CN107703247A - Method that is a kind of while detecting volatile organic matter in coating - Google Patents
Method that is a kind of while detecting volatile organic matter in coating Download PDFInfo
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- CN107703247A CN107703247A CN201710990651.3A CN201710990651A CN107703247A CN 107703247 A CN107703247 A CN 107703247A CN 201710990651 A CN201710990651 A CN 201710990651A CN 107703247 A CN107703247 A CN 107703247A
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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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
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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
- G01N30/16—Injection
- G01N30/20—Injection using a sampling valve
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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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
- G01N2030/884—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample organic compounds
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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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
- G01N2030/884—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample organic compounds
- G01N2030/8854—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample organic compounds involving hydrocarbons
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- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The present invention relates to analysis detection field, more particularly to method that is a kind of while detecting volatile organic matter in coating, methods described sampling operation mixes operating process due to improving as defined in national standard method component, reduce coating each component mix operate when evaporation rate differ and the uncertainty that factor brings to sampling operation such as be difficult to judge with Blending Efficiency of Blending；Using the special quantitative capillary tube sampling of thin-layer chromatography point sample, the sealing for avoiding damage to head space bottle cap is placed before there is easy to operation, sealing；Sample introduction volume is few in method ml headspace bottle, almost all volatilization, contributes to ml headspace bottle to keep preferable inertia in the case of reusing；Gas sampling can avoid gas chromatography system from being introduced into non-volatile matter, help to extend the maintenance period and running stores service life of chromatographic system；Methanol, benzene homologues, halogenated hydrocarbons etc. and other volatile components in sample can be efficiently separated identification by mass spectrograph well, and meet quantitative testing requirements.
Description
Technical field
The present invention relates to analysis detection field, and in particular to a kind of while method that detects volatile organic matter in coating.
Background technology
Standard GB/T 18581-2009 at present《Limits of harmful substances in indoor decorating and refurnishing materials solvent-borne type woodcare paint》
In the related detection method of gas-chromatography is defined to the middle methanol in solvent-borne type woodcare paint, benzene homologues, halo hydrocarbon content.Method
Using for methanol, benzene homologues, halo hydrocarbon content internal standard method, but the practice of practice examining is shown, such detection method is deposited
In following deficiency：1. gas chromatographic detection lacks the object qualitative tool in addition to retention time, false positive also can be often caused
Or the test result that content increases emptily；2. halogenated hydrocarbons and benzene homologues belong to lower boiling organic compound, during the test of two projects
Need also exist for separating by long period relatively low column temperature program, the possibility for merging detection in principle be present；3. Paint dilution dissolves
Liquid sample introduction afterwards, it can cause to remain more nonvolatile matter at injection port, these nonvolatile matters are mainly resin and metallochrome
Material etc., they can cause to adsorb to the test of subsequent sample, and then cause the repeated not good enough of sample detection；4. current standard gauge
The method of fixed different target thing separate detection, the efficiency of detection work is significantly reduced, the work for adding operation repeats
Property, while consumed with larger amount of reagent, do not meet the test industry development trend of environmental protection and energy saving.
Headspace sampling technology has cleaning sample introduction, does not pollute injection port, is advantageous to extend using life of chromatographic column and reduction
A variety of benefits such as mass spectrograph component frequency of maintenance.Mass spectrometric full scan and selection ion scan can also meet chromatographic peak simultaneously
The qualitative and quantitative testing requirement of object.It is high that this patent can provide cleaning for the detection of the chromatogram class harmful substance in coating
Effect, reproducible, the good method of testing of selectivity, checked on product for decorating and renovating material buying side selection material and manufacturing enterprise
Quality provides Fast Detection Technique, and the method foundation of technology upgrading is provided for coating test job.
The content of the invention
It is an object of the invention to overcome above-mentioned problems of the prior art, there is provided a kind of high sensitivity, specificity
By force, the detection method of volatile organic matter in coating simple to operate, versatile, applicability is wide.
