微波常压法制备三聚氰酸

研究了在常压条件下尿素与助溶剂通过微波辐射制备三聚氰酸的反应条件，结果表明，采用594W微波辐射3min，转化率达83．5％。     

血液中循环肿瘤细胞捕获与释放方法研究进展

血液中的循环肿瘤细胞(CTCs)与癌症转移密切相关,对CTCs进行检测有利于实现癌症早期诊断。但由于血液中CTCs个数稀少且存在异质性,因此急需发展血液中CTCs的高效分离及检测方法。此外,释放被捕获的细胞并进行后续培养及基因水平分析,将会进一步推进癌症的个性化治疗。本文综述了近年来CTCs捕获及释放的相关研究进展,并展望了其应用前景及发展方向。     

静态顶空/气相色谱-质谱法同时测定化妆品中22种有毒挥发性有机溶剂残留

以2015版《化妆品安全技术规范》中规定的常见禁用及限用有毒挥发性有机溶剂为研究对象,建立了静态顶空/气相色谱-质谱法(SHS/GC-MS)同时测定化妆品中22种有毒挥发性有机溶剂(VOC)(二氯甲烷、顺式-1,2-二氯乙烯、反式-1,2-二氯乙烯、2-氯-1,3-丁二烯、三氯甲烷、1,2-二氯乙烷、苯、四氯化碳、三氯乙烯、甲苯、四氯乙烯、氯苯、乙苯、三溴甲烷、间二甲苯、对二甲苯、苯乙烯、邻二甲苯、异丙苯、1,4-二氯苯、1,2-二氯苯、六氯丁二烯)残留的检测方法。试样在80℃下30 min静态顶空,经DB-1柱分离后,采用选择离子监测模式(SIM)进行定性定量分析。优化了顶空、色谱和质谱参数,结果表明:22种VOC在0.5~50 ng/m L浓度范围内均呈良好的线性关系,相关系数均大于0.99,在1.0,2.0,5.0 ng/m L 3个浓度加标水平下的平均回收率为80.3%~102.7%,相对标准偏差(RSD,n=6)为6.4%~9.9%,检出限为0.2~5.0 ng/g。结果表明,该方法简便、灵敏、准确,具有良好的重现性和稳定性,适合于化妆品中22种VOC残留的筛查和确证检测。     

Hydrothermal Synthesis and Crystal Structure of a Novel Hexanuclear Copper（Ⅱ） Complex：[Cu_6（DPPZ）_4（btc）_4（H_2O）_8]·5H_2O

A new hexanuclear copper(Ⅱ) complex,[Cu 6 (DPPZ) 4 (btc) 4 (H 2 O) 8 ]·5H 2 O (1,DPPZ=dipyrido[3,2-a:2,3-c]phenazine,H 3 btc=1,3,5-benzenetricarboxylic acid),has been hydrothermally synthesized and structurally characterized by X-ray single-crystal diffraction,elemental analyses,IR,and thermogravimetric analysis.Its crystal structure is of triclinic system,space group P1 with a=12.489(4),b=14.234(5),c=14.484(5),α=82.848(4),β=79.399(4),γ=73.646(4)°,V=2421.2(13) 3,Z=1,Cu 6 C 108 H 78 N 16 O 37,M r=2573.17,D c=1.752 g/cm 3,μ=1.398 mm-1,F(000)=1308,GOOF=1.011,the final R=0.0495 and wR=0.1030 for 5420 observed reflections with I > 2σ(Ⅰ).In 1,four btc 3ligands act as bridges between six neighboring Cu atoms to form an unusual hexanuclear copper cluster.The clusters are further connected by two types of O-H···O and O-H···N hydrogen bonds,generating a three-dimensional supramolecular structure.In addition,intermolecular and intramolecular π-π stacking interactions further consolidate the three-dimensional supramolecular framework of 1.     

茂铁基二氢吡唑类衍生物的液相色谱分离研究

本文利用梯度洗脱进行溶剂强度的优化,确定分离一组化合物的最佳二元流动相体系,即甲醇-水、四氢呋喃-水和乙腈-水,将这三种二元流动相的最佳组成作为溶剂选择性三角形的三个顶点,利用ORM法对流动相进行优化选择,得到流动相的最佳组成和配比为V乙腈:V四氢呋喃:V水=33.75:33:33.25,有效地分离了六种二茂铁取代二氢...     

