CN112557540A - Method for measuring toluene-2, 6-diisocyanate in memory health care pillow by gas chromatography-mass spectrometry - Google Patents
Method for measuring toluene-2, 6-diisocyanate in memory health care pillow by gas chromatography-mass spectrometry Download PDFInfo
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Abstract
The invention discloses a method for measuring toluene-2, 6-diisocyanate in a memory health care pillow by a gas chromatography-mass spectrometry method, which comprises the following instruments and reagents: agilent 7890B/7000DGC-QQ, Agilent MassHunter 4.2 workstation, capillary column: HP-5MS (15m 0.250mm 0.25Um), multifunctional nitrogen blower: n-20, microsyringe: 10uL of the steel bar, a toluene-2, 6-diisocyanate standard substance and toluene; the determination method comprises the following steps: s1, sample treatment, S2, standard solution preparation, S3, analytical determination and S4 and sample recovery, wherein the S1 sample treatment comprises the following steps: a1, crushing and preparing liquid, a2, concentrating and processing, wherein the step of preparing the standard solution by S2 comprises the following steps: b1, primary configuration and b2 multi-stage dilution. The method has the advantages of high accuracy, simple and convenient operation and low cost, is suitable for rapid qualitative and quantitative determination of toluene-2, 6-diisocyanate in the memory health care pillow, has high sample recovery rate and small relative standard deviation, and can improve the sensitivity of analysis by adopting ion Scanning (SIM) to acquire data.
Description
Technical Field
The invention relates to the technical field of chromatographic analysis, in particular to a method for measuring toluene-2, 6-diisocyanate in a memory health-care pillow by a gas chromatography-mass spectrometry method.
Background
The main material of the memory health care pillow is polyurethane, and the toluene-2, 6-diisocyanate is mainly used in polyurethane products, so that respiratory mucosa is directly damaged by high-concentration contact, asthmatic bronchitis is generated, and pneumonia and pulmonary edema can be caused. Vapors and liquids are irritating to the eye. Some people generate allergy after contacting the product for many times, and even if the contact is extremely trace, typical asthma attack can be caused, and the product has sensitization on the skin. Therefore, the detection of the toluene-2, 6-diisocyanate on the memory health care pillow commonly used by people is of great significance.
Disclosure of Invention
The invention aims to provide a method for measuring toluene-2, 6-diisocyanate in a memory health-care pillow by a gas chromatography-mass spectrometry method, so as to solve the problems in the background technology.
A method for measuring toluene-2, 6-diisocyanate in a memory health care pillow by a gas chromatography-mass spectrometry method comprises the following instruments and reagents: agilent 7890B/7000DGC-QQ, Agilent MassHunter 4.2 workstation, capillary column: HP-5MS (15m 0.250mm 0.25Um), multifunctional nitrogen blower: n-20, microsyringe: 10uL of the steel bar, a toluene-2, 6-diisocyanate standard substance and toluene; the determination method comprises the following steps: s1, sample treatment, S2, standard solution preparation, S3, analytical determination and S4 and sample recovery, wherein the S1 sample treatment comprises the following steps: a1, crushing and preparing liquid, a2, concentrating and processing, wherein the step of preparing the standard solution by S2 comprises the following steps: b1, primary configuration and b2 multi-stage dilution.