The purpose of the present invention is achieved by the following technical programs：
Method that is a kind of while detecting volatile organic matter in coating, methods described is using side associated with static headspace-GC-MS
Method, comprise the following steps：
S1 is sampled
5 ~ 10 ml containing the internal standard thing dilute solutions are taken with colorimetric cylinder, adding construct ratio successively in the sign of coating in the solution
Host, curing agent and diluent are weighed to gross mass in 1~2g, 5 ~ 10 ml is settled to and is vortexed and shake up, it is standby after centrifugation；
S2 headspace samplings prepare
The special quantitative capillary tube of μ L thin-layer chromatography point samples of 2 μ L ~ 5 is taken, draws the test sample supernatant after centrifugal treating, it is small
The heart is placed in be measured after ml headspace bottle seals；
S3 static headspace-GC-MSs instrument is analyzed；
Wherein, static headspace-GC-MS instrument condition of work is：a）150 ~ 200 DEG C of head space furnace temperature, balance 5 ~ 15min, sampling probe
200 ~ 220 DEG C, transmission line temperature is 220 DEG C, and carrier gas is high-purity helium；Head space flow rate of carrier gas is 20ml/min；Gas-chromatography is entered
230 DEG C of sample mouth temperature；Injection port split ratio is 1:1；Chromatographic column is the capillary chromatographic column of 60m × 0.25mm × 0.25 μm, is gathered
Ethylene glycol capillary column；Column temperature is by temperature control programme-control；Flow rate of carrier gas：1.0ml/min；Electron impact ionization source：70eV；Ion gun
Temperature：230℃；Level Four bar temperature：150℃；GC-MS interface temperatures：250℃.
Preferably, the temperature control program is：+ 5 DEG C ~ 30 DEG C of column temperature initial temperature room temperature 8 ~ 15min of holding, then with 6 ~
10 DEG C/min is warming up to 150 ~ 180 DEG C of holdings 2 ~ 5min, 20 ~ 50 DEG C/min and is warming up to 180 ~ 210 DEG C of 1 ~ 3min of holding.
Preferably, solution, constant volume solvent for use are glyceryl triacetate, DMF or DMA in the step S1.
Preferably, the gas chromatography combined with mass spectrometry method, poly- second of the chromatographic column for 60m × 0.25mm × 0.25 μm is used
Glycol capillary chromatographic column.
Preferably, the purity of the carrier gas is more than 99.999%.
Preferably, the gas chromatography combined with mass spectrometry method, mass spectrograph is using full scan and selection ion detection double mode.
Qualitative foundation is used as using full scan total ion chromatogram；Corrected with target compound characteristic ion abundance internal standard method
It is quantitative.
Sample volatilizees under selected headspace autosampler balance furnace temperature in ml headspace bottle, is uniformly distributed in ml headspace bottle.
Sample flows with inert carrier gas and is full of quantitative loop in ml headspace bottle after pressurized, after Vavle switching by transmission line lead into
It is detected after sample mouth, then selected chromatogram post separation into mass spectrograph, test result is recorded by work station and is used to analyze.
The present invention is distinguished using two standard mixed solutions of Methanol-benzene system thing-internal standard and halogenated hydrocarbons-internal standard of known content
Sample introduction, by it by introducing gas chromatograph-mass spectrometer with the sampling of sample identical and injection procedure, record the complete of test compound
Scanning and Salbutamol Selected Ion Monitoring collection of illustrative plates, by the standard retention time library searching result and characteristic ion that contrast test compound
Abundance ratio determines whether there is the compound, then by the response of response target compound close in sample with select from
Sub- internal standard method correction is quantitative.Retention time is basically identical, when chromatographic peak still has a question, using automatic mass spectrogram deconvolution and identification
System software (AMDIS) confirms chromatographic peak details.
When sampling amount is 1.00g, methanol 0.01%, halogenated hydrocarbons 0.01% or 0.1g/kg, benzene homologues 0.02g/kg（External standard method）
Or 0.01%（Internal standard method）, n-hexane 0.1g/kg.Benzene homologues, halogenated hydrocarbons detection collection of illustrative plates Interference Peaks can clearly be sentenced in the invention simultaneously
Fixed, sample detection is reproducible, volatile harmful material in coating is analyzed comprehensive；Test solvent dosage is small, completes all to survey
The chromatographic time of examination also greatly shortens compared with national standard method；Select ion quantitatively accurate, HS GC mass spectrograph versatility
By force, therefore the invention has wide applicability and realistic meaning.