Glucose oxidase as a blocking agent-based signal amplification strategy for the fabrication of label-free amperometric immunosensors

An effective electrochemical signal amplification strategy based on enzyme membrane modification and redox probe immobilization was proposed to construct an amperometric immunosensor.L-cysteine@ferrocene functionalized chitosan,which possessed not only efficient redox-activity but also excellent film-forming ability,was coated on the bare glass carbon electrode. Moreover,the thiol groups(SH)in the ferrocenyl compound were used for gold nanoparticles immobilization via the strong bonding interaction,which co...     

Numerical study on scanning radiation acoustic field in formations generated from a borehole

The directivity of acoustic transducers used in conventional acoustic logging tools is uncontrollable[1,2], which inevitably affects investigation depth and resolution. At present, deep and wide range of investigation in petroleum exploration is urgently re- quired. It is important to improve the exploration capability to find more complex and fine reservoirs[3], for which the direction of the radiated acoustic energy is a direct factor. Acoustic field in the formations generated by the source…     

亚像元动态成像技术中系统的调制传递函数

亚像元动态成像技术是国际上目前实现遥感器小型化非常有效的新方法，因而研究亚像元动态成像系统的调制传递函数（MTF）显得非常必要和重要。本文分析亚像元动态成像系统的MTF模型，并给出亚像元动态成像系统MTF的数学表达式。     

Nd-Fe-B(B≤50at.％)三元系相图的研究

本文用X射线衍射、热学分析、磁性测量等手段研究了Nd-Fe-B(B≤50at.％)三元系相图,主要结果如下:1.重新测定了Nd-Fe二元系相图,确证NdFe₂相是不存在的。2.测定了Nd-Fe-B(B≤50at.％)三元系室温横截面。在该三元系中存在三个化合物:Nd₂Fe₁₄B,Nd₈Fe₂₇B₂₄,Nd₂FeB₃。 指出:在未经退火的Nd-Fe-B三元母合金中,存在有过冷液相(非晶)的可能性。实用Nd-Fe-B新型永磁合金,由三相构成,主相为Nd₂Fe₁₄B,次相为Nd和Nd₈Fe₂₇B₂₄。3.测定了Fe₉₄B₆-Nd₁₂Fe₈₂B₆-Nd_33.5Fe_60.5B₆和Nd₂Fe₁₇-Nd₂Fe₁₄B-Nd₈Fe₂₇B₂₄纵截面。指出:在制备Nd-Fe-B三元永磁合金时,最高烧结温度不得高于1100℃,而后热处理的温度在600℃左右为宜。4.研究了Nd₂Fe₁₄B,Nd₈Fe₂₇B₂₄的结构和Nd₂Fe₁₄B的单相区。Nd₂Fe₁₄B为四方晶系,a=8.800,c=12.190,z=4,空间群为P4₂/mnm,X射线密度D_X=7.60g/cm³,测量密度D_O=7.50g/cm³。在测量精度范围内,观测不到Nd₂Fe₁₄B有单相区存在。Nd₈Fe₂₇B₂₄为四方晶系,a=7.12,c=27.40,z=2,D_X=7.01g/cm³,D_O=7.00g/cm³,可能的空间群为P4₂/n。5.在实验的基础上,讨论了Nd₂Fe₁₄B的热稳定性,并对制备Nd-Fe-B永磁合金的粉末冶金工艺提供了解释。     

碱金属碘酸盐赝二元系固溶体的研究

碱金属碘酸盐形成的二十一个赝二元系中,六个体系为机械混合物,九个体系是形成化合物的(其中三个是离子化合物),其余六个体系形成连续固溶体。本文对KIO₃-NH₄IO₃,RbIO₃-NH₄IO₄等赝二元系形成的连续固溶体进行了研究。NH₄IO₃中加入KIO₃或RbIO₃时,随加入量增加,NH< 关键词：