S1, sample treatment: selecting a memory testing health care pillow by a sampling investigation method, collecting a plurality of parts of polyurethane in a sample for later use, and treating the collected polyurethane by steps of a1, crushing and preparing a liquid, a2, concentrating, processing on a machine and the like;
a1, crushing and preparing liquid: crushing a polyurethane sample by a crushing device, weighing 1g of the sample in a 50mL colorimetric tube, adding 25mL of toluene, adding a stopper, shaking for 2min, standing for 10min, taking the liquid in a 50mL volumetric flask, and repeating for 1 time;
a2, concentrating and processing: selecting 10mL of sample liquid which is subjected to a1 and crushed liquid preparation, concentrating to 1mL, and passing through a membrane and loading on a machine;
s2, preparing a standard solution: weighing a plurality of parts of a quantitative standard toluene-2, 6-diisocyanate standard substance for later use, and respectively processing the weighed quantitative standard toluene-2, 6-diisocyanate standard substance through b1, primary preparation, b2 multistage dilution and other steps;
b1, primary configuration: selecting 0.025g of standard substance, adding the standard substance into a 25mL volumetric flask, adding toluene to a constant volume to a scale, and preparing a toluene-2, 6-diisocyanate solution with the concentration of 1 mg/mL;
b2 multistage dilution: taking a quantitative standard solution which is subjected to b1 and is primarily prepared, and gradually diluting the standard solution with toluene to obtain a toluene-2, 6-diisocyanate solution standard solution, wherein the concentrations of the diluted toluene-2, 6-diisocyanate solution are respectively as follows: 0.1mg/L, 0.2mg/L, 0.3mg/L, 0.4mg/L, 0.5mg/L, and 0.6 mg/L;
s3, analysis and measurement: calculating a regression equation of toluene-2, 6-diisocyanate solution which is subjected to multistage dilution through b2 by using the mean value of ion abundance to the concentration of toluene-2, 6-diisocyanate, selecting an HP-5MS column as a separation column, collecting data of sample solution which is subjected to a2 and concentrated processing by using ion Scanning (SIM), using an m/z90.0 fragment peak as a quantitative peak, calculating the regression equation by using the mean value of ion abundance to the concentration of toluene-2, 6-diisocyanate, preparing 0.1mg/L standard solution, adopting no-split sample injection, measuring signal noise, weighing 1g of sample amount, determining the volume to be 50mL, and concentrating 10mL to 1mL of sample amount to 1uL (same standard sample);
s4, sample recovery: respectively adding 5uL, 10uL and 20uL of toluene-2, 6-diisocyanate standard stock solution (20mg/L) into a sample with the concentration of 0.1mg/L, wherein the adding amount is 100ug, 200ug and 400 ug;
as a further improvement of the invention, in the determination method, after the step a1, the crushing liquid preparation is crushed, the crushed sample is heated, the temperature of the heating treatment is controlled to be 13-15 ℃, the heating time is 5min, and the temperature is controlled to be about 13 ℃ in the process of adding toluene and shaking for fusion.
As a further improvement of the invention, the experimental conditions in the determination method are as follows: the sample inlet temperature is 220 ℃, the sample injection mode is not divided, and the column temperature is as follows: 50 ℃, column flow rate: 1.0mL/min, the spacer purge flow rate is 3mL/min, the ion source temperature is 230 ℃, the MS1 quadrupole temperature is 150 ℃, and the MS2 quadrupole temperature is 150 ℃; SCAN mode: the mass range is 30-300, m/z for qualitative use is 174.0, and an SIM mode is selected; the quantitative determination was carried out at m/z 90.0.
As a further improvement of the present invention, the toluene-2, 6-diisocyanate standard in the present assay is Michael CAS91-08-7, where toluene is the chromatographic alcohol.
As a further improvement of the present invention, the toluene-2, 6-diisocyanate solution after dilution in the multi-stage dilution of step b2 in the present measurement method was repeated 2 times per concentration for characterization of retention time and abundance ratio of mass spectrum peaks, 0.1mg/L, 0.2mg/L, 0.3mg/L, 0.4mg/L, 0.5mg/L, and 0.6 mg/L.
As a further improvement of the invention, in the measuring method, in step S3, the factors of the column temperature of the separation column, the temperature of the vaporizing chamber, the flow rate of the carrier gas and the like are analyzed and measured to carry out orthogonal comparison experiments.
As a further improvement of the present invention, in step S3, the regression equation is calculated as the average value of the ion abundance in the analytical measurement for the concentration (ug/L) of p-toluene-2, 6-diisocyanate as y 3092.352785 × 17488.341902, and the correlation coefficient r is 0.9996.
As a further improvement of the present invention, in the present measurement method, 6 samples at each concentration in the sample collection at step S4 are subjected to sample treatment in accordance with the sample treatment method.
As a further improvement of the invention, in the determination method, in the step a1, the preheating treatment is carried out before the toluene in the crushing liquid preparation is added, the oscillation temperature of the added toluene is ensured to be 13 ℃, and the temperature reduction treatment is carried out after the oscillation is static, so that the temperature of the liquid is ensured to be about 0 ℃.
