Method for detecting 1-vinyl imidazole in chemical product
A technology of vinylimidazole and detection method, which is applied in the directions of measuring devices, instruments, scientific instruments, etc., to achieve the effects of simple operation, symmetrical peak shape, high accuracy and precision
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Embodiment 1
[0017] Embodiment one 1-vinylimidazole standard curve
[0018] a. Reagent preparation
[0019] 50mM Potassium Dihydrogen Phosphate Buffer: Accurately weigh 6.8g of Potassium Dihydrogen Phosphate and 1g of Sodium Heptane Sulfonate into a 1L volumetric flask, add 900mL of water, adjust the pH to 3.5 with phosphoric acid, dilute to the mark with water, and mix well;
[0020] Standard stock solution: Accurately weigh an appropriate amount (accurate to 0.1mg) of the standard substance in a volumetric flask, dissolve in water and dilute to the mark, prepare a standard stock solution with a concentration of 1000μg / mL, store at 4°C, and have a validity period of 6 months ;
[0021] Standard intermediate solution: measure a certain volume of standard stock solution in a volumetric flask, dilute it with water and adjust the volume to the mark, prepare a standard intermediate solution of 100 μg / mL, store at 4°C, and have a validity period of 3 months;
[0022] Standard working solution...
Embodiment 2
[0027] The detection of 1-vinylimidazole in the sample of embodiment two
[0028] a. Sample pretreatment
[0029] Take a rubber product as a sample, cut it into small pieces below 3mm×3mm, then freeze and pulverize it to a powder sample with a particle size of no more than 1mm for use. Weigh about 1g of the sample into a 50mL centrifuge tube, add 40mL of methanol, mix well, ultrasonically extract for 20min, centrifuge at 4000r / min for 10min, take the supernatant and filter it through a filter membrane for testing.
[0030] b. Sample testing
[0031] The detection conditions are the same as in "Example 1".
[0032] c. Test results
[0033] Spectrum of the sample solution as image 3 As shown, it can be seen from the figure that the rubber sample does not detect a peak near the retention time of 1-vinylimidazole, that is, the rubber sample does not contain 1-vinylimidazole.
Embodiment 3
[0034] Embodiment three method accuracy and precision test
[0035] Select the above negative rubber sample as the matrix, and do two levels of standard addition experiments at 400mg / kg and 120mg / kg, with 6 parallels in each group. The spectrum diagram is for example Figure 4 The precision and accuracy results are shown in Table 1.
[0036] The recovery rate of this method is between 98.2-112.1%, and the RSD is 2.28-3.33%, which shows that this method has relatively good accuracy and precision.
[0037] Table 1. Accuracy and precision detection of 1-vinylimidazole spiked samples
[0038]
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