CN106198772A - Measure the method for low free toluene diisocyanate content in base polyurethane prepolymer for use as - Google Patents
Measure the method for low free toluene diisocyanate content in base polyurethane prepolymer for use as Download PDFInfo
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- CN106198772A CN106198772A CN201610424674.3A CN201610424674A CN106198772A CN 106198772 A CN106198772 A CN 106198772A CN 201610424674 A CN201610424674 A CN 201610424674A CN 106198772 A CN106198772 A CN 106198772A
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- 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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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G—PHYSICS
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- 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
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Abstract
A kind of measure the method for low free toluene diisocyanate content in base polyurethane prepolymer for use as be use high performance liquid chromatograph, detection wavelength be 220nm to 237nm, the mode of gradient elution, directly dissolve mensuration, peak area quantified by external standard method.The present invention has simple to operate, highly sensitive, and separating degree is good, and detection range is wide, the free TDI of energy Accurate Determining low concentration.
Description
Technical field
The invention belongs to a kind of method measuring toluene diisocyanate content, a kind of high performance liquid chromatography being specifically related to
Method measures the method for low free toluene diisocyanate (TDI) content in base polyurethane prepolymer for use as.
Technical background
TDI system polyurethane prepolymer exists unreacted toluene di-isocyanate(TDI) (i.e. free TDI), has strong thorn
Swashing abnormal smells from the patient, human body is worked the mischief after sucking by human body.Under the situation that the world today is the strictest to environmental requirement, in performed polymer
Free monomer content must control below 0.5%, have reaches less than 0.1%, and this allows for trace even microscratch amount
Analyze detection TDI content to necessitate.
At present, the detection method of free TDI content has three kinds: chemical method, gas chromatogram spectrometry, high performance liquid chromatography,
But all there are some problems in every kind of method.
Chemical method (1.Free Toluene Diisocyanatein Urelymers, ASTM method D2615-70,
American Society fo Testing and Materials, Phidelphia pa, 1974.) it is to use n-hexane extraction,
Dibutyl amine titrates, and the method process is simple, but is difficult to Accurate Determining.
During the content of gas chromatography and Gas Chromatography-Mass Spectrometry free TDI, (2.N.R.Neubauer,
G.R.Skreckoski, R.G.White and A.J.Kane, Anal.Chem.35 1647.) due to the heating of TDI prepolymer easily
Decomposing, during injector temperature height, prepolymer decomposes generation TDI, affects testing result；When vaporizer temperature is low, TDI can not be complete
Full gasification.So, there are serious problems in accuracy and precision.
High performance liquid chromatography comprises two kinds, one be with methanol derivative after with anti-phase C18 post (3.K.Marcali,
Anal.Chem., 29 552.), first alcohol and water does flowing phase, and UV-detector detects.This method to derive, cumbersome,
And pilot process can introduce error；Another kind is to use (4.Von Uwe Lotz fared+lack
Heft.Quantitative Bestimmung monomerer Isocyanate85:172-75) high performance liquid chromatography positive silicon
Glue post directly detects, but it is the highest all to there is separating degree, and detection sensitivity is low, and low concentration detects inaccurate problem.
Summary of the invention
It is an object of the invention to provide a kind of directly, quickly, easy, measure wide ranges, highly sensitive, accuracy is high, weight
The method of low-free TDI content in the high-performance liquid chromatogram determination base polyurethane prepolymer for use as that renaturation is good.
