CN108008025A - Method that is a kind of while detecting a variety of volatile organic matters in marking pen - Google Patents
Method that is a kind of while detecting a variety of volatile organic matters in marking pen Download PDFInfo
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- CN108008025A CN108008025A CN201710990698.XA CN201710990698A CN108008025A CN 108008025 A CN108008025 A CN 108008025A CN 201710990698 A CN201710990698 A CN 201710990698A CN 108008025 A CN108008025 A CN 108008025A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/60—Construction of the column
- G01N30/6052—Construction of the column body
- G01N30/6073—Construction of the column body in open tubular form
- G01N30/6078—Capillaries
-
- 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
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
- G01N30/7206—Mass spectrometers interfaced to gas chromatograph
Abstract
The present invention relates to analysis detection field, more particularly to method that is a kind of while detecting a variety of volatile organic matters in marking pen, the method is sampled using absorbent cotton, with easy to operation, part marking pen sample is avoided can not directly to obtain the rough sledding of ink from ink sac, it with the addition of high boiling matrix Equilibration in ml headspace bottle, equilibrium liquid and analysis object retention time gap are larger, chromatography will not be had an impact again when playing the role of stable vapor liquid equilibrium, injector temperature is arranged to 120 DEG C, transmission line temperature is 110 ~ 120 DEG C, ideal gas sample introduction can avoid gas chromatography combined with mass spectrometry system from being introduced into interfering material, help to extend chromatographic column and the maintenance period and consumables service life at mass spectrum end, so as to reduce detection job costs.Volatile component 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 detect a variety of volatile organic matters in marking pen
Method.
Background technology
It is domestic:QB/T 21027《The safety general requirement of students' supplies》、HJ 572-2010《Environmental labelling product text
Tool》、QB/T 2777-2015《Marking pen》Deng marking pen relevant criterion in all its bearings all to safe to use, the product of marking pen
Quality is made that constraint, but the requirement for wherein ink all lacks for specific requirement.More without suitable correlative measurement
The method that method for testing is measured the species and content of volatile organic compounds present in MARKER INK is used and is directed to
Methanol, benzene homologues, halo hydrocarbon content internal standard method, but the practice of practice examining is shown, such detection method there are it is following not
Foot:1. gas chromatographic detection lacks the object qualitative tool outside retention time, often false positive or content can be caused to increase emptily
Test result;2. halogenated hydrocarbons and benzene homologues belong to low-boiling organic compound, when test also need by the long period compared with
, there is the possibility for merging detection in low column temperature program separation;3. the dissolved Liquid sample introduction of Paint dilution, can cause at injection port
More nonvolatile matter is remained, these materials can cause to adsorb to subsequent sample, and then cause the repeated not good enough of sample detection;4.
Classification as defined in standard detects, and the efficiency of detection work is significantly reduced while detection accuracy has been shown consideration for, and increases
Add the complexity of operation, while consumed with substantial amounts of experiment reagent, do not meet the development trend of environmental protection and energy saving.
Headspace sampling technology has cleaning sample introduction, does not pollute injection port, do not reduce using life of chromatographic column and reduce mass spectrum
A variety of benefits such as instrument component frequency of maintenance.Mass spectrometric full scan and selection ion scan can meet at the same time perk purity and
The quantitative testing requirement of object.This patent can provide clean and effective, again for the detection of the chromatography class harmful substance in coating
The test method that renaturation is good, selectivity is good, checks on product quality for decorating and renovating material buying side selection material and manufacturing enterprise
Fast Detection Technique is provided, 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 upper deficiency of the prior art to provide one kind while detect a variety of in marking pen wave
The method of hair property organic matter, the method high sensitivity, specificity are strong, easy 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 a variety of volatile organic matters in marking pen, the method use the side of Gas-phase acidity
Method, comprises the following steps:
S1. sample
Solvent is added in head space, drawing MARKER INK with absorbent cotton is dissolved in solvent, addition equilibrium liquid, head space furnace temperature 80 ~
90 DEG C, 30 ~ 45 min of equilibration time;
S2 HS GCs mass spectrometer is analyzed,
Wherein, the operating condition of the HS GC mass spectrometry analysis is:90 ~ 110 DEG C of sampling probe temperature, transmission line
110 ~ 120 DEG C of temperature, carrier gas are high-purity helium or hydrogen;Head space flow rate of carrier gas is 20ml/min;Gas chromatographic sample introduction mouth temperature
For 120 DEG C, injection port split ratio is 10 ~ 20:1;Post case is heated up using temperature control program;Carrier gas stream element is 1.0ml/min;Electricity
Son bombardment ionization source 70eV;230 DEG C of ion source temperature;150 DEG C of level Four bar temperature;GC-MS makes an excuse 250 DEG C of temperature;Solvent delay
3 ~ 4 min of time.
