水杨醛—5—溴—水杨酰腙与锌的高灵敏度荧光反应及其应用

合成了新荧光试剂水杨醛－５－溴－水杨酰腙（ＳＡＢＳＨ），详细研究了试剂与锌的荧光反应新体系的最适宜条件．在ｐＨ７．９的异丙醇／水（体积比１∶１）溶液中，该试剂与Ｚｎ２＋形成配合物，组成比为１∶２（金属∶试剂），λｅｘ／λｅｍ＝３９３ｎｍ／４６５ｎｍ．所建立锌的荧光分析方法的线性范围为０～４００μｇ／Ｌ，相对标准偏差为１．２％，检出限为１．３μｇ／Ｌ．考察了３６种离子的干扰情况．方法成功地用于面粉、大米、人尿和矿泉水中痕量锌的测定．     

二溴水杨醛异烟酰腙的合成及其与钪的荧光反应研究

合成了新荧光试剂３，５－二溴水杨醛异烟酰腙（简称ＤＢＳＩＮ），研究了该试剂与钪的荧光反应，在ｐＨ４．７～５．５乙醇／水溶液中，试剂与钪所形成的荧光络合物的λｅｘ＝３３５．４ ｎｍ、λｅｍ＝５１０ｎｍ．提出了混合稀土氧化物中微量钪的测定法。     

钪—水杨醛苯甲酰腙高灵敏度荧光反应及其应用

研究了水杨醛苯甲酰腙（ＳＡＢＨ）与钪荧光反应新体系的最佳条件。在ｐＨ＝６．４乙醇／水（６．２：３．８）溶液介质中，形成络合物的组成比１：３（钪、试剂），λｅｘ／λｅｍ＝３８５ｎｍ／４５５ｎｍ，建立钪荧光分析法的线性范围为０￣１００μｇ／Ｌ；相对标准偏差１．５％；检出下限为０．０２５μｇ／Ｌ。考察了３０种共存离子的干扰情况，方法成功用于地质中样中痕量钪的测定。     

水杨醛水杨酰腙与镓的荧光反应及其应用

测定了水杨醛水杨酰腙的离解常数。研究了试剂与镓荧光反应体系的最佳条件，观察到在ＰＨ３．２－氯乙酸缓冲液和乙醇：水＝２：３介质中，络合物组成比为１：３（镓：试剂），λｅｘ／λｅｍ＝３７０／４５５ｎｍ。建立镓分析方法的线性范围为０－１４０μｇ／Ｌ，相对标准偏差２．４％，检测限为１．４μｇ／Ｌ。考察了３６种共存组分的干扰情况，方法用于适当分离的半导体材料硅和地质样品中痕量镓的测定，结果满意。     

水杨醛异烟酰腙与镓荧光反应的研究

本文研究了荧光新试剂水杨醛异烟酰腙与镓的荧光反应,用紫外光谱法测定了试剂离解常数。在此荧光体系中,荧光配合物λ_(ex)=395nm、λ_(em)=480nm。在pH3.8、60％(V/V)乙醇介质中,测定的线性范围为0～1.0 μg/10mL,方法灵敏度为4×10~(-4)ppm。用荧光法测定了配合物的组成比及表观稳定常数。建立了镓的新荧光光度法,将其用于地质样品分析,精密度和准确度良好。     

Zn的3，5-二溴水杨醛水杨酰腙配合物的合成、表征及晶体结构

The title complex [Zn(C₁₄H₈N₂O₃Br₂)(C₅H₅N)₃] was synthesized in DMF and pyridine. It has been characterized by IR, element analysis and X-ray diffraction analysis. The crystal structure of the title complex belongs to monoclinic space group P2₁/c with cell parameters: a=0.999 78(6) nm, b=1.951 11(13) nm, c=1.496 02(10) nm, β=97.126 0(10)°, and V=2.895 7(3) nm³, Dc=1.639 g·cm^-3, Z=4, F(000)=1 424, μ=3.647 mm^-1, the final R=0.061 0 and wR=0.140 2 for 3 528 observed reflections with I>2σ(I). The X-ray crystal structure analysis revealed that the center zinc(Ⅱ) is bonded to two oxygen atoms and one nitrogen atom from a tridentate ligand and three nitrogen atoms from three solvent pyridine molecules to form a six-coordinate octahedron. CCDC: 261047.     

铝-水杨醛苯甲酰腙荧光反应的研究及应用

本文研究了Al~(3+)-水杨醛苯甲酰腙高灵敏度荧光体系,络合物的荧光激发波长=375nm,发射波长=450nm。铝量在0～1.4μg/10ml范围内,荧光强度与其含量成正比,灵敏度为0.4ppb。方法可用于试剂中微量铝的检测,结果令人满意。     

β—环糊精增敏邻羟基萘醛水杨酰腙—锶荧光反应及其应用

合成了新荧光试剂邻羟基萘醛水杨酰腙，并研究了β－环糊精对试剂与锶形成包络物的最佳条件。确定了形成包络物的包结比为１：１、包络常数为１．１７×１０＾４，在λｅｘ／λｅｍ＝３７０／４８０ｎｍ，测定锶的线性范围为０．０￣０．０１８ｍｇ／Ｌ检测限０．０８３μｇ／Ｌ，检测限０．０８３μｇ／Ｌ，是目前测定锶最灵敏的方法，成功的应用于海产品和矿泉水中痕量锶的测定。     

水杨醛苯腙与铜荧光反应的研究及其应用

水杨醛苯腙与铜荧光反应的研究及其应用江崇球，唐波，傅红燕，曹红，张晓刚（山东师范大学化学系，济南，２５００１４）关键词铜，水杨醛苯腙，荧光分析胺类试剂是一类理想的荧光分析试剂［１］，用其测定Ａｌ３＋［２］、Ｇａ３＋［３］、Ｚｎ２＋［４］已显示出其灵敏...     

