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Calibrated solvent test

We use the ENCAD macromolecular potential model with the F3C water model. The combined model explicitly represents all of the atoms with the protein, allowing for dynamic freedom of all the atoms. The balance in explicit description and flexibility between the solute and solvent avoids the inadvertent introduction of unexpected and undetected systematic error into the simulations. This is especially problematic in simulations of biological macromolecules for which there are relatively few experimental observations available for calibration and testing. [Pg.2212]

When the correct solvent for recrystallisation is not known a procedure similar to that given on pp. 15-16 should be followed, but on the semi-micro scale not more than 10 mg. of the solid should be placed in the tapered-end test-tube (Fig. 29(B)) and about o i ml. of the solvent should be added from the calibrated dropping-pipette (Fig. 30(B)). If the compound dissolves readily in the cold, the solvent is unsuitable, but the solution should not be discarded. [In this case recourse should be had to the use of mixed solvents (p. 18). For example if the substance is very soluble in ethanol, water should be added from a calibrated pipette with shaking to determine whether crystallisation will now take place, indicated by a cloudiness or by the separation of solid.]... [Pg.67]

The choice of solvent cannot usually be made on the basis of theoretical considerations alone (see below), but must be experimentally determined, if no information is already available. About 0 -1 g. of the powdered substance is placed in a small test-tube (75 X 11 or 110 X 12 mm.) and the solvent is added a drop at a time (best with a calibrated dropper. Fig. 11, 27, 1) with continuous shaking of the test-tube. After about 1 ml. of the solvent has been added, the mixture is heated to boiling, due precautions being taken if the solvent is inflammable. If the sample dissolves easily in 1 ml. of cold solvent or upon gentle warming, the solvent is unsuitable. If aU the solid does not dissolve, more 11,27,1. solvent is added in 0-5 ml. portions, and again heated to boiling after each addition. If 3 ml. of solvent is added and the substance... [Pg.124]

Amount of material required. It is convenient to employ an arbitrary ratio of 0 10 g. of solid or 0 20 ml. of liquid for 3 0 ml. of solvent. Weigh out 0 10 g. of the finely-powdered solid to the nearest 0 01 g. after some experience, subsequent tests with the same compound may be estimated by eye. Measure out 0-20 ml. of the liquid either with a calibrated dropper (Fig. 11,27, 1) or a small graduated pipette. Use either a calibrated dropper or a graduated pipette to deliver 3 0 ml. of solvent. Rinse the delivery pipette with alcohol, followed by ether each time that it is used. [Pg.1055]

A double-beam atomic absorption spectrophotometer should be used. Set up a vanadium hollow cathode lamp selecting the resonance line of wavelength 318.5 nm, and adjust the gas controls to give a fuel-rich acetylene-nitrous oxide flame in accordance with the instruction manual. Aspirate successively into the flame the solvent blank, the standard solutions, and finally the test solution, in each case recording the absorbance reading. Plot the calibration curve and ascertain the vanadium content of the oil. [Pg.808]

Calibration data (e.g., linearity or sensitivity) are not discussed in detail between laboratories, but a typical calibration starts with 50% of the lowest fortification level and requires at least three additional calibration levels. Another point of calibration is the use of appropriate standards. In 1999 a collaborative study tested the effect of matrix residues in final extracts on the GC response of several pesticides.Five sample extracts (prepared for all participants in one laboratory using the German multi-residue procedure) and pure ethyl acetate were fortified with several pesticides. The GC response of all pesticides in all extracts was determined and compared with the response in the pure solvent. In total, 20 laboratories using 47 GC instruments... [Pg.125]

The test procedure can be performed by pumping HPLC grade water at a specified flow rate under a controlled back-pressure, using a commercial back-pressure device connected in-line just after the pump. A f 000 psi back-pressure device is recommended. It is also advised that about f % MeOH be added to the water in order to minimize biological growth. While timing the process with a calibrated stop watch, the pump effluent should then be collected in a volumetric flask. From this, one can calculate the actual solvent flow at each flow rate. [Pg.315]

