Eluents flow rate

Experimental part was provided by device Model Knauer-Compact with UV-detector (b=3 mm) at 250 nm and column Spherisorb-ODS-2 (250x4,6 mm). Sample volume was 1-2 p.1 injected by Reodyne 7725. Concentration range was 0.4-0.5 mg/ml for solutions of studied substances in DMSO. The organic modificator concentration range was 75-85 % w for methanol and 40-60 % w for acetonitrile in eluent (flow rate -1 ml/min). 

Solid flow rate Recycling flow rate Eluent flow rate Extract flow rate Eeed flow rate Raffinate flow rate ... 

The vertex of a separation region points out the better operating conditions, since it is the point where the purity criteria are fulfilled with a higher feed flow rate (and so lower eluent flow rate). Hence, in the operating conditions specified by the vertex point, both solvent consumption and adsorbent productivity are optimized. Comparing the vertex points obtained for the two values of mass transfer coefficient, we conclude that the mass transfer resistance influences the better SMB operating conditions. Moreover, this influence is emphasized when a higher purity requirement is desired [28]. 

Following the procedure presented earlier, the y values for sections I and IV were fixed, in such a way that constraints concerning these zones were fulfilled Yj = 3.8657 and 7 = 2.6901. Since the liquid flow rates in sections I and IV are constants in this study, the eluent flow rate is also constant and equal to Q) - Q y = 7.49 inL miirf... 

Figure 5.1 Pesticides included in the systematic investigations on APCI-MS signal response dependence on eluent flow rate the parameter IsTow represents the distribution coefficient of the pesticide between n-octanol and water. Reprinted from J. Chromatogr, A, 937, Asperger, A., Efer, 1., Koal, T. and Engewald, W., On the signal response of various pesticides in electrospray and atmospheric pressure chemical ionization depending on the flow rate of eluent applied in liquid chromatography-mass spectrometry , 65-72, Copyright (2001), with permission from Elsevier Science.

Analyses were performed by gel permeation chromatography (GPC) and by high performance liquid chromatography (HPLC). Gel filtration of oligosaccharides was effected in a thermostated (65 <>C) column (210 X 1.5 i.d.) filled with polycrylamide gel (Bio-gel P2, 200-400 mesh Bio Rad-USA), using stilled water as eluent (flow rate 30 ml.h-1). 

Vasanits, A. and Molnar-Perl, I., Temperature, eluent flow-rate and column effects on the retention and quantitation properties of phenylthiocarbamyl derivatives of amino acids in reversed-phase high-performance liquid chromatography, J. Chromatogr., A, 832,109, 1999. 

FIGURE 13.3 Comparison of relationship between column inlet pressure and eluent flow rate using 4.6 mm inner diameter x 25 cm columns packed with 1, 2, 3, and 5 pm particles. Solid lines = 100% water. Dashed lines = 50 50 acetonitrile water. Dotted lines = 60 40 methanobwater. In the case of 1 pm particles, only 100% water is shown. 

Chromatographic System. The isocratic liquid chromatograph used was a Waters Associates (Milford, MA) Model 24A alc which included a Model 6000A Solvent Delivery System, a Model 401 Differential Refractometer and a Model 440 Absorbance Detector operating at 254 nm and was fitted with a WISP automatic injector. The analog outputs of the UV absorbance detector or differential refractometer were recorded with a Model 730 Data Module (printer, plotter, integrator)(Waters). Eluent flow rate was 1.0 ml/min unless otherwise noted. 

Aqueous Size Exclusion Chromatography (ASEC) A Pharmacia system with superose TM12 gel as packing, TRIS-HC1 50 mM as eluent (flow rate 0.4 ml min-1), was used, detection being by UV at 280 nm. 

Surprisingly enongh, the above processes are very fast and separation of macromolecnles on this principle can be considered an equilibrium process. The precise measurements of retention volumes of polymers under conditions of their partial pore permeation in absence of enthalpic interaction did not reveal practically any effect of the eluent flow rate [55]. On the contrary, in a review, Aubert and Tirrell [66] have demonstrated that the SEC exclusion volumes can be flow rate dependent due to both anomalous and physical effects. The former are caused by... 

The instruments for polymer HPLC except for the columns (Section 16.8.1) and for some detectors are in principle the same as for the HPLC of small molecules. Due to sensitivity of particular detectors to the pressure variations (Section 16.9.1) the pumping systems should be equipped with the efficient dampeners to suppress the rest pulsation of pressure and flow rate of mobile phase. In most methods of polymer HPLC, and especially in SEC, the retention volume of sample (fraction) is the parameter of the same importance as the sample concentration. The conventional volumeters— siphons, drop counters, heat pulse counters—do not exhibit necessary robustness and precision [270]. Therefore the timescale is utilized and the eluent flow rate has to be very constant even when rather viscous samples are introduced into column. The problems with the constant eluent flow rate may be caused by the poor resettability of some pumping systems. Therefore, it is advisable to carefully check the actual flow rate after each restarting of instrument and in the course of the long-time experiments. A continuous operation— 24h a day and 7 days a week—is advisable for the high-precision SEC measurements. THE or other eluent is continuously distilled and recycled. 

System (8) has been described for quantitation of corticosteroids as common adulterants in local drugs [156]. The sample is extracted from its matrix by methanol, and the resulting supernatant layer subjected to the HPLC analysis. The column used was an ODS-Zorbax column (25 cm x 4.6 mm), and the mobile phase 7 2 11 acetonitrile-methanol-aqueous 1% phosphoric acid. An eluent flow rate of 0.8 mL/min was used, and the analyte detection was performed using the UV absorbance at 240 nm. The calibration graph was found to be linear in the ranges of 1-15 pg/mL for betamethasone, 0.5-20 pg/mL for prednisolone, and 1-30 pg/mL for cortisone acetate. 

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