Gas chromatography of caprolactam polyamide resin residue.docVIP

 PAGE \* MERGEFORMAT 2 Gas chromatography of caprolactam polyamide resin residue Author: Yang Xianjiong Wang Aimin Lan Yanyu Li Yongjun He Xun [Abstract] Objective To establish a gas chromatography of caprolactam polyamide resin residue method. Methods A sample internal standard method in order to FFAP capillary column (30 m * 0.53 mm, 1 μ m) for the column, column temperature 175 ℃ , carrier gas nitrogen, pre-column pressure 20 kPa, inlet temperature of 220 ℃ , FID detector, detector temperature is 280 ℃ , the air flow rate 400 ml * min-1, hydrogen flow rate 40 ml * min-1. The results of caprolactam in the 5.85 ~ 374 μ g * ml-1 (r = 0.999 9) within the concentration range showed good linearity. The average recoveries were polyamide resin, caprolactam 100.6% (RSD = 2.7%), elution of caprolactam 99.96% (RSD = 3.0%). Conclusion The method is reproducible, accurate, easy to operate. [Keywords:] Gas chromatography of caprolactam polyamide resin residue Polyamide is a ε -caprolactam polymerization of a polymer material, due to ε -caprolactam ring-opening polymerization is a complex irreversible process, the reaction equilibrium of the products contain a certain amount of monomer and low molecular weight cyclic oligomerization material. Xin Shao injection preparation of freeze-dried powder injection process used in polyamide resin, polyamide in the caprolactam due to human eyes and central nervous stimulus, especially in the brain stem, can cause substantial damage to internal organs [1 ], so it must right to control residues of caprolactam. Reference to the relevant literature [2 ~ 6], we use gas chromatography polyamide resin residual ε -caprolactam monomer content, thus the evaluation of treatment effect for the polyamide one of the indicators. An instrument and reagent Shimadzu-14B gas chromatograph, hydrogen flame ionization detector; column: SE-54, OV-1701, FFAP large-diameter quartz capillary column (30 m * 0.53 mm, 1 μ m, homemade), high purity nitr