洋葱中多种农药残留的双柱双检测器气相色谱分析法

洋葱中含有许多对人类有用的成分包括:水分、蛋白、脂肪、膳食纤维、碳水化合物、胡萝卜素、视黄醇、硫胺素、核黄素、抗坏血酸、维生素总E、K、Na、Ca、Mg、Fe、Mn、Zn等[1].近来的许多研究表明,洋葱具有消炎抑菌,预防心血管疾病、糖尿病等生物活性[2].由于洋葱的医疗价值和保健作用,洋葱现在已经成为人们喜爱的蔬菜,受到人们的重视,尤其在欧美,洋葱被称为"蔬菜皇后".目前,国内外对洋葱的研究越来越多,但是主要集中在研究它的生物活性和成分上[2-4].由于洋葱中合有油类物质,因此给农药残留分析带来许多困难.至今,对洋葱中的农药残留分析还未有成熟的方法.目前,用气相色谱分析多组分农药残留的报道已经有了很多[5,6],关于用双检测器分析多组分农药残留的研究,已越来越引起研究人员的关注[7-9].Jatiender Kumar Dubey等[7]用GC-NPD和GC-ECD检测了食品中乙烯基硫脲的含量.Jiménez等[8]利用GC-NPD和GC-ECD分析了蜂蜜中的农药残留.但是用GC-FPD和GC-ECD分析洋葱中的农药残留还未见报道.本文报道了一种简便、快速的洋葱中多种有机磷和菊酯类农药残留的提取净化及其双柱双检测器测定方法.采用乙睛提取洋葱中的农药,二氯甲烷/乙酸乙酯(20:1,V:V)为淋洗剂,经过Florisil和活性炭净化后,用气相色谱-火焰光度检测器和气相色谱-电子捕获检测器分别直接测定各种农药残留含量.结果表明,采用程序升温,所测定的有机磷和菊酯类农药在DB-1701和BPX608弹性石英毛细管柱上得到了很好的分离,且方法快速、灵敏,完全符合实际应用需要.各种农药的加标回收率范围为86.3～103%,变异系数范围为0.67～4.6%,最低检测浓度范围为0.001～0.005 mg/kg.     

痕量钒的分析进展

综述近年来测定痕量钒的主要方法,包括光度法如常规光度法、流动注射光度法、催化动力学光度法、萃取光度法、导数光度法以及原子吸收法、荧光法、交流示波极谱法、催化动力学离子选择电极法和流动注射化学发光法等。     

电位滴定法测定铜镁合金中镁

建立电位滴定法测定铜镁合金中的镁含量.以光度电极为指示电极,乙二胺四乙酸二钠溶液为滴定剂.试料用王水溶解,在pH 4.0～4.5时,用硫化钠和铜试剂将大量基体铜和杂质元素沉淀分离.在pH约为10的环境下,以铬黑T为指示剂,用乙二胺四乙酸二钠溶液滴定至电位突跃记为终点,计算镁含量.考察滴定参数的影响,确定了滴定波长为61...     

Electric gating of the multichannel conduction in LaAlO_3/SrTiO_3 superlattices

The electric gating on the transport properties of two-dimensional electron gas(2DEG) at the interface of LaAlO₃/SrTiO₃(LAO/STO) heterostructure has attracted great research interest due to its potential application in fieldeffect devices. Most of previous works of gate effect were focused on the LAO/STO heterostructure containing only one conductive interface. Here, we systematically investigated the gate effect on high-quality LAO/STO superlattices(SLs)fabricated on the TiO₂-terminated(001) STO substrates. In addition to the good metallicity of all SLs, we found that there are two types of charge carriers, the majority carriers and the minority carriers, coexisting in the SLs. The sheet resistance of the SLs with a fixed thickness of the LAO layer increases monotonically as the thickness of the STO layer increases. This is derived from the dependence of the minority carrier density on the thickness of STO. Unlike the LAO/STO heterostructure in which minority and majority carriers are simultaneously modulated by the gate effect, the minority carriers in the SLs can be tuned more significantly by the electric gating while the density of majority carriers is almost invariable. Thus, we consider that the minority carriers may mainly exist in the first interface near the STO substrate that is more sensitive to the back-gate voltage, and the majority carriers exist in the post-deposited STO layers. The SL structure provides the space separation for the multichannel conduction in the 2 DEG, which opens an avenue for the design of field-effect devices based on LAO/STO heterostructure.     

镍钛铂合金中铂量的测定

样品以混酸溶解,在酸性介质中,NH_4Cl与Pt~(4+)形成(NH_4)2PtCl_6沉淀,静置,过滤,在900℃马弗炉中,灼烧至恒量。以电感耦合等离子体原子发射光谱仪(ICP-AES)测定滤液中残留Pt的质量,以沉淀出的Pt与滤液中残留Pt的质量之和,计算Pt的质量分数。     

GDMS法和ICP-MS法测定太阳能级多晶硅中杂质元素含量

采用辉光放电质谱法(GD-MS)测定太阳能级多晶硅中B,P,Fe,Co,Ni,Cu,Zn等痕量杂质元素,并优化和选择了GD-MS工作参数。考察了在半定量分析的情况下,GD-MS测定痕量杂质的精密度。结果表明,GD-MS对B,P,Na,Al,K,Ca,Fe,Ni,Cu,Co,Zn等元素测定结果的RSD都小于30%。用ICP-MS法进行验证,检出限0.14~2.85 ng/mL,RSD为1.6%~12%,加标回收率85.2%~125%。