Hydrogen peroxide(H2O2)precipitation from sodium aluminate(SA)solution at close-ambient temperature is an efficient method to synthesize boehmite and its derived alumina with high surface area,but the precipitation yi...Hydrogen peroxide(H2O2)precipitation from sodium aluminate(SA)solution at close-ambient temperature is an efficient method to synthesize boehmite and its derived alumina with high surface area,but the precipitation yield of Al2O3 is usually below 50%in highly alkaline SA solutions.Here the synthesis of boehmite is enhanced through a precarbonization-assisted H2O2 route in highly alkaline SA solutions.It is found that the crystal structure of the precipitation product is evidently influenced by the precipitation conditions.As the precipitation temperature increases from 273 to 325 K,a small amount of gibbsite by-product is formed.As the aging temperature increases from 301 to 333 K,the crystallinity of boehmite decreases and part of the boehmite dissolves due to an increase in the pH value.Based on the above results,a precarbonization-assisted H2O2 route is proposed to obtain pure boehmite with more complete recovery of Al2O3 from highly alkaline SA solutions.The route includes a controllable precarbonization step of SA solutions with a molar ratio of Na2O to Al2O3 higher than 2:1,followed by the H2O2-precipitated step with a molar ratio of H2O2 to Al2O3 less than 7:1.Because of its facile operation conditions,no extraneous impurity,time saving and a possible recycle of the filtrate,the route has great potential to be an alternative method for preparation of boehmite and its derived alumina.展开更多
建立了不使用离子对试剂,液质联用技术检测鳗鱼中链霉素和双氢链霉素残留量的检测方法。样品经三氯乙酸溶液提取,碱性氧化铝快速净化,弱阳离子交换柱固相萃取,CAPCELL PAK ST柱分离。链霉素和双氢链霉素检出限为1.5μg/kg,在10.0-500 ng...建立了不使用离子对试剂,液质联用技术检测鳗鱼中链霉素和双氢链霉素残留量的检测方法。样品经三氯乙酸溶液提取,碱性氧化铝快速净化,弱阳离子交换柱固相萃取,CAPCELL PAK ST柱分离。链霉素和双氢链霉素检出限为1.5μg/kg,在10.0-500 ng/m L质量浓度范围内链霉素和双氢链霉素呈线性相关,相关系数为0.9999和0.9994,回收率在78.3%-105.9%之间,相对标准偏差在3.1%-6.6%之间。方法采用碱性氧化铝基质分散固相萃取,除去样液中油脂同时也降低样液中酸的浓度,进而降低固相萃取上样液中碱金属离子强度,提高了链霉素和双氢链霉素残留检测的绝对回收率。展开更多
基金Supported by the China Postdoctoral Science Foundation （20080440142）. ACKNOWLEDGEMENTS We thank Dr. Stacy M. Morris, Kent State University, for her reviews and improvement of the manuscript.
文摘Hydrogen peroxide(H2O2)precipitation from sodium aluminate(SA)solution at close-ambient temperature is an efficient method to synthesize boehmite and its derived alumina with high surface area,but the precipitation yield of Al2O3 is usually below 50%in highly alkaline SA solutions.Here the synthesis of boehmite is enhanced through a precarbonization-assisted H2O2 route in highly alkaline SA solutions.It is found that the crystal structure of the precipitation product is evidently influenced by the precipitation conditions.As the precipitation temperature increases from 273 to 325 K,a small amount of gibbsite by-product is formed.As the aging temperature increases from 301 to 333 K,the crystallinity of boehmite decreases and part of the boehmite dissolves due to an increase in the pH value.Based on the above results,a precarbonization-assisted H2O2 route is proposed to obtain pure boehmite with more complete recovery of Al2O3 from highly alkaline SA solutions.The route includes a controllable precarbonization step of SA solutions with a molar ratio of Na2O to Al2O3 higher than 2:1,followed by the H2O2-precipitated step with a molar ratio of H2O2 to Al2O3 less than 7:1.Because of its facile operation conditions,no extraneous impurity,time saving and a possible recycle of the filtrate,the route has great potential to be an alternative method for preparation of boehmite and its derived alumina.
文摘建立了不使用离子对试剂,液质联用技术检测鳗鱼中链霉素和双氢链霉素残留量的检测方法。样品经三氯乙酸溶液提取,碱性氧化铝快速净化,弱阳离子交换柱固相萃取,CAPCELL PAK ST柱分离。链霉素和双氢链霉素检出限为1.5μg/kg,在10.0-500 ng/m L质量浓度范围内链霉素和双氢链霉素呈线性相关,相关系数为0.9999和0.9994,回收率在78.3%-105.9%之间,相对标准偏差在3.1%-6.6%之间。方法采用碱性氧化铝基质分散固相萃取,除去样液中油脂同时也降低样液中酸的浓度,进而降低固相萃取上样液中碱金属离子强度,提高了链霉素和双氢链霉素残留检测的绝对回收率。
