气相色谱法测定卷烟主流烟气气相物中的甲烷、乙烯和乙炔

 建立了测定卷烟主流烟气气相物中的甲烷、乙烯和乙炔气体的气相色谱法,用外标法定量,同时考查了捕集条件和仪器的稳定性.所建立的方法简便、快速、准确,并具有良好的线性关系(r_甲烷²=0.9993,r_乙烯²=0.9998,r_乙炔²=0.9994)及较好的准确度与精密度,回收率均>85%,相对标准偏差<3%.将该方法应用于实际样品检测,结果令人满意.     

聚二甲基硅烷的热裂解-气相色谱-质谱研究

聚二甲基硅烷(PDMS)具有不溶不熔的特性,本文使用热裂解-气相色谱-质谱(Py-GC-MS)研究了PDMS热裂解行为.通过对2种PDMS热裂产物差异的比较,试图获取与PDMS化学结构特征相关的信息,为聚碳硅烷(PCS)原料质量控制标准的制订提供基础信息.     

剑叶金鸡菊花部分挥发油化学成分分析

研究剑叶金鸡菊（Coreopsis Lanceolata L.）花中挥发油的组成及含量。采用水蒸气蒸馏法提取剑叶金鸡菊花部分挥发油,并用毛细管气相色谱-质谱（GC-MS）对提取成分进行定性定量研究。分析鉴定了21个化合物,并确定其化学结构和百分含量。揭示了剑叶金鸡菊花部分的药理作用,为综合开发利用剑叶金鸡菊提供了科学依据。     

Near-infrared spectroscopy-based quantification of substrate and aqueous products in wastewater anaerobic fermentation processes

In this study, a Fourier transform near-infrared （FT-NIR） technique was used for process monitoring of anaerobic fermentation. Orthogonal signal correction （OSC） method was used as NIR spectral pre- processing options. Calibration models were established and the validation of the method was per- formed with the sucrose, ethanol and volatile fatty acids （VFAs） contents determined by the anthrone and gas chromatography methods, respectively. Spectral range and the number of internal latent variables were optimized for the best correlation coefficient. Test set validation of sucrose resulted in excellent measurement of prediction performance and the correlation coefficient of determination is 0.930. Similar prediction statistics for individual VFA and total VFA contents were obtained. These re- sults proved that the NIR spectroscopy technology is able to quantify the contents of both volatile fatty acids and sucrose in wastewater anaerobic fermentation process.     

Direct observations of reaction zone structure in shock-induced ignition of methane air mixture

Ignition of methane/air mixture by the passage of a shock wave is an important issue for understanding more details of its gaseous detonation. The experiments of shock-induced ignition of stoichiometric methane/air mixture were conducted on a shock tube platform, The reaction zone structure in weak and strong ignition cases were investigated by digital chemiluminescence imaging and planar laser induced fluorescence （PLIF） techniques. Due to smaller gradients in induced time in weak ignition, which provided more time to nonlinear chemical reaction process, the results show that the reaction structures are highly nonuniform in those weak ignition cases, which become more regular while induced shock waves become stronger. In strong ignition case, it gives a typical detonation structure. The characteristics of reaction zone released by single-pulsed OH PLIF technique agreed well with other experimental measurements in this paper and were also in accord with the conclusions of previous researches. The successful implementation of the PLIF system has explored a new high temporally and spatially resolved method for the study of interaction between shock wave and gaseous matter in shock tube.     

拟康氏木霉产胞外多糖的分离纯化及组成初步研究

以拟康氏木霉（Trichoderma pseudokoningii SDTP1）产胞外多糖粗品为材料,经木瓜蛋白酶-Sevag法除蛋白、凝胶柱层析分离纯化,得到一种水溶性的拟康氏木霉产胞外多糖纯品（TPP-0）,并研究了其单糖组成.采用紫外光谱和红外光谱法对拟康氏木霉产胞外多糖进行了定性分析.结果表明,拟康氏木霉产胞外多糖具有多糖特征性的紫外和红外吸收峰 高效凝胶渗透色谱法测定结果表明,拟康氏木霉产胞外多糖的峰值分子量为1.8×104 采用气相色谱法测定拟康氏木霉产胞外多糖中单糖的种类和构成比例,结果表明,拟康氏木霉产胞外多糖主要由鼠李糖、葡萄糖、半乳糖等3种单糖组成,含有葡萄糖醛酸,并计算出3种单糖的摩尔组成比例.     

液相色谱质谱联用法快速测定配方奶粉中的三聚氰胺

应用液相色谱质谱联用法测定配方奶粉样品中的三聚氰胺.试样用三氯乙酸溶液提取,经阳离子交换固相萃取柱净化后,用液相色谱质谱法测定和确证,外标法定量.采用电喷雾离子源,定性离子对为127/85和127/68;定量离子对为127/85.样品的三聚氰胺标准加入回收率为91.6%～104.2%;相对标准偏差(RSD)1.2%～2.6%;检出限为0.2 mg/kg.     

铟掺杂一维半导体氧化锌纳米螺旋制备及表征

利用化学气相沉积的方法,在硅衬底上生长了铟掺杂的氧化锌纳米螺旋结构.通过X-射线衍射仪、扫描电子显微镜、透射电子显微镜、选区电子衍射等手段对样品的形貌和结构进行了表征.结果表明,合成的纳米螺旋由纳米带旋转而成,曲率半径为几个微米.纳米带宽约200 nm,厚约几十纳米,铟杂质的引入使其生长方向沿(1010)方向.     

汽油辛烷值促进剂的有效成分研究

采用柱层析、高效液相色谱等手段对产自澳大利亚的汽油辛烷值促进剂进行分离,利用气相色谱质谱联用(GC-MS)对分离组分进行定性分析,依据各馏分的定性分析结果,对含有有效成分的馏分进行进一步制备分离及提纯,得到2种有效成分的单体化合物.利用气相色谱质谱联用(GC-MS)、傅立叶变换红外光谱(FIR)对分离得到的化合物进行结构表征,证实其分别为甲基环戊二烯三羰基锰(MMT)和N-甲基苯胺.经质量法定量分析,确定其质量分数为7.38 mg/mL和20.45 mg/mL.     

顶空毛细管气相色谱法测定头孢他美钠中4种有机溶剂的残留量

采用顶空毛细管气相色谱法,测定了头孢他美钠中乙醇、丙酮、二氯甲烷和四氢呋喃四种溶剂的残留量.用DB-624毛细管气相色谱柱顶空进样法,FID检测器.乙醇、丙酮、二氯甲烷和四氢呋喃的线性范围分别为0.2～7.0 mg·mL-1(r=0.9995),0.2～7.0 mg·mL-1(r=0.9994),0.03～1.0mg·mL-1(r=0.9993),0.02～0.9 mg·mL-1(r=0.9994);乙醇、丙酮、二氯甲烷和四氢呋喃的平均回收率分别为100.5%、99.6%、99.0%、98.4%;RSD(n=5)分别为1.2%、2.3%、1.8%、2.8%.本方法简单、准确、灵敏度高、重现性好,适用于头孢他美钠中有机溶剂残留量的测定.