Experimental filtering

To simplify FECO evaluation, it is conmion practice to experimentally filter out one of the components by the use of a linear polarizer after the interferometer. Mica bireftingence can, however, be useftil to study thin films of birefringent molecules [49] between the surfaces. Rabinowitz [53] has presented an eigenvalue analysis of birefringence in the multiple beam interferometer. 

Measurements of filtration rates should be repeated at different pressures or different vacuum levels. This gives information on the influence of pressure on the specific cake resistance. The specific resistance of cakes that are difficult to filter is often pressure-dependent. Thus, use of excessive pressure can result in blocking of the cake, causing filtration to stop. In the case of compressible cakes, information is needed over the whole range of pressures being considered for industrial filters since extrapolation of compressibility beyond the experimentally covered region is always risky. The larger the scale of an experimental filter, the less risky predictions based on the experimental data. 

Fig. 11. Experimental filter pressure drop as a function of soot mass loading compared with the model taking into account the effect of gas compressibility (dashed line) and the effect of soot deposit compaction (continuous line). The indicative example is given for a soot aggregate size of 129 nm.

Equations (27) and (29) can be used to calculate the total PNS of replicated experimental filter challenges. For example, five filter membrane media are to be challenged at the following / . diminuta levels. 

Cori, C.B., S.P Battista, P.S. Thayer, M.R. Cuerin, and C.J. Lynch Chemistry and in vitro bioassay of smoke from experimental filter cigarettes DHEW Publ. No. (NIH) 76-1076 (1976). 

Weston, E.B. (1896). Report of the results obtained with experimental filters at the Pettaconset pumping station of the Providence water works. Freeman Providence RI. 

Constant-Pressure Filtration and fVashing in a Leaf Filter. An experimental filter press having an area of 0.0414 (Rl) is used to filter an aqueousBaC03 slurry at a constant pressure of 267 kPa. The filtration equation obtained was... 

The experimental conditions used to determine the CFPP do not exactly reflect those observed in vehicles the differences are due to the spaces in the filter mesh which are much larger in the laboratory filter, the back-pressure and the cooling rate. Also, research is continuing on procedures that are more representative of the actual behavior of diesel fuel in a vehicle and which correlate better with the temperature said to be operability , the threshold value for the Incident. In 1993, the CEN looked at two new methods, one called SFPP proposed by Exxon Chemicals (David et al., 1993), the other called AGELFI and recommended by Agip, Elf and Fina (Hamon et al., 1993). 

In fig. 2 an ideal profile across a pipe is simulated. The unsharpness of the exposure rounds the edges. To detect these edges normally a differentiation is used. Edges are extrema in the second derivative. But a twofold numerical differentiation reduces the signal to noise ratio (SNR) of experimental data considerably. To avoid this a special filter procedure is used as known from Computerised Tomography (CT) /4/. This filter based on Fast Fourier transforms (1 dimensional FFT s) calculates a function like a second derivative based on the first derivative of the profile P (r) ... 

The filter according equation (1) allows a practical application of a second derivative, because it has only the noise amplification like a first derivative. This is shown in fig. 3 on a experimental data set. The SNR of the true second derivative is too low for correct edge detection, whereas the CT filter gives reliable results. 

A number of experimental and physical realities cloud this rosy picture. Inevitably many emitted photons are lost due to the finite solid angle over which the fluorescence is collected, losses at the various filters, lenses, windows, and other... 

The ethereal extracts are then united, dried with a suitable drying agent and filtered. The filtrate is then cautiously distilled, the ether being first distilled and finally the organic compound if volatile if the compound is solid, the crude residue is purified by recrystallisation. Very great care must be taken on all occasions when ether is distilled because of the risk of fire or of an explosion full experimental details for this operation are given, both on p. 8o (Preparation of Ether) and on p. 164 (Pre-... 

Benzene. The analytical reagent grade benzene is satisfactory for most purposes if required dry, it is first treated with anhydrous calcium chloride, filtered, and then placed over sodium wire (for experimental details, see under Diethyl ether, 1). 

Drop 1 g. of sodium into 10 ml. of ethyl alcohol in a small flask provided with a small water condenser heat the mixture until all the sodium has dissolved. Cool, and add 1 g. of the ester and 0-5 ml. of water. Frequently the sodium salt of the acid will be deposited either at once or after boiling for a few minutes. If this occurs, filter oflF the solid at once, wash it with a little absolute ethyl alcohol (or absolute methylated spirit), and convert it into the p-bromophenacyl ester, p-nitro-benzyl ester or S-benzyl-tso-thiuronium salt (for experimental details, see Section 111,85). If no solid separates, continue the boiling for 30-60 minutes, boil oflF the alcohol, allow to cool, render the product just neutral to phenolphthalein with dilute sulphuric or hydrochloric acid, convert the sodium salt present in solution into a crystalline derivative (Section 111,85), and determine its melting point. 

Place 18 g. (12 ml.) of fuming nitric acid, sp. gr. 1 5, and 30 g. (16-5 ml.) of concentrated sulphuric acid and a few fragments of broken glass in a 250 or 500 ml. round-bottomed flask. Add gradually, in small portions, 14 g. of p-nitrotoluene do not allow the temperature to rise above 50 and cool the flask, if necessary, by immersion in cold water. Place a small funnel in the mouth of the flask and heat on a water bath at 90-95° for 30 minutes. Allow to cool almost to the laboratory temperature and pour the reaction mixture slowly into about 500 ml. of ice water containing a few small pieces of ice. Filter the crude dinitrotoluene through a Buchner funnel at the pump, wash it thoroughly with cold water, and drain as completely as possible. RecrystalUse from the minimum volume of hot methyl alcohol (flask, reflux condenser, and water bath experimental details as in Section IV,12). The yield of pure 2 4-dinitrotoluene, m.p. 71°, is 12 -5 g. 

