基于顶空固相微萃取(head space solid phase microextraction,HS-SPME)结合全二维气相色谱-飞行时间质谱(comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry,GC×GC-TOFMS)建立了一种准确定量...基于顶空固相微萃取(head space solid phase microextraction,HS-SPME)结合全二维气相色谱-飞行时间质谱(comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry,GC×GC-TOFMS)建立了一种准确定量白酒中氨基甲酸乙酯(ethyl carbamate,EC)的方法。实验对HS-SPME方法进行了优化,在酒精度12%vol、加NaCl 3 g、萃取温度70℃,萃取时间40 min的条件下,能够显著提高目标物的响应值。实验以D_(5)-氨基甲酸乙酯(D_(5)-EC)为内标,对不同浓度的样品溶液进行GC×GC-TOFMS定量分析。结果表明,EC在10~500μg/L范围内线性关系良好,回归系数(R^(2))>0.998,检出限为0.19μg/L,定量限为0.64μg/L,平均回收率为97.57%,精密度为8.66%。测定结果与国标方法相比无显著性差异(P>0.05)。该方法前处理简单,检测灵敏度更高,为白酒中EC自动化定量测定提供了新思路。展开更多
To investigate the assumptions proposed in this paper,the evolution law governing the strength and expansion performance of MgO and nano-MgO micro-expansive concrete in the environment of mineral powder was firstly ob...To investigate the assumptions proposed in this paper,the evolution law governing the strength and expansion performance of MgO and nano-MgO micro-expansive concrete in the environment of mineral powder was firstly observed in this study.Secondly,SEM,XRD,and TG-DSC microscopic tests were conducted to reveal the effects of the active mineral-powder admixture on the hydration degree and expansion performance of MgO and nano-MgO in HPC.Our experimental results successfully verified our hypothesis,which indicated that the expansion performance of macro-MgO and nano-MgO was indeed depressed by the addition of active mineral power admixtures,even though the mechanical property of concrete composites was effectively improved.Furthermore,the hydration test also demonstrated the negative interference on the mineral powders,which was induced by the expansion agents.It is found the amounts of hydrates tend to decrease because the mineral powder ratio reaches and exceeds 40%.Moreover,it is also concluded the effect of expansion agents is governed by the alkalinity cement paste,especially for the nano-MgO.In other words,the expansion performance of nano-MgO will vary more obviously with the hydration process,than MgO.The results of this study provide that effective experimental and theoretical data support the hydration-inhibition mechanism of magnesium expansive agents.展开更多
文摘基于顶空固相微萃取(head space solid phase microextraction,HS-SPME)结合全二维气相色谱-飞行时间质谱(comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry,GC×GC-TOFMS)建立了一种准确定量白酒中氨基甲酸乙酯(ethyl carbamate,EC)的方法。实验对HS-SPME方法进行了优化,在酒精度12%vol、加NaCl 3 g、萃取温度70℃,萃取时间40 min的条件下,能够显著提高目标物的响应值。实验以D_(5)-氨基甲酸乙酯(D_(5)-EC)为内标,对不同浓度的样品溶液进行GC×GC-TOFMS定量分析。结果表明,EC在10~500μg/L范围内线性关系良好,回归系数(R^(2))>0.998,检出限为0.19μg/L,定量限为0.64μg/L,平均回收率为97.57%,精密度为8.66%。测定结果与国标方法相比无显著性差异(P>0.05)。该方法前处理简单,检测灵敏度更高,为白酒中EC自动化定量测定提供了新思路。
基金Funded by the National Natural Science Foundation of China(No.51578325)。
文摘To investigate the assumptions proposed in this paper,the evolution law governing the strength and expansion performance of MgO and nano-MgO micro-expansive concrete in the environment of mineral powder was firstly observed in this study.Secondly,SEM,XRD,and TG-DSC microscopic tests were conducted to reveal the effects of the active mineral-powder admixture on the hydration degree and expansion performance of MgO and nano-MgO in HPC.Our experimental results successfully verified our hypothesis,which indicated that the expansion performance of macro-MgO and nano-MgO was indeed depressed by the addition of active mineral power admixtures,even though the mechanical property of concrete composites was effectively improved.Furthermore,the hydration test also demonstrated the negative interference on the mineral powders,which was induced by the expansion agents.It is found the amounts of hydrates tend to decrease because the mineral powder ratio reaches and exceeds 40%.Moreover,it is also concluded the effect of expansion agents is governed by the alkalinity cement paste,especially for the nano-MgO.In other words,the expansion performance of nano-MgO will vary more obviously with the hydration process,than MgO.The results of this study provide that effective experimental and theoretical data support the hydration-inhibition mechanism of magnesium expansive agents.
