Polystyrene calibration standard

Most frequently, SEC with dextran-, pullulan-, or polystyrene calibration standards has been used to characterize the molecular properties of xylans. However, as for viscometric studies [108], a sufficient solvent ionic strength is a prerequisite for useful SEC measurements of charged polysaccharides, including glucuronoxylans [111-113]. An advantage of the SEC technique is that the presence of protein and phenolic components or oxidative changes can be detected by simultaneous ultraviolet (UV) detection. 

Table 2. Quantum yields for oolymer scission and crosslinking for some representative polysilanes (SiR R )n (a) Molecular weights were measured by GPC using polystyrene calibration standards (b) Ban, H Sukegawa, K. J. Polym. Sci., Polym. Chem. Ed., 1988, 26, 521...

Polystyrene calibration standards we from Pressure Chemical Co. and all had polydispersities (Mw/Mn) less than 1.1. 

Figure 26-15 Larger CdSe quantum dots are eluted before smaller quantum dots by 0.1 M trioctylphosphine in toluene at 1.0 mL/min in size exclusion chromatography on a 7.5 x 300 mm cross-linked polystyrene column of 100-nm pore size Polymer Labs PLgel 5 (im. Triangles are CdSe and squares are polystyrene calibration standards. The size of the CdSe core was measured with a transmission electron microscope and the length of 1-dodecanethiol endcaps (0.123 nm) was added to the radius. [Data from K. M. Krueger. A. M. Al-Somall, J. C. Falkner, and V. L. Colvin, "Characterization of Nanocrystalline CdSe by Size Exclusion Chromatography," Anal. Chem. 2005, 77,3511.]...

If the Mark-Houwink coefficients are not available, a universal calibration curve is established using polystyrene calibration standards and the SEC-vis-cometer combination. The basic steps involved in the MMD analysis are summarized in Fig. 11. First, the universal calibration curve of the SEC separation system has to be established by using narrow molar mass standards as indicated by the top arrow pointing to the right. Once the universal calibration curve is established, the procedure can then be reversed, by going from right to left following the bottom arrow, to obtain the molar mass calibration curve of any unknown... 

Molecular weights he samples were The samples were were determined by GPC and are relative to polystyrene calibration standards, studied only in solutions, studied only as solid films. ... 

Figure 6. Calibration curves for SEC columns packed with CPG (D = 31.0nm Vp= 1.12cm /g dp = 12/rm) (solid line) and silica gel (D = 29.1 nm Vp = 1.09cm /g dp = 10/rm) (dashed line). Column 300 x 6 mm. Polystyrene calibration standards. Mobile phase-tetrahydrofuran.

IR spectrometers must be calibrated for wavelength accuracy. FTIRs are usually calibrated by the manufacturer and checked on installation. Wavelength calibration can be checked by the analyst by taking a spectrum of a thin film of polystyrene, which has well-defined absorption bands across the entire mid-IR region, as seen in Fig. 4.1. Polystyrene calibration standard films are generally supplied with an IR instrument or can be purchased from any instmment manufacturer. Recalibration of the spectrometer should be left to the instmment service engineer if required. 

It can be stated that the situation with SEC separation of polar polymers employing PS/DVB column is ambiguous. Polystyrene calibration standards are... 

Polystyrene calibration standards are most frequently used, and with polymers of different chemical structure, molecular masses are reported relative to polystyrene. 

Determinarion of MW and MWD by SEC using commercial narrow molecular weight distribution polystyrene as calibration standards is an ASTM-D5296 standard method for polystyrene (11). However, no data on precision are included in the 1997 edition of the ASTM method. In the ASTM-D3536 method for gel-permeation chromatography from seven replicates, the M of a polystyrene is 263,000 30,000 (11.4%) for a single determination within the 95% confidence level (12). A relative standard deviation of 3.9% was reported for a cooperative determination of of polystyrene by SEC (7). In another cooperative study, a 11.3% relative standard deviation in M, of polystyrene by GPC was reported (13). 

