日化用多糖产品中阳离子醚化剂残留量的检测

通过高效液相色谱仪联用线性离子阱质谱建立了阳离子多糖产品中醚化剂残留量的检测方法。以阳离子瓜尔胶为例,采用硼砂-NaOH水溶液对残留醚化剂进行了提取,以C18为分析色谱柱,甲醇-水(0.1%三氟乙酸TFA)作为流动相进行梯度洗脱分离。质谱采用电喷雾正离子(ESI+)电离模式,选择反应检测(SRM)模式检测。结果表明:QUAB-151和QUAB-188在0.5~100μg·mL-1范围内呈良好的线性关系,相关系数(r2)均大于0.998.检出限分别为0.12和0.14μg·mL-1,定量限分别为0.39和0.46μg·mL-1。从0.5~100μg·mL-1的添加浓度的检测结果可以看出,平均回收率均在99.6%~103.2%之间,相对标准偏差(RSD,n=3)均为3.51%以下。该方法操作简便快速,定量准确,可适用于化妆品中QUAB-151和QUAB-188的残留测定。     

CNAS认可实验室质量安全风险管理

随着人们生活质量的提高和科学技术的进步,消费品的质量安全已经成为各个国家关注的焦点,很多国家都制定了相应的技术法规来确保本国消费品的质量安全。美国、欧盟等发达国家对消费品中有毒、有害物质的限量正在逐步降低,这就对公共检测机构的技术水平提出了更高的要求,检得出、检得快、检得准,并出具权威、公正、可信、准确的试验报告,必然要求公共检测机构进行严格、规范、科学的质量安全风险管理,以确保公共检测机构对实验室     

Synthesis and Crystal Structure of Novel Mixed-metal Alkoxide Clusters of Ytterbium and Sodium: Yb4O4（OiPr）16Na12

The mixed-metal cluster Yb4O4(OiPr)16Na12 has been synthesized and structurally determined by IR, elemental analysis, and single-crystal X-ray diffraction. The crystal belongs to the cubic system, space group P23 with a = b = c = 13.9788(3), V = 2731.55(10)3 , Z = 1, Dc = 1.202 g/cm 3 , Mr = 1977.42, = 3.480 mm-1 , F(000) = 972, the final R = 0.0288 and wR = 0.1511 for 1677 observed reflections with Ⅰ > 2σ(Ⅰ). X-ray analysis reveals that Yb4O4 (OiPr)16Na12 is centrosym-metric and the structure contains four ytterbium metals and twelve sodium metals, and each ytterbium atom is coordinated by six oxygen atoms. In addition, an ancillary computational analysis of the optimized molecular unit was provided. The large energy gap (3.31 eV) between HOMO and LUMO indicates that the structure framework is particularly stable.     

[(ButC5H4)2NdMe]2催化聚合甲基丙烯酸甲酯

茂基钕甲基化合物;亲核取代反应;[(ButC5H4)2NdMe]2催化聚合甲基丙烯酸甲酯     

新型的双阴离子型镱(Ⅲ)胺化物{[Me_2Si(NPh)_2]_2Yb[(N~iPr)_2CN(SiMe_3)_2]}{Li(THF)_2}_2的合成及晶体结构

结构新颖的双阴离子型桥联胺基胍基镱(Ⅲ)配合物{[Me2Si(NPh)2]2Yb[(NiPr)2CN(SiMe3)2]}{Li(THF)2}2是通过二胍基镱氯化物[(SiMe2)2NC(N'Pr)2]2Yb(μ-Cl)2Li(THF)2和桥联胺基锂盐PhLiNSiMe2NLiPh反应制得,该配合物经过了IR、元素分析和X-ray晶体结构的测定.该晶体为单斜晶系,P 21/c空间群,a=14.0001(8),b=17.6808(9),c=24.9565(16)A,B=95.994(3),V=6143.8(6)A3,Dc=1.287g/cm3,Z=4.     

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.     

Lanthanide Complexes for Oligomerization of Phenyl Isocyanate

IntroductionThestudyonthereactivitiesoflanthanidecomplexesto wardisocyanateshasattractedmuchattention .Ithasbeenre portedthatlanthanidealkoxides,1anddivalentdiaza pentadi enyllanthanidecomplexes2 canbeusedasthesinglecompo nentinitiatorsforisocyanatespolymerization .Recentlyourre searchgrouphasalsofoundthatlanthanoceneamide ,3diva lentaryloxideofsamarium4 ,5anddivalentsamarocene6 areallactivefortheoligomerizationofphenylisocyanate,andtheactivespeciesforthesethreesystemswereallsuccessfullyisolat…     

二(环戊二烯基)(双烯酮亚胺基)镱配合物的合成和晶体结构

双烯酮亚胺基作为辅助配体在金属有机化学中的应用已经引起了广泛注意，并且发现部分双烯酮亚胺基金属配合物在催化一些极性和非极性单体的聚合中显示良好的催化活性。我们曾经报道具有大体积的双烯酮亚胺亚[{C6H3-2，6-i-Pr2NC（Me）}2CH]^-（L^-）是合成混配型稀土金属化合物的理想配体，为了进一步研究这类稀土金属化合物的合成及反应性能，本文通过双烯酮亚胺基镱二氯化物LYbCl2（THF）2与2倍量的环戊二烯基钠反应，分离得到了标题化合物，并测定了其晶体结构。     

[Li（DME）3][η^5—MeCp）Nd（t—Bu）3[的合成及其对苯乙烯的催化聚合

将ＭｅＣｐＮｄＣｌ１．２ＬｉＣｌ，ｎＴＨＦ和２摩尔（ｇ－ＢｕＬｉ于四氢呋喃和戊烷混合溶剂中反应，合成得到一种新的阴离子型配合物用元素分析，红外光谱等作了表征，配合物溶于苯乙烯，可单独引发苯乙烯本体聚合，得无规聚苯乙烯。