Compared with the prior art, the invention has the beneficial effects that:
1. in the present invention, the determination is performed by setting up the steps of S1, sample treatment, S2, preparing standard solution and S3, analysis, wherein the S1 sample treatment comprises: a1, crushing and preparing liquid, a2, concentrating and processing, wherein the step of preparing the standard solution by S2 comprises the following steps: b1, primary preparation and b2 multi-stage dilution, high determination accuracy, simple and convenient operation and low cost, and is suitable for rapid qualitative and quantitative determination of toluene-2, 6-diisocyanate in the memory health care pillow;
2. according to the invention, step a1, after the crushing liquid preparation is finished, the crushed sample is heated, the heating temperature is controlled to be 13-15 ℃, the heating time is 5min, the toluene-2, 6-diisocyanate can be melted and enter a liquid state, the extraction can be more effectively and thoroughly carried out, and the detection accuracy is further improved;
3. in the invention, the step S4 is arranged, the sample is recovered, the sample recovery rate is high, and the relative standard deviation is small;
4. in the invention, the step S3 is set, analysis and measurement are carried out, the data of the sample solution which is processed by a2 and a concentrating machine are collected through ion Scanning (SIM), and the data are collected through the ion Scanning (SIM), so that the analysis sensitivity can be improved.
Drawings
FIG. 1 is a general flowchart of a method for determining toluene-2, 6-diisocyanate in a memory health pillow by using a gas chromatography-mass spectrometry method according to the present invention;
FIG. 2 is a linear view of a method for measuring toluene-2, 6-diisocyanate in the memory health pillow by using a gas chromatography-mass spectrometry method according to the present invention;
FIG. 3 is a chromatogram of a method for determining toluene-2, 6-diisocyanate in a memory health pillow by using a gas chromatography-mass spectrometry method;
FIG. 4 is a line mass spectrum of a method for determining toluene-2, 6-diisocyanate in the memory health care pillow by using a gas chromatography-mass spectrometry method according to the present invention;
FIG. 5 is a full scan of a method for determining toluene-2, 6-diisocyanate in the memory health care pillow by using a gas chromatography-mass spectrometry method.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Examples
Referring to fig. 1-5, the present invention provides the following technical solutions: a method for measuring toluene-2, 6-diisocyanate in a memory health care pillow by a gas chromatography-mass spectrometry method comprises the following instruments and reagents: agilent 7890B/7000DGC-QQ, Agilent MassHunter 4.2 workstation, capillary column: HP-5MS (15m 0.250mm 0.25Um), multifunctional nitrogen blower: n-20, microsyringe: 10uL of the steel bar, a toluene-2, 6-diisocyanate standard substance and toluene; the determination method comprises the following steps: s1, sample treatment, S2, standard solution preparation, S3, analytical determination and S4 and sample recovery, wherein the S1 sample treatment comprises the following steps: a1, crushing and preparing liquid, a2, concentrating and processing, wherein the step of preparing the standard solution by S2 comprises the following steps: b1, primary configuration and b2 multi-stage dilution.
S1, sample treatment: selecting a memory testing health care pillow by a sampling investigation method, collecting a plurality of parts of polyurethane in a sample for later use, and treating the collected polyurethane by steps of a1, crushing and preparing a liquid, a2, concentrating, processing on a machine and the like;
a1, crushing and preparing liquid: crushing a polyurethane sample by a crushing device, weighing 1g of the sample in a 50mL colorimetric tube, adding 25mL of toluene, adding a stopper, shaking for 2min, standing for 10min, taking the liquid in a 50mL volumetric flask, and repeating for 1 time;
a2, concentrating and processing: selecting 10mL of sample liquid which is subjected to a1 and crushed liquid preparation, concentrating to 1mL, and passing through a membrane and loading on a machine;
s2, preparing a standard solution: weighing a plurality of parts of a quantitative standard toluene-2, 6-diisocyanate standard substance for later use, and respectively processing the weighed quantitative standard toluene-2, 6-diisocyanate standard substance through b1, primary preparation, b2 multistage dilution and other steps;
b1, primary configuration: selecting 0.025g of standard substance, adding the standard substance into a 25mL volumetric flask, adding toluene to a constant volume to a scale, and preparing a toluene-2, 6-diisocyanate solution with the concentration of 1 mg/mL;
b2 multistage dilution: taking a quantitative standard solution which is subjected to b1 and is primarily prepared, and gradually diluting the standard solution with toluene to obtain a toluene-2, 6-diisocyanate solution standard solution, wherein the concentrations of the diluted toluene-2, 6-diisocyanate solution are respectively as follows: 0.1mg/L, 0.2mg/L, 0.3mg/L, 0.4mg/L, 0.5mg/L, and 0.6 mg/L;
s3, analysis and measurement: calculating a regression equation of toluene-2, 6-diisocyanate solution which is subjected to multistage dilution through b2 by using the mean value of ion abundance to the concentration of toluene-2, 6-diisocyanate, selecting an HP-5MS column as a separation column, collecting data of sample solution which is subjected to a2 and concentrated computer processing through ion Scanning (SIM), using an m/z90.0 fragment peak as a quantitative peak, calculating the regression equation by using the mean value of ion abundance to the concentration of toluene-2, 6-diisocyanate, preparing 0.1mg/L standard solution, adopting non-split sample injection, wherein the sample injection amount is 1uL, the measured signal-to-noise ratio is 3.6, the detection limit is calculated by using 3 times of noise, and the detection limit of an instrument is obtained as:
s4, sample recovery: 5uL, 10uL and 20uL of toluene-2, 6-diisocyanate standard stock solution (20mg/L) are respectively added into a sample with the concentration of 0.1mg/L, the adding amount is respectively 100ug, 200ug and 400ug, the recovery rate of the sample is 94.6-97.7%, and the Relative Standard Deviation (RSD) is 0.5-1.7%.
