total organic carbon is analyzed
Instrument TOC-L, with oxidizing fire infrared analysis, a certain amount of water sample is injected separately into 680 DEG C of high temperature for filling oxidation catalyst
In combustion tube and low-temp reaction pipe, the water sample in high-temperature combustion tube is turned by high-temperature S removal, organic carbon and inorganic carbonate
It is melted into CO2；Water sample in low-temp reaction pipe is made inorganic carbonate resolve into CO by the acidification of hydrochloric acid2, the carbon dioxide of the two generation
Non-dispersive infrared NDIR detectors are imported successively, measure total carbon TC in water respectively and inorganic carbon IC, difference are as water-soluble
Potassium Hydrogen Phthalate, sodium bicarbonate and sodium carbonate are selected in the preparation of property organic carbon WSOC, TC, IC standard solution respectively, and
The r of standard curve2Reach 0.999 or more, apparatus measures range：4 μ g/L-30000 μ g/L, detection are limited to：4 μ g/L carrier gas：
Compressed air or oxygen, carrier gas supply pressure：200 ± 10kPa, carrier gas flux：150mL/min.
After the present invention is by optimizing extraction conditions and sample detection condition, this method is used for Atmospheric particulates
Minimum detectability when HULIS concentration mensurations is 0.5-0.7mg/L, corresponds to concentration (sampling 20h, sampling volume in air
1200m3) it is 5.0-7.0 μ g/m3；The minimum detectability of HULIS-C is 0.3-0.6mg/L, a concentration of (sampling in corresponding air
20h, sampling volume 1200m3)0.1-0.3μg/m3, relative standard deviation 2.0-6.3%.
Description of the drawings
Fig. 1：Real atmosphere PM2.5The HPLC spectrograms of sample HULIS concentration mensurations
Fig. 2：The HPLC spectrograms of standard substance Sa Wang mud river fulvic acid (SRFA)
Fig. 3：Evaporative light-scattering method measures the standard curve of SRFA
Specific implementation mode
Embodiment 1：Air PM2.5HULIS method for measurement of concentration in particle, includes the following steps：
(1) sample collection：Using big flow sampler (KB-1000 types, Qingdao Electronic Science and Technology Co., Ltd. of Kingstar) with
1.05m3/ min flows acquire PM in two sampled points2.5Sample is to quartz filter (20.3cm × 25.4cm, Whatman QM-
A on), continuous acquisition 7 days acquires 20h daily.Before sampling, quartz filter is pre-placed 500 DEG C of degree roasting 4h of Muffle furnace, places
48h is balanced in constant temperature and humidity drying device (22 DEG C of temperature, humidity 45%), the balance for being 0.01mg with precision is weighed, then used
Aluminium foil encapsulation be stored in -20 DEG C of low temperature refrigerators preserve it is to be analyzed.The flow of sampler is corrected before spot sampling, according to
It is secondary to install filter membrane clip, adsorbent sleeve, it is connected to sampler, sampling flow is adjusted, starts to sample.It opens and adopts after sampling
Filter membrane clip on sample head gently removes filter membrane with tweezers, samples towards inner doubling, be placed in previously baked good aluminium foil and protect
It deposits.Same method collection site blank sample.Acquire blank sample when, in addition to not starting sampling instrument, remaining operation with
The sampling operation process of actual sample is identical.The filter membrane of particle concentrations object sample will be cut into 4 or 8 with ceramic scissors
Equal portions gather according to sampling quantity and filter membrane size selection 1/8,1/4,1/2 or whole filter membrane, the high density that filter membrane is placed in 60mL
Ethylene sample bottle is added 50mL ultra-pure waters, sample bottle is placed in ultrasonic cleaner, and adds packed ice cube in wherein, low
Temperature extraction 60min.The syringe filter extracted by filtration liquid in 0.45 μm of aperture is selected, removes and suspends and insoluble particulate matter, transfer
Into 50mL volumetric flasks, sample lysate is obtained.