The method of the present invention comprises the steps of:
One, determining instrument and reagent:
(1) instrument
High performance liquid chromatograph (waters company) is used to include breeze 1525 pump, 2487 dual wavelength ultraviolet detectors,
Nova-Pak SiO2Chromatographic column (3.9x150mm, id 604 μm, waters company), analysis software is empower；
(2) reagent
Standard sample TDI, purchased from Bayer company of Germany；Flowing phase 2,2,4-trimethylpentane and 1,4-dioxane
For high-efficiency liquid chromatographic-grade reagent, purchased from Merck KGaA company；
Two, the quantitative analysis of low-free TDI in TDI base polyurethane prepolymer for use as
(1) configuration of standard solution
Accurately weigh TDI standard reagent 10mg-1g, be placed in the volumetric flask of 100ml, add initial flow phased soln and dilute
To scale, shake up, as standard solution storing solution, take above-mentioned storing solution 0.5ml, 1ml, 1.5ml, 2ml, 3ml, 5ml respectively, use
Initial flow phase dilution constant volume, in the volumetric flask of 50ml, is configured to 6 standard solution, is used for doing standard quantitative curve；
(2) testing sample configuration
Accurately weighing quality is MSampleTesting sample, be configured to liquid to be measured with initial flow phased soln, volume is VSample, to be measured
The concentration range of liquid is 20mg/ml-100mg/ml；
(3) measure
A () standard solution measures
Measuring the absorption value of each standard solution, draw standard curve, two absorption values of each METHOD FOR CONTINUOUS DETERMINATION take its meansigma methods
As result, 6 standard solution of above-mentioned configuration are taken 10 μ l high performance liquid chromatographs respectively and carries out gradient elution, initial flow
Dynamic be mutually volume ratio be pure isooctane and the Isosorbide-5-Nitrae-dioxane of 75:25, flow when being eluted to 4 minutes mutually direct
Become the Isosorbide-5-Nitrae-dioxane of 100%, the when of by 10 minutes, change to pure isooctane and Isosorbide-5-Nitrae-dioxane again
Mixed liquor, volume ratio is 75:25, flow velocity 0.6ml/min, and chromatogram column temperature is 25 DEG C, UV-detector detection wavelength can be
220nm to 237nm, integral area and concentration obtaining standard curve is y=a+bx；
B () liquid to be measured measures
Being taken by the liquid to be measured of above-mentioned configuration and carry out gradient elution on 10 μ l high performance liquid chromatographs, initial flow is body mutually
Long-pending ratio is pure isooctane and the Isosorbide-5-Nitrae-dioxane of 75:25, and flowing when being eluted to 4 minutes is directly changed mutually
Isosorbide-5-Nitrae-the dioxane of 100%, changes to the mixed of pure isooctane and Isosorbide-5-Nitrae-dioxane again when of by 10 minutes
Closing liquid, volume ratio is 75:25, flow velocity 0.6ml/min, and chromatogram column temperature is 25 DEG C, and UV-detector detection wavelength can be 220nm
To 237nm, utilize empower software to be obtained free TDI concentration in liquid to be measured by TDI standard curve, measure and average for twice
CSample；
(4) calculate
By formula, free TDI %=CSample╳VSample/MSample100%, it is calculated free TDI quality in performed polymer
Percent.
By the ultraviolet spectra of TDI solution is tested, obtain three ultraviolet absorption peaks, be respectively 207nm, 237nm and
284nm, but owing to the cutoff wavelength of flowing phase Isosorbide-5-Nitrae-dioxane is 215nm, so this patent has selected 220nm, but
Owing to 284nm absorption peak strength is little, so this patent has selected 220nm-237nm scope.
This patent have employed gradient elution, is primarily due in base polyurethane prepolymer for use as in addition to having free TDI, major part
Being polymer, Isosorbide-5-Nitrae-dioxane is big to the dissolubility of polymer, and eluting power is strong, so energy quickly eluting is complete, no
Residual and hangover can be caused.
This patent method has the advantage that compared with the conventional method
1. using and detect the wavelength that TDI uv absorption is the strongest, detection limit is low, highly sensitive, between each component
Separating degree is big, and testing result is accurate, and detection range is wide.
2. use gradient elution, save the testing time, the problem solving chromatographic peak hangover, reproducible, make to survey continuously
Try multiple sample to be possibly realized.
3. sample does not process through derivative grade, direct configuration testing, does not has middle loss and process simple, operation side
Just.
Accompanying drawing explanation
Fig. 1 TDI standard solution is at the standard curve of 220nm wavelength.
The high-efficient liquid phase chromatogram that Fig. 2 performed polymer LF950A obtains at 220nm ultraviolet wavelength gradient elution.
The high-efficient liquid phase chromatogram that Fig. 3 performed polymer LF800A obtains at 237nm ultraviolet wavelength gradient elution.
The high-efficient liquid phase chromatogram that Fig. 4 performed polymer LF800A obtains at 254nm ultraviolet wavelength isocratic elution.