The measurement results are shown in Table 1;
TABLE 1
In some embodiments of the present invention, in the step a1, after the pulverization of the pulverization solution, the pulverized sample is heated, the temperature of the heating is controlled to be 13 ℃ to 15 ℃, the heating time is 5min, and the temperature is controlled to be about 13 ℃ during the process of adding toluene and shaking for fusion.
In some embodiments of the invention, the assay conditions in the assay are: the sample inlet temperature is 220 ℃, the sample injection mode is not divided, and the column temperature is as follows: 50 ℃, column flow rate: 1.0mL/min, the spacer purge flow rate is 3mL/min, the ion source temperature is 230 ℃, the MS1 quadrupole temperature is 150 ℃, and the MS2 quadrupole temperature is 150 ℃; SCAN mode: the mass range is 30-300, m/z for qualitative use is 174.0, and an SIM mode is selected; the quantitative determination was carried out at m/z 90.0.
In some embodiments of the invention, the toluene-2, 6-diisocyanate standard in the assay is Michael CAS91-08-7, where toluene is the chromatographic alcohol.
In some embodiments of the present invention, the toluene-2, 6-diisocyanate solution after dilution in the multi-stage dilution of step b2 in the present assay method was repeated 2 times per concentration for characterization by retention time and abundance ratio of mass spectrum peaks, 0.1mg/L, 0.2mg/L, 0.3mg/L, 0.4mg/L, 0.5mg/L, and 0.6 mg/L.
In some embodiments of the present invention, step S3 of the determination method, the analysis determination, and the like, perform orthogonal comparison experiments on the column temperature, the vaporization chamber temperature, the carrier gas flow rate, and the like of the separation column.
In some embodiments of the present invention, in step S3 of the assay, the regression equation is calculated as the mean value of the ion abundance for the concentration of p-toluene-2, 6-diisocyanate (ug/L) in the assay as y 3092.352785 x +17488.341902 and the correlation coefficient r 0.9996.
In some embodiments of the present invention, the 6 samples at each concentration in the sample recovery in step S4 of the present assay method are processed according to the sample processing method.
In some embodiments of the present invention, in the step a1, the preheating treatment is performed before adding the toluene in the pulverization solution, so as to ensure that the oscillation temperature of toluene is 13 ℃, and the temperature reduction treatment is performed after oscillation and standing, so as to ensure that the temperature of the liquid is about 0 ℃.
In the invention, a gas chromatography-mass spectrometer is used for detecting toluene-2, 6-diisocyanate in the memory health care pillow to calculate a regression equation of y being 3092.352785 x +17488.341902, a correlation coefficient r being 0.9996, the detection limit being 0.016mg/g, the recovery rate being 94.6-97.7%, and the Relative Standard Deviation (RSD) being 0.5-1.7%. The detection method has the advantages of high accuracy of qualitative and quantitative analysis results, simplicity and convenience in operation, sensitivity, rapidness, high determination accuracy, simplicity and convenience in operation and low cost, is suitable for rapid qualitative and quantitative determination of toluene-2, 6-diisocyanate in the memory health care pillow, is high in sample recovery rate and small in relative standard deviation, and can improve analysis sensitivity and further improve detection accuracy by collecting data through ion Scanning (SIM).
