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3.
Forensic Sci Int ; 266: 139-147, 2016 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-27262685

RESUMO

The effects on the separation of writing ink dyes and the repeatability of the Rf values from using different grades of chemicals used in solvent system I (SSI) and solvent system II (SSII) for thin-layer chromatographic (TLC) ink analysis were studied. Solvent system I consists of a 70:35:30 mixture of ethyl acetate, ethanol, and water. Solvent system II consists of a 50:10:15 mixture of ethanol, water, and n-butanol. Since 1991, the ASTM International Guideline E 1422 has recommended that the purity of solvents should be "reagent grade" and that water quality should be "distilled or equivalent." A total of 25 blue and 25 black inks were selected for analysis. Thirteen of each color ink were ballpoint and the remainder were non-ballpoint. The observations show that there is a solvent grade effect on both the separation and clarity of the ink dyes and the repeatability of their Rf values. These results indicate that the grades and manufacturers of solvents used in solvent systems for thin-layer chromatography must be consistent. This is especially critical for searching TLC plates against those from a large ink library in casework. Overall, the combination of solvents that produced the best results for solvent system I consisted of denatured ethanol, HPLC grade water, and ACS grade ethyl acetate. There was no consensus for the best combination of solvent grades for solvent system II; however, it was shown that different grades did have an effect on the separation of ink components.

4.
Inorg Chem ; 47(7): 2264-6, 2008 Apr 07.
Artigo em Inglês | MEDLINE | ID: mdl-18338851

RESUMO

The reaction of Ru2(OAc)4Cl with 2.2 equiv of H2esp (esp = alpha,alpha,alpha',alpha'-tetramethyl-1,3-benzenedipropionate) resulted in a new compound, Ru2(esp)2Cl (1), that is soluble in organic media. 1 is an active catalyst for the oxygenation of organic sulfides by tert-butyl hydroperoxide (TBHP) in both an acetonitrile solution or neat (solvent-free) conditions. Solvent-free reactions display the quantitative utility of TBHP and hence excellent chemical selectivity for sulfoxide formation.


Assuntos
Compostos Organometálicos/química , Oxigênio/química , terc-Butil Hidroperóxido/química , Catálise , Cristalografia por Raios X , Ligantes , Modelos Moleculares , Estrutura Molecular , Ésteres do Ácido Sulfúrico/química
5.
Inorg Chem ; 45(19): 7973-80, 2006 Sep 18.
Artigo em Inglês | MEDLINE | ID: mdl-16961393

RESUMO

A novel Cu(II)2 complex of the [18]ane-N6 macrocycle ([18]ane-N6 = 1,4,7,10,13,16-hexaazacyclooctadecane) was prepared from the reaction between [18]ane-N6 and Cu(II) salts such as Cu(NO3)2 and Cu(OAc)2. A structural study of the complex derived from Cu(OAc)2 (1) revealed a Cu(II)2 core encircled by a [18]ane-N6 ligand and two mu-O-OAc ligands. The facile replacement of mu-O-OAc by a phosphate monoester [PO3(OR)2-] yielded a number of bis(phosphate monoester)dicopper complexes with ROPO3(2-) as hydrogen phosphate (HPO4(2-), 3a), phenyl phosphate [PO3(OPh)2-, 3b], glycerol 2-phosphate [PO3(OCH(CH2OH)2)2-, 3c], alpha-d-gluocose phosphate [PO3(C6H11O6)2-, 3d], and dl-alpha-glycerol phosphate [PO3(OCH2CHOHCH2OH)2-, 3e]. Structural studies of compounds 3a-d confirmed both the retention of the Cu2{[18]ane-N6} core and a mu-O-PO3(OR) coordination mode. Displacement of acetate by a phosphate monoester in an aqueous solution was accompanied by a significant change in the visible absorption, which enables the establishment of relative association constants of PO3(OR)2- on the order of 10(4) in the unbuffered solution and 10(3) in the buffered solution (HEPES). Measurement of the magnetic susceptibility of compound 3a over the temperature range of 5-300 K and subsequent modeling revealed a weak antiferromagnetic coupling (J = -1.1 cm(-1)) between two Cu(II) centers.


Assuntos
Carbono/química , Cobre/química , Ésteres/química , Magnetismo , Nitrogênio/química , Fosfatos/química , Cristalografia por Raios X , Íons/química , Modelos Moleculares , Estrutura Molecular , Titulometria
6.
J Am Chem Soc ; 125(44): 13332-3, 2003 Nov 05.
Artigo em Inglês | MEDLINE | ID: mdl-14583009

RESUMO

Dicopper-[18]ane-N6 complex functions as a broad spectrum receptor for phosphate monoesters.

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