高效液相色谱法测定烟草料液中的糖、甘油和丙二醇

研究了用高效液相色谱法测定烟草料液样品中糖、甘油和丙二醇的方法。烟草料液用Sep-Park-C18固相萃取小柱预分离，以Waters Surar-Pakl钙型阳离子交换柱为固定相，0．05g/L EDTA钙钠水溶液为流动相，示差折光仪为检测器，一次进样测定烟草料液样品中的糖、甘油和丙二醇。线性范围为0．005－5g/L,检测限在1．5－2．5mg/L之间，相对标准偏差为0．89％－1．3％，标准回收率在96．0％－103％之间。方法用于几种烟草料液样品测定，结果令人满意。     

C-410树脂分离富集-电感耦合等离子体质谱法测定地质样品中的金、铂、钯

研究了地质样品中超痕量Au,Pt和Pd的测定方法。采用C－410阴离子交换树脂在1．5mol/L HCl条件下对Au,Pt,Pd的吸附率分别为91．2％、100．0％、95．7％。共存离子除Ge^4 ,Cr^6 ,Ti^4 外，无显著性干扰，用ICP－MS测定Au,Pt,Pd的检出限分别为0．27、0．40和0．19μg/L。当n=8时，Au的RSD为19．2％；Pt的RSD为28．1％；Pd的RSD为15．6％。     

离子色谱荧光检测法测定废水中痕量2-氨基联苯和4-氨基联苯

采用离子色谱荧光检测法测定废水中的2－氨基联苯（2－ADP）和4－氨基联苯（4－ADP），流动相为1．0mL/min的0．06mol/L NaCl,0.08mol/L HCl,40%(V/V)ACN，分离柱为Dinoex OmniPac PCX-500，该法具有良好的重现性和线性关系，2－ADP和4－ADP的回收率分别为98．5％－101．4％和102．2％－104．0％，检测限分别为0．006mg/L和0．10mg/L。     

氢化物发生-原子吸收法测定饮用水中的砷、硒

建立了测定饮用水中砷、硒的氢化物发生－原子吸收法，探讨了盐酸、硼氢化钠溶液的浓度以及样品还原处理对测定结果的影响，测定结果的相对标准偏差（n=7)小于3％，回收率为89．1％－110．7％，测定砷的线性范围为0－40ug/L(r=0.9990)，测定硒的线性范围为0－50ug/L(r=0.9990)，砷、硒的检出限分别为1．06，0．78ug/L。     

导数恒基体强度同步荧光分析法同时测定光谱严重重叠的1-氯蒽和9-溴蒽

通过选择适合测定路径,应用恒基体强度同步及荧光法同时测定了两种光谱严重重叠的蒽衍生物1－氯蒽和9－溴蒽。混合物中1－氯蒽和9－溴蒽不必预分离就能直接同时测定。在混合物中1－氯蒽和9－溴蒽的回收率分别为83．5％－94．0％,90．0％－94．0％,检出限分别为0．69μg/L,10μg/L。     

巯基棉分离富集、石英缝管FAAS法测定河水中痕量铋

研究了巯基棉分离富集、单缝石英管FAAS法测定铋的最佳条件。以盐酸作介质,巯基棉富集铋的最佳吸附酸度为0．1－0．2mol/L(盐酸）,定量洗脱酸度为2mol/L(盐酸）。该法用于测定水中痕量的铋,回收率为96％－102％,相对标准偏差为4．8％。     

4种喹诺酮类药物滤纸基质室温Lin光法研究

提出了以滤纸为基质的环丙沙星、氟罗沙星、洛美沙星和氧氟沙星4种喹诺酮类药物的滤纸基质室温Lin光（PS-RTP)分析的新方法。方法取样量少（1．5μL).其线性动力学范围依次为0．11－55．2、0．35－211、2．10－526、1．03－411（ng/斑点）；灵敏度高，其检出限分别为0．082、0．070、0．080、0．123（ng/斑点）；标准回收率在97．70％－102．2％之间。相对标准偏差RSD＜1．8％。     

流动注射冷蒸气发生法测定环境样品中痕量汞

以气体扩散膜为分离装置，流动注射进样冷蒸气发生法测定了土壤中的汞。试验了载流种类，流速，浓度，还原剂的浓度，流速，载气及春流速等分析参数对测定的影响。实验中观察到Cr(Ⅵ）对汞的响应信号有负干扰。方法的线范围为0－20μg/L，检出限为0．01μg/L，在2μg/L、5μg/L含量水平测定，方法的相对标准偏差（RSD）分别为1．5％和0．54％，回收率在91％－110％之间。     

吡虫啉极谱吸附波的研究及应用

在0．04mol/LNH3－0．2mol/LNH4Cl（pH＝8．0）的介质中,吡虫啉在单扫描极谱仪上于-0．95V（vs,SCE）处产生一灵敏的吸附还原波,其浓度在1．2×10－4~5．0×10-6mol/L之间与峰电流呈良好的线性关系（r＝0．9941）。对于4．0×10-5mol/L吡虫啉,平行测定（n＝6）的RSD为1．38％,回收率为100．0％~101．1％。建立了单扫描极谱测定吡虫啉的新方法,该法对吡虫啉工业品进行测定取得满意的结果。同时对电极反应机理进行了研究。     

