离子色谱法测定浓磷酸中的Cl~–,SO_4~(2–),NO_3~–

采用离子色谱法测定浓磷酸中的Cl~–,SO_4~(2–),NO_3~–。将浓磷酸稀释至400倍体积,以0.22μm滤膜过滤,使用阴离子交换色谱–抑制电导检测器测定浓磷酸中的Cl~–,SO_4~(2–),NO_3~–。采用高容量色谱柱,以1.0 mmol/L Na_2CO_3–24 mmol/L Na OH混合液为流动相,将无机阴离子与浓磷酸基体分离,以标准加入法定量。氯离子、硝酸盐、硫酸盐的检出限为0.05~0.12 mg/L,加标回收率为96.6%~100.0%,测定结果的相对标准偏差为7.0%~10.0%(n=5)。该方法分离效果好,可用于浓磷酸中Cl~–,SO_4~(2–),NO_3~–的同时测定。     

以脉冲萃取柱利用三异辛胺从高浓度铀溶液中回收铀

利用三异辛胺(TOA)纯化Gattar小型试验工厂的高浓度铀溶液(洗脱液的铀浓度7 g·L^-1),研究了脉冲萃取柱的性能。利用实验室级脉冲萃取柱进行了实验室规模的溶剂萃取实验和后续实验。结果表明,在室温、pH=1和有机相与水相的比例(V_O/V_A)约为1.8：1时,加入二(2-乙基己基)磷酸(D2EHPA)使其与TOA的比例(V_D2EHPA/V_TOA)为2：3,可使萃取克服Cl-的抑制效应,提高效率。将结论用于考察试验工厂级萃取柱的流体力学和传质性能,结果表明用脉冲萃取柱萃取铀可以达到97%的萃取效率,具有可行性。     

硅胶柱与凝胶柱净化/气相色谱-质谱联用测定植物叶片中多环芳烃

建立了索氏提取-硅胶柱和凝胶柱净化/气相色谱-质谱联用(GC-MS)测定植物叶片中多环芳烃的分析方法。叶片中的多环芳烃经二氯甲烷-正己烷(体积比1∶1)索氏提取,提取液采用硅胶柱和凝胶柱两步净化(手填硅胶柱和GPC柱)后,进行GC-MS测定,根据保留时间和特征离子进行定性,内标法定量。方法检出限为0.025 1~5.80 ng/g,加标回收率为82.2%~130%,相对标准偏差不大于11%。该方法能有效去除植物叶片中的色素与油脂,适用于植物叶片中多组分多环芳烃的痕量分析,为测定植物组织内多环芳烃的含量提供了技术支撑。     

Electrospray ionization mass spectrometric detection of low polar compounds by adding NaAuCl4

Liquid chromatography electrospray ionization mass spectrometry (LC/ESI/MS) has been widely used for various analyses. However, it is difficult to use LC/ESI/MS for the analysis of low polar compounds, such as polycyclic aromatic hydrocarbons. It is well known that AuCl₄^? ion decomposes to AuCl₃ by heating, and AuCl₃ is a strong π‐electrophilic Lewis acid. Low polar compounds (pyrene, benzo[a]pyrene, perylene, benzo[ghi]perylene, dibenzothiophene and p‐dimethoxybenzene) were detected by ESI/MS in the positive ion mode by adding NaAuCl₄. The low polar compound interacts with AuCl₃ formed at the ESI interface, and undergoes electron transfer to AuCl₃. The radical cation of the low polar compound was then detected by MS. In addition, the LC/ESI/MS determination of polycyclic aromatic hydrocarbons by the post‐column addition of NaAuCl₄ was studied. © 2016 The Authors Journal of Mass Spectrometry Published by John Wiley & Sons Ltd     

Alloying effects of the elements with a positive heat of mixing on the glass forming ability of Al-La-Ni amorphous alloys

The effects of Sn and Ga additions on the glass forming ability(GFA)of(Al86La5Ni9)100 xSnx(x=0,0.2,0.3,0.5,0.7,1 and 2at.%)and(Al86La5Ni9)100 xGax(x=0,0.2,0.5,1 and 1.5 at.%)alloys were systematically investigated.Unlike common microalloying methods,both Sn and Ga have a positive heat of mixing with the main component of Al.Our analysis confirmed that proper Sn addition can suppress the strong formation ofα-Al and enhance the GFA due to the positive heat of mixing between Sn and Al and the large difference in their atomic sizes.While the addition of Ga to the base alloy acted as the nucleation cites forα-Al and accelerated precipitation of theα-Al phase,thus deteriorating the GFA.     