苯偶氮水杨醛异烟酰腙与镉的高灵敏度荧光反应及其应用

1引言镉是一种剧毒重金属。长期接触镉,能引起多种癌症。人们急需各种改进的方法来检测各种环境样品、工业废水以及生物组织里的Cd2 含量。本研究合成了新荧光试剂苯偶氮水杨醛异烟酰腙(BSIH),实验了试剂与镉的荧光反应新体系的最适宜条件。建立了一个新的测定痕量镉的荧光分析方法,方法的线性范围为0.6~120.0μg/L;检出限为0.32μg/L,方法成功地应用于自来水、河水和废水中镉的测定。2实验部分2.1仪器与试剂RF-5000型荧光光度计(日本岛津公司);PHS-2C型pH计(上海雷磁仪器厂);Cd2 标准溶液1 g/L;标准工作液:1μg/L;1×10-4mol/L苯偶…     

Fluorescence Enhancement of Samarium－Thenoyl－trifluoroacetone－Cetyltrimethylammonium Bromide－Triton X－100 by Scandium

ＦｌｕｏｒｅｓｃｅｎｃｅＥｎｈａｎｃｅｍｅｎｔｏｆＳａｍａｒｉｕｍ－Ｔｈｅｎｏｙｌ－ｔｒｉｆｌｕｏｒｏａｃｅｔｏｎｅ－ＣｅｔｙｌｔｒｉｍｅｔｈｙｌａｍｍｏｎｉｕｍＢｒｏｍｉｄｅ－ＴｒｉｔｏｎＸ－１００ｂｙＳｃａｎｄｉｕｍＺＨＵＧｕｉ－ｙｕｎ，ＬＩＵＰ...     

A Study on the Fluorescence System of Sc-BPMPHD-CTMAB and Its Analytical Application

IntroductionThe fluorescence of Sc(3+) itself in solution is not observed. After complexed with an organic ligand with a chromophore, Sc(3+) makes the ligand, which has no or has weak fluorescence, emit strong fluorescence. The fluorescence reagents of Sc~(3+) have been summarized inreferences[1,2], but the derivative of diacylated pyrazolone as a fluorescence reagent of Sc~(3+) hasnot been reported. The experiments indicated that the synthetic derivative of diacylated pyrazolone, 1, 6-bi (1…     

Fluorimetric Determination of Trace Amounts of Scandium with Di-2-pyridyl-ketone 2-Furoylhydrazone

Abstract

The reaction of Di-2-pyridyl-ketone 2-furoylhydrazone (DPFH) with scandium in an aqueous ethanolic medium (4% v/v of ethanol) has been studied. A spectrofluorimetric method based on the formation of a fluorescent complex is proposed for the determination of scandium. With excitation at 387 nm, the scandium (III) chelate has an emission maximum at 492 nm; the reaction is carried out at pH 6.5–7.5. The accuracy and precision of the method are demonstrated by the analysis of synthetic mixtures containing various amounts of scandium. 10 – 140 ng/ml of scandium can be determined with a relative error of ±1.3%.     

Scandium Reduced Arene Complex: Protonation and Reaction with Azobenzene

The reactivity of the reduced anthracene complex of scandium [Li(thf)₃][Sc{N(tBu)Xy}₂(anth)] ( 2-anth-Li ) (Xy=3,5-Me₂C₆H₃; anth=C₁₄H₁₀²⁻, thf=tetrahydrofuran) toward Brønsted acid [NEt₃H][BPh₄] and azobenzene is reported. While a stepwise protonation of 2-anth-Li with two equivalents of [NEt₃H][BPh₄] afforded the scandium cation [Sc{N(tBu)Xy}₂(thf)₂][BPh₄] ( 3 ), reduction of azobenzene gave a thermolabile, anionic scandium reduced azobenzene complex [Li(thf)][Sc{N(tBu)Xy}₂(η²-PhNNPh)] ( 4 ), which slowly lost one of the anilide ligands to form the neutral scandium azobenzene complex dimer [Sc{N(tBu)Xy}(μ-η²:η²-Ph₂N₂)]₂ ( 5 ). Exposure of 3 to CO₂ produced the scandium carbamate complex [Sc{κ²-O₂CN(tBu)(Xy)}₂][BPh₄] ( 6 ) as a result of CO₂ insertion into the Sc−N bonds. In an attempt to prepare scandium hydrides, the reaction of 3 with the hydride sources LiAlH₄ and Na[BEt₃H] led to the terminal aluminum hydride [AlH{N(tBu)Xy}₂(thf)] ( 7 ) and the scandium n-butoxide [Sc{N(tBu)(Xy)}₂(μ-OnBu)] ( 8 ) after Sc/Al transmetalation and nucleophilic ring-opening of THF, respectively. All reported compounds isolated in moderate to good yields were fully characterized.     