The present invention has following technique effect compared with prior art：
The sampling operation of the present invention mixes operating process, coating when reducing sampling due to improving component as defined in national standard method
Each component possible evaporation rate when mixing operation is variant；The sample preparation efficiency that simple sample blending is brought, and component mixing
The uncertainty that the factors such as effect is undesirable introduce to detection work；Upper strata is taken using the special quantitative capillary tube of thin-layer chromatography point sample
Liquid-like, have the advantages that easy to operation, representative strong；The special quantitative capillary tube of thin-layer chromatography point sample takes supernatant liquid sample
Also have and easily obtain certain volume sample, and ml headspace bottle is placed into ml headspace bottle, in general liquid sample feeding device can also be avoided
Sampling needs to puncture head space bottle cap, so as to influence the deficiency of ml headspace bottle sealing property；Sample introduction volume is few in method ml headspace bottle, can
All to volatilize, help still to keep preferable inertia in the case where ml headspace bottle is reused, so as to reduce sample introduction
Link testing cost；Gas sampling can effectively avoid gas chromatographic sample introduction mouth and chromatographic column from introducing non-volatile matter, contribute to
Extend the maintenance period and running stores service life of chromatographic system；Mass spectrometric full scan function can be very good methanol, benzene
It is that thing, halogenated hydrocarbons etc. are efficiently separated with other volatile components in sample, identified, while can be entered using quantitative example scanning
One step meets quantitative detection demand.
Brief description of the drawings
The total ion current figure of Fig. 1 halogenated hydrocarbons and the trichloropropane mixed solution of internal standard 1,2,3-.
Fig. 2 methanol, benzene homologues, normal heptane, diethylene adipate and repefral total ion current figure.
Embodiment
With reference to Figure of description and specific embodiment, the present invention is expanded on further.These embodiments are merely to illustrate
The present invention rather than limitation the scope of the present invention.The experimental method of unreceipted actual conditions in lower example embodiment, generally according to
This area normal condition or the condition suggested according to manufacturer.What those skilled in the art was done on the basis of the present invention
The change and replacement of any unsubstantiality belong to scope of the present invention.
Embodiment 1
（1）The detection of methanol, benzene homologues, halogenated hydrocarbons, TOVC content in polyurethane coating
Take 5ml containing the internal standard things（Normal heptane, 1,2,3- trichloropropanes, repefral）With 250 DEG C of temperature marker things（Oneself
Diethyl adipate）Ethyl acetate solution in colorimetric cylinder, then colorimetric cylinder is placed in balance sample weighting disk and is zeroed, by the mark of coating
Show construction ratio component A（Mian paint）, B component（Curing agent）And component C（Tianna solution）=1:0.5:0.5 weighs A, B, component C successively
Gross mass 1g, it is vortexed and mixes with same solvent constant volume and after being capped, it is standby to survey.
After 4000 turns/min of sample liquid centrifugations, the 5 special quantitative capillary tubes of μ l thin-layer chromatography point samples are taken with tweezers, make capillary
Upper strata sample liquid is immersed in pipe one end, and pause 5s treats that sample liquid is full of whole capillary automatically.Then whole branch capillary is carefully placed into
In 20ml headspace samplings bottle and seal.
（2）HS GC mass spectrograph condition of work
a）200 DEG C of head space furnace temperature, 5min, 210 DEG C of sampling probe are balanced, transmission line temperature is 220 DEG C, and carrier gas is high-purity helium；Top
Unloaded gas velocity is 20ml/min；
b）230 DEG C of gas chromatographic sample introduction mouth temperature；Injection port split ratio is 1:1；
c）Chromatographic column:The capillary chromatographic column of 60m × 0.25mm × 0.25 μm, polyethylene glycol capillary column；
d）Column temperature：30 DEG C of holding 12min of initial temperature, then 150 DEG C of holding 2min, 30 DEG C/min heatings are warming up to 10 DEG C/min
To 180 DEG C of holding 1min；
e）Flow rate of carrier gas：1.0ml/min；
f）Electron impact ionization source：70eV；
g）Ion source temperature：230℃；
h）Level Four bar temperature：150℃；
i）GC-MS interface temperatures：250℃；
j）Select ion detection：Every kind of target compound selects 3 or more qualitative ions, wherein comprising a quota ion,
Target compound monitors ion referring to subordinate list 1,2.
（3）Analysis result calculation
By contrasting object appearance time and characteristic ion abundance ratio, determine to contain 1,1- dichloroethanes, three chloroethenes in sample
Alkene, calculated using the Internal standard correction methods factor, it is respectively 0.025%, 0.018% to measure content；Toluene, ethylbenzene, xylene content difference
It is 3.21%, 2.69%, 12.19%；TOVC content is 512.5g/kg.