(2) Solid Phase Extraction：Take the half of sample lysate 50mL solution obtained by step (1) with the hydrochloric acid tune pH of 2mol/L extremely
It after 2, is added in the HLB solid-phase extraction columns for having activated and having balanced, the adjustment rate of filtration is 2mL/min, to be filtered to finish, into column
2mL pure water is added and removes the inorganic or organic matter not adsorbed, then, it is that 2% ammonium hydroxide methanol is molten that 3mL volume ratios are added into column
Liquid elutes target compound (HULIS), obtains eluent.
(3) sample concentration：Eluent obtained by step (2) is subjected to liquid nitrogen drying, 1mL or so pure water is added, quantitatively arrives
1.5mL is transferred in the brown liquid chromatogram sample bottle of 2mL, and -20 DEG C of preservations of temperature obtain sample solution, to be analyzed.
(4) Specification Curve of Increasing：Matched with pure water and is set to 0, the SRFA standard solution of 1,5,10,25,75 μ g/mL, with efficient liquid
Phase chromatography (LC-2030C 3D, Shimadzu) cascade evaporation light scattering apparatus (ELSD-LT II, Shimadzu) measures its concentration.Draw signal-
Relationship between concentration obtains standard curve.
(5) chromatographic condition：With the HPLC with ESLD detectors to HULIS quantitative analyses, chromatographic column C18Column, mobile phase are
Acetonitrile-water 20-80, flow velocity 0.6mL/min, sampling volume are 60 μ L；ELSD setup parameters are as follows：Use N2As carrier gas,
Flow velocity 1.5L/min, 80-90 DEG C of drift tube temperature, GAIN is set as 6；With high performance liquid chromatography cascade evaporation light scattering apparatus to step
Suddenly the sample solution that prepared by (3) is detected, and is quantified according to SRFA standard curves, and PM is measured2.5Middle humic-like substance it is dense
Degree, the results are shown in Table 1.
2 TOC of embodiment measures air PM2.5Middle HULIS-C concentration methods include the following steps：
(1) sample collection：Using big flow sampler (KB-1000 types, Qingdao Electronic Science and Technology Co., Ltd. of Kingstar) with
1.05m3/ min flows acquire PM in two sampled points2.5Sample is to quartz filter (20.3cm × 25.4cm, Whatman QM-
A on), continuous acquisition 7 days acquires 20h daily.Before sampling, quartz filter is previously positioned at 500 DEG C of degree roasting 4h of Muffle furnace, puts
It sets and balances 48h in constant temperature and humidity drying device (22 DEG C of temperature, humidity 45%), the balance for being 0.01mg with precision is weighed, then
With aluminium foil encapsulation be stored in -20 DEG C of low temperature refrigerators preserve it is to be analyzed.The flow of sampler is corrected before spot sampling,
Filter membrane clip, adsorbent sleeve are installed successively, is connected to sampler, are adjusted sampling flow, are started to sample.It is opened after sampling
Filter membrane clip on sampling head gently removes filter membrane with tweezers, samples towards inner doubling, be placed in previously baked good aluminium foil and protect
It deposits.Same method collection site blank sample.Acquire blank sample when, in addition to not starting sampling instrument, remaining operation with
The sampling operation process of actual sample is identical.The filter membrane of particle concentrations object sample will be cut into 4 or 8 with ceramic scissors
Equal portions gather according to sampling quantity and filter membrane size selection 1/8,1/4,1/2 or whole filter membrane, the high density that filter membrane is placed in 60mL
Ethylene sample bottle is added 50mL ultra-pure waters, sample bottle is placed in ultrasonic cleaner, and adds packed ice cube in wherein, low
Temperature extraction 60min.The syringe filter extracted by filtration liquid in 0.45 μm of aperture is selected, removes and suspends and insoluble particulate matter, transfer
Into 50mL volumetric flasks, sample lysate is obtained.
