Cooling molecular weight

Separation of low-molecular-weight materials. Low-molecular-weight materials are distilled at high pressure to increase their condensing temperature and to allow, if possible, the use of cooling water or air cooling in the column condenser. Very low... 

This method of Molecular Weight determination should be used only with solvents in which the particular substance is freely soluble, since it is essential that, on cooling, the solvent, and hot the solute, should crystallise out. 

Benzene. Pure benzene (free in particular from toluene) must be used, otherwise the freezing-point is too low, and crystallisation may not occur with ice-water cooling alone. On the other hand, this benzene should not be specially dried immediately before use, as it then becomes slightly hygroscopic and does not give a steady freezing-point until it has been exposed to the air for 2-3 hours. Many compounds (particularly the carboxylic acids) associate in benzene, and molecular weights determined in this solvent should therefore be otherwise confirmed. 

Place a mixture of 0-5 g. of finely powdered thiourea, 0-5 g. of the alkyl halide and 5 ml. of alcohol in a test-tube or small flask equipped with a reflux condenser. Reflux the mixture for a j)eriod depending upon the nature of the halide primary alkyl bromides and iodides, 10-20 minutes (according to the molecular weight) secondary alkyl bromides or iodides, 2-3 hours alkyl chlorides, 3-5 hours polymethy lene dibromides or di-iodides, 20-50 minutes. Then add 0 5 g. of picric acid, boil until a clear solution is obtained, and cool. If no precipitate is obtained, add a few drops of water. RecrystaUise the resulting S-alkyl-iso-thiuronium picrate from alcohol. 

To a solution of 0-5 g. of the salt in 5 ml. of water and 2-3 drops of O li hydrochloric acid (or to a solution of the acid treated as above), add a shght excess of a cold, 15 per cent, aqueous solution of benzyl-wo-thiourea hydrochloride (if the molecular weight of the compound is not known, use a solution of 1 g. of the reagent in 5 ml. of water), and cool in ice. Filter off the crystaUine derivative and recrystaUise it from 50 per cent, alcohol. 

Reflux gently in a test-tube under a short air condenser 1 g. of the base with 2 5 mols or 3 0 g. (3 0 ml.) if the molecular weight is unknown of redistilled acetic anhydride for 10-15 minutes. Cool the reaction mixture and pour it into 20 ml. of cold water (CAUl ION). Boil to decompose the excess of acetic anhydride. When cold, filter the residual insoluble acetyl derivative and wash it with a little cold water. Recrystal-/ise from water or from dilute alcohol. 

The following alternative procedure is sometimes useful. Heat the amine with the theoretical quantity of benzoyl chloride (if the molecular weight is unknown, use an equal weight of benzoyl chloride in the preliminary experiment) to 100° for 20-30 minutes. Allow to cool, add excess of 5 per cent, sodium hydroxide solution and shake, if necessary,... 

Chains of polybutadiene were trapped in the network formed by cooling a butadiene-styrene copolymer until phase separation occurred for the styrene, effectively crosslinking the copolymer. At 25°C the loss modulus shows a maximum which is associated with the free chains. This maximum occurst at the following frequencies for the indicated molecular weights of polybutadiene ... 

In a typical adiabatic polymerization, approximately 20 wt % aqueous acrylamide is charged into a stainless steel reactor equipped with agitation, condenser, and cooling jacket or coils. To initiate the polymerization, an aqueous solution of sodium bisulfite [7631-90-5] is added, followed by the addition of a solution of ammonium persulfate [7727-54-0] N2HgS20g. As the polymerization proceeds, the temperature rises to about 90°C, and then begins to fall at the end of the polymerization. The molecular weight obtained depends primarily on the initiator concentration employed. 

Melting and recrystallization behavior of virgin PTEE has been studied by dsc (64). A quantitative relationship was found between and the heat of crystallization (A/T) in the molecular weight range of 5.2 x 10 to 4.5 X 1 0, where is heat of crystallization in J/g, which is independent of cooling... 

The preparation of high molecular weight PPT in HMPA/NMP shows a strong dependence of inherent viscosity on reactant concentrations. In 2 1 (by volume) HMPA/NMP, the highest inherent viscosity polymer is obtained when each reactant is present in concentrations of ca 0.25 M higher and lower concentrations result in the formation of polymer of lower inherent viscosities. A typical procedure is as foUows 1,4-phenylenediamine, HMPA, and NMP are added to an oven-dried resin ketde equipped with a stirrer and stirred for ca 15 min with cooling to — 15°C, foUowed by the addition of powdered terephthaloyl chloride to the rapidly stirred solution. The reaction mixture changes to a thick, opalescent, paste-like gel in ca 5 min. 

The composition of an oxidizing mixture is altered extensively by the passage of a cool flame (66,83,84). Before passage of the flame, oxygenated materials are present. In the case of hexane oxidation, ROO radicals are reportedly displaced by HOO radicals above 563 K (85), in concordance with previous work (86,87). After the passage of a cool flame, olefins, some conjugate and others of lower molecular weight, are observed. 

The majority of thermal polymerizations are carried out as a batch process, which requires a heat-up and a cool down stage. Typical conditions are 250—300°C for 0.5—4 h in an oxygen-free atmosphere (typically nitrogen) at approximately 1.4 MPa (200 psi). A continuous thermal polymerization has been reported which utilizes a tubular flow reactor having three temperature zones and recycle capabiHty (62). The advantages of this process are reduced residence time, increased production, and improved molecular weight control. Molecular weight may be controlled with temperature, residence time, feed composition, and polymerizate recycle. 

Polymerization. The polymerization of aziridines takes place ia the presence of catalytic amounts of acid at elevated temperatures. The molecular weight can be controlled by the monomer—catalyst ratio, the addition of amines as stoppers, or the use of bifimctional initiators. In order to prevent a vigorous reaction, the heat Hberated during the highly exothermic polymerization must be removed by various measures, ie, suitable dilution, controlled metering of the aziridine component, or external cooling after the reaction has started. 

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