The experimental conditions for conducting the above reaction in the presence of dimethylformamide as a solvent are as follows. In a 250 ml. three-necked flask, equipped with a reflux condenser and a tantalum wire Hershberg-type stirrer, place 20 g. of o-chloronitrobenzene and 100 ml. of diinethylform-amide (dried over anhydrous calcium sulphate). Heat the solution to reflux and add 20 g. of activated copper bronze in one portion. Heat under reflux for 4 hours, add another 20 g. portion of copper powder, and continue refluxing for a second 4-hour period. Allow to cool, pour the reaction mixture into 2 litres of water, and filter with suction. Extract the solids with three 200 ml. portions of boiling ethanol alternatively, use 300 ml. of ethanol in a Soxhlet apparatus. Isolate the 2 2- dinitrodiphenyl from the alcoholic extracts as described above the 3ueld of product, m.p. 124-125°, is 11 - 5 g. 

To isolate pure p-dibromobenzene, filter the second portion of the steam distillate through a small Buchner funnel with suction press the crystals as dry as possible. Combine these crystals with the residue (R) and recrystaliise from hot ethyl alcohol (for experimental details, see Section IV,12) with the addition of 1-2 g. of decolourising charcoal use about 4 ml. of alcohol (methylated spirit) for each gram of material. Filter the hot solution through a fluted filter paper, cool in ice, and filter the crystals at the pump. The yield of p-dibromobenzene, m.p. 89°, is about 12 g. 

The experimental details for mono-M-propylanillne are as follows. Reflux a mixture of 230 g. of aniline and 123 g. of n-propyl bromide for 8-10 hours. Allow to cool, render the mixture alkafine, and add a solution of 150 g. of zinc chloride in 150 g. of water. Cool the mixture and stir after 12 hours, filter at the pump and drain well. Extract the thick paste several times with boiling light petroleum, b.p. 60-80° (it is best to use a Soxhlet apparatus), wash the combined extracts successively with water and dilute ammonia solution, and then dry over anhydrous potassium carbonate or anhydrous magnesium sulphate. Remove the solvent on a water bath, and distil the residue from a Claisen flask with fractionating side arm (well lagged). Collect the n-propyl-aniline at 218-220° the yield is 80 g. Treat the pasty solid zincichloride with an excess of. sodium hydroxide solution and steam distil 130 g. of pure aniline are recovered. 

Add 25 g. of finely-powdered, dry acetanilide to 25 ml. of glacial acetic acid contained in a 500 ml. beaker introduce into the well-stirred mixture 92 g. (50 ml.) of concentrated sulphuric acid. The mixture becomes warm and a clear solution results. Surround the beaker with a freezing mixture of ice and salt, and stir the solution mechanically. Support a separatory funnel, containing a cold mixture of 15 -5 g. (11 ml.) of concentrated nitric acid and 12 -5 g. (7 ml.) of concentrated sulphuric acid, over the beaker. When the temperature of the solution falls to 0-2°, run in the acid mixture gradually while the temperature is maintained below 10°. After all the mixed acid has been added, remove the beaker from the freezing mixture, and allow it to stand at room temperature for 1 hour. Pour the reaction mixture on to 250 g. of crushed ice (or into 500 ml. of cold water), whereby the crude nitroacetanilide is at once precipitated. Allow to stand for 15 minutes, filter with suction on a Buchner funnel, wash it thoroughly with cold water until free from acids (test the wash water), and drain well. Recrystallise the pale yellow product from alcohol or methylated spirit (see Section IV,12 for experimental details), filter at the pump, wash with a httle cold alcohol, and dry in the air upon filter paper. [The yellow o-nitroacetanihde remains in the filtrate.] The yield of p-nitroacetanihde, a colourless crystalline sohd of m.p. 214°, is 20 g. 

Place a solution of 10 -4 g. of benzalacetophenone, m.p. 57° (Section IV,130) in 75 ml. of pure ethyl acetate (Section 11,47,15) in the reaction bottle of the catalytic hydrogenation apparatus and add 0 2 g. of Adams platinum oxide catalyst (for full experimental details, see Section 111,150). Displace the air with hydrogen, and shake the mixture with hydrogen until 0 05 mol is absorbed (10-25 minutes). Filter oflF the platinum, and remove the ethyl acetate by distillation. RecrystaUise the residual benzylacetophenone from about 12 ml. of alcohol. The yield of pure product, m.p. 73°, is 9 g. 

The hydrolysis by alkali is illustrated by the following experimental details for benzamido. Place 3 g. of benzamide and 50 ml. of 10 per cent, sodium hydroxide solution in a 150 ml. conical or round-bottomed flask equipped with a reflux condenser. Boil the mixture gently for 30 minutes ammonia is freely evolved. Detach the condenser and continue the boiling in the open flask for 3-4 minutes to expel the residual ammonia. Cool the solution in ice, and add concentrated hydrochloric acid until the mixture is strongly acidic benzoic acid separates immediately. Leave the mixture in ice until cold, filter at the pump, wash with a little cold water and drain well. RecrystaUise the benzoic acid from hot water. Determine the m.p., and confirm its identity by a mixed m.p. test. 

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