Fining procedures

Incipient hazes may not be removed at all by simple filtration. An array of fining procedures have been developed to achieve stable clarity in such cases. Fining agents ate substances that ate or become insoluble in wines, and, as they precipitate, adsorb or coptecipitation incipient sources of cloudiness. Ptopedy used, the fining agents themselves ate not retained in the wines and thein effect is subtractive rather than additive. 

Another major fining procedure in Interior Valley table wine production is use of the compound PVPP (polyvinylpolypyrrolidone) (12). This reacts principally with tannins and is used to reduce browning in white wines. This results from its affinity for catechin, the main substrate for browning reactions. This compound also is used widely in the brewing industry. 

Fig. 5.1 Effect of different fining procedures on the turbidity of a Chardonnay wine. Measurements were made 28 h after treatments...

None of the bottled pear juices or reconstituted pear juice samples showed particular problems of haze or sediment formation (Table IV). SO2 addition, which protected phenolics from oxidation, had no influence on the clarity of these samples. Juice from ripened d Anjou and Cornice fruit had slightly higher % haze readings than juice from unripe fruit. All of these samples were subjected to standard fining procedures which may account for their stability and clarity (6). 

Let us consider the calculation of sensitivity threshold in the case when the cracks are revealing by PT method. Constant distance H between crack s walls along the whole defect s depth is assumed for the simplicity. The calculation procedure depends on the dispersity of dry developer s powder [1]. Simple formula has to be used in the case when developer s effective radius of pores IC, which depends mainly on average particle s size, is smaller than crack s width H. One can use formula (1) when Re is small enough being less than the value corresponding maximum sensitivity (0,25 - 1 pm). For example. Re = 0,25 pm in the case when fine-dispersed magnesia oxide powder is used as the developer. In this case minimum crack s width H that can be detected at prescribed depth lo is calculated as... 

It is instructive for the student to construct a rough melting point diagram (compare Section 1,13 and Fig. 1,12, 1) for mixtures of cinnamic acid and urea. Weigh out 1 00 g. each of the two finely powdered components, and divide each into ten approximately equal portions on a sheet of clean, smooth paper. Mix 4 portions of cinnamic acid (A) with 1 portion of urea B) intimately with the aid of a spatula on a glass slide, and determine the melting point (the temperature at which the mixture just becomes completely fluid is noted). Repeat the procedure for 3 parts of A and 2 parts oiB 2 parts of A and 3 parts of B and 1 part of A and 4 parts of B. Tabulate your results as follows —... 

Place 125 ml. of glacial acetic acid, 7 -5 g. of purifled red phosphorus (Section II,50,d) and 2 5 g. of iodine in a 500 ml, round-bottomed flask fitted with a reflux condenser. Allow the mixture to stand for 15-20 minutes with occasional shaking until aU the iodine has reacted, then add 2 5 ml. of water and 50 g, of benzilic acid (Section IV,127). Boil the mixture under reflux for 3 hours, and filter the hot mixture at the pump through a sintered glass funnel to remove the excess of red phosphorus. Pour the hot filtrate into a cold, weU-stirred solution of 12 g. of sodium bisulphite in 500 ml, of water the latter should be acid to litmus, pro duced, if necessary, by passing sulphur dioxide through the solution. This procedure removes the excess of iodine and precipitates the diphenyl-acetic acid as a fine white or pale yellow powder. Filter the solid with suction and dry in the air upon filter paper. The yield is 45 g., m.p. 

This procedure may be used for the preparation of finely-divided sodamide If the sodamide is to be used in any other solvent than liquid ammonia, the ammonia is allowed to evaporate whilst the new solvent is slowly added from a dropping funnel alternatively, the new solvent may be added before the ammonia evaporates. If dry sodamide is required, the product may be freed from the last traces of ammonia by evacuation at 100°. The sodamide prepared by this method must be used immediately if allowed to stand, it rapidly changes into explosive substances. 

A more active product is obtained by the following slight modification of the above procedure. Dissolve the succinimide in a slight molar excess of sodium hydroxide solution and add the bromine dissolved in an equal volume of carbon tetrachloride rapidly and with vigorous stirring. A finely crystalline white product is obtained. Filter with suction and dry thoroughly the crude product can be used directly. It may be recrystallised from acetic acid. 

If filtration is slow, the following procedure may be used. Place the fine suspension in a large evaporating dish and evaporate to dryness on a water bath. Dissolve the resulting sticky mass in the minimum volume of dilute alcohol (1 volume of water 3 volumes of methylated spirit about 200-260 ml.) and allow... 

