Substances laboratory

For working with small amounts of substances, laboratory ware of a small size and capacity is used, for example, 2- and 10-ml flasks, 20-, 10-, and 5-ml beakers, etc. 

Ifa laboratory is properly designed and operated,withadequateventilationandefficientfume hoods or other types of safety cabinets, additional respiratory protection normally will not be needed formostprocedures. However, in theevent ofan accident oran unusual operation which cannot be performed in ahood,orwhenworkingwithhighly toxic substances, laboratory persons working with toxic materials should be included in a respiratory protection program, managed by the institution or corporation. There are a few situations which should require the availability of respiratory protection immediately at hand. 

Although benzenesulphonyl chloride has for simplicity been used in the above discussion, tolucne-/>- sulphonyl chloride, CHaCeH SO Cl, is more frequently used in the laboratory, owing to its much lower cost, the latter being due in turn to the fact that toluene-p-sulphonyl chloride is a by-product in the commercial preparation of saccharin. Toluene-p sulphonyl chloride is a crystalline substance, of m.p. 68° the finely powdered chloride will, however, usually react readily with amines in the Schotten-Baumann reaction it does not react so readily with alcohols, but the reaction may be promoted considerably by first dissolving the chloride in some inert water-soluble solvent such as acetone. 

The term distillation is applied to vaporisation and subsequent condensation according to (i) it should also be applied to (ii) since it is really the liquid which is converted into vapour and is first formed by condensation. Strictly speaking, the term sublimation should be applied to changes according to (iii). However, in practice, a substance when heated may first melt and then boil, but on cooling it may pass directly from the vapour to the solid the process is then also called sublimation. Indeed the mode of vaporisation, whether directly from solid to vapour or through the intermediate formation of a liquid, is of secondary importance it is the direct conversion of vapour to solid which is really the outstanding feature of sublimation in the laboratory. 

The theory of the process can best be illustrated by considering the operation, frequently carried out in the laboratory, of extracting an orgaiuc compound from its aqueous solution with an immiscible solvent. We are concerned here with the distribution law or partition law which, states that if to a system of two liquid layers, made up of two immiscible or slightly miscible components, is added a quantity of a third substance soluble in both layers, then the substance distributes itself between the two layers so that the ratio of the concentration in one solvent to the concentration in the second solvent remains constant at constant temperature. It is assumed that the molecular state of the substance is the same in both solvents. If and Cg are the concentrations in the layers A and B, then, at constant temperature ... 

The theory underlying the removal of impurities by crystaUisation may be understood from the following considerations. It is assumed that the impurities are present in comparatively small proportion—usually less than 5 per cent, of the whole. Let the pure substance be denoted by A and the impurities by B, and let the proportion of the latter be assumed to be 5 per cent. In most instances the solubilities of A (SJ and of B (/Sb) are different in a particular solvent the influence of each compound upon the solubility of the other will be neglected. Two cases will arise for an3 particular solvent (i) the impurity is more soluble than the compound which is being purified (/Sg > SA and (ii) the impurity is less soluble than the compound Sg < S ). It is evident that in case (i) several recrystallisations will give a pure sample of A, and B will remain in the mother liquors. Case (ii) can be more clearly illustrated by a specific example. Let us assume that the solubility of A and 5 in a given solvent at the temperature of the laboratory (15°) are 10 g. and 3 g. per 100 ml. of solvent respectively. If 50 g. of the crude material (containing 47 5 g. of A and 2-5 g. of B) are dissolved in 100 ml. of the hot solvent and the solution allowed to cool to 15°, the mother liquor will contain 10 g. of A and 2-5 g. (i.e., the whole) of B 37-5 g. of pure crystals of A will be obtained. 

The most desirable characteristics of a solvent for recrystalhsation are (a) a high solvent power for the substance to be purified at elevated temperatures and a comparatively low solvent power at the laboratory temperature or below (6) it should dissolve the impurities readily or to only a very small extent (c) it should yield well-formed crystals of the purified compound and (d) it must be capable of easy removal from the crystals of the purified compound, i.e., possess a relatively low boiling point. It is assumed, of course, that the solvent does not react chemically with the substance to be purified. If two or more solvents appear to be equally suitable for the recrystallisation, the final selection will depend upon such factors as ease of manipulation, inflammability and cost. 

