A method for separation and determination of polycyclic aromatic hydrocarbons in hot melt adhesives
A polycyclic aromatic hydrocarbon and hot melt adhesive technology, applied in the field of analytical chemistry, can solve the problems of unreported determination of polycyclic aromatic hydrocarbons, and achieve the effects of low detection limit, good precision and feasible method
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Embodiment 1
[0029] A method for the separation and determination of polycyclic aromatic hydrocarbons in hot melt adhesive includes the following steps:
[0030] Step (1), extraction: accurately weigh 0.5g of the chopped sample into a 50mL round bottom flask, add 20mL n-hexane, and add 20μL of perylene-d at a concentration of 100μg / mL 12 The internal standard solution is heated and refluxed in a 70℃ water bath for 20 minutes until the hot melt adhesive sample is dissolved;
[0031] Step (2), purification: transfer the extract to a 50mL Erlenmeyer flask, put it in the refrigerator at -10°C and freeze for 10 minutes, and collect the supernatant after centrifugation; the supernatant is concentrated by evaporation under reduced pressure to 2mL, and then subjected to solid phase extraction Column, control the flow rate to 0.5 drops / s, add 5 mL of a mixture of n-hexane and dichloromethane for elution, where the volume ratio of n-hexane to dichloromethane is 3:2, collect and combine the column solution...
Embodiment 2
[0035] A method for the separation and determination of polycyclic aromatic hydrocarbons in hot melt adhesive includes the following steps:
[0036] Step (1), extraction: accurately weigh 0.2g of the chopped sample into a 25mL round bottom flask, add 8mL n-hexane, and add 20μL of perylene-d at a concentration of 100μg / mL 12 The internal standard solution was heated to reflux in a water bath at 70°C for 20 minutes, and the undissolved sample was added with 8 mL of n-hexane and extracted again for 20 minutes;
[0037] Step (2), purification: transfer the extract to a 50mL Erlenmeyer flask, put it in the refrigerator at -10°C and freeze for 10 minutes, and collect the supernatant after centrifugation; the supernatant is concentrated by evaporation under reduced pressure to 2mL, and then subjected to solid phase extraction Column, control the flow rate to 0.5 drops / s, add 5 mL of a mixture of n-hexane and dichloromethane for elution, where the volume ratio of n-hexane to dichloromethane...
Embodiment 3
[0041] A method for the separation and determination of polycyclic aromatic hydrocarbons in hot melt adhesive includes the following steps:
[0042] Step (1), extraction: accurately weigh 1.0g of the chopped sample into a 100mL round bottom flask, add 40mL n-hexane, and at the same time add 20μL of 100μg / mL perylene-d 12 The internal standard solution is heated and refluxed in a 70℃ water bath for 20 minutes until the sample is dissolved;
[0043] Step (2), purification: transfer the extract to a 50mL Erlenmeyer flask, put it in the refrigerator at -10°C and freeze for 10 minutes, and collect the supernatant after centrifugation; the supernatant is concentrated by evaporation under reduced pressure to 2mL, and then subjected to solid phase extraction Column, control the flow rate to 0.5 drops / s, add 5 mL of a mixture of n-hexane and dichloromethane for elution, where the volume ratio of n-hexane to dichloromethane is 3:2, collect and combine the column solution and elution Liquid t...
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