A detection method for the simultaneous determination of three isocyanates by pre-column derivatization-gas chromatography-mass spectrometry
A gas chromatography and pre-column derivatization technology, which is used in the field of product detection and analysis, can solve problems such as ineffective application detection, and achieve the effects of cheap equipment, high test accuracy and high purity.
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Embodiment 1
[0051] Selection and optimization of gas chromatography-mass spectrometry parameters
[0052] In order to obtain suitable gas chromatography-mass spectrometry parameters, selection and optimization of experimental conditions and instrument parameters: Japan Shimadzu GC-MS-QP2010 gas chromatography-mass spectrometer, equipped with an automatic sampler;
[0053] (1) Selection of chromatographic column
[0054] Considering that DB-5ms (30m×0.25mm×0.25μm) has the largest amount of use in each testing center, it is found through experiments that the chromatographic peak shape under this chromatographic column is symmetrical and correspondingly high, so this chromatographic column is preferred as the experimental chromatographic column, Other chromatographic columns with comparable performance can also be selected;
[0055] (2) Optimization of the inlet temperature
[0056] Select different inlet temperatures and observe the change of the chromatographic peak area of each target...
Embodiment 2
[0066] Determination of 2,4-TDI, 2,6-TDI and MDI Content in Leather Samples
[0067] (1) Sample preparation
[0068] Take a leather sample, cut it into pieces with a side length of 2mm~4mm, and mix well;
[0069] (2) Extraction and reaction of samples
[0070] Accurately weigh 1.0g of the above-mentioned leather sample (accurate to 0.0001g) and place it in a 50mL glass conical flask, add 20mL of acetone to mix well, close the lid tightly, place it in an ultrasonic cleaner for extraction for 30min, filter out the solvent, and then add 20mL Acetone, repeat the extraction once, combine the extracts in a 100mL rotary evaporator, and slowly evaporate to dryness with a rotary evaporator in a 30°C water bath;
[0071] (3) Derivatization reaction
[0072] Accurately pipette 10mL of the residue in the acidic aqueous reaction rotary steamer, vortex for 3min, pipette 2mL of the reacted test solution into a 10mL test tube, add sodium hydroxide solution to neutralize the excess acid, mi...
Embodiment 3
[0099] Establishment of 2,4-TDA, 2,6-TDA or MDA linear relationship in the detection of leather, artificial leather and textiles
[0100] Using the method in Example 2, use the standard solution of 2,4-TDA, 2,6-TDA or MDA diluted with blank matrix solution for GC-MS analysis, the prepared concentrations are: 1 mg / L, 2 mg / L , 5mg / L, 10 mg / L, the measurement results were analyzed by the workstation software, the measurement linear range was 1~10mg / L, and the detection limit LOD was 1mg / L. Taking leather as an example, the standard curve diagram obtained is shown in Figure 6~8, the abscissa in the figure represents the concentration (mg / L), and the ordinate of the total ratio represents the peak area. For the actual sample, the bottom line LOQ of the measurement is all less than 2 μg / mL. Under the experimental conditions determined by this method, the linear equations and correlation coefficients of other matrices are shown in Table 3 (where Y is the peak area, X is the concent...
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