Polystyrene calibration

Figure 2. Intrinsic viscosity-molecular weight data for polystyrene and polyvinyl chloride measured by osmometry and by SEC using broad MWD standard calibration (polystyrene (m) M = 7,06 X 10 in THF/1% PPG (O) [ ] =...

Conners Advantage (Frequency Precision). The dispersive instrument depends on calibration (polystyrene at 1601 cm 0, and the ability of gears and levers to move slits and gratings in a reproducable fashion. The FTIR carries its own internal frequency standard, usually a He-Ne gas laser, that serves as the master timing clock, tracking mirror movement and frequency calibration to a precision and accuracy of better than 0.01 wavenumbers (cm ). 

Adapter, T type, 24/40 Adapters, hose connection with stopcocks, 24/40 joints, one inner, one outer Beaker, 30 mL Beaker, plastic, 400 mL Bottles, wash, 250 mL Card, calibration, polystyrene Cell, NaCl, sandwich Cell, NaCl, wedge Clamps, buret... 

Characterization. The polymers were characterized with IR, NMR spectroscopy. Molecular weight and molecular weight distribution were measured with GPC using tetrahydrofuran/formacetoamide and phosphoric acid/lithium bromide as an eluant, calibrated polystyrene standard. 

Determined by gel permeation chromatography, relative to calibrated polystyrene standards. 

Fig. 3. Calibration curves for columns of PLgel for organic SEC at ambient temperature (a) a range of individual pore size columns designated 50 A to 10E6 A, (b) a range of mixed gel columns designated A to E. Eluent THF, flow rate 1 mL/min, calibrants polystyrene standards.

Figure 9.17 Plot of log [i ]M versus retention volume for various polymers, showing how different systems are represented by a single calibration curve when data are represented in this manner. The polymers used include linear and branched polystyrene, poly(methyl methacrylate), poly(vinyl chloride), poly(phenyl siloxane), polybutadiene, and branched, block, and graft copolymers of styrene and methyl methacrylate. [From Z. Grubisec, P. Rempp, and H. Benoit, Polym. Lett. 5 753 (1967), used with permission of Wiley.]...

Both preparative and analytical GPC were employed to analyze a standard (NBS 706) polystyrene sample. Fractions were collected from the preparative column, the solvent was evaporated away, and the weight of each polymer fraction was obtained. The molecular weights of each fraction were obtained usmg an analytical gel permeation chromatograph calibrated in terms of both and M. The following data were obtained ... 

Susceptibility to radiation damage must be considered seriously if reference samples are to be calibrated for use in place of absolute systems. For the measurement of absolute C He, H) cross sections, films of polystyrene (CH) (which is relatively radiation hard) have been used successfiiUy, the RBS determination of carbon providing implied quantitation for the hydrogen present in the film. For a durable laboratory reference sample, however, there is much to recommend a known ion-implanted dose of H deep within Si or SiC, where the loss of hydrogen under room temperature irradiation will be neghgible. 

H type resins are available in different pore sizes. Examples of calibration curves for polystyrene standards are shown in Figs. 4.38 and 4.39. Other series of H type columns have similar calibration curves. Exclusion limits are listed in Tables 4.12-4.16. 

FIGURE 4.38 Calibration curves for TSK-GEL Hxl columns with polyst/rene standards. Column TSK-GEL Hxl series, two 7.8 mm x 30 cm columns in series. Sample Polystyrene standards. Elution Tetrahydrofuran. Flow rate 1.0 ml/min. Detection Rl. 

Figure 6.3 shows a comparison of elution patterns of standard polystyrene between a linear-type column and a standard-type column. Because of the high linearity of its calibration curve, the linear series has improved the efficiency of oligomer domain separation. 

FIGURE 6.1 Calibration curves of Shodex GPC KF-BOO series. Column Shodex GPC KF-800 series 8 mm i.d. X 300 mm. Eluent THF. Sample Polystyrene standards. 

FIGURE 10.3 Calibration curves for sulfonated polystyrenes on SynChropak GPC columns. Mobile phase 0.1 A1 sodium sulfate. (From MICRA Scientific, Inc., with permission.)... 

A range of individual pore size PLgel packing materials is produced and their pore size distribution is conveniently represented by a SEC calibration curve as illustrated in Fig. 12.1. It should be pointed out that the descriptors used for the different pore sizes, 50 A, 100 A, and so on, are not the actual pore sizes of the beads but relate to the size of a polystyrene molecule just excluded from the packing material. This nomenclature comes from the original work carried out by Moore (3) and should only be viewed in the context of differentiating... 

FIGURE 12.1 SEC calibration curves for PLgel individual pore size columns (300 X 7.5 mm), eluent THE at 1.0 ml/min, polystyrene calibrants. 

Figures 13.8 and 13.9 show the separation of polystyrene standards using a typical mixed-bed column and its calibration plot, respectively. The major advantages of using a large i.d. 10-mm column are low hack pressure and relatively short run times. As seen in Fig. 13.8,10 standards from toluene thru 8.4 X 10 MW can be resolved in a mere 21 min. Because of the large 10-mm i.d. columns, 1.5-ml/min flow rates give a linear velocity equivalent to that of only 0.9 ml/min using a 7.6-mm i.d. column. Also, the gel volume contained in one 10 mm i.d. X 500 mm column is 39.3 ml, whereas a 7.6 mm i.d. X 300 mm column contains only 13.6 ml of gel volume. This bulk volume factor, combined with the large pore volumes of gels, obtains essentially the same resolution as that obtained on three standard 7.6 X 300-mm columns in series, but in about one-half the usual time required using the smaller columns.

The ISO method prescribes polystyrene standards with tetrahydrofuran as the eluent, but this equation can also be used with other narrow distribution standards, provided the same elution solvent and the same standards are used for a comparison. Further, the ISO method requires the result to be greater than 6 for one decade of the molar mass. Because calibration curves are usually not linear, this decade should lie nearly symmetrically around the peak maxima of the samples in question. The required value of 6 is easy to fulfill, as results of 10 or more are usual with modern columns. If so-named linear or mixed... 

PMMA, on the unmodified porous glass and silica gel, and the universal calibration curves for polystyrenes and poly(methyl methacrylates) did not coincide (10,12,19). 

FIGURE 15.3 Column No. 2. Calibration dependences for polystyrenes in THF ( ), chloroform (9), and toluene C ) eluents. Samples were dissolved in eluent. 

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). 

Commercial narrow standards [such as poly(ethylene glycol) (pEG), polystyrene sulfonate, pAA, poly w-vinyl pyrrolidinone, dextrans] are available from American Polymer Standards Corporation, Polymer Laboratories, Polymer Standards Service USA, Toyo Soda, and others. While these standards are often not as narrow as pSty or pMMA that has been anionically polymerized, they are acceptable for narrow standard calibrations. 

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