Gee, that all sounds fine and dandy. But Strike saved the best for last. Without a doubt, the cleanest, fastest and easiest method for isomerizing safrole and other allylbenzenes is to use CaOH. Someone who is Not Tim (Strike s name for her) emailed Strike the Chemical Abstracts entry for the procedure ... 

But that is not the case. What the Korean lab found out was that when this procedure is performed, the OH stabilizes on the alpha carbon. That is the carbon right next to the phenyl ring. If one has any use for it as is then that is fine. But what is most preferable is to reduce the OH to get the propenylbenzene (say isoelemicin for our example). Using the simple potassium bisulfate reduction recipe, one can get rid of the OH with no problems at all. 

Ether - Starting fluid (works great - Quaaaaack ) 2. Home made mercuric acetate (Now this stuff can be special ordered from ones chem supplier but there s a delay, may look funny - Quaaaaack , and is more expensive. So what is the solution to this Make it yourself Its easy, quantitative, and cheaper. Strike mentions this in the book and points ducks to a reference. Follow the EXACT same procedure for Mercuric Propionate except use glacial acetic acid...quack ). You ll need to use 20 to 25% more of the home brew mercuric acetate since it is a little contaminated with acetic (ducks can t get it totally dry without a vacuum oven). 3. NaOH washed Brazillian is fine Quack No need to purify further for starting material ... 

Hove 1. The procedure described in Ref. 1 was modified. To a solution of 2.0 mol of lithium acetylide in 1.2 1 of liquid ammonia in a 4-1 round-bottomed, three-necked flask (see Fig. 2) was added 1.5 mol of freshly distilled benzaldehyde with cooling at about -45°C. After an additional 30 min finely powdered ammonium chloride (2 mol) was introduced in 15 min. The ammonia was allowed to evaporate, then water (1.1 1) was added and the product was extracted with diethyl ether. After drying over magnesium sulfate the extract was concentrated in a water-pump vacuum. High-vacuum distillation,... 

An interesting example of a large specific surface which is wholly external in nature is provided by a dispersed aerosol composed of fine particles free of cracks and fissures. As soon as the aerosol settles out, of course, its particles come into contact with one another and form aggregates but if the particles are spherical, more particularly if the material is hard, the particle-to-particle contacts will be very small in area the interparticulate junctions will then be so weak that many of them will become broken apart during mechanical handling, or be prized open by the film of adsorbate during an adsorption experiment. In favourable cases the flocculated specimen may have so open a structure that it behaves, as far as its adsorptive properties are concerned, as a completely non-porous material. Solids of this kind are of importance because of their relevance to standard adsorption isotherms (cf. Section 2.12) which play a fundamental role in procedures for the evaluation of specific surface area and pore size distribution by adsorption methods. 

A Type II isotherm indicates that the solid is non-porous, whilst the Type IV isotherm is characteristic of a mesoporous solid. From both types of isotherm it is possible, provided certain complications are absent, to calculate the specific surface of the solid, as is explained in Chapter 2. Indeed, the method most widely used at the present time for the determination of the surface area of finely divided solids is based on the adsorption of nitrogen at its boiling point. From the Type IV isotherm the pore size distribution may also be evaluated, using procedures outlined in Chapter 3. 

It would be difficult to over-estimate the extent to which the BET method has contributed to the development of those branches of physical chemistry such as heterogeneous catalysis, adsorption or particle size estimation, which involve finely divided or porous solids in all of these fields the BET surface area is a household phrase. But it is perhaps the very breadth of its scope which has led to a somewhat uncritical application of the method as a kind of infallible yardstick, and to a lack of appreciation of the nature of its basic assumptions or of the circumstances under which it may, or may not, be expected to yield a reliable result. This is particularly true of those solids which contain very fine pores and give rise to Langmuir-type isotherms, for the BET procedure may then give quite erroneous values for the surface area. If the pores are rather larger—tens to hundreds of Angstroms in width—the pore size distribution may be calculated from the adsorption isotherm of a vapour with the aid of the Kelvin equation, and within recent years a number of detailed procedures for carrying out the calculation have been put forward but all too often the limitations on the validity of the results, and the difficulty of interpretation in terms of the actual solid, tend to be insufficiently stressed or even entirely overlooked. And in the time-honoured method for the estimation of surface area from measurements of adsorption from solution, the complications introduced by... 

In the laboratory or process research section a laboratory procedure for a fine chemical is worked out. The resulting process description provides the necessary data for the determination of preliminary product specifications, the manufacture of semicommercial quantities in the pilot plant, the assessment of the ecological impact, an estimation of the manufacturing cost in an industrial-scale plant, and the vaHdation of the process and determination of raw material specifications. 

---