The high-efficient liquid phase chromatogram that Fig. 5 performed polymer LF800A obtains at 220nm ultraviolet wavelength gradient elution.
Table 1LF800A sample is in 220nm and 254nm detection six measurement results of wavelength and relative standard deviation.
Detailed description of the invention:
Embodiment 1:
(1) instrument
High performance liquid chromatograph (waters company) is used to include breeze 1525 pump, 2487 dual wavelength ultraviolet detectors,
Nova-Pak SiO2Chromatographic column (3.9x150mm, id 604 μm, waters company), analysis software is empower；
(2) reagent
Standard sample TDI, purchased from Bayer company of Germany；Flowing phase 2,2,4-trimethylpentane and 1,4-dioxane
For high-efficiency liquid chromatographic-grade reagent, purchased from Merck KGaA company；
(3) mensuration of standard curve
Accurately weigh TDI standard reagent 0.0980g to 100ml volumetric flask, add initial flow phased soln, be configured to standard
Solution storing solution.Taking above-mentioned storing solution 0.5ml the most respectively, 1ml, 1.5ml, 2ml, 3ml, 5ml initial flow phased soln arrives
In the volumetric flask of 50ml, configuration standard series, takes each standard serial solution 10 μ l high performance liquid chromatograph respectively and carries out ladder
Degree eluting, initial flow be mutually volume ratio be pure isooctane and the Isosorbide-5-Nitrae-dioxane of 75:25, be eluted to 4 points
During clock flowing be directly changed mutually 100% Isosorbide-5-Nitrae-dioxane, change to again the when of by 10 minutes pure isooctane and
The mixed liquor of Isosorbide-5-Nitrae-dioxane, volume ratio is 75:25.Flow velocity 0.6ml/min, chromatogram column temperature is 25 DEG C, UV-detector
Detection, wavelength can be 220nm, integral area and concentration obtaining standard curve is y=228351+98750x, R2=0.9992,
Standard curve is shown in Fig. 1.
(4) testing sample measures
Accurately weigh 2.8148g sample LF950A (Chemtura Corporation, free TDI≤0.1wt%) flowing phased soln fixed
Hold and obtain liquid to be measured in 50ml volumetric flask.Take liquid 10 μ l to be measured and carry out gradient elution, fore flow with high performance liquid chromatograph
Dynamic be mutually volume ratio be pure isooctane and the Isosorbide-5-Nitrae-dioxane of 75:25, flow when being eluted to 4 minutes mutually direct
Become the Isosorbide-5-Nitrae-dioxane of 100%, the when of by 10 minutes, change to pure isooctane and Isosorbide-5-Nitrae-dioxane again
Mixed liquor, volume ratio is 75:25.Flow velocity 0.6ml/min, chromatogram column temperature is 25 DEG C, and UV-detector detects, and wavelength can be
220nm, the chromatogram recorded is shown in Fig. 2, it can be seen that the peak of TDI component can reach baseline separation, by peak area external standard method
Quantitatively, the concentration obtaining double mensuration is 25.34ug/ml and 25.13ug/ml, exists by being calculated free TDI monomer
Content in performed polymer is 0.045wt%.
Embodiment 2:
Accurately weigh 4.7148g sample LF800A (Chemtura Corporation, free TDI≤0.1wt%) flowing phased soln fixed
Hold and obtain liquid to be measured in 50ml volumetric flask.Use high performance liquid chromatograph gradient elution, ultraviolet detection wavelength 237nm, obtain
Chromatogram is shown in Fig. 3, it can be seen that the peak of TDI component can reach baseline separation, by peak area quantified by external standard method, obtains continuously
The concentration recording twice is 28.32ug/ml and 28.26ug/ml, is calculated free TDI monomer content in performed polymer and is
0.030%.Remaining is with embodiment 1.
Embodiment 3:
Accurately weigh 1.0215g sample LF950A (Chemtura Corporation, free TDI≤0.1wt%) flowing phased soln fixed
Hold and obtain liquid to be measured in 50ml volumetric flask.By liquid to be measured inject chromatograph of liquid gradient elution, ultraviolet detection wavelength 220nm,
The peak of TDI component can reach baseline separation, by peak area quantified by external standard method, obtains free TDI monomer in performed polymer
Content is 0.043%.Remaining is with embodiment 1.
