CN108693365A - Styrene and butyl acrylate method are measured using gas-mass spectrometer - Google Patents
Styrene and butyl acrylate method are measured using gas-mass spectrometer Download PDFInfo
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- CN108693365A CN108693365A CN201810889257.5A CN201810889257A CN108693365A CN 108693365 A CN108693365 A CN 108693365A CN 201810889257 A CN201810889257 A CN 201810889257A CN 108693365 A CN108693365 A CN 108693365A
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Abstract
Styrene and butyl acrylate method are measured using gas-mass spectrometer, belong to analysis method technical field, including gas chromatograph is arranged, mass spectrograph is set, by styrene and butyl acrylate, with carbon disulfide desorption, it is detached through gas chromatograph, mass spectrograph detection is qualitative by retention time and mass spectrogram, peak height or peak area quantification complete the measurement of styrene and butyl acrylate.The present invention overcomes the overlap of peaks occurred when styrene and butyl acrylate exist simultaneously, the phenomenon that inferior separating effects such as hangover, it is improved with Gas-phase acidity instrument on the basis of existing method, qualitative and quantitative analysis is carried out to meet the requirement that styrene and butyl acrylate quickly, accurately detect in air place to sample by gas-mass spectrometer, makes the separating degree higher of sample;The detection limit for improving experimental method, reduces the purpose of the interference of other organic matters.
Description
Technical field
The invention belongs to analysis method technical field, styrene is especially related to and when butyl acrylate exists simultaneously,
The method that qualitative and quantitative analysis is carried out to it with gas-mass spectrometer.
Background technology
At this stage, it with the fast development of production technology, in Pre-assessment of Occupational Disease Hazards, also brings over and did not occurred
New material, new process, and the generation of new material also brings difficulty to the identification of hazard factor and accurate quantitative analysis.Styrene and
Butyl acrylate copolymer is in building coating, metal surface latex paint, floor coating, paper adhesives, adhesive, leather
The fields such as finishing agent, ink have a wide range of applications.The boiling point of styrene is 146 DEG C, and the boiling point of butyl acrylate is 145.7
DEG C, boiling point is close.And GBZ/T300.127-2017"Workplace air noxious material measures the 127th part:Acrylate
Class",GBZ/T300.68-2017"Workplace air noxious material measures the 68th part:Styrene, methyl styrene and two
Vinyl benzene"Method be solvent desorption or Thermal Desorption with Gas Chromatography, styrene and butyl acrylate sampling media, sample streams
It measures identical, acquisition and detection can be analyzed accurately to single substance sample.But when styrene and propylene in public place
When acid butyl ester exists simultaneously, it may appear that phenomena such as hangover, accurately identification and difficulty is quantitatively brought to it for overlap of peaks.Therefore
There is an urgent need for a kind of novel technical solutions to solve the problems, such as this in the prior art.
Invention content
The technical problem to be solved by the present invention is to:It provides and styrene and acrylic acid is measured using gas-mass spectrometer
Butyl ester method carries out qualitative and quantitative analysis to meet styrene and third in air place by gas-mass spectrometer to sample
The requirement that olefin(e) acid butyl ester is quick, accurately detects, makes the separating degree higher of sample;The detection limit for improving experimental method, reduces it
The purpose of the interference of his organic matter.
Styrene and butyl acrylate method are measured using gas-mass spectrometer, it is characterized in that:Include the following steps,
And following steps sequentially carry out,
Step 1: the chromatographic column for choosing gas chromatograph is HP-VOC, the operation reference conditions of gas chromatograph are set;Column
Temperature is 38 DEG C, keeps 3min;80 DEG C are risen to 15 DEG C/min, keeps 2min;140 DEG C are risen to 5 DEG C/min, keeps 3min;Gas
It is 270 DEG C to change room temperature;Gas of carrier gas is nitrogen, flow 1mL/min;Split ratio is 10:1;
Step 2: setting mass spectrograph operates reference conditions;Electron impact ion source is EI;Ion source energy is 70eV;From
Source temperature is 230 DEG C;Quadrupole rod temperature is 150 DEG C;Interface temperature is 270 DEG C;Scanning range is 35amu~350amu;It is molten
Agent delay is 3min;
Step 3: preparing standard solution, styrene and butyl acrylate are taken, with carbon disulfide desorption and constant volume, is marked
Quasi- solution concentration is 0.0 μ of μ g/mL~600.0 g/mL;
Step 4: the standard solution 4~7 that step 3 is obtained, sample introduction to the gas-chromatography after step 1 is arranged
The measurement of each concentration quantitative ion of standard series is carried out in mass spectrograph after instrument and step 2 setting, styrene characteristic ion is
78,103,104, quota ion 104;The characteristic ion of n-butyl acrylate is 55,56,73, and quota ion 55 draws mark
Directrix curve calculates regression equation, completes the measurement of styrene and butyl acrylate.