复方维生素B片中主要成分的高效毛细管电泳电化学法检测

采用高效毛细管电泳－电化学检测法同时测定复方维生素B片中的主要成分维生素B1，B12，B6和C的含量；研究了电极电位，运行缓冲溶液的浓度和酸度，电泳电压和进样时间等对电泳的影响，以微铂电极为工作电极，检测电位＋0．5V（vs SCE)，在pH9.0的15mmol/L Tris-1mmol/L H3BO3缓冲溶液中，上述4组分在5min内获得基线分离；维生素B1，B12，B6和C的线性范围分别为2．1mg/L-1.0g/L,6.0mg/L-0.80g/L,1.4mg/L-0.72g/L和0．97mg/L-0.44g/L检出限分别为0．50mg/L,1.0mg/L,,0.65mg/L和0．40mg/L；5次测定峰高的相对标准偏差分别为2．4％，3．0％，3．1％，和2．5％，5次测定的平均回收率分别为99％，102％，98％和100％。     

5-[(偶氮苯基)偶氮]-8-氨基喹啉的合成、性质及其应用的研究

本文报道了新试剂5-[(偶氮苯基)偶氯]-8氨基喹啉的合成方法。研究了该试剂的理化性质,分析性能及其与钯显色反应的条件。从而拟定了直接分光光度法测定微量钯的新方法,结果满意。     

4-[(1,3-二氧代丁基)氨基]苯甲酸稀土配合物的合成、表征及发光性质

在乙醇体系中,由主配体4-[(1,3-二氧代丁基)氨基]苯甲酸(H2L,C11H11NO4)、稀土硝酸盐及辅助配体邻菲啰啉(phen)反应合成了两个系列8个配合物[Ln2(L)3(H2O)4]n(Ln=Sm(1),Eu(2),Tb(3),Dy(4));[Ln2(NO3)2(L)2(phen)2]n(Ln=Sm(5),Eu(6),Tb(7),Dy(8))。用元素分析、红外光谱、摩尔电导、热重分析进行表征,确定了产物的化学组成,推断了相应的结构。测定了室温时固体产物的激发和发射光谱,结果表明:由主辅配体共同配位的三元配合物的发光强度好于无辅助配体参与的二元配合物。测定了三元配合物的荧光寿命,其中铕和铽配合物显示较长的荧光寿命。     

Microwave Synthesis and Crystal Structure of Bis {2- [（2,4-dichloro-phenylimino）- methyl]-4,6-diiodo-phenol}-copper（II）

Bis{2-[(2,4-dichloro-phenylimino)-methyl]-4,6-diiodo-phenol}-copper(II) (1) has been synthesized and its structure determined by X-ray diffraction. It crystallizes in the monoclinic system, space group P2 1 /n with a=14.7558(17), b=20.770(2), c=20.3260(19) , β=90.6110(10)°, V=6229.2(11) 3 and Z=8. The Cu atom is surrounded by two O atoms and two N atoms from two 2-[(2,4-dichloro-phenylimino)-methyl]-4,6-diiodo-phenol molecules to form a tetrahedral coordination environment. The complex is linked into a column by weak intermolecular interactions.     

Synthesis and Crystal Structure of 2-[（4-Methoxy- 6-methylthio-2-pyrimidinyl）aminocarbonyl- aminosulfonyl] Benzoic Acid Methyl Ester

1 INTRODUCTION The sulfonylurea herbicides are characterized by broad-spectrum weed control at very low use rates (c.2~75g ai ha-1), good crop selectivity and very low acute and chronic animal toxicity (acute oral LD50 to rat >4000 mg/kg)[1]. They are e…     

Resonance Rayleigh scattering spectra of ion-association nanoparticles of [Co(4-[(5-Chloro-2-pyridyl) azo]-1, 3-diaminobenzene)2]-sodium dodecyl benzene sulfonate system and its analytical application

In pH 1.8-3.0 Britton-Robinson (BR) buffer solution, cobalt (II) reacts with 4-[(5-Chloro-2-pyridyl) azo]-1, 3-diaminobenzene (5-Cl-PADAB, L) to form a cationic chelate [CoL₂]²⁺. When interacting with anionic surfactants (AS) such as sodium dodecyl benzene sulfonate (SDBS), sodium dodecyl sulfate (SDS) or sodium dodecyl sulfonate (SLS), the chelate can only react with SDBS to form ternary ion-association complexes ([CoL₂][SDBS]₂). By virtue of the extrusion action of water and Van der Waals force, the hydrophobic ion-association complexes draw close to each other and further aggregate to form {[CoL₂][SDBS]₂}_n nanoparticles with an average diameter of 30 nm. As a result, resonance Rayleigh scattering (RRS) is enhanced greatly and new RRS spectra appear. Under the same conditions, both SDS and SLS exhibit no similar reactions and do not result in obvious change of RRS. Therefore, SDBS can be determined selectively by RRS method in the presence of SDS or SLS. The wavelength of 516 nm was chosen as a detection wavelength, the linear range and the detection limit (3σ) are 0.05-6.0 μg mL⁻¹ and 0.015 μg mL⁻¹ for the determination of SDBS, respectively. The characteristics of RRS spectra of the [CoL₂]²⁺-SDBS system, the optimum conditions of the reaction and the influencing factors have been investigated. The effects of coexisting substances have been examined too, indicating a good selectivity of the method for the determination of SDBS. The method can be used for the determination of SDBS in waste water and river water samples, and the results are satisfactory compared with those of standard samples of SDBS. Based on the formation of {[CoL₂][SDBS]₂}_n nanoparticles, a sensitive, simple and rapid method has been developed for the determination of SDBS in environmental water samples using a RRS technique. Moreover, the reaction mechanism was discussed.     

