Poly HPLC analysis

Other hand, when an equimolar mixture of 2,5-DSP and l OEt is recrystallized from benzene, yellow crystals, comprising 2,5-DSP and l OEt in a molar ratio of 1 2, deposit. In the DSC curve of this crystal, a single endothermic peak is observed at 166°C, which is different from the melting point of either 2,5-DSP (223°C) or l OEt (156°C). Furthermore, the X-ray powder diffraction pattern of the crystal is quite different from those of the homocrystals 2,5-DSP and l OEt. Upon irradiation the cocrystal 2,5-DSP-l OEt affords a crystalline polymer (77i h = 1.0 dl g in trifluoroacetic acid). The nmr spectrum of the polymer coincides perfectly with that of a 1 2 mixture of poly-2,5-DSP and poly-1 OEt. In the dimer, only 2,5-DSP-dimer and l OEt-dimer are detected by hplc analysis, but the corresponding cross-dimer consisting of 2,5-DSP and l OEt is not detected at all (Hasegawa et al., 1993). These observations by nmr and hplc indicate that the photoproduct obtained from the cocrystal 2,5-DSP-l OEt is not a copolymer but a mixture of poly-2,5-DSP and poly-l OEt in the ratio 1 2. 

Polyethers Poly(propylene glycol) M = 2000-4000) HPLC Analysis Optical density Soi -Corynebacterium sp. Alcaligen denitrificans [103]... 

Fig. 1. (left) Effect of poly L-lysine, L-arginine or both on incoiporadon from [adenylate-32p] NAD into proteins of SR vesicles. The reaction mixture containing 0.88 mg/ml of SR and 0.5 mM labeled NAD (2 ci/mol) in the absence and presence of 50 mM L-arginine was incubated, with or without 100 [ig/ml of poly L-lysine, at 25 C for 30 min, and radioactivity of the acid-insoluble fraction was measured by filter assay (2). The minute amount of [32p]NAD which bound to poly L-lysine during the incubation was detected. Thus, this radioactivity was subtracted fiom the value obtained in the presence of SR plus poly L-lysine. The ADP-ribosylation of L-arginine was determined by HPLC analysis (6). 

Tables Deposition of collagen-glycosaminoglycan conjugates on poly(octadecen-a/f-maleic anhydride)-coated substrates. Fibrillogenesis and immobilization of fibrillar collagen (1.2 mg/ml) was performed for 2 h at 37 ° C in the presence of heparin and hyaluronic acid (0.4, 1.2 and 5.0 mg/ml, respectively). Thickness of the layers was determined ellip-sometrically using the refractive index of 1.6035 for the dried collagen layer. The collagen amount was determined by amino acid-based HPLC analysis after acidic hydrolysis of surface-bound collagen...

An application of an LC-SFC system has been demonstrated by the separation of non-ionic surfactants consisting of mono- and di-laurates of poly (ethyleneglycol) (23). Without fractionation in the precolumn by normal phase HPLC (Figure 12.18 (a)) and transfer of the whole sample into the SFC system, the different homologues coeluted with each other. (Figure 12.18(b)). In contrast with prior fractionation by HPLC into two fractions and consequent analysis by SFC, the homologues in the two fractions were well resolved (Figures 12.18(c) and 12.18(d)). 

Figure 12.18 LC-SFC analysis of mono- and di-laurates of poly (ethylene glycol) ( = 10) in a surfactant sample (a) normal phase HPLC trace (b) chromatogram obtained without prior fractionation (c) chromatogram of fraction 1 (FI) (d) chromatogram of fraction 2 (F2). LC conditions column (20 cm X 0.25 cm i.d.) packed with Shimpak diol mobile phase, w-hexane/methylene chloride/ethanol (75/25/1) flow rate, 4 p.L/min UV detection at 220 nm. SFC conditions fused-silica capillary column (15 m X 0.1 mm i.d.) with OV-17 (0.25 p.m film thickness) Pressure-programmed at a rate of 10 atm/min from 80 atm to 150 atm, and then at arate of 5 atm/min FID detection. Reprinted with permission from Ref. (23).

The identification and quantification of potentially cytotoxic carbonyl compounds (e.g. aldehydes such as pentanal, hexanal, traw-2-octenal and 4-hydroxy-/mAW-2-nonenal, and ketones such as propan- and hexan-2-ones) also serves as a useful marker of the oxidative deterioration of PUFAs in isolated biological samples and chemical model systems. One method developed utilizes HPLC coupled with spectrophotometric detection and involves precolumn derivatization of peroxidized PUFA-derived aldehydes and alternative carbonyl compounds with 2,4-DNPH followed by separation of the resulting chromophoric 2,4-dinitrophenylhydrazones on a reversed-phase column and spectrophotometric detection at a wavelength of378 nm. This method has a relatively high level of sensitivity, and has been successfully applied to the analysis of such products in rat hepatocytes and rat liver microsomal suspensions stimulated with carbon tetrachloride or ADP-iron complexes (Poli etui., 1985). 