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (9)
1. A method for measuring toluene-2, 6-diisocyanate in a memory health care pillow by a gas chromatography-mass spectrometry method is characterized by comprising the following steps: the determination method comprises the following instruments and reagents: agilent 7890B/7000DGC-QQ, Agilent MassHunter 4.2 workstation, capillary column: HP-5MS (15m 0.250mm 0.25Um), multifunctional nitrogen blower: n-20, microsyringe: 10uL of the steel bar, a toluene-2, 6-diisocyanate standard substance and toluene; the determination method comprises the following steps: s1, sample treatment, S2, standard solution preparation, S3, analytical determination and S4 and sample recovery, wherein the S1 sample treatment comprises the following steps: a1, crushing and preparing liquid, a2, concentrating and processing, wherein the step of preparing the standard solution by S2 comprises the following steps: b1, primary configuration and b2 multi-stage dilution.
S1, sample treatment: selecting a memory testing health care pillow by a sampling investigation method, collecting a plurality of parts of polyurethane in a sample for later use, and treating the collected polyurethane by steps of a1, crushing and preparing a liquid, a2, concentrating, processing on a machine and the like;
a1, crushing and preparing liquid: crushing a polyurethane sample by a crushing device, weighing 1g of the sample in a 50mL colorimetric tube, adding 25mL of toluene, adding a stopper, shaking for 2min, standing for 10min, taking the liquid in a 50mL volumetric flask, and repeating for 1 time;
a2, concentrating and processing: selecting 10mL of sample liquid which is subjected to a1 and crushed liquid preparation, concentrating to 1mL, and passing through a membrane and loading on a machine;
s2, preparing a standard solution: weighing a plurality of parts of a quantitative standard toluene-2, 6-diisocyanate standard substance for later use, and respectively processing the weighed quantitative standard toluene-2, 6-diisocyanate standard substance through b1, primary preparation, b2 multistage dilution and other steps;
b1, primary configuration: selecting 0.025g of standard substance, adding the standard substance into a 25mL volumetric flask, adding toluene to a constant volume to a scale, and preparing a toluene-2, 6-diisocyanate solution with the concentration of 1 mg/mL;
b2 multistage dilution: taking a quantitative standard solution which is subjected to b1 and is primarily prepared, and gradually diluting the standard solution with toluene to obtain a toluene-2, 6-diisocyanate solution standard solution, wherein the concentrations of the diluted toluene-2, 6-diisocyanate solution are respectively as follows: 0.1mg/L, 0.2mg/L, 0.3mg/L, 0.4mg/L, 0.5mg/L, and 0.6 mg/L;
s3, analysis and measurement: calculating a regression equation of toluene-2, 6-diisocyanate solution which is subjected to multistage dilution through b2 by using the mean value of ion abundance to the concentration of toluene-2, 6-diisocyanate, selecting an HP-5MS column as a separation column, collecting data of sample solution which is subjected to a2 and concentrated processing by using ion Scanning (SIM), using an m/z90.0 fragment peak as a quantitative peak, calculating the regression equation by using the mean value of ion abundance to the concentration of toluene-2, 6-diisocyanate, preparing 0.1mg/L standard solution, adopting no-split sample injection, measuring signal noise, weighing 1g of sample amount, determining the volume to be 50mL, and concentrating 10mL to 1mL of sample amount to 1uL (same standard sample);
s4, sample recovery: 5uL, 10uL and 20uL of toluene-2, 6-diisocyanate standard stock solution (20mg/L) are respectively added into a sample with the concentration of 0.1mg/L, and the adding amount is respectively 100ug, 200ug and 400 ug.
2. The method for determining toluene-2, 6-diisocyanate in the memory health care pillow by using the gas chromatography-mass spectrometry as claimed in claim 1, wherein the method comprises the following steps: in the determination method, the step a1, after the crushing liquid preparation is finished, the crushed sample is heated, the heating temperature is controlled to be 13-15 ℃, the heating time is 5min, and the temperature is controlled to be about 13 ℃ in the process of adding toluene and shaking and fusing.
3. The method for determining toluene-2, 6-diisocyanate in the memory health care pillow by using the gas chromatography-mass spectrometry as claimed in claim 1, wherein the method comprises the following steps: the experimental conditions in the determination method are as follows: the sample inlet temperature is 220 ℃, the sample injection mode is not divided, and the column temperature is as follows: 50 ℃, column flow rate: 1.0mL/min, the spacer purge flow rate is 3mL/min, the ion source temperature is 230 ℃, the MS1 quadrupole temperature is 150 ℃, and the MS2 quadrupole temperature is 150 ℃; SCAN mode: the mass range is 30-300, m/z for qualitative use is 174.0, and an SIM mode is selected; the quantitative determination was carried out at m/z 90.0.
