高纯溶剂制备纯化及标准化研究

Purification and Standardization of High Purity Grade Solvents

在科技部与质检总局资助下,开展色谱级、农残级、质谱级以及电子级等高纯溶剂制备纯化及标准化关键技术研究。在纯化关键技术方面,通过双塔精密精馏去除痕量同分异构体、同系物等杂质专利技术,从工业级直接制备得到农残级、质谱级高纯溶剂。在高纯试剂标准化方面,制订了《仪器分析用高纯水规格及试验方法》国家标准;建立了GB/T30301《高纯试剂试验方法通则》、GB/T 32263《高纯化合物农残级试剂的测定气相色谱-电子捕获检测器(ECD)法》等系列高纯试剂国家方法标准,以及HG/T 4747《农药残留检测用试剂正己烷》等高纯溶剂行业产品标准,填补了国内高纯试剂检测标准的空白。

With the support of the general administration of quality supervision,inspection and quarantine of the people＇s republic of China（ AQSIQ） and the ministry of science and technology of the people＇s public of China（ MOST）,this work was aimed to develop the key purification standardization techniques of high purity grade solvents including HPLC grade,pesticide analysis grade,LC-MS grade and electronic grade high purity solvents. In the term of key purification standardization technologies,works were performed with twin towers precision distillation to isolate trace level impurities,including isomers and homologue,patent processes were developed scaled up in which the high purity solvent such as pesticide analysis grade n-hexane can be directly produced from industrial crudes. Further,series of standards related to high purity solvents were developed including ultra pure water for instrumental analysis-specification test methods,GB / T 30301 General Rule for Test Methods of Highly Purified Reagents,GB / T 32263 High purity grade compound,determination of pesticide analysis grade reagent with gas chromatographyelectron capture detector（ ECD） method and HG / T 4747 Reagent n-Hexane for Pesticide Residue Analysis. All these standards meet the needs of domestic test methods of highly purified reagents,which can help to regulate the domestic market,play a key role in promoting solvents market.