A new method for rapid degree of substitution and purity determination of chloroform-soluble cellulose esters, using 31P NMR
[摘要] Chloroform-solublepalmiticanddecanoicacidestersofcelluloseweresynthesizedfromthereactionofMCCwithacidchloridesinLiCl/DMAandtheionicliquid[amim]Cl,asnovelcellulosesolvents.Aprocessofderivatizationoftheremaininghydroxylgroups,asphosphiteestersandsubsequent31PNMRanalysis,allowedforsimultaneousdegreeofsubstitution(DS)determinationandquantificationoftheaqueous-quenchacidby-productimpurity,aftertheappropriatecalculation.ThefullmathematicaltreatmentforDSdeterminationispresented,includingscriptsforthePythonandJavaprogramminglanguagesforrapidinterpretationofresults.ThismethodforDSdeterminationwasvalidatedagainsttraditionalanalysesofthepalmitoylcelluloseandthefullysubstitutedp-nitrobenzoylpalmitoyldiesterproduct,fromadditionalreactionwithp-nitrobenzoylchloride.DOSYNMRandSCOREanalyseswerealsoemployedtodemonstratetheutilityofthisrapid31Pderivatizationandanalyticalprocessovertraditional1DNMRanalyses...
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[效力级别] [学科分类] 分析化学
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