Sampled using absorbent cotton, have it is easy to operation, avoid part marking pen sample from not obtained from ink sac directly
The rough sledding of ink is obtained, high boiling matrix Equilibration, equilibrium liquid and analysis object retention time are with the addition of in ml headspace bottle
Gap is larger, chromatography will not be had an impact again when playing the role of stable vapor liquid equilibrium, injector temperature is arranged to 120
DEG C, transmission line temperature is 110 ~ 120 DEG C, using gas sampling gas chromatography-mass spectrography system can be avoided to be introduced into completely
Interfering material, helps to extend chromatographic column and the maintenance period and consumables service life at mass spectrum end, so as to reduce detection work
Cost.Volatile component in sample can be efficiently separated identification by mass spectrograph well, and meet quantitative testing requirements.
Preferably, the temperature control program is:Initial temperature keeps 9 ~ 12min from+5 DEG C ~ 40 DEG C of room temperature;Again with 6 ~
The speed of 10 DEG C/min rises to 55 ~ 65 DEG C and keeps 3 ~ 5min;Then 70 ~ 90 DEG C and holding 3 are raised to the speed of 3 ~ 5 DEG C/min
~6min;120 DEG C are risen to the speed of 6 ~ 9 DEG C/min and keep 5min again;Then 200 DEG C of guarantors are risen to the speed of 20 DEG C/min
Hold 11min;260 DEG C are risen to the speed of 20 DEG C/min again, keeps 5min;Afterwards equilibrium temperature be set as keeping after 40 DEG C of stabilizations 1 ~
2min。
Preferably, the solvent is glyceryl triacetate.
Preferably, the gas chromatography combined with mass spectrometry method, uses poly- second of the chromatographic column for 60m × 0.25mm × 0.25 μm
Glycol capillary chromatographic column.
Chromatographic column is using chromatographic column Agilent DB-624 (60m × 0.32mm × 1.40mm) or the filler of equivalent effect
Such as:The capillary of AT-624, Rxi-624 Sil MS, Rtx-624, PE-624,007-624,007-502, ZB-624
Column.
Preferably, the purity of the carrier gas is more than 99.999%.
Post case uses temperature programming;Carrier gas high-purity helium(He)Or high-purity hydrogen(H2), purity is more than 99.999%;Top
Empty injector split ratio is adjustable;Head-space sampler quantitative loop 1mL or 3mL.
Preferably, the gas chromatography combined with mass spectrometry method, mass spectrograph is using full scan and selection ion detection double mode.
Mass spectrograph is using full scan and selection ion detection double mode;Using full scan total ion current mass spectrogram as it is qualitative according to
According to;It is quantitative with the correction of target compound characteristic ion automatic integration area-method.
The present invention adds sample introduction in ml headspace bottle using 16 kinds of volatile organic matter standard mixed solutions series of known content,
It is introduced into gas chromatograph-mass spectrometer by the sampling identical with sample and injection procedure, records the full scan of test compound
With Salbutamol Selected Ion Monitoring collection of illustrative plates, by the standard retention time library searching result and characteristic ion abundance that contrast test compound
Than determining whether there is the compound, then by the response of response target compound close in sample to select outside ion
The correction of mark method is quantitative.Retention time is basically identical, when chromatographic peak still suffers from query, is using automatic mass spectrogram deconvolution and identification
Software (AMDIS) unite to distinguish chromatographic peak detail.