Embodiment 4:
Accurately weigh 2.8148g sample LF950A (Chemtura Corporation, free TDI≤0.1wt%) flowing phased soln fixed
Hold and obtain liquid to be measured in 50ml volumetric flask.By liquid to be measured inject chromatograph of liquid gradient elution, ultraviolet detection wavelength 230nm,
The peak of TDI component can reach baseline separation, by peak area quantified by external standard method, obtains free TDI monomer in performed polymer
Content is 0.045%.
Embodiment 5:
Accurately weigh 4.7148g sample LF800A (Chemtura Corporation, free TDI≤0.1wt%) flowing phased soln fixed
Hold and obtain liquid to be measured in 50ml volumetric flask.Use high performance liquid chromatograph gradient elution, ultraviolet detection wavelength 220nm, obtain
Chromatogram is shown in Fig. 5, and remaining is with embodiment 1.Use external standard method peak area quantification, obtain the average result of six measurements and relative mark
Quasi-deviation RSD is shown in Table 1.
Comparative example 1:
Accurately weigh 4.7148g sample LF800A (Chemtura Corporation, free TDI≤0.1wt%) flowing phased soln fixed
Hold and obtain liquid to be measured in 50ml volumetric flask.Liquid to be measured injection high performance liquid chromatograph, the method in employing document, 2,2,4-
Trimethylpentane and Isosorbide-5-Nitrae-dioxane 4:1 isocratic elution by volume, ultraviolet detection wavelength 254nm, obtain liquid chromatogram
See Fig. 4.Use peak height quantified by external standard method, measure the average result obtained six times and relative standard deviation RSD is shown in Table 1.From figure
Can be seen that the peak of TDI component is smaller with the separating degree at other peak, the chromatographic peak peak height response of component TDI is the least, test
Result sensitivity and separating degree are the most bad, and quantitative Analysis time error is very big, and six test results show that repeatability is bad.Separately
Outward, the testing time is long, is eluted to 15 minutes elute the most completely.
From figure 5 it can be seen that the separating degree at the peak of TDI component and other peak is big in embodiment 5, response value is very big,
Absorption value is three times of comparative example 1, and sensitivity and the separating degree of test result are the highest, and six times test result shows reproducible.
And when 8 minutes, all of component can be eluted out in performed polymer, save elution time.
Table 1 LF800A sample is in 220nm and 254nm detection six measurement results of wavelength and relative standard deviation
Claims (1)
1. one kind measures the method for low free toluene diisocyanate content in base polyurethane prepolymer for use as, it is characterised in that include as follows
Step:
One, determining instrument and reagent:
(1) instrument
Use high performance liquid chromatograph, including breeze 1525 pump, 2487 dual wavelength ultraviolet detectors, Nova-Pak SiO2Color
Spectrum post, analysis software is empower；
(2) reagent
Standard sample TDI, purchased from Bayer company of Germany；Flowing phase 2,2,4-trimethylpentane and 1,4-dioxane are
High-efficiency liquid chromatographic-grade reagent, purchased from Merck KGaA company；
Two, the quantitative analysis of low-free TDI in TDI base polyurethane prepolymer for use as
(1) configuration of standard solution
Accurately weigh TDI standard reagent 10mg-1g, be placed in the volumetric flask of 100ml, add initial flow phased soln and be diluted to
Scale, shakes up, and as standard solution storing solution, takes above-mentioned storing solution 0.5ml, 1ml, 1.5ml, 2ml, 3ml, 5ml respectively, with just
The flowing phase dilution constant volume that begins, in the volumetric flask of 50ml, is configured to 6 standard solution, is used for doing standard quantitative curve；
(2) testing sample configuration
Accurately weighing quality is MSampleTesting sample, be configured to liquid to be measured with initial flow phased soln, volume is VSample, liquid to be measured