Synthesis,Structure and Fluorescent Property of Coordination Polymer from 4-[（8-Hydroxy-5-quinolinyl）azo]-benzoic Acid

One new coordination polymer based on 4-[（8-hydroxy-5-quinolinyl）azo]-benzoic acid（H2L）, { [CdL（H20）]·H2O}n（1） was solvothermally synthesized and structurally characterized by single-crystal X-ray diffrac- tion, infrared spectrometry, elemental analysis, powder X-ray diffraction（PXRD） and thermogravimetric analysis （TGA）. In compound 1, L2- ligands link Cd（II） to form a sinusoidal ruffling layer, in which the carboxylic groups connect Cd（II） into an infinite Cd--O chain. And the layers are further stabilized by hydrogen bonding and π-π in- teractions, forming a three-dimensional（3D） supramolecular network. In addition, the fluorescent property of compound 1 was also investigated.     

2-[2-(6-Methylbenzothiazolyl)azo]-5-Diethylaminobenzoic acid as a new analytical reagent for the spectrophotometric determination of nickel

A new thiazolylazo chromogenic reagent, 2-[2-(6-methylbenzo-thiazoly)azo]-5-diethylaminobenzoic acid (6-Me-BTAEB), has been synthesized. Its chromogenic reaction with microamounts of nickel in the presence of sodium dodecylsulfate (SDS) has been thoroughly studied. 6-Me-BTAEB reacts with nickel(II) in weak acid medium containing appropriate amounts of SDS to form a blue-violet complex with high sensitivity, good selectivity and high stability. The composition is found to be 1:2 (nickel to 6-Me-BTAEB) and its absorption maximum is at 650 nm with an apparent molar absorptivity of 1.67 × 10⁵l mole^–1 cm^–1. Beer's law is obeyed over the range 0-0.4 g of nickel per ml. The proposed method has been applied to the direct determination of nickel in aluminium alloys, pure magnesium and low alloy steels at the 0.2–0.3% (w:w) level with satisfactory results.     

Synthesis of 2-Aryl and 2-Hetaryl Derivatives of 2'-Aminospiro[(1,3-dioxane)-5,5'-thiazolin]-4'-one and Spiro[(1,3-dioxane)-5,5'-thiazolidine]2',4'-dione

2-(Het)aryl derivatives of 2'-aminospiro[(1,3-dioxane)-5,5'-thiazolin]-4'-one or spiro[(1,3-dioxane)-5,5'-thiazolidine]-2',4'-dione are formed by the acid catalyzed interaction of 2-amino-5,5-bis(hydroxymethyl)-4-thiazolinone or its oxo analog 5,5-bis(hydroxymethyl)thiazolidine-2,4-dione with (hetero)aromatic aldehydes.     

Enamine Configuration of 5-Methyl-2-phenyl-4-[（Z）-3-tolylamino-phenylmethylene]pyrazol-3（2H）-one

1 INTRODUCTION In contrast to the old-line academic and practical studies of 1-phenyl-3-methyl-4-benzoyl-5-pyrazo- lone (PMBP) on the metal coordination chemistry[1], the complexes of β-ketoamines derivated from PMBP received little attention due to its complicated com- plexation. However, in recent years, there has a sudden growth of this area as a result of its timely interest in biological activities[2]. Recently, a series of β-ketoamines[3] containing PMBP have been prepared fro…     

Synthesis and Crystal Structure of 1-[(1-Phenyl-4-cyano)pyrazol-5-yliminomethyl]- 2-nitroiminoimidazolidine

1　INTRODUCTIONNeonicotinoids[1～2]areanovelanddistinctclassofinsecticides.Theycombineselectiveactivityagainstinsectswithafavourablesafetyprofile.Neonicotinoidsactatthenicotinicacetylcholinereceptor(nAChR)[3～4].Sincethefirstneonicotinoid,imi-dacloprid(IMI)1wasintroducedtothemarketbyBayerin1991,alotofitsanalogswerereported.Thesecompoundshavethesamestructuralunit,asshowedindashedlineareainIMI.AccordingtothemodelproposedbyYamamotoetal[5],thedistancebetweenthetwonitrogenatomsofIMIisthe…