Use the carbon disulfide desorption time for 30min in the step 3.
By above-mentioned design scheme, the present invention can bring following advantageous effect:Benzene is measured using gas-mass spectrometer
Ethylene and butyl acrylate method overcome styrene and overlap of peaks that when butyl acrylate exists simultaneously occurs, and trail decile
The phenomenon poor from effect, is improved with Gas-phase acidity instrument on the basis of existing method, passes through gas-mass spectrometer pair
Sample carries out qualitative and quantitative analysis to meet the requirement that styrene and butyl acrylate quickly, accurately detect in air place, makes
The separating degree higher of sample;The detection limit for improving experimental method, reduces the purpose of the interference of other organic matters.
Description of the drawings
Below in conjunction with the drawings and specific embodiments, the present invention is further illustrated:
Fig. 1 is styrene regression equation related coefficient curve synoptic diagram of the present invention.
Fig. 2 is butyl acrylate regression equation related coefficient curve synoptic diagram of the present invention
Specific implementation mode
The present invention measures the instrument and equipment needed for styrene and butyl acrylate method such as using gas-mass spectrometer
Under:In standard livery shopwork place by taking 100ml/min samples the sample detection that 15 minutes obtain as an example,
Required instrument and equipment:5mL solvent desorptions bottle, 50ml volumetric flasks, 10uL micro syringes, gas chromatograph-mass spectrometer,
Has hydrogen flame ionization detector;
Wherein gas chromatograph operation reference conditions be:
A) chromatographic column:60m × 200um × 1.1um, HP-VOC;
B) column temperature:38 DEG C, keep 3min;80 DEG C are risen to 15 DEG C/min, keeps 2min;140 DEG C are risen to 5 DEG C/min,
Keep 3min;
C) gasify room temperature:270℃;
D) carrier gas (nitrogen) flow:1mL/min;
E) split ratio:10:1.
Mass spectrograph operates reference conditions:
A) electron impact ion source:EI;
B) ion source energy:70eV;
C) ion source temperature:230℃;
D) quadrupole rod temperature:150℃;
E) interface temperature:270℃;
F) scanning range:35amu~350amu;
G) solvent delay:3min.
Reagent:Carbon disulfide, the noiseless miscellaneous peak in chromatography identification.
Standard solution processing:Add a small amount of carbon disulfide in volumetric flask, accurately measure or take a certain amount of styrene and
N-butyl acrylate, with two sulphur constant volumes.The concentration of each determinand in solution is calculated, is the standard solution of determinand.Ice after sealing
Case freezen protective.
Sample treatment:Front and back section activated carbon is poured into respectively in two solvent desorption bottles, it is each that 1.0mL curing carbon lids are added
After tight bottle cap, 30min is desorbed, is shaken frequently, sample solution is for measuring.
The preparation of standard curve:Take 4~7 volumetric flasks, with carbon disulfide working solution at 0.0 μ g/mL~
The standard series of the determinand of 600.0 μ g/mL concentration ranges.With reference to instrumentation condition, gas chromatograph-mass spectrometer is adjusted to
Optimum determining state reference condition, 1.0 μ L of sample introduction, the quota ion of each concentration of bioassay standard series, styrene are characterized respectively
Ion 78,103,104, quota ion 104;N-butyl acrylate characteristic ion 55,56,73, quota ion 55, to measure to phase
The testing concentration (μ g/mL) answered draws standard curve or calculates regression equation, and related coefficient answers >=0.999.
