Apiezon

Lubrication of all ground glass surfaces is essential for distillations under reduced pressure. Suitable lubricants are Apiezon grease L, M or N and Silicone stopcock grease also Alkathene (a polyethylene plastic), which is especially suitable for high temperatures. 

These values are practically temperature independant, and they are very close to those found for the Apiezon L column. Comparison with the values of a series of alkybenzenes shows that the 5-position of thiazole possesses behavior analogous to that of a benzenic position in gas-liquid chromatography. 

Instmmental methods of analysis provide information about the specific composition and purity of the amines. QuaUtative information about the identity of the product (functional groups present) and quantitative analysis (amount of various components such as nitrile, amide, acid, and deterruination of unsaturation) can be obtained by infrared analysis. Gas chromatography (gc), with a Hquid phase of either Apiezon grease or Carbowax, and high performance Hquid chromatography (hplc), using siHca columns and solvent systems such as isooctane, methyl tert-huty ether, tetrahydrofuran, and methanol, are used for quantitative analysis of fatty amine mixtures. Nuclear magnetic resonance spectroscopy (nmr), both proton ( H) and carbon-13 ( C), which can be used for quaHtative and quantitative analysis, is an important method used to analyze fatty amines (8,81). 

Pyrazolines Imidazoles Thiazoles Oxadiazoles 1 -Phenylpyrazoles Purines Dioxolanes Ox azolines 10% Cyanethylated mannite on Celite 545. 5% OV-17 on Chromosorb W, AW-DMCS (H.P.). Carbowax 4000, dioleate on firebrick, 190 °C. Silicone grease on Chromosorb P. Apiezon L on firebrick C-22, 220 °C. 15% Hallcomid M-18 on firebrick. Carbowax 20M on Gas-Chrom P. Ethyleneglycol succinate on Diatoport-S. 

Apiezon grease 50-200° Volatile hydrocarbons and polar molecules... 

Diphenyl carbonate [102-09-0] M 214.2, m 80 . Purified by sublimation, and by preparative gas chromatography with 20% Apiezon on Embacel, and crystn from EtOH. 

Di-p-tolyl carbonate [621-02-3] M 242.3, m 115 . Purified by GLC with 20