应变液晶的负压光效应和反式压光效应

介绍聚合物分散液晶和应变液晶概念,给出聚合物分散液晶调光玻璃的"正压光效应"、"负压光效应"和"反式压光效应"三种效应定义.实验制备出负压光效应和反式压光效应新型应变调光玻璃样品,测试样品散射态雾度90%以上,半透明态透光率接近30%.用偏光显微术研究压光效应原理,表明对样品施加垂面按压或拉伸的应力诱导作用会引起液晶微滴中液晶分子具有某些特殊排列方式,导致样品光学性质发生显著变化.建立垂面拉伸液晶微滴模型,计算模拟所绘出的图形与偏光显微镜照片独特花样十分相似,进而合理解释了实验现象.应变液晶压光效应研究具有聚合物分散液晶基础研究意义和开发非电控调光玻璃的实际应用价值.     

由正负磁单极对相互作用诱导的孤立狄拉克弦

基于三维旋量Gross-Pitaevskii(GP)方程研究在含时周期性外磁场作用下玻色-爱因斯坦凝聚体的动力学行为.结果显示,在含时周期外磁场的作用下,铁磁态自旋为1的玻色-爱因斯坦凝聚体将发生拓扑形变.当磁场的两个零点进入凝聚体后,自旋向上态的密度布居图在z轴上分别形成向上和向下的凸起.随着磁场的两个零点在凝聚体内逐渐重合,向上和向下的凸起被拉长,最终自旋向上态在z轴上呈线状分布,这与理论分析预测得到的孤立狄拉克弦相对应.最后,通过计算凝聚体的超流涡度给出磁单极的表征图.结果显示,凝聚体在磁场的两个零点处形成正、负磁单极对,分别对应着自旋向上态在z轴上向上和向下的凸起.随着磁场的两个零点重合,正、负磁单极对中的两条狄拉克弦逐渐靠近,之后大约经5 ms,它们完全相连,最终形成孤立的狄拉克弦.     

Direct evaluation of the equivalent linear damping for TLCD systems in random vibration for pre-design purposes

Passive control of structural vibrations has received in recent years a great attention from researchers concerned with vibration control. Several types of devices have been proposed in order to reduce the dynamic responses of different kinds of structural systems. Among them, the Tuned Liquid Column Damper (TLCD) proved to be very effective in reducing vibration of structures. Since the increasing use of TLCDs in practical realizations, this paper aims at developing an approximate formulation, by means of a statistical linearization technique, able to estimate the parameters of a structure equipped with a TLCD subjected to random loads for pre-design purposes. Moreover, it is shown that results obtained via Monte Carlo approach on the non-linear system are in good agreement with those obtained by means of the proposed formulation.     

EXISTENCE OF POSITIVE SOLUTIONS TO A THREE-POINT BOUNDARY VALUE PROBLEM FOR SECOND ORDER DYNAMIC EQUATIONS WITH DERIVATIVE ON TIME SCALES

In this paper, we consider the existence of positive solutions to a three-point boundary value problem for second order dynamic equations with derivative on time scales.Applying Leggett-Williams fixed point theorem, we obtain at least three positive solutions to the problem. An example is also presented to illustrate the applications of the results obtained.     

六角柱形NaErF_(4)和NaErF_(4)@NaYF_(4)核壳微粒制备及多色上转换荧光调控性能EI北大核心CSCD

采用简单的水热法合成了六角柱形NaErF_(4)和NaErF_(4)@NaYF_(4)核壳上转换发光材料,利用扫描电镜(SEM)、X射线粉末衍射(XRD)和荧光光谱(PL)等表征对材料的形貌、结构和上转换发光性能进行了研究。结果表明,纯NaErF_(4)样品为六角柱形,边长和厚度均为1μm左右,样品表面光滑。随着NaYF_(4)壳层的包覆,六角相NaErF_(4)周围出现了大量的立方相NaYF_(4)纳米颗粒,得到了NaErF_(4)@NaYF_(4)核壳结构。荧光光谱表明,通过在六角柱形NaErF_(4)表面包覆NaYF_(4)壳层,可以有效增强上转换发光强度,其中,位于527,543,663 nm处的3个发射峰分别对应于Er^(3+)的^(2)H_(11/2)→^(4)I_(15/2)、^(4)S_(3/2)→^(4)I_(15/2)和^(4)F_(9/2)→^(4)I1_(5/2)能级跃迁。随着壳层中Y∶F比例的增加,立方相NaYF_(4)的晶体衍射峰逐渐增强;同时,对应的NaErF_(4)@NaYF_(4)样品发射光谱中红绿比(R/G)逐渐增大,发光颜色也从绿色、经黄绿色逐渐向黄色过渡,实现了多色发光。