The present invention has following technique effect compared with prior art:
The present invention uses HS GC-mass spectrography detection technique, measures volatile organic compounds in MARKER INK and contains
Amount, has the following advantages that:A. contained volatility under MARKER INK sample substrate complex situations can be suitable for by establishing one kind
The method of organic compound qualitative, quantitative;B. using absorbent cotton sample, have it is easy to operation, avoid part marking pen sample
Product can not directly obtain the rough sledding of ink from ink sac;C. it with the addition of high boiling matrix Equilibration in ml headspace bottle, balance
Liquid and analysis object retention time gap are larger, and shadow will not be produced to chromatography again when playing the role of stable vapor liquid equilibrium
Ring;D. ideal gas sample introduction can avoid gas chromatography-mass spectrography system from being introduced into interfering material, help to extend chromatography
Column and the maintenance period and consumables service life at mass spectrum end, so as to reduce detection job costs;E. mass spectrograph can well by
Volatile component in sample efficiently separates identification, and meets quantitative testing requirements.
Brief description of the drawings
16 kinds of VOCs total ion current figures of Fig. 1, methanol, ethanol, propyl alcohol, isopropanol, butanone, second are followed successively by by peak sequence
Acetoacetic ester, benzene, isopropyl acetate, n-butyl alcohol, two acetaldehyde of second contracting, ethylene glycol monoethyl ether, dihydroxypropane single-ether, ethyl lactate, benzene
Formaldehyde, 2- ethyl -1- hexanols and benzyl carbinol, last peak are glyceryl triacetates.
VOCs total ion current figures in Fig. 2 mark pen ink samples.
Specific embodiment
With reference to Figure of description and specific embodiment, the present invention is further explained.These embodiments are merely to illustrate
The present invention rather than limit the scope of the invention.The experimental method of actual conditions is not specified in lower example embodiment, usually 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 content of volatile organic compound in MARKER INK
Take the glyceryl triacetate solution that 5ml analyzes pure or more rank a small amount of again by head space in 20mL specification ml headspace bottles, taking
Bottle is placed in balance sample weighting disk and is zeroed, and disassembles out marking pen ink sac, gross mass 0.5g, is vortexed with same solvent constant volume and after being capped
Mix, it is standby to survey.
(2)HS GC mass spectrograph operating condition
a)80 DEG C of head space furnace temperature, balances 30min, 110 DEG C of sampling probe, and transmission line temperature is 120 DEG C, and carrier gas is high-purity helium;Top
Unloaded gas velocity is 20ml/min;
b)120 DEG C of gas chromatographic sample introduction mouth temperature;Injection port split ratio is 10:1;
c)Chromatographic column:The capillary chromatographic column of 60m × 0.25mm × 0.25 μm, polyethylene glycol capillary column;
d)Heating schedule is as follows:40 DEG C of initial temperature, keeps 9min;60 DEG C are risen to the speed of 8 DEG C/min and keep 3min again;
Then 90 DEG C are raised to the speed of 4 DEG C/min and keep 5min;120 DEG C are risen to the speed of 8 DEG C/min and keep 5min again;So
200 DEG C of holding 11min are risen to the speed of 20 DEG C/min afterwards;260 DEG C are risen to the speed of 20 DEG C/min again, keeps 5min;Afterwards
Equilibrium temperature keeps 1min after being set as 40 DEG C of stabilizations;
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 table 1;
k)Solvent delay 4min.