The selected factors are either mixture-related, quantitative (continuous), or qualitative (discrete).A mixture-related factor is, for instance, the fraction organic solvent in the buffer system. Examples of quantitative factors are the electrolyte concentration, the buffer pH, the capillary temperature, and the voltage, and of qualitative factors the manufacturer or the batch number of a reagent, solvent, or capillary. Sample concentration (see Table 1) is a factor sometimes included. However, the aim of the method tested is to determine this concentration through the measured signal, from a calibration procedure. Thus, one evaluates the influence of the sample concentration on the sample concentration, which we do not consider a good idea. [Pg.189]

Fig. 3.2 Sono-square-wave anodic stripping voltammetric traces for an insonated deposition of 60 s at —1.5 V. Traces show background corrected standard additions to sono-solvent extracted laked horse blood solution (test solution 0.05%, by volume-blood). Each 10 (tl addition corresponds to an increase in copper concentration of 0.22 pg/1. Calibration graph shown inset (R = 0.9972) gives concentration of 1.637 mg/1 (reprinted from [64] with permission)... Fig. 3.2 Sono-square-wave anodic stripping voltammetric traces for an insonated deposition of 60 s at —1.5 V. Traces show background corrected standard additions to sono-solvent extracted laked horse blood solution (test solution 0.05%, by volume-blood). Each 10 (tl addition corresponds to an increase in copper concentration of 0.22 pg/1. Calibration graph shown inset (R = 0.9972) gives concentration of 1.637 mg/1 (reprinted from [64] with permission)...
Based on the 96-well format, OCT-PAMPA was proposed and has proved its ability to determine (indirectly) log Poet [87]. PAM PA is a method, first developed for permeability measurements, where a filter supports an artificial membrane (an organic solvent or phospholipids) [88, 89]. With this method, the apparent permeability coefficient (log P ) of the neutral form of tested compounds is derived from the measurement of the diffusion between two aqueous phases separated by 1-octanol layer (immobilized on a filter). A bilinear correlation was found between log Pa and log Poct> therefore log Poet of unknown compounds can be determined from log Pa using a calibration curve. Depending on the detection method used a range oflog P within —2 to +5 (with UV detection) and within —2 to +8 (with LC-MS detection) was successfully explored. This method requires low compound amounts (300 pi of 0.04 mM test compound) and, as for the previous method, samples can be prepared in DM SO stock solutions. For these experiments, an incubation time of 4h was determined as the best compromise in term of discrimination. The limitation of the technique lies in the lower accuracy values... [Pg.99]

The most useful method of testing the efficiency of a test is by means of a conventional calibration in which the response of the instrument is plotted against the concentration of a compound selected as a suitable model for the suspected impurity (if the nature of this is not known), with the main compound being used as the solvent. The concentration range should be carried down as far as possible to ascertain the lowest detection limit for the impurity. [Pg.134]

The Karl Fischer titration requires 20 to 45 min (depending on sample being tested) to complete calibration, blank determination, sample equilibration (extraction in Karl Fischer solvent), and final testing. [Pg.16]

Fig. 11.1. Blind test for the COSMO-RS relative solubility prediction of commercial drugs from Merck Co., Inc. [119] All values are calibrated against the experimental solubility in ethanol. The 14 solvents are water, 1-propanol, 2-propanol, dimethylformamide, ethyl acetate, methanol, heptane, toluene, chlorobenzene, acetone, ethanol, acetonitrile, triethylamine, and 1-butanol. Fig. 11.1. Blind test for the COSMO-RS relative solubility prediction of commercial drugs from Merck Co., Inc. [119] All values are calibrated against the experimental solubility in ethanol. The 14 solvents are water, 1-propanol, 2-propanol, dimethylformamide, ethyl acetate, methanol, heptane, toluene, chlorobenzene, acetone, ethanol, acetonitrile, triethylamine, and 1-butanol.
Different references give variations to the values for the different bands. These vary depending on the calibration of the instrument used, the exact chemistry of the system, and the method of preparation and testing of the sample. Samples tested in a solvent may indicate the carbonyl band at a wave number of 1745 cm-1, whereas the solid material will be at approximately 1730 cm-1. [Pg.33]


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