7428-48-0Relevant articles and documents
Preparation of PbS and PbSe nanocrystals by a new solvothermal route
Gautam, Ujjal K.,Seshadri, Ram
, p. 669 - 676 (2004)
A new solvothermal route for the preparation of nanocrystals of PbS and PbSe, involving the reaction of lead stearate with sulfur or selenium and tetralin (tetrahydronaphthalene) in toluene solvent is described. Tetralin in the presence of S/Se gives H2S/H2Se and gets aromatized to naphthalene. The nanocrystals have been characterized by powder X-ray diffraction and electron microscopy. Use of surfactant Triton X-100 (polyoxyethylene(10)isooctylphenyl ether) resulted in both nanorods and nanoparticles of PbSe. Capping by citric acid and malonic acid reduce the particle sizes to less than 10nm.
Preparation and Structure of Q-State Lead Sulfide Monolayers in Metastable Stearic Acid Langmuir-Blodgett Films
Peng, Xiaogang,Guan, Shiquan,Chai, Xiangdong,Jiang, Yueshun,Li, Tiejin
, p. 3170 - 3174 (1992)
Monolayers of Q-state PbS were prepared by exposure of Langmuir-Blodgett (LB) films of lead stearate to H2S at a pressure of 1 Torr.Its long spacing measured by X-ray diffraction is 50.5 +/- 0.2 Angstroem which is just the same with that of lead stearate LB films.It was determined by X-ray diffraction and IR that the hydrocarbon chains are still packed in an orthorhombic unit cell after the reaction.The carboxylic groups yielded by the reaction form a ring structure by hydrogen bonds which controls PbS within a monolayer.A structured UV-visible absorption spectrum of the PbS monolayer was obtained.The PbS monolayer consists of a two-dimensional domain or linear form of PbS.The latter is more possible.Their size is almost homogeneous.The onset of the absorption of PbS monolayer is blue-shifted by 1.4 eV with respect to bulk PbS.
Scanning Tunneling Microscopy and UV-Visible Spectroscopy Studies of Lead Sulfide Ultrafine Particles Synthesized in Langmuir-Blodgett Films
Zhu, Rong,Min, Guangwei,Wei, Yu,Schmitt, Hans J.
, p. 8210 - 8211 (1992)
Ultrafine semiconductor particles of lead sulfide were synthesized by exposing lead stearate Langmuir-Blodgett films to hydrogen sulfide gas.By heating the Langmuir-Blodgett films containing PbS ultrafine particles in nitrogen gas at 120 deg C for 1 h, the molecules for stearic acid were evaporated and the lead sulfide particles were left.The PbS ultrafine particles before and after evaporation were analyzed by using a scanning tunneling microscope and a UV-visible spectrophotometer.
Lead(ii) soaps: Crystal structures, polymorphism, and solid and liquid mesophases
Martínez-Casado,Ramos-Riesco,Rodríguez-Cheda,Redondo-Yélamos,Garrido,Fernández-Martínez,García-Barriocanal,Da Silva,Durán-Olivencia,Poulain
, p. 17009 - 17018 (2017/07/24)
The long-chain members of the lead(ii) alkanoate series or soaps, from octanoate to octadecanoate, have been thoroughly characterized by means of XRD, PDF analysis, DSC, FTIR, ssNMR and other techniques, in all their phases and mesophases. The crystal structures at room temperature of all of the members of the series are now solved, showing the existence of two polymorphic forms in the room temperature crystal phase, different to short and long-chain members. Only nonanoate and decanoate present both forms, and this polymorphism is proven to be monotropic. At higher temperature, these compounds present a solid mesophase, defined as rotator, a liquid crystal phase and a liquid phase, all of which have a similar local arrangement. Since some lead(ii) soaps appear as degradation compounds in oil paintings, the solved crystal structures of lead(ii) soaps can now be used as fingerprints for their detection using X-ray diffraction. Pair distribution function analysis on these compounds is very similar in the same phases and mesophases for the different members, showing the same short range order. This observation suggests that this technique could also be used in the detection of these compounds in disordered phases or in the initial stages of formation in paintings.
Coordination geometry of lead carboxylates - Spectroscopic and crystallographic evidence
Catalano, Jaclyn,Murphy, Anna,Yao, Yao,Yap, Glenn P. A.,Zumbulyadis, Nicholas,Centeno, Silvia A.,Dybowski, Cecil
, p. 2340 - 2347 (2015/01/30)
Despite their versatility, only a few single-crystal X-ray structures of lead carboxylates exist, due to difficulties with solubility. In particular, the structures of long-chain metal carboxylates have not been reported. The lone electron pair in Pb(ii) can be stereochemically active or inactive, leading to two types of coordination geometries commonly referred to as hemidirected and holodirected structures, respectively. We report 13C and 207Pb solid-state NMR and infrared spectra for a series of lead carboxylates, ranging from lead hexanoate (C6) to lead hexadecanoate (C18). The lead carboxylates based on consistent NMR parameters can be divided in two groups, shorter-chain (C6, C7, and C8) and longer-chain (C9, C10, C11, C12, C14, C16, and C18) carboxylates. This dichotomy suggests two modes of packing in these solids, one for the short-chain lead carboxylates and one for long-chain lead carboxylates. The consistency of the 13C and 207Pb NMR parameters, as well as the IR data, in each group suggests that each motif represents a structure characteristic of each subgroup. We also report the single-crystal X-ray diffraction structure of lead nonanoate (C9), the first single-crystal structure to have been reported for the longer-chain subgroup. Taken together the evidence suggests that the coordination geometry of C6-C8 lead carboxylates is hemidirected, and that of C9-C14, C16 and C18 lead carboxylates is holodirected.