(3)Analysis result calculation
By contrasting object appearance time and characteristic ion abundance ratio, determine in sample containing ethanol, isopropanol, acetic acid second
Ester, n-butyl alcohol, concrete content are shown in Table 2
Embodiment 2
(1)The detection of content of volatile organic compound in black MARKER INK can be added
Take the glyceryl triacetate solution that 5ml analyzes pure or more rank a small amount of again by head space in 20mL specification ml headspace bottles, taking
Bottle is placed in balance sample weighting disk and is zeroed, and disassembles out marking pen ink sac, gross mass 0.2g, is vortexed with same solvent constant volume and after being capped
Mix, it is standby to survey.
(2)HS GC mass spectrograph operating condition
a)90 DEG C of head space furnace temperature, balances 40min, 90 DEG C of sampling probe, and transmission line temperature is 110 DEG C, and carrier gas is high-purity helium;Head space
Flow rate of carrier gas is 20ml/min;
b)120 DEG C of gas chromatographic sample introduction mouth temperature;Injection port split ratio is 10:1;
c)Chromatographic column:The capillary chromatographic column of 60m × 0.25mm × 0.25 μm, polyethylene glycol capillary column;
d)Heating schedule is as follows:40 DEG C of initial temperature, keeps 9min;60 DEG C are risen to the speed of 8 DEG C/min and keep 3min again;
Then 90 DEG C are raised to the speed of 4 DEG C/min and keep 5min;120 DEG C are risen to the speed of 8 DEG C/min and keep 5min again;So
200 DEG C of holding 11min are risen to the speed of 20 DEG C/min afterwards;260 DEG C are risen to the speed of 20 DEG C/min again, keeps 5min;Afterwards
Equilibrium temperature keeps 2min after being set as 40 DEG C of stabilizations;
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 table 1;
k)Solvent delay 4min.
(3)Analysis result calculation
By contrasting object appearance time and characteristic ion abundance ratio, determine in sample containing ethanol, isopropanol, ethylene glycol list
Ether, concrete content are shown in Table 2
Embodiment 3
(1)The detection of content of volatile organic compound in blank pen inks
Take the glyceryl triacetate solution that 10ml analyzes pure or more rank a small amount of again by head space in 20mL specification ml headspace bottles, taking
Bottle is placed in balance sample weighting disk and is zeroed, and disassembles out white board marker ink sac, gross mass 0.3g, is vortexed with same solvent constant volume and after being capped
Mix, it is standby to survey.
(2)HS GC mass spectrograph operating condition
a)90 DEG C of head space furnace temperature, balances 45min, 100 DEG C of sampling probe, and transmission line temperature is 110 DEG C, and carrier gas is high-purity helium;Top
Unloaded gas velocity is 20ml/min;
b)120 DEG C of gas chromatographic sample introduction mouth temperature;Injection port split ratio is 20:1;
c)Chromatographic column:The capillary chromatographic column of 60m × 0.25mm × 0.25 μm, polyethylene glycol capillary column;
d)Heating schedule is as follows:40 DEG C of initial temperature, keeps 9min;60 DEG C are risen to the speed of 8 DEG C/min and keep 3min again;
Then 90 DEG C are raised to the speed of 4 DEG C/min and keep 5min;120 DEG C are risen to the speed of 8 DEG C/min and keep 5min again;So
200 DEG C of holding 11min are risen to the speed of 20 DEG C/min afterwards;260 DEG C are risen to the speed of 20 DEG C/min again, keeps 5min;Afterwards
Equilibrium temperature keeps 2min after being set as 40 DEG C of stabilizations;
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 2 or more qualitative ions, wherein comprising a quota ion,
Target compound monitors ion referring to table 1;
k)Solvent delay 3min.
(3)Analysis result calculation
By contrasting object appearance time and characteristic ion abundance ratio, determine in sample containing ethanol, propyl alcohol, isopropanol, second
Acetoacetic ester and n-butyl alcohol, concrete content are shown in Table 2.
