碘化物-罗丹明B体系荧光猝灭反应测定痕量亚硝酸根

拟定了一个荧光猝灭法测定痕量亚硝酸根的新方法。在盐酸介质中，亚硝酸根氧化 碘化钾的反应，其反应产物Ｉ３－使罗丹明Ｂ荧光猝灭。方法的检出限为３．６μｇ／Ｌ；测定范围为 １０～１２０μｇ／Ｌ。方法简便快速、选择性好，用于自来水，矿泉水及合成样品中亚硝酸根的测定， 结果满意。     

Syntheses and Crystal Structures of Homleptic Lanthanide Complexes [C_6H_5COCHC(CH_3)N-(p-ClC_6H_4)]_3Ln(THF)_n (Ln =Yb,Y,Nd)

Three homoleptic lanthanide complexes, [C6H5COCHC(CH3)N(p-ClC6H4)]3Ln(THF)n(n = 0, Ln = Yb(1); n = 0, Ln = Y(2); n = 1, Ln = Nd(3)), were synthesized by amine elimination reaction of Ln[N(SiMe3)2]3 with 1-phenyl-3-N-(p-chlorophenylimino)-1-butanone. These complexes crystallize in triclinic, space group P1 with a = 9.805(3), b = 14.831(6), c = 16.075(6) A, α = 111.996(9), β = 91.570(7), γ = 93.744(6)°, V = 2159.4(13) A3, Z = 2, D3 c = 1.515 g/cm, F(000) = 986, μ(MoKα) = 2.396 mm-1, R = 0.0360 and wR = 0.0850 for 9548 observed reflections with I 2σ(I) for complex 1; a = 9.861(5), b = 14.852(9), c = 16.111(9) A, α = 112.362(13), β = 91.949(11), γ = 93.678(14)°, V = 2173(2) A3, Z = 2, Dc = 1.377 g/cm3, F(000) = 924, μ(MoKα) = 1.570 mm-1, R = 0.0735 and wR = 0.1389 for 8015 observed reflections with I 2σ(I) for complex 2; and a = 9.308(3), b = 15.357(3), c = 17.419(4) A, α = 66.493(13), β = 88.61(2), γ = 86.664(19)°, V = 2279.4(9) A3, Z = 2, Dc = 1.499 g/cm3, F(000) = 1046, μ(MoKα) = 1.364 mm-1, R = 0.0843 and wR = 0.2280 for 8433 observed reflections with I 2σ(I) for complex 3. Each central metal in complexes 1 and 2 is six-coordinated by three nitrogen and three oxygen atoms from three β-ketoiminate ligands to give a distorted octahedral geometry, while the central metal in 3 is seven-coordinated by three nitrogen and three oxygen atoms from three β-ketoiminate ligands and one oxygen atom from the solvated THF molecule to complete a distorted monocapped trigonal prism.     

席夫碱稀土配合物(3,5-t-Bu_2-2-OC_6H_2CH=N-8-C_9H_6N)_3Ln(Ln=Eu,Yb)的合成及晶体结构

以席夫碱钠盐[NaL(THF)]2(L=3,5-t-Bu2-2-OC6H2CH=N-8-C9H6N)(1)为前体,与无水LnCl3(Ln=Eu,Yb)按物质的量比3∶2在四氢呋喃体系中室温反应24 h,高产率地得到均配型席夫碱稀土配合物LnL3[Ln=Eu(2),Yb(3)].两个配合物都通过了元素分析、红外光谱及单晶X射线衍射表征,其中配合物2属于三斜晶系,P 1空间群,a=1.28670(14)nm,b=1.32775(14)nm,c=2.3254(2)nm,α=93.435(2)°,β=96.487(2)°,γ=112.692(2)°.配合物3属于单斜晶系,P21/c空间群,a=1.72004(9)nm,b=1.81911(9)nm,c=2.85093(15)nm,β=106.376(1)°.     

(ArO)2Sm(THF)4催化N-苯基马来酰亚胺聚合

发现二价稀土配合物二 ( 2 ,6 二叔丁基 4 甲基苯氧基 )钐 [(ArO) 2 Sm (THF) 4]能较好地引发N 苯基马来酰亚胺 (N PMI)的聚合 ,溶剂对聚合的影响较大 ,在四氢呋喃中聚合转化率最高 ,且聚合转化率随单体浓度的提高而提高 ,而温度对聚合的影响不大。     

Polymerization of methyl methacrylate by diphenylamido bis (methylcyclopentadienyl) ytterbium complex

Methyl methacrylate (MMA) was effectively polymerized by diphenylamido bis (methylcyclopentadienyl) ytterbium complex (MeCp)2YbNPb2(THF). The reaction can be carried out over a range of polymerization temperature from - 40℃ to 40℃ and gives the poly MMA with high molecular weights. The initiation mechanism was demonstrated by diphenylamido-terminated methyl methacrylate oligomer.     