Characterisation of metal carboxylates by Raman and infrared spectroscopy in works of art
Otero, Vanessa,Sanches, Diogo,Montagner, Cristina,Vilarigues, Mrcia,Carlyle, Leslie,Lopes, Joo A.,Melo, Maria J.
, p. 1197 - 1206 (2015/02/19)
This work introduces the complementary use of μ-Raman and μ-Fourier transform infrared (IR) spectroscopy for the detection of specific carbon chains and cations for the identification of metal carboxylates within oil paint microsamples. Metal carboxylates (metal soaps) form naturally when free fatty acids react with metal cations and may also be found as additives or degradation products. Twenty-two metal carboxylates were synthesised, and their spectra assembled in a reference database. Metal salts of cations commonly present in oil paintings were used, including lead, zinc, calcium, cadmium, copper and manganese. The fatty acids selected were the saturated acids palmitic (C1 6:0) and stearic (C18:0) and the polyunsaturated oleic acid (C1 8:1). Azelaic acid (C9 diacid), a product resulting from autoxidation of polyunsaturated acids, was also included. Metal carboxylates were characterised by Raman and IR spectroscopy, and their structures were confirmed by X-ray diffraction. Raman and IR spectroscopy proved to be complementary techniques for a full identification of the metal carboxylates in complex aged paint. Raman enables the differentiation of the carbon chain length in the C-C stretching region (1120-1040 cm-1), and IR distinguishes the metal cation in the COO- stretching absorption region (1650-1380cm-1). Principal component analysis was applied to the spectra in order to facilitate a fast and accurate method to discriminate between the different metal carboxylates and to aide in their identification. Finally, spectra from case studies were successfully projected in the principal component analysis models built, enabling a higher confidence level for the identification of copper palmitate and copper azelate in two 19th-century Portuguese oil paintings.
Synthesis of biodiesel via homogeneous Lewis acid catalyst
Di Serio,Tesser,Dimiccoli,Cammarota,Nastasi,Santacesaria
, p. 111 - 115 (2008/10/09)
Nowadays, most biodiesel (fatty acids methyl esters, FAME) is produced by the transesterification of triglycerides (TG) of refined/edible type oils using methanol and an homogeneous alkaline catalyst. However, production costs are still rather high compared with the ones of petroleum-based diesel fuel. To lower costs and make biodiesel competitive less-expensive feedstocks such as waste fats or non-edible type oils could be used. The use of homogeneous alkaline catalysts in the transesterification of such types of fats and oils poses great difficulties due to the presence of large amounts of free fatty acids (FFA). This paper studies the use of carboxylic salts as a possible alternative, because these catalysts are active also in the presence of high FFA concentrations. The most active catalyst (Cd, Mn, Pb, Zn carboxylic salts) have been individuated and a correlation of the activities with the cation acidity has been found.
Preparation of metal carboxylates and their stabilizing performance under intense high-pressure shear treatment
Akhmetkhanov,Kolesov,Kadyrov,Karmilov,Zaikov
, p. 842 - 845 (2007/10/03)
Solid-phase synthesis of certain metal carboxylates and their effect on stabilization of polyvinyl chloride under intense high-pressure shear treatment were studied.
The characterisation of lead fatty acid soaps in 'protrusions' in aged traditional oil paint
Plater, M. John,De Silva, Ben,Gelbrich, Thomas,Hursthouse, Michael B.,Higgitt, Catherine L.,Saunders, David R.
, p. 3171 - 3179 (2008/10/08)
Lead(II) carboxylate soaps of two fatty acids, palmitic (C 15H31COOH) and stearic acids (C17H 35COOH), and a dicarboxylic acid, azelaic acid (HOOCC 7H14COOH), have been synthesised and characterised by FTIR spectroscopy. These acids are all encountered in aged traditional oil paint, the azelaic acid resulting from the oxidative degradation of unsaturated fatty acids in the oil. Lead(II) azelate synthesised by hydrothermal methods was characterised by single crystal structure determination. This has a 3D polymeric structure with lead(II) ions linked by carboxylate bridges to form an infinite stack of (PbO4)n units. These layers are connected to adjacent layers by an infinite number of parallel C(CH 2)7C chains arranged perpendicularly to the stacks. The lead(II) ions display an unusual 7-fold coordination. The first direct evidence that the 'protrusions' encountered in aged traditional lead-containing oil paints contain lead soaps is reported. Their mechanism of formation is discussed.