Concentration range is 20mg/ml-100mg/ml；
(3) measure
A () standard solution measures
Measuring the absorption value of each standard solution, draw standard curve, two absorption values of each METHOD FOR CONTINUOUS DETERMINATION take its meansigma methods conduct
As a result, 6 standard solution of above-mentioned configuration are taken 10 μ l high performance liquid chromatographs respectively and carry out gradient elution, initial flow phase
Be volume ratio be pure isooctane and the Isosorbide-5-Nitrae-dioxane of 75:25, when being eluted to 4 minutes flowing be directly changed mutually
Isosorbide-5-Nitrae-the dioxane of 100%, changes to pure isooctane and the mixing of Isosorbide-5-Nitrae-dioxane again when of by 10 minutes
Liquid, volume ratio is 75:25, flow velocity 0.6ml/min, and chromatogram column temperature is 25 DEG C, UV-detector detection wavelength can be 220nm extremely
237nm, integral area and concentration obtaining standard curve is y=a+bx；
B () liquid to be measured measures
Being taken by the liquid to be measured of above-mentioned configuration and carry out gradient elution on 10 μ l high performance liquid chromatographs, initial flow is volume ratio mutually
For pure isooctane and the Isosorbide-5-Nitrae-dioxane of 75:25, when being eluted to 4 minutes, flowing is directly changed the 1 of 100% mutually,
4-dioxane, changes to pure isooctane and the mixed liquor of Isosorbide-5-Nitrae-dioxane, volume again when of by 10 minutes
Ratio is 75:25, flow velocity 0.6ml/min, and chromatogram column temperature is 25 DEG C, and UV-detector detection wavelength can be 220nm to 237nm,
Utilize empower software to be obtained free TDI concentration in liquid to be measured by TDI standard curve, measure the C that averages for twiceSample；
(4) calculate
By formula, free TDI %=CSample╳VSample∕MSample100%, it is calculated free TDI mass percent in performed polymer.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106596772A (en) * | 2016-12-14 | 2017-04-26 | 东莞市凯欣电池材料有限公司 | Method for detecting aggregated double-bone compounds in lithium hexafluorophosphate electrolyte solution |
| CN108279276A (en) * | 2017-03-10 | 2018-07-13 | 泰州市产品质量监督检验中心 | The assay method of toluene di-isocyanate(TDI) residual quantity in a kind of sponge brassiere |
| CN110068616A (en) * | 2018-01-22 | 2019-07-30 | 联化科技股份有限公司 | The normal-phase chromatography analysis method of chloro- 2 nitrophenyl isocyanate of 4- and its reaction solution |
| CN111521695A (en) * | 2020-04-14 | 2020-08-11 | 中国建材检验认证集团苏州有限公司 | Method for rapidly detecting free toluene diisocyanate in polyurethane coating |
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| CN105367743A (en) * | 2015-12-21 | 2016-03-02 | 中国科学院山西煤炭化学研究所 | Synthetic method of waterborne polyurethane emulsion |
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| CN105367743A (en) * | 2015-12-21 | 2016-03-02 | 中国科学院山西煤炭化学研究所 | Synthetic method of waterborne polyurethane emulsion |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106596772A (en) * | 2016-12-14 | 2017-04-26 | 东莞市凯欣电池材料有限公司 | Method for detecting aggregated double-bone compounds in lithium hexafluorophosphate electrolyte solution |
| CN108279276A (en) * | 2017-03-10 | 2018-07-13 | 泰州市产品质量监督检验中心 | The assay method of toluene di-isocyanate(TDI) residual quantity in a kind of sponge brassiere |
| CN110068616A (en) * | 2018-01-22 | 2019-07-30 | 联化科技股份有限公司 | The normal-phase chromatography analysis method of chloro- 2 nitrophenyl isocyanate of 4- and its reaction solution |
| CN110068616B (en) * | 2018-01-22 | 2022-06-03 | 联化科技股份有限公司 | Normal phase chromatographic analysis method for 4-chlorine-2 nitrophenyl isocyanate and reaction liquid thereof |
| CN111521695A (en) * | 2020-04-14 | 2020-08-11 | 中国建材检验认证集团苏州有限公司 | Method for rapidly detecting free toluene diisocyanate in polyurethane coating |
| CN111521695B (en) * | 2020-04-14 | 2022-09-16 | 中国建材检验认证集团苏州有限公司 | Method for rapidly detecting free toluene diisocyanate in polyurethane coating |
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