1. the retention time of the compound of table, qualitative/quantitative ion and No. CAS
2. sample tests of table(mg/g)
Claims (6)
1. method that is a kind of while detecting a variety of volatile organic matters in marking pen, it is characterised in that the method uses gas phase
The method of mass spectrometry, comprises the following steps:
S1. sample
Solvent is added in head space, drawing MARKER INK with absorbent cotton is dissolved in solvent, addition equilibrium liquid, head space furnace temperature 80 ~
90 DEG C, 30 ~ 45 min of equilibration time;
S2 HS GCs mass spectrometer is analyzed,
Wherein, the operating condition of the HS GC mass spectrometry analysis is:90 ~ 110 DEG C of sampling probe temperature, transmission line
110 ~ 120 DEG C of temperature, carrier gas are high-purity helium or hydrogen;Head space flow rate of carrier gas is 20ml/min;Gas chromatographic sample introduction mouth temperature
For 120 DEG C, injection port split ratio is 10 ~ 20:1;Post case is heated up using temperature control program;Carrier gas stream element is 1.0ml/min;Electricity
Son bombardment ionization source 70eV;230 DEG C of ion source temperature;150 DEG C of level Four bar temperature;GC-MS makes an excuse 250 DEG C of temperature;Solvent delay
3 ~ 4 min of time.
2. the method for detecting a variety of volatile organic matters in marking pen at the same time according to claim 1, it is characterised in that described
Temperature control program is:Initial temperature keeps 9 ~ 12min from+5 DEG C ~ 40 DEG C of room temperature;Again 55 are risen to the speed of 6 ~ 10 DEG C/min
~ 65 DEG C and 3 ~ 5min of holding;Then 70 ~ 90 DEG C are raised to the speed of 3 ~ 5 DEG C/min and keep 3 ~ 6min;Again with 6 ~ 9 DEG C/min
Speed rise to 120 DEG C and keep 5min;Then 200 DEG C of holding 11min are risen to the speed of 20 DEG C/min;Again with 20 DEG C/min
Speed rise to 260 DEG C, keep 5min;Equilibrium temperature keeps 1 ~ 2min after being set as 40 DEG C of stabilizations afterwards.
3. the method for detecting a variety of volatile organic matters in marking pen at the same time according to claim 1, it is characterised in that described
Equilibrium liquid is glyceryl triacetate.
4. the method for detecting a variety of volatile organic matters in marking pen at the same time according to claim 1, it is characterised in that described
Gas chromatography combined with mass spectrometry method, uses polyethylene glycol capillary chromatographic column of the chromatographic column for 60m × 0.25mm × 0.25 μm.
5. the method for detecting a variety of volatile organic matters in marking pen at the same time according to claim 1, it is characterised in that described
The purity of carrier gas is more than 99.999%.
6. the method for detecting a variety of volatile organic matters in marking pen at the same time according to claim 1, it is characterised in that described
Gas chromatography combined with mass spectrometry method, mass spectrograph is using full scan and selection ion detection double mode.
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Cited By (2)
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CN111103374A (en) * | 2019-08-07 | 2020-05-05 | 南京生命能科技开发有限公司 | Method for determining content of 2,2,6, 6-tetramethylpiperidine oxide in cinacalcet hydrochloride |
CN111812244A (en) * | 2020-07-22 | 2020-10-23 | 北京印刷学院 | Method for detecting content of VOCs (volatile organic compounds) in water-based ink based on ionic liquid |
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CN111103374A (en) * | 2019-08-07 | 2020-05-05 | 南京生命能科技开发有限公司 | Method for determining content of 2,2,6, 6-tetramethylpiperidine oxide in cinacalcet hydrochloride |
CN111103374B (en) * | 2019-08-07 | 2023-11-28 | 南京生命能科技开发有限公司 | Method for measuring content of 2, 6-tetramethylpiperidine oxide in cinacalcet hydrochloride |
CN111812244A (en) * | 2020-07-22 | 2020-10-23 | 北京印刷学院 | Method for detecting content of VOCs (volatile organic compounds) in water-based ink based on ionic liquid |
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