水杨醛缩2-茚(芴)基乙胺席夫碱的合成及其晶体结构

茚基(芴基)锂与2-溴乙胺氢溴酸盐在乙醚中按2:1物质的量比反应,分别得到2-茚基(芴基)乙胺氢溴酸盐(1)和3,1和3再与水杨醛缩合,分别得到水杨醛缩2-茚基(芴基)乙胺席夫碱2和4.通过1H NMR,IR.MS和元素分析等手段对产物进行了表征,X射线分析确定了2,4的晶体结构.其中化合物2属于单斜晶系,P21/c空间群,a＝0.9771(2)nm,b＝1.9561(4)nm,c＝1.1901(3)nm,β＝99.955(5)°,Mr＝375.53,V＝2.2404(8)nm3,Dc＝1.113 g/cm3,Z＝4,F(000)＝816,μ＝0.066 mm-1,R1＝0.0769,wR2＝0.1625.化合物4属于三斜晶系,P-1空间群,a＝0.9688(3)nm,b＝0.9699(3)nn,c＝1.3535(5)nm,α＝95.280(7)°,β＝105.394(11)°,y＝90.987(12)°,Mr＝425.59,V=1.2197(8)nm3,Dc＝1.159g/cm3,Z=2,F(000)＝460,μ＝0.069mm-1,R1＝0.0589,wR2＝0.1312..     

离子对型[O,N,N]三齿席夫碱镱氯化物的合成及其晶体结构

无水YbCl3和席夫碱[HL=3,5-(t-Bu)2-2-HOC6H2CH=N-8-C9H6N]锂盐按1∶1物质的量比在THF中反应,得到离子对席夫碱镱氯化物YbLCl3Li(DME)3(1).标题配合物1经元素分析、IR光谱和X射线衍射结构表征.配合物1属单斜晶系,P21/n空间群,晶胞参数:a=1.4855(16)nm,b=1.3696(13)nm,c=2.1816(2)nm,α=90.00°,β=98.217(3)°,γ=90.00°,V=4.3748(8)nm3,Z=4,F(000)=1868,Mr=916.17,Dc=1.397 g.cm-3,μ=2.364 mm-1,R1=0.0855,wR2=0.1863.     

Synthesis and Crystal Structure of Tetra（（8-quinolyl）-amido-N）ytterbium Bi（tetrahydrofuran-O）lithium

The treatment of the mixture of n-BuLi with 1 equiv.8-aminoquinoline in THF in situ,which reacted further with 1/3 equiv.of YbCl3 in THF,to give the homoleptic lanthanide amide ate complex Yb(NH-C9H6N)4Li(C4H8O)2(1).The crystal structure was determined by X-ray diffraction and the following crystallographic data were obtained:C44H44N8O2YbLi,Mr = 896.85,monoclinic,space group C2/c,a = 7.8384(16),b = 22.294(5),c = 22.668(5),β = 97.614(5)°,V = 3926.3(14)3,Z = 4,Dc = 1.517 g/cm3,F(000)= 1812,μ(MoKα)= 2.431 mm-1,R = 0.0542 and wR = 0.1523 for 3372 observed reflections with I > 2σ(I).The structure of molecule 1 consists of one ytterbium atom,one lithium atom,four 8-aminoquinoline ligands and two THF molecules.The ytterbium atom is coordinated by eight nitrogen atoms of four 8-aminoquinoline ligands,forming a distorted dodecahedral geometry.     

（ArO02Sm（THF）4催化N—苯基马来酰亚胺聚合

发现了二价稀土配合物二（２，６－二叔丁基－４－甲基苯氧基）钐「ＡｒＯ）２Ｓｍ（ＴＨＦ）４」能较好地引发Ｎ－苯基马来酰亚胺（Ｎ－ＰＮＩ）的聚合，溶剂对聚合的影响较大，在四氢呋喃中聚合转化率最高，且聚合转化率随单体浓度的提高而提高，而温度对温度响不大。     

硒(Ⅳ)-碘化物-罗丹明6G体系荧光猝灭反应测定茶叶中痕量硒

拟定了一个荧光猝灭法测定痕量硒（Ⅳ）的新方法。在盐酸介质中，硒（Ⅳ）氧化碘化钾的反应，其反应产物使罗丹明６Ｇ荧光猝灭。方法的检出限为１．２μｇ／Ｌ，线性范围为０～８０μｇ／Ｌ，方法简便快速，选择性好，用于茶叶样品中硒的测定，结果满意。