Grades boron trifluoride

Boron trichloride, technical grade Boron trifluoride, technical grade... 

Electronic-grade boron trifluoride gas (99.99-1-%), anhydrous pyridine (99.8%), anhydrous dichloromethane (99.8-1-%). It is essential to use dry solvents and reactants (including the mercury placed at the bottom of the calorimetric cell, to be dried under vacuum) because traces of humidity (and also other impurities) tend to induce an additional heat of reaction. Moreover, boron trifluoride releases hydrogen fluoride by slow hydrolysis, resulting in etching of the glass parts of the system. 

The submitters use the purified, redistilled grade of boron trifluoride etherate available from Aldrich Chemical Company, Inc. 

Reagent grade tetrahydrofuran (Fisher Scientific Company) was either freshly distilled from sodium metal and benzophenone or dried for at least 24 hr over activated Linde 4 A molecular sieves. Boron trifluoride etherate was redistilled prior to use. Fresh bottles of redistilled boron trifluoride etherate purchased from Aldrich Chemical Company, Inc., also usually give good results. 

Dimethyl ether and nitrogen were dried by passage through columns of Drierite. Boron trifluoride etherate (Eastman Practical Grade) was redistilled. Epichlorohydrin (Eastman Organic Chemicals) and methylene chloride (Fisher Scientific Company) were used as received. 

A practical grade of boron trifluoride etherate, purchased from Eastman Kodak Company, was redistilled before use. The pure etherate boils at 126°. 

Other Technologies. Ethylbenzene can he recovered from mixed Cs aromatics by superfractionalion. The Alkar process, commercialized in 1960, uses boron trifluoride on alumina support as the catalyst. It has been used for polymer-grade as well as dilute ethylene feeds. 

Alkylphenol. Alkylphenol is a common surfactant intermediate used to produce alkylphenol ethoxylates. Phenol reacts with an olefin thermally without a catalyst but with relatively poor yields. Catalysts for the reaction include sulfuric acid p-toluene sulfonic acid (PTSA), strong acid resins, and boron trifluoride (BF3). Of these, strong acid resins and BF3 are mostly widely used for the production of surfactant-grade alkylphenols. The most common alkylphenols are octylphenol, nonylphenol, and dodecylphe-nol. Mono nonylphenol (MNP) is by far the most common hydrophobe. It is produced by the alkylation of phenol with nonene under acid conditions. All commercially produced MNP is made with nonene based on propylene trimer. Because of the skeletal rearrangements that occur during propylene oligomerization, MNP is a complex mixture of branched isomers. 

Identification Transfer about 100 mg of sample into a small, conical flask fitted with a suitable reflux condenser. Transfer 50 mg each of USP Palmitic Acid Reference Standard and USP Stearic Acid Reference Standard into a similar flask to serve as the Standard Solution. Treat the contents of each flask as follows Add 5.0 mL of a solution prepared by dissolving 14 g of boron trifluoride in methanol to make 100 mL [commercial reagent, 14% w/v, may be used (Applied Science, or equivalent)]. Swirl to mix, andrefluxfor 15 min. Cool, transfer the reaction mixture with the aid of 10 mL of chromatographic-grade hexane to a 60-mL separator, and add 10 mL of water and 10 mL of saturated sodium chloride solution. Shake, allow the mixture to separate, then drain and discard the lower, aqueous layer. Pass the hexane layer through 6 g of anhydrous sodium sulfate into a suitable flask. 

Boron trifluoride etherate is freshly distilled over CaH2 or used directly when obtained as an analytical grade chemical. This reagent is kept at 4°C under nitrogen as it is a moisture-sensitive reagent. 

Boron trifluoride-diethyl etherate solution, 48%, is commercially available and was used without prior purification. Both the submitters and checkers used reagent grade material from Fluka Chemie AG. 

Boron Trifluoride (commercial grade) may be purchased in cylinders from various suppliers and it should be used with Great Caution. 

The following chemicals were obtained from Aldrich Chemical Company, Inc. and used without further purification 1,3-dimethoxybenzene (99%) butyl lithium (1.6 M in hexanes) 1-formylpiperdine (99%) boron trifluoride-diethyl ether (purified, redistilled) 2,3-dichloro-5,6-dicyano-l,4-benzo-quinone (98%), and pyridine hydrochloride (98%). All solvents were reagent grade and were obtained from Fisher Scientific and used without further purification except where noted. Silica gel (230-4(X) mesh) was obtained from EM Scientific. Chloroform was stored over activated, 4-A molecular sieves for at least 24 h prior to use. Tetrahydrofuran (optima grade) was distilled from sodium benzophenone. Pyrrole (99%) was obtained from Aldrich Chemical Company, Inc. and distilled from calcium hydride. 

Boron trifluoride is available for commercial and industrial use in technical grades having much the same component proportions from one producer to another. The specification for a typical technical grade is as follows ... 

Boron trifluoride is also available in high-purity grades for use in the electronics industry. Gas purity guidelines have been developed and published by the Semiconductor Equipment and Materials International and can be found in the Book of SEMI Standards, Gases Volume [1]. 

Materials. Krypton (Linde, Research grade or Spectra Gases Inc. 99.995% purity) was used as received without further purification. Fluorine (Air Products and Chemicals Inc., nominal 98%) was purified by passing the gas through two NaF traps to remove HF and SiF. Ultrapure fluorine was prepared by the method of Asprey (24). Boron trifluoride (Ozark-Mahoning) was used as received after verification of its infrared spectrum. 

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