Plasticiser/oil in rubber is usually determined by solvent extraction (ISO 1407) and FTIR identification [57] TGA can usually provide good quantifications of plasticiser contents. Antidegradants in rubber compounds may be determined by HS-GC-MS for volatile species (e.g. BHT, IPPD), but usually solvent extraction is required, followed by GC-MS, HPLC, UV or DP-MS analysis. Since cross-linked rubbers are insoluble, more complex extraction procedures must be carried out. The determination of antioxidants in rubbers by means of HPLC and TLC has been reviewed [58], The TLC technique for antidegradants in rubbers is described in ASTM D 3156 and ISO 4645.2 (1984). Direct probe EIMS was also used to analyse antioxidants (hindered phenols and aromatic amines) in rubber extracts [59]. ISO 11089 (1997) deals with the determination of /V-phenyl-/9-naphthylamine and poly-2,2,4-trimethyl-1,2-dihydroquinoline (TMDQ) as well as other generic types of antiozonants such as IV-alkyl-AL-phenyl-p-phenylenediamines (e.g. IPPD and 6PPD) and A-aryl-AL-aryl-p-phenylenediamines (e.g. DPPD), by means of HPLC. 

Various techniques have been used for the determination of oligomers, including GC [135], HPLC [136-138], TLC for polystyrene and poly a-methyl-styrene [139] and SEC for polyesters [140,141]. GC and PyGC-MS can also profitably be used for the analysis of the compositions of volatile products formed using different flame retardants (FRs). Takeda [142] reported that volumes and compositions of the volatile products and morphology of the char were affected by FRs, polymers (PC, PPE, PBT) and their reactions from 300... 

Applications Van der Maeden et al. [646] first used GE-HPLC for the qualitative and quantitative analysis of oligomeric mixtures, such as low-MW resins (epoxy up to 16-mer, o-cresol novolak up to 16-mer, p-cresol novolak up to 13-mer), prepolymers (poly-(2,6-diphenyl-p-phenylene oxide) up to 20-mer), PET (up to 14-mer) and ethoxylated octaphenol surfactants (up to 19-mer). In many GE-HPLC separations of oligomeric mixtures, a compromise has to be found between sample loading, injection volume and compatibility of the sample solvent and the initial phase system. Therefore,... 

Off-line coupling of HPLC with FD-MS has been used by several authors [118-121] for the determination of oligomers, oligomeric antioxidants (such as poly-TMDQ), ozonation and vulcanisation products. Pausch [122] reported on rubbers, cyclic polyurethane oligomers, as well as on the determination of the molecular weight distribution (up to 5300 Da) and oligomer analysis of polystyrene. Also the components of an aniline-acetone resin were deduced from FD-MS molecular weights [122]. 

Trathnigg, B., Kollroser, M.J. (1997). Liquid chromatography of polyethers using universal detectors V. Quantitative aspects in the analysis of low-molecular mass poly(ethylene glycols) and their derivatives by reversed-phase HPLC with an evaporative light scattering detector. J. Chromatogr. A 768, 223-238. 

Beginning in the late forties, copolymers were fractionated by adsorption chromatography poly (butadiene-co-styrene)32 34), poly(butadiene-co-acrylonitrile)32), polystyrene- -vinyl acetate)35), poly(styrene-h-ethylene oxide)36) and poly(styrene-co-acrylonitrile) 37). HPLC adsorption chromatography was first applied to copolymer analysis by Teramachi et al. in 1979 38>. 

The analysis of TNT in wastewaters is made simple and direct by LC using a UV detector at 220nm (Refs 81 158). An LC method suitable for the low level determination of Tetrvl in the presence of TNT, RDX and HMX is described (Ref 91). The adsorptive LC of TNT was demonstrated using poly(styrene-divinyl benzene) adsorbent and ethanol as the moving phase (Ref 112). HPLC was used for the separation of TNT from purification by-products of hexanitro-bibenzyl (Ref 69). Enzymatic action on TNT was supported by HPLC (Ref 155). HPLC chromatograms of TNT are included, together with data on TLC and color reactions of TNT in mixts (Ref 153). Pollutants in wastewater... 

Method for diamines and poly amines by HPLC. To a mixture of one volume of amine solution (less than 1 nmole/pl) is added an equal volume of 0.1 M borate buffer (pH 8.0) [101]. The solutions are mixed and one volume of fluorescamine solution (20 mg/10 ml in acetone) is added with rapid shaking using a vortex mixer or the equivalent. An aliquot portion of this mixture is then subjected to chromatography for separation and analysis. 

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