Analysis of Resin

The most common methods for monitoring solid phase reactions utilized in normal research laboratories are Infrared analysis of resin 

This is a destructive method in which the resin is ground and pelleted as a KBr disc and analysed by FT-IR analysis. This method works best for systems where distinct functional group transformations (C=0, C-OH, C=C, etc) are expected. No special equipment is needed. 

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Characterization. In many cases, ftir is a timely and cost-effective method to identify and quantify certain functionaHties in a resin molecule. Based on developed correlations, ftir is routinely used as an efficient method for the analysis of resin aromaticity, olefinic content, and other key functional properties. Near infrared spectroscopy is also quickly becoming a useful tool for on-line process and property control. 

Feller, R. L., "Identification and Analysis of Resins and Spirit Varnishes", in "Application of Science in Examination of Works of Art", Museum of Fine Arts, Boston, 1959, pp. 51-76. 

Analysis of resins described by Poisson distributions shows the validity of this constraint for standards. A cumulative, molar distribution of macromolecules is determined from the normalized... 

Cure Rate of the Phenolated SEL Resins. 13C NMR spectra of the phenolated SEL formaldehyde-treated resins revealed the formation of methylol groups. A similar cure reaction to resole type phenolic resins is expected to occur with the phenolated lignin-based resins. Since cure rate normally determines production capacity of a board mill, it is important that new types of adhesives have at least the same cure rate as the conventional phenolic adhesives. Cure analysis of resins has usually been examined by... 

Figure 1. Capillary GC analysis of resin-cleaning Soxhlet extraction solvents 900 mL of solvent/700 mL of resin was successively extracted with methanol, acetonitrile, and ethyl ether for 24 h each. Direct injection of 1.5 xL was used. (See Table 11 for GC-MS...

The conclusion of this study is that semiquantitative (order of magnitude) analysis is possible for broad spectrum analysis of resin lots cleaned by a consistent method and blanked with Milli-Q water. The concentrations of the resin impurities will vary as a function of the following ... 

Broad Spectrum Analysis of Resin Extracts A Base Extraction Cleanup Procedure... 

Teas, J. P. 1968. Graphic analysis of resin solubilitieS aintTechnol40 19-25. 

Lauterbach, J., Snively, C. M. and Oskarsdottir, G. (2002) Chemically sensitive high-throughput parallel analysis of resin bead supported combinatorial libraries. In Combinatorial Materials Development (R. Malhotra, ed.), American Chemical Society, Washington, DC. 

While solid-phase chemistry is valuable, it is not without its problems such as difficulties in the analysis of resin-bound products, low loading capacities of many resins, and physical properties of resins which can severely affect reaction rates and site accessibility. 

Most of the mass spectrometry applications for combinatorial chemistry will be described in the following sections of this chapter. Here we will give a short overview of MS techniques utilized for the characterization of resin-bound molecules. The majority of publications in this field describe applications of matrix-assisted laser desorption ionization (MALDI), combined with time-of-flight (TOF) detection. The major difference of MS application for analysis of resin-bound molecules from the above-described NMR and IR applications is that analyte should not be covalently bound to solid support prior to mass measurement. Detachment of compound molecules from resin can be done chemically (for example, by bead exposure to TFA vapors) [30,31] or photochemically, such that cleavage, desorption, and ionization of molecules occur simultaneously upon stimulation by laser radiation [32], Since the... 

Wood et al. [174] analysed long-chain fatty hydroxy acids. After esterification with diazomethane, hydroxyl groups were silylated with HMDS. DEGS and Apiezon L were used as the stationary phases and even the partial resolution of some diastereoisomers was achieved. TMS esters have similarly been applied to the analysis of resin acids, and retention data have been reported for several of them on SE-30, Apiezon L, QF-1, etc. [175]. 

GC (with or without identification of constituents by MS) remains the most precise, quantitative method for the detailed analysis of resinous remains and the choice when a relatively small number of samples must be studied in depth. It provides information about the method of preparation, that is, about early resin and pitch technology. The analyses reported in this chapter and elsewhere (20) have been the impetus for current work in this laboratory on replication of ancient pitch manufacturing methods and identification of the types of pine resins that were used. 

DSA analysis of Resin 5208 exhibits two dispersion regions. The first is related to gelation and the second is related to vitrification. The first DSA peak occurs on the attainment of a value for the resin storage modulus slightly lower than that of the rubbery plateau. The first TBA peak occurs at the point where the composite (braid and resin) attains measurable rigidity. 

Although spectroscopic analysis of resins does not lead to a quantitative determination of the loading, spectroscopic techniques can be very useful for the characterization of resins, as well as for the identification of possible undesired functional groups arising from incomplete reactions. 

Amino Add Analysis of Resin-Bound Peptide Mixtures ... 

While IR transmission spectroscopy is a general analytical method for resin samples, internal reflection spectroscopy is especially suited for solid polymer substrates known as pins or crowns. Single-bead analysis is best done by IR microspectroscopy, whereas photoacoustic spectroscopy allows totally nondestructive analysis of resin samples. 

From a practical point of view, if running parallel reactions is quite straightforward in SPS, the analysis of resin-bound substrates and resin-bound products is not. For solution-phase synthesis the experimenter has at his disposal a wide panel of routine analytical techniques that give rapid and readable information. In contrast, for solid-phase reactions, analysis is not routine and chemists often do not have the know-how and the experimental background to analyse reactions in solid support. 

C. P. A. Kappelmeier Chemical Analysis of Resin-Based Coaling Materials, Interscience Publishers Inc., New York 1959. 

White, R., A review with illustrations of resin/oU varnish mixtures, methods applicable to the analysis of resin/oil varnish mixtures, report 2/16/81, in ICOM Committee for Conservation, 6th Triennial Meeting, Ottawa, 1981. 

After the sample was taken, the sample port cover was replaced on its bolts but not bolted down as the procedure specified. The agitator was started and almost simultaneously the contents of the reactor erupted, forcing off the 6.8 kg sampling port cover. The analysis of resin samples from the reactor, erupted resin on the equipment and a sample taken from the reactor 15 minutes prior to the accident indicated that, during the time the technician was taking the reactor sample, the vessel contents were still reacting and essentially at the boiling point of the mass. 

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