Embodiment 2
（1）The detection of methanol, benzene homologues, halogenated hydrocarbons, TOVC content in nitro paint
Take 5ml containing the internal standard things（Normal heptane, 1,2,3- trichloropropanes, repefral）With 250 DEG C of temperature marker things（Oneself
Diethyl adipate）Ethyl acetate solution in colorimetric cylinder, then colorimetric cylinder is placed in balance sample weighting disk and is zeroed, by the mark of coating
Show construction ratio component A（Mian paint）, B component（Tianna solution）=1:0.5 weighs A, B component gross mass 1.5g successively, uses same solvent
It is vortexed and mixes after constant volume and capping, it is standby to survey.
Sample liquid takes the 2 special quantitative capillary tubes of μ l thin-layer chromatography point samples after 4000 turns/min centrifuges 5min with tweezers,
Capillary one end is set to immerse upper strata sample liquid, pause 5s treats that sample liquid is full of whole capillary automatically.It is then that whole branch capillary is careful
It is put into 20ml headspace samplings bottle and seals.
（2）HS GC mass spectrograph condition of work
a）200 DEG C of head space furnace temperature, 5min, 210 DEG C of sampling probe are balanced, transmission line temperature is 220 DEG C, and carrier gas is high-purity helium；Top
Unloaded gas velocity is 20ml/min；
b）230 DEG C of gas chromatographic sample introduction mouth temperature；Injection port split ratio is 1:1；
c）Chromatographic column:The capillary chromatographic column of 60m × 0.25mm × 0.25 μm, polyethylene glycol capillary column；
d）Column temperature：30 DEG C of holding 12min of initial temperature, then 150 DEG C of holding 2min, 30 DEG C/min heatings are warming up to 10 DEG C/min
To 180 DEG C of holding 1min；
e）Flow rate of carrier gas：1.0ml/min；
f）Electron impact ionization source：70eV；
g）Ion source temperature：230℃；
h）Level Four bar temperature：150℃；
i）GC-MS interface temperatures：250℃；
j）Select ion detection：Every kind of target compound selects 3 or more qualitative ions, wherein comprising a quota ion,
Target compound monitors ion referring to subordinate list 1,2.
（3）Analysis result calculation
By contrasting object appearance time and characteristic ion abundance ratio, determine to contain 1,2- dichloroethanes in sample, using interior
Calibration positive divisor calculates, and measures content as 0.032%；Toluene, ethylbenzene, xylene content are 2.39%, 3.14%, 10.06% respectively；
TOVC content is 467.2g/kg.
Embodiment 3
（1）The detection of methanol, benzene homologues, halogenated hydrocarbons, TOVC content in unsaturated-resin coating
Take 5ml containing the internal standard things（Normal heptane, 1,2,3- trichloropropanes, repefral）With 250 DEG C of temperature marker things（Oneself
Diethyl adipate）Ethyl acetate solution in colorimetric cylinder, then colorimetric cylinder is placed in balance sample weighting disk and is zeroed, by the mark of coating
Show construction ratio component A（Mian paint）, B component（Tianna solution）=1:0.5 weighs A, B component gross mass 1.5g successively, uses same solvent
It is vortexed and mixes after constant volume and capping, it is standby to survey.
After 4000 turns/min of sample liquid centrifugations, the 5 special quantitative capillary tubes of μ l thin-layer chromatography point samples are taken with tweezers, make capillary
Upper strata sample liquid is immersed in pipe one end, and pause 5s treats that sample liquid is full of whole capillary automatically.Then whole branch capillary is carefully placed into
In 20ml headspace samplings bottle and seal.
（2）HS GC mass spectrograph condition of work
a）200 DEG C of head space furnace temperature, 5min, 210 DEG C of sampling probe are balanced, transmission line temperature is 220 DEG C, and carrier gas is high-purity helium；Top
Unloaded gas velocity is 20ml/min；
b）230 DEG C of gas chromatographic sample introduction mouth temperature；Injection port split ratio is 1:1；
c）Chromatographic column:The capillary chromatographic column of 60m × 0.25mm × 0.25 μm, polyethylene glycol capillary column；
d）Column temperature：30 DEG C of holding 12min of initial temperature, then 150 DEG C of holding 2min, 30 DEG C/min heatings are warming up to 10 DEG C/min
To 180 DEG C of holding 1min；
e）Flow rate of carrier gas：1.0ml/min；
f）Electron impact ionization source：70eV；
g）Ion source temperature：230℃；
h）Level Four bar temperature：150℃；
i）GC-MS interface temperatures：250℃；
j）Select ion detection：Every kind of target compound selects 3 or more qualitative ions, wherein comprising a quota ion,
Target compound monitors ion referring to subordinate list 1,2.