An alternative method of calibration involves the dispersion of monodisperse polystyrene microparticles. This has recently been made an efficient process by the incorporation of these particles in pMDI suspension to allow for metering of small well-dispersed boluses sufficient for use as aerosol calibration standards [43]. 

The Q-factor approach is based upon the weight-to-size ratios (Q-factors) of the calibration standard and the polymer to be analyzed. The Q-factors are employed to transform the calibration curve for the chemical type of the standards (e.g. polystyrene) into a calibration curve for the chemical type of polymer under study. The inherent assumption In such a calibration approach is that the weight-to-size ratio is not a function of molecular weight but a constant. The assumption is valid for some polymer types (e.g. polyvinylchloride) but not for many polymer types. Hence the Q-factor method is generally referred to as an approximation technique. 

Sample Preparation. Calibration standards and test solutes were injected ai dilute solutions in the eluent. Polystyrene standards were 0.03 (w/v). Styrene, ODCB and normal hydrocarbons were 0.15 (w/v), except for dodecane and tridecane (0.65 ). Samples involving more complex matrices were prepared by crushing (if necessary), dissolving a weighed amount in the eluent, and filtering through a 0.45 Millex-SR filter cartridge (Millipore, Bedford, ma). 

The calibration standards included sodium form polystyrene sulfonates obtained from Pressure Chemical Co., Pittsburgh, Pa., and sodium toluene sulfonate. Measurements were taken at 0.5 to I.Oml/mln flow rates. The logarithm of the molecular weight of the standards was linear it suggests a framework for approaching an interpretion of the structure of the scission products. This application of size exclusion chromatography measurements must be viewed as a first approximation because of the unmeasured differences between the chromatographic behavior of the linear standards and the expected branched structure of the scission products. 

Calibration of Gel Permeation Chromatograph Polystyrene Calibration. A plot of molecular size in (S) versus elution volume for polysty-rene standards in dichloromethane showed deviation from linearity at about 2,200 which may be attributed to Imperfect column resolution, peak broadening, axial dispersion and skewing. The extensive tailing of the chromatograms of high molecular weight polystyrene standards observed in dichloromethane has also been reported in the literature (23-26). 

As explained in Sections 16.3.4, 6.4.1, and 16.4.2, SEC is a nonabsolute method, which needs calibration. The most popular calibration materials are narrow molar mass distribution polystyrenes (PS). Their molar mass averages are determined by the classical absolute methods—or by SEC applying either the absolute detection or the previously calibrated equipment. The latter approach may bring about the transfer and even the augmentation of errors. Therefore, it is recommended to apply exclusively the certified well-characterized materials for calibrations. These are often called PS calibration standards and are readily available from numerous companies in the molar mass range from about 600 to over 30,000,000g moL. Their prices are reasonable and on average (much) lower than the cost of other narrow MMD polymers. Other available homopolymer calibration materials include various poly(acrylate)s and poly(methacrylate)s. They are, similar to PS, synthesized by anionic polymerization. Some calibration materials are prepared by the methods of preparative fractionation, for example, poly(isobutylene)s and poly(vinylchloride)s. 

FIG. 1.8 Electron micrograph of cross-linked monodisperse polystyrene latex particles. The latex is a commercial product (d = 0.500 jun) sold as a calibration standard. (Photograph courtesy of R. S. Daniel and L. X. Oakford, California State Polytechnic University, Pomona, CA.)... 

Figure 3. Typical calibration curve using a polystyrene (PS) standard.

Monodispersed polystyrene sols are used as calibration standards for electron microscopes, light scattering photometers, Coulter counters, particle sieves, etc. Monodispersed silica is used for antireflection lens coatings. Monodispersity (even at a modest level) can usefully be exploited in photographic film, magnetic devices, pharmaceutical preparations and catalysis. 

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