As depicted in figs. 1 and 2, styrene equation be response=5.146e4*C+2.603e5 related coefficients (R2)=
0.999254;N-butyl acrylate equation is response=3.429e4*C+9.555e5 related coefficients (R2)=0.999576;
It is respectively 0.025mg/L, 0.136mg/ to obtain styrene and n-butyl acrylate detection limit according to three times signal-to-noise ratio
L, 10 times of signal-to-noise ratio obtain lower limit of quantitation 0.08mg/L, 0.45mg/L;Respectively less than GBZ/T300.127-2017"Workplace is empty
Gas noxious material measures the 127th part:Esters of acrylic acid",GBZ/T300.68-2017"Workplace air noxious material is surveyed
Fixed 68th part:Styrene, methyl styrene and divinylbenzene"Detection limit and lower limit of quantitation.
Claims (2)
1. styrene and butyl acrylate method are measured using gas-mass spectrometer, it is characterized in that:Include the following steps, and
Following steps sequentially carry out,
Step 1: the chromatographic column for choosing gas chromatograph is HP-VOC, the operation reference conditions of gas chromatograph are set;Column temperature is
38 DEG C, keep 3min;80 DEG C are risen to 15 DEG C/min, keeps 2min;140 DEG C are risen to 5 DEG C/min, keeps 3min;Vaporizer
Temperature is 270 DEG C;Gas of carrier gas is nitrogen, flow 1mL/min;Split ratio is 10:1;
Step 2: setting mass spectrograph operates reference conditions;Electron impact ion source is EI;Ion source energy is 70eV;Ion source
Temperature is 230 DEG C;Quadrupole rod temperature is 150 DEG C;Interface temperature is 270 DEG C;Scanning range is 35amu~350amu;Solvent prolongs
It is 3min late;
Step 3: preparing standard solution, styrene and butyl acrylate are taken, with carbon disulfide desorption and constant volume, it is molten to obtain standard
A concentration of μ of 0.0 μ g/mL~600.0 g/mL of liquid;
Step 4: by step 3 obtain standard solution 4~7, sample introduction to after step 1 is arranged gas chromatograph with
The measurement of each concentration quantitative ion of standard series is carried out in mass spectrograph after step 2 setting, styrene characteristic ion is 78,
103,104, quota ion 104;The characteristic ion of n-butyl acrylate is 55,56,73, and quota ion 55 draws standard
Curve calculates regression equation, completes the measurement of styrene and butyl acrylate.
2. according to claim 1 measure styrene and butyl acrylate method, feature using gas-mass spectrometer
It is:Use the carbon disulfide desorption time for 30min in the step 3.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113671046A (en) * | 2020-05-13 | 2021-11-19 | 昆山石梅新材料科技有限公司 | Method for low-temperature separation and determination of styrene and butyl acrylate by gas chromatography |
Citations (3)
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| CN103487542A (en) * | 2013-09-11 | 2014-01-01 | 湖南中烟工业有限责任公司 | Method for concurrently detecting 23 ester compounds in cigarette water-base adhesive |
| CN107515264A (en) * | 2017-08-31 | 2017-12-26 | 中国检验检疫科学研究院 | Benzene homologues migrate quantity measuring method in food processing electrical appliance based on Dynamic headspace |
| CN107607639A (en) * | 2017-08-28 | 2018-01-19 | 浙江云广检测技术服务有限公司 | A kind of method that Solvent desorption Gas phase chromatography method surveys Air toxic substance |
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2018
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Patent Citations (3)
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|---|---|---|---|---|
| CN103487542A (en) * | 2013-09-11 | 2014-01-01 | 湖南中烟工业有限责任公司 | Method for concurrently detecting 23 ester compounds in cigarette water-base adhesive |
| CN107607639A (en) * | 2017-08-28 | 2018-01-19 | 浙江云广检测技术服务有限公司 | A kind of method that Solvent desorption Gas phase chromatography method surveys Air toxic substance |
| CN107515264A (en) * | 2017-08-31 | 2017-12-26 | 中国检验检疫科学研究院 | Benzene homologues migrate quantity measuring method in food processing electrical appliance based on Dynamic headspace |
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| 徐鑫等: "工作场所空气中39种有机溶剂的大口径毛细管气相色谱同时测定法", 《职业与健康》 * |
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| CN113671046A (en) * | 2020-05-13 | 2021-11-19 | 昆山石梅新材料科技有限公司 | Method for low-temperature separation and determination of styrene and butyl acrylate by gas chromatography |
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Application publication date: 20181023 |