（3）Analysis result calculation
By contrasting object appearance time and characteristic ion abundance ratio, determine in sample containing toluene, ethylbenzene, xylene content
It is 6.24%, 1.05%, 8.12% respectively；TOVC content is 674.9g/kg.
The halogenated hydrocarbons of table 1 and internal standard retention time and corresponding selection quota ion
The methanol of table 2, benzene homologues, normal heptane, diethylene adipate and repefral selection ion, quota ion
Claims (6)
1. method that is a kind of while detecting volatile organic matter in coating, it is characterised in that methods described uses headspace gas color
The method for composing mass spectrometry, comprises the following steps：
S1 is sampled
5 ~ 10 ml containing the internal standard thing dilute solutions are taken with colorimetric cylinder, adding construct ratio successively in the sign of coating in the solution
Weigh host, curing agent and diluent 1~2g of gross mass, constant volume and shake up rear standby；
S2 headspace samplings prepare
The special quantitative capillary tube of μ L thin-layer chromatography point samples of 2 μ L ~ 5 is taken, draws the test sample supernatant after being diluted processing
It is placed in be measured after ml headspace bottle seals；
S3 static headspace-GC-MSs instrument is analyzed；
Wherein, static headspace-GC-MS instrument condition of work is：a）200 DEG C of head space furnace temperature, 5min is balanced, 210 DEG C of sampling probe, is passed
Defeated line temperature is 220 DEG C, and carrier gas is high-purity helium；Head space flow rate of carrier gas is 20ml/min；Gas chromatographic sample introduction mouth temperature 230
℃；Injection port split ratio is 1:1；Chromatographic column be 60m × 0.25mm × 0.25 μm capillary chromatographic column, polyethylene glycol capillary
Post；Column temperature is by temperature control programme-control；Flow rate of carrier gas：1.0ml/min；Electron impact ionization source：70eV；Ion source temperature：230
℃；Level Four bar temperature：150℃；GC-MS interface temperatures：250℃.
2. the method for detecting volatile organic matter in coating simultaneously according to claim 1, it is characterised in that the temperature control
Processing procedure sequence is：30 DEG C of holding 12min of column temperature initial temperature, then 150 DEG C of holding 2min, 30 DEG C/min liters are warming up to 10 DEG C/min
Warm to 180 DEG C holding 1min.
3. the method for detecting volatile organic matter in coating simultaneously according to claim 1, it is characterised in that the step S1
Middle solution, constant volume solvent for use are glyceryl triacetate, DMF or DMA.
4. the method for detecting volatile organic matter in coating simultaneously according to claim 1, it is characterised in that the gas phase color
Mass spectrometry combination method is composed, uses polyethylene glycol capillary chromatographic column of the chromatographic column for 60m × 0.25mm × 0.25 μm.
5. the method for detecting volatile organic matter in coating simultaneously according to claim 1, it is characterised in that the carrier gas
Purity is more than 99.999%.
6. the method for detecting volatile organic matter in coating simultaneously according to claim 1, it is characterised in that the gas phase color
Mass spectrometry combination method is composed, mass spectrograph is using full scan and selection ion detection double mode.
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| CN108827998A (en) * | 2018-05-30 | 2018-11-16 | 中国计量科学研究院 | A method of volatile substances purity is accurately measured using quantitative nuclear magnetic resonance spectroscopy |
| CN109813795A (en) * | 2018-12-26 | 2019-05-28 | 宁波大学 | Ion source mass spectrum combination method |
| CN113176363A (en) * | 2021-04-14 | 2021-07-27 | 宁波检验检疫科学技术研究院 | Method for measuring total volatile organic compounds in recycled plastics |
| CN114414693A (en) * | 2022-01-21 | 2022-04-29 | 珠海格力电工有限公司 | Method for detecting content of organic volatile matter in enameled wire |
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