Pentaerythritol chromatography

Determination of Acetone In Pentaerythritol-trinitrate By Gas Chromatography , NAVORD 7014, AD 231855 (I960) 110) J. Carol,... 

Initial work was carried out with 3,9-bis(methylene-2,4,8,10-tetraoxaspiro[5,5] undecane) where R = H (11). However, this monomer contains two electron donor alkoxy groups on one double bond which is thus highly susceptible to a cationic polymerization. For this reason, the monomer is extremely difficult to handle and cannot be analyzed by gas chromatography since it does not survive passage through the column. It is prepared by the dehydrohalogen-ation reaction of the reaction product of pentaerythritol and chloro-acetaldehyde,... 

If simple sample pretreatment procedures are insufficient to simplify the complex matrix often observed in process mixtures, multidimensional chromatography may be required. Manual fraction collection from one separation mode and re-injection into a second mode are impractical, so automatic collection and reinjection techniques are preferred. For example, a programmed temperature vaporizer has been used to transfer fractions of sterols such as cholesterol and stigmasterol from a reversed phase HPLC system to a gas chromatographic system.11 Interfacing gel permeation HPLC and supercritical fluid chromatography is useful for nonvolatile or thermally unstable analytes and was demonstrated to be extremely useful for separation of compounds such as pentaerythritol tetrastearate and a C36 hydrocarbon standard.12... 

A flame-dried 1-liter reactor was charged with ethoxylated pentaerythritol tetrakis-(3-mercaptopropionate) (46.3 mmol), the step 1 product (185 mmol), and 300 ml of dioxane and then treated with 2,2 -azobisisobutyronitrile (4 mmol). The mixture was then heated to 70°C for 36 hours and concentrated. The residue was purified by column chromatography with hexane/acetone, 30 70, respectively, and the product isolated as a dark orange viscous liquid. 

Fig. 5. Solvating gas chromatography (SGC) separation of a standard explosive mixture. Injected amounts 0.33 pg nitroglycerine (NG), 3.3 pg all others. Peaks (1) nitroglycerine, (2) 2,6-dinitrotolene, (3) 2,4-dinitrotoluene, (4) 2,4,6-trinitrotoluene, (5) pentaerythritol tetranitrate (PETN). Reprinted from Bowerbank et al. [48], Copyright (2000), with permission from Elsevier.

BTT and BTN, butane-1,2,4-triol-trinitrate DNT, dinitrotoluene EGDN, ethylene glycol dinitrate HPLC, high-performance liquid chromatography LOD, limits of detection MDQ, minimum detectable quantities NB, nitrobenzene NG, nitroglycerine NN, nitronaphthalene NT, nitrotoluene PETN, pentaerythritol tetranitrate RDX, cyclotrimethylene trinitramine SFE, supercritical fluid extraction SGC, solvating gas chromatography TDM, thermal desorption modulator TNB, trinitrobenzene and TNT, trinitrotoluene. 

Quantification. Gas Chromatography. In blood or urine pentaerythritol tetranitrate and de-esterified metabolites, detec-... 

Chromatography (TLC) showed very small spots of hexanitrate of dipenta-ecyihiilol (DPEHN), and in some cases octonitrate of tripcntaerythritol (TPEON)and pentaerythritol trinitrate. 

The crude reaction mixtures were deprotected with aqueous ammonia and purified by preparative TLC and ion-exchange chromatography. So far, compounds of type 73 have been obtained as diastereomeric mixtures since the attempts at separation of diastereomers of 72 have failed. The ratio of substrates used in all condensation reactions depicted in Scheme 19 is important and determines the structure of final products, what can be well illustrated in the case of pentaerythritol (76).The reaction of 76 with less that four molar equivalents of 72 provided a mixture of mono-, di-, or tri- adenosine 5 -0-phosphorothioy-lated pentaerythritols, still containing free OH function(s) (77, Scheme 20). 

Yu, W.C. Goff, E.U. Determination of vasodilators and their metabolites in plasma by liquid chromatography with a nitrosyl-specific detector. Anal.Chem., 1983,55,29-32 [TEAdetection plasma SPE extracted isosorbide dinitrate, isosorbide mononitrate, pentaerythritol tetranitrate LOD 0.1 ng]... 

Carlson, M. Thompson, R.D. Determination of pentaerythritol tetremitrate in pharmaceuticals hy high performance liquid chromatography. J.Liq.Chromatogr., 1988, 11, 2603—2620 [simultaneous pen-taeiythritol tetranitrate tablets capsules nitroglycerin is IS]... 

Figure 3.9 Reaction of polyethers with p-toluene sulfonic acid - gas chromatography. Gas chromatogram of reaction products of polyurethane polyethers (1) propylene glycol diacetate (2) glycerol triacetate (3) trimethylpropane triacetate (4) triethylanolamine triacetate (5) pentaerythritol tetracetate. Gas chromatographic conditions column 1 m x 3 mm, coated with 15% FFAQ on Uniport B, oven 170 °C chart speed 1 cm/s. (b) Gas chromatogram of reaction products of polyurethane polyethers based on amines (1) pyropylene glycol diacetate (2) derivative from 1,2 diaminoethane (3) derivative from 2,2 -diaminodiethylamine. Gas chromatographic conditions Column 1 m x 3 mm packed with 15% SE-30 on Uniport B oven 230 "C chart speed, 1 cm/min.

Such a procedure yielded pentaerythritol-/ /M tetraester with an average MW of 4.5-4.9 kDa according to H-NMR and gel permeation chromatography (GPC) analyses (25). Matrix-assisted laser desorption ionization-time of flight-mass spectroscopy, or MALDI-TOF-MS, and C-NMR confirmed the NMR-and GPC-derived molecular structure and composition of the product (25). Esterification of the polyol acyl acceptor s hydroxyl groups occurred at 78%,... 

Taking advantage of the more traditional cyclic ester formation between boronic acids and 1,2- and 1,3-diols can also lead to macrocyclic structures. It has been shown by NMR, FTIR, and size exclusion chromatography (SEC) that reaction between phenylene-l,3-diboronic acid and pentaerythritol principally produces 6 6, hexameric cycles (Fig. 16a)." As before, the crude reaction mixture was a dynamic mixture of cyclic and oligomeric products, but the... 

---