Synthesis and Crystal Structure of the Rubidium Scandium Telluride RbSc5Te8

During attempts to synthesize the rubidium dicopper triscandium hexatelluride RbCu₂Sc₃Te₆ in analogy to CsCu₂Sc₃Te₆ from 2:3:6‐molar mixtures of the elements (Cu, Sc and Te) with an excess of RbBr as flux and rubidium source, after 14 days at 900 °C in torch‐sealed evacuated silica tubes brown lath‐shaped crystals of RbSc₅Te₈ did form instead. This new compound crystallizes monoclinically in space group C2/m (no. 12) with two formula units in a unit cell of the dimensions a = 2130.61(9) pm, b = 413.94(2) pm, c = 1022.03(5) pm and β = 104.392(4)°. The crystal structure of RbSc₅Te₈ consists of a three‐dimensional anionic framework of face‐, edge‐ and vertex‐sharing [ScTe₆]⁹⁻ octahedra that provides one‐dimensional tunnels with a distorted square shape. For charge compensation they are occupied with Rb⁺ cations (CN = 10) coordinated in a trans‐face bicapped cubic fashion by Te²⁻ anions.     

Fluorescence Reaction of 5- (p-Methoxyphenylazo)-8-(p-tolylsulfonamido)quinoline with Cobalt(II) and Its Analytical Application

Abstract

5-(p-Methoxyphenylazo)-8-(p-tolylsulfonamido) quinoline(MTAQ) has been synthesized. The product was checked by IR, theroograviae-try, NMR and elemental analysis. A highly sensitive spectrofluorim-etric method has been developed for the determination of cobalt(II) based on the formation of a complex with MTAQ in slightly basic medium aqueous solution and In the presence of nonionic surfactant, tween-80. The complex shows two excitation maxima at 304 nm and 338 nm, its emission maximum is centred at 402 nm. The fluorescence intensity is proportional to cobalt(II) concentration in the range of 0-85 ppb. The method has good selectivity and has been applied to the direct fluorimetric determination of trace cobalt(II) in pig's liver, Dianchi shrimp and celery.     

水杨醛-1H-苯并三唑-1-乙酰腙与镧(Ⅲ)配合物的制备、表征及热化学

在甲醇中,利用水杨醛-1H-苯并三唑-1-乙酰腙(C15H13N5O2,简称SBTH)与高氯酸镧反应,制得一新配合物,经元素分析、化学分析并结合热分析确定了其组成为La(C15H12N5O2)( C15H11N5O2)•2.5H2O.利用电导测定、红外光谱、1H NMR和TG-DTG等手段推测了配合物的结构.用微热量计测定了配合物在不同浓度(b)时的溶解焓,用计算机拟合求得该配合物的标准摩尔溶解焓(ΔsolHmΘ=－135.62 kJ•mol－1)及溶解焓(ΔsolH)的经验公式(ΔsolH=－135.62－11633b＋3761.5b1/2),并由此分别推导出配合物的相对表观摩尔焓(Li)、相对偏摩尔焓(Li)以及配合物稀释焓(ΔdilH1,2)的经验公式:Li=－11633b＋3761.5b1/2；Li=－23266b＋5642.2b1/2和ΔdilH1,2=－11633(b21/2－b11/2)＋3761.5(b2－b1).还研究了配合物的热分解过程,利用Kissinger公式计算了配合物主要分解阶段的表观活化能(Ea=470.24 kJ•mol－1).     

Water-based Synthesis and Properties of a Scandium 1,4-Naphthalenedicarboxylate

A new scandium naphthalenedicarboxylate with the framework composition [Sc₂(1,4-NDC)₃] (H₂-1,4-NDC = 1,4-naphthalenedicarboxylic acid) was obtained under hydrothermal synthesis conditions. A structure model could be developed by a combination of 3D electron diffraction measurements and computationally assisted structure determination, which was further validated by a good agreement with the experimental powder X-ray diffraction pattern. The structure consists of isolated ScO₆ octahedra interconnected by the carboxylate groups of linker molecules to form chains. These chains are connected by the naphthalene-moieties to form a three-dimensional framework with square-shaped pores and the organic group pointing into the pores. Although very similar synthesis conditions were chosen, [Sc₂(1,4-NDC)₃] is not isostructural to aluminum naphthalenedicarboxylate [Al(OH)(1,4-NDC)], which crystallizes in a MIL-53 type structure. This can be traced back to the different inorganic building units that are observed. The compound was thoroughly characterized by elemental analysis, IR spectroscopy, sorption measurements, thermogravimetric analysis and luminescence measurements. [Sc₂(1,4-NDC)₃] exhibits a high thermal stability and a ligand-based blue luminescence in the solid state at room temperature.