Frequently the water or other solvent is so firmly held that it cannot be completely removed in a vacuum desiccator at the ordinary temperature. These substances are dried in a vacuum oven at a higher temperature. A convenient laboratory form of vacuum oven is the so-called... 

The preparation of these compounds in the laboratory is not recommended and is rarely worth while because of the cheapness of the commercial products. Dimethyl sulphate is a heavy liquid, boiling at 188-6°, and is practically without odour. The vapour is highly poisonous and the substance should only be used in a fume cupboard with a good draught. The liquid itself is readily absorbed through the skin, with toxic results. 

A large number of polycyclic aromatic hydrocarbons are known Many have been synthesized m the laboratory and several of the others are products of com bustion Benzo[a]pyrene for example is present m tobacco smoke contaminates food cooked on barbecue grills and collects m the soot of chimneys Benzo[a]pyrene is a carcinogen (a cancer causing substance) It is converted m the liver to an epoxy diol that can induce mutations leading to the uncontrolled growth of certain cells... 

The field of fullerene chemistry expanded in an unexpected direction in 1991 when Sumio lijima of the NEC Fundamental Research Laboratories in Japan discovered fibrous carbon clusters in one of his fullerene preparations This led within a short time to substances of the type portrayed in Figure 11 7 called single-walled nanotubes The best way to think about this material IS as a stretched fullerene Take a molecule of Ceo cut it in half and place a cylindrical tube of fused six membered carbon rings between the two halves... 

Classical methods for separation and purifica tion include fractional distillation of liquids and re crystallization of solids and these two methods are routinely included in the early portions of laboratory courses in organic chemistry Because they are capa ble of being adapted to work on a large scale frac tional distillation and recrystallization are the preferred methods for purifying organic substances in the pharmaceutical and chemical industries... 

In the area of municipal and iadustrial wastewater treatment, the principal environmental issue is the toxicity of residual flocculating agents ia the effluent. Laboratory studies have shown that cationic polymers are toxic to fish because of the iateraction of these polymers with giU. membranes. Nonionic and anionic polymers show no toxicity (82,83). Other studies have shown that ia natural systems the suspended inorganic matter and humic substances substantially reduce the toxicity of added cationic polymer, and the polymers have been used successfully ia fish hatcheries (84—86). Based on these results, the EPA has added a protocol for testing these polymers for toxicity toward fish ia the presence of humic acids (87). The addition of anionic polymers to effluent streams containing cationic polymers to reduce their toxicity has been mentioned ia the patent Hterature (83). 

Local and state forensic laboratories generally do not engage ia excipient testing. Most provide quaUtative and quantitative analysis of the evidence to determine if an Ulegal substance is present and if so, the amount of the dmg present. The quantity of dmg seized by the authorities may be important ia jurisdictions which give enhanced sentences for larger amounts of the pure dmg, or ia some cases the total weight on the dmg and diluent ia possession of the defendant. 

The posterior lobe of the pituitary, ie, the neurohypophysis, is under direct nervous control (1), unlike most other endocrine organs. The hormones stored in this gland are formed in hypothalamic nerve cells but pass through nerve stalks into the posterior pituitary. As early as 1895 it was found that pituitrin [50-57-7] an extract of the posterior lobe, raises blood pressure when injected (2), and that Pitocin [50-56-6] (Parke-Davis) causes contractions of smooth muscle, especially in the utems (3). Isolation of the active materials involved in these extracts is the result of work from several laboratories. Several highly active posterior pituitary extracts have been discovered (4), and it has been deterrnined that their biological activities result from peptide hormones, ie, low molecular weight substances not covalendy linked to proteins (qv) (5). 

Time to Result. The time required to submit samples to a laboratory, have the samples analy2ed, and receive the results is not usually a critical health issue, although promptness in reporting the results of an evaluation adds credibiUty and impact. On the other hand, some evaluations of acutely acting substance may require immediate results such as a direct on the spot reading. 

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