4. The method for determining toluene-2, 6-diisocyanate in the memory health care pillow by using the gas chromatography-mass spectrometry as claimed in claim 1, wherein the method comprises the following steps: in the determination method, the toluene-2, 6-diisocyanate standard is Michael CAS91-08-7, wherein toluene is chromatographic alcohol.
5. The method for determining toluene-2, 6-diisocyanate in the memory health care pillow by using the gas chromatography-mass spectrometry as claimed in claim 1, wherein the method comprises the following steps: in the determination method, the toluene-2, 6-diisocyanate solution after dilution in the step b2 multi-stage dilution is repeated for 2 times at each concentration of 0.1mg/L, 0.2mg/L, 0.3mg/L, 0.4mg/L, 0.5mg/L and 0.6mg/L, and is characterized by retention time and abundance ratio of mass spectrum peaks.
6. The method for determining toluene-2, 6-diisocyanate in the memory health care pillow by using the gas chromatography-mass spectrometry as claimed in claim 1, wherein the method comprises the following steps: in the measuring method, in step S3, the factors such as the column temperature of the separation column, the temperature of the vaporizing chamber, the flow rate of the carrier gas and the like are analyzed and measured to carry out an orthogonal comparison experiment.
7. The method for determining toluene-2, 6-diisocyanate in the memory health care pillow by using the gas chromatography-mass spectrometry as claimed in claim 1, wherein the method comprises the following steps: in the step S3 of the present measurement method, the mean value of the ion abundance in the analytical measurement of the concentration (ug/L) of p-toluene-2, 6-diisocyanate is used to calculate the regression equation of y 3092.352785 x +17488.341902, and the correlation coefficient r 0.9996.
8. The method for determining toluene-2, 6-diisocyanate in the memory health care pillow by using the gas chromatography-mass spectrometry as claimed in claim 1, wherein the method comprises the following steps: in the present measurement method, in step S4, samples of 6 concentrations were collected, and the samples were processed according to the sample processing method.
9. The method for determining toluene-2, 6-diisocyanate in the memory health care pillow by using the gas chromatography-mass spectrometry as claimed in claim 2, wherein the method comprises the following steps: in the determination method, in the step a1, the toluene is preheated before being added into the crushing liquid preparation, the oscillation temperature of toluene addition is ensured to be 13 ℃, and meanwhile, the temperature is reduced after oscillation and standing, and the temperature of liquid is ensured to be about 0 ℃.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5670573A (en) * | 1996-08-07 | 1997-09-23 | E. I. Du Pont De Nemours And Company | Coatings containing fluorinated esters |
| JP2000019166A (en) * | 1998-06-30 | 2000-01-21 | Nippon Polyurethane Ind Co Ltd | Tolylene diisocyanate analysis method |
| 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 |
| 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 |
-
2020
- 2020-12-04 CN CN202011397189.4A patent/CN112557540A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5670573A (en) * | 1996-08-07 | 1997-09-23 | E. I. Du Pont De Nemours And Company | Coatings containing fluorinated esters |
| JP2000019166A (en) * | 1998-06-30 | 2000-01-21 | Nippon Polyurethane Ind Co Ltd | Tolylene diisocyanate analysis method |
| 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 |
| 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 |
Non-Patent Citations (5)
| Title |
|---|
| OH, CHANG-HWAN 等: "Analysis of toluene diisocyanate of adhesives in food contact materials by GC/MS", 《ANALYTICAL SCIENCE AND TECHNOLOGY》 * |
| 中华人民共和国国家质量监督检验检疫总局: "《中华人民共和国出入境检验检疫行业标准 SN/T 3802-2014》", 30 November 2014, 中国标准出版社出版 * |
| 刘昌宁等: "聚氨酯防水涂料中游离甲苯二异氰酸酯的气相色谱分析法优化", 《中国建筑防水》 * |
| 张燕红等: "聚氨酯涂料中游离TDI的毛细管气相色谱分析", 《聚氨酯工业》 * |
| 龙尚俊等: "内标曲线法测定聚氨酯胶粘剂中游离甲苯二异氰酸酯含量", 《贵州科学》 * |
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