(2) Solid Phase Extraction：Take the half of sample lysate 50mL solution obtained by step (1) with the hydrochloric acid tune pH of 2mol/L extremely
It after 2, is added in the HLB solid-phase extraction columns for having activated and having balanced, the adjustment rate of filtration is 2mL/min, to be filtered to finish, into column
2mL pure water is added and removes the inorganic or organic matter not adsorbed, then, it is that 2% ammonium hydroxide methanol is molten that 3mL volume ratios are added into column
Liquid elutes target compound (HULIS), obtains eluent.
(3) sample concentration：Eluent obtained by step (2) is subjected to liquid nitrogen drying, pure water constant volume is added to 25mL, transfer
Sample after to constant volume is transferred to progress HULIS-C measurement in the sample injection bottle of Shimadzu, and the instrument used is the model of Shimadzu
TOC-VCPHAnalyzer, with oxidizing fire infrared analysis, a certain amount of water sample is injected separately into the height for filling oxidation catalyst
In warm (680 DEG C) combustion tube and low-temp reaction pipe, the water sample in high-temperature combustion tube is by high-temperature S removal, organic carbon and inorganic carbon
Hydrochlorate is transformed into CO2；Water sample in low-temp reaction pipe is made inorganic carbonate resolve into CO by acidification (hydrochloric acid)2, what the two generated
Carbon dioxide imports non-dispersive infrared (NDIR) detector successively, measures total carbon (TC) and inorganic carbon in water respectively
(IC), difference is Water Soluble Organic Carbon (WSOC).Potassium Hydrogen Phthalate, carbon are selected in the preparation of TC, IC standard solution respectively
Sour hydrogen sodium and sodium carbonate, and the r of standard curve2Reach 0.999 or more, linear fit is preferable.Apparatus measures range：4μg/
L-30000μg/L；Detection is limited to：4μg/L；Carrier gas：Compressed air or oxygen (free from dust, mist of oil, water droplet etc.)；Carrier gas supply pressure
Power：200±10kPa；Carrier gas flux：150mL/min.The two sampled point PM measured2.5Middle HULIS-C concentration is shown in Table 1.
Table 1：2 sampled point PM of Changzhou winter2.5Concentration (the μ g/m of middle HULIS, HULIS-C3)
Test example 1, the rate of recovery, standard deviation and minimum detectability measure
(1) the detection method rate of recovery of humic-like substance, standard deviation and minimum detectability measure：Take 8 part of 1/8 blank quartz
Filter membrane is added the SRFA solution of a concentration of 1mg/mL of 1mL, is handled with the method in embodiment 1.Extraction column selects HLB, washes
De- agent elutes for 2% ammonium hydroxide methanol solution of volume ratio；Extraction column selects ENVI-18, and eluant, eluent is methanol；Extraction column selects XAD-
8, eluant, eluent is that volume ratio is 6:4 methanol-water solution.With the HPLC with ESLD detectors to HULIS quantitative analyses, calculate back
Yield, standard deviation and minimum detectability, the results are shown in Table 2.
(2) the detection method rate of recovery of carbon content, standard deviation and minimum detectability measure in humic-like substance：Take 8 part 1/8
Blank quartz filter is handled with the method in embodiment 2, and it is 2% ammonium hydroxide first of volume ratio that extraction column, which selects HLB, eluant, eluent,
Alcoholic solution elutes；Extraction column selects ENVI-18, and eluant, eluent is methanol；Extraction column selects XAD-8, and eluant, eluent is that volume ratio is 6：4
Methanol-water solution.Air PM is measured with TOC2.5Middle HULIS-C concentration calculates the rate of recovery, standard deviation and minimum detectability,
It the results are shown in Table 2.
Table 2：The HULIS and HULIS-C rate of recovery, relative standard deviation and minimum detectability when difference extraction column extracting
Claims (9)
1. the detection method of humic-like substance in a kind of Atmospheric particulates, which is characterized in that this method comprises the steps of：
(1) sample collection：Use band PM2.5The big flow of cutter or middle traffic sampling device acquire Atmospheric particulates, take collection big
The filter membrane of aerated particle object is set in pure water, ultrasonic extraction, and extracting solution filtering, constant volume obtains sample lysate；
(2) Solid Phase Extraction：By sample lysate obtained by step (1), it is adjusted with acid pH=2, preactivated and balance consolidate is added
It is extracted in phase extraction column, first plus pure water is eluted, and eluent discards, then is eluted with eluant, eluent, collects eluent；
(3) prepared by sample solution：Eluent obtained by step (2) is subjected to liquid nitrogen drying, brown volumetric flask is settled to pure water
In, -20 DEG C of preservations obtain sample solution；
(4) Specification Curve of Increasing：With pure water with setting to 0, the SRFA standard solution of 1,5,10,25,75 μ g/mL uses high-efficient liquid phase color
Spectrum cascade evaporation light scattering apparatus is measured, and draws the relationship between signal-concentration, and standard curve is made；
(5) chromatographic condition：Chromatographic column is C18Column, mobile phase are acetonitrile-water 20-80, flow velocity 0.6mL/min, and sampling volume is
60μL；ELSD setup parameters are as follows：Use N2As carrier gas, flow velocity 1.5L/min, 80-90 DEG C of drift tube temperature, GAIN settings
It is 6；The sample solution prepared to step (3) with high performance liquid chromatography cascade evaporation light scattering apparatus is detected, and is marked according to SRFA
Directrix curve is quantified, and the concentration of humic-like substance is measured.
2. the detection method of humic-like substance in Atmospheric particulates according to claim 1, which is characterized in that step (1) institute
The filter membrane stated is quartz filter, and filter membrane toasts 5h using being preceding put into Muffle furnace, removes organic principle, use aluminum foil sealing at 450 DEG C
It is sealed in constant temperature and humidity drying case after putting；The time of the ultrasonic extraction is 45-60min；The extracting solution mistake
The method of filter is：With the syringe filter filtering in 0.45 μm of aperture, removes and suspend and insoluble particulate matter.
3. the detection method of humic-like substance in Atmospheric particulates according to claim 1, which is characterized in that step (2) institute
The acid stated is the hydrochloric acid of 2mol/L.
4. the detection method of humic-like substance in Atmospheric particulates according to claim 1, which is characterized in that step (2) institute
The solid-phase extraction column stated is reverse phase hydrophilic lipophilicity column, non-polar hydrophobic C18It is any one in column or nonionic macroreticular resin
Kind.
5. the detection method of humic-like substance in Atmospheric particulates according to claim 4, which is characterized in that step (2) is：
By sample lysate obtained by step (1), it is adjusted with acid pH=2, preactivated and balance reverse phase hydrophilic lipophilicity solid phase is added
It is extracted in extraction column, first plus pure water is eluted, and eluent discards, then is eluted for 2% ammonium hydroxide methanol solution with volume ratio, is collected
Eluent.
6. the detection method of humic-like substance in Atmospheric particulates according to claim 4, which is characterized in that step (2) is：
By sample lysate obtained by step (1), it is adjusted with acid pH=2, preactivated and balance non-polar hydrophobic C is added18Solid phase
It is extracted in extraction column, first plus pure water is eluted, and eluent discards, and eluent is collected in again with methanol elution.
7. the detection method of humic-like substance in Atmospheric particulates according to claim 4, which is characterized in that step (2) is：
By sample lysate obtained by step (1), it is adjusted with acid pH=2, it is solid that preactivated and balance nonionic macroreticular resin is added
Extracted in phase extraction column, first plus pure water eluted, eluent discards, then with volume ratio be 6:4 methanol-water solution is washed
It is de-, collect eluent.
8. in a kind of Atmospheric particulates in humic-like substance carbon content detection method, which is characterized in that this method is：According to power
Profit requires the step of any one of 1-7 (1) to (3) to prepare sample solution, is detected in humic-like substance with the analyzer of TOC-L
Carbon content.
9. detection method according to claim 8, which is characterized in that the analyzer of the TOC-L is detected class humic
The parameter of carbon content is in matter：Shimadzu total organic carbon analyzer TOC-L, with oxidizing fire infrared analysis, a certain amount of water
Sample is injected separately into the 680 DEG C of combustion tubes of high temperature and low-temp reaction pipe for filling oxidation catalyst, the water sample in high-temperature combustion tube by
High-temperature S removal, organic carbon and inorganic carbonate are transformed into CO2；Water sample in low-temp reaction pipe is made nothing by the acidification of hydrochloric acid
Machine carbonate decomposition is at CO2, the two generate carbon dioxide import non-dispersive infrared NDIR detectors successively, measure respectively
Total carbon TC in water and inorganic carbon IC, difference are Water Soluble Organic Carbon WSOC, and neighbour is selected in the preparation of TC, IC standard solution respectively
Potassium hydrogen phthalate, sodium bicarbonate and sodium carbonate, and the r of standard curve2Reach 0.999 or more, apparatus measures range：4μ
G/L-30000 μ g/L, detection are limited to：4 μ g/L carrier gas：Compressed air or oxygen, carrier gas supply pressure：200 ± 10kPa, carrier gas
Flow：150mL/min.
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| CN110346480A (en) * | 2019-08-09 | 2019-10-18 | 新乡双鹭药业有限公司 | The method of organic carbon method measurement workshop air total hydrocarbon |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008051618A (en) * | 2006-08-24 | 2008-03-06 | National Agriculture & Food Research Organization | Determination method for degree of compost decay, and solution for determination |
| CN102056976A (en) * | 2008-05-05 | 2011-05-11 | 卡普图尔技术有限责任公司 | Novel crosslinked polymeric substrates methods of preparation and end use applications of the substrates |
| CN104458997A (en) * | 2014-12-19 | 2015-03-25 | 中国环境科学研究院 | Method for analyzing composition of humic-like functional groups with different molecular weights |
| CN106093259A (en) * | 2016-06-29 | 2016-11-09 | 常州大学 | A kind of water solublity humic-like substance aerosol (HULIS) containing carbon ratio detection method |
-
2018
- 2018-05-31 CN CN201810552881.6A patent/CN108760925A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008051618A (en) * | 2006-08-24 | 2008-03-06 | National Agriculture & Food Research Organization | Determination method for degree of compost decay, and solution for determination |
| CN102056976A (en) * | 2008-05-05 | 2011-05-11 | 卡普图尔技术有限责任公司 | Novel crosslinked polymeric substrates methods of preparation and end use applications of the substrates |
| CN104458997A (en) * | 2014-12-19 | 2015-03-25 | 中国环境科学研究院 | Method for analyzing composition of humic-like functional groups with different molecular weights |
| CN106093259A (en) * | 2016-06-29 | 2016-11-09 | 常州大学 | A kind of water solublity humic-like substance aerosol (HULIS) containing carbon ratio detection method |
Non-Patent Citations (4)
| Title |
|---|
| JIHUA TAN 等: "Chemical characterization of humic-like substances (HULIS) in PM 2.5 in Lanzhou, China", 《SCIENCE OF THE TOTAL ENVIRONMENT》 * |
| PENG LIN 等: "Abundance and size distribution of HULIS in ambient aerosols at a rural site in South China", 《JOURNAL OF AEROSOL SCIENCE》 * |
| XINGJUN FAN 等: "Comparison of isolation and quantification methods to measure humic-like substances (HULIS) in atmospheric particles", 《ATMOSPHERIC ENVIRONMENT》 * |
| 周雪明 等: "北京APEC期间大气颗粒物中类腐殖酸的污染特征及来源", 《环境科学》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110346480A (en) * | 2019-08-09 | 2019-10-18 | 新乡双鹭药业有限公司 | The method of organic carbon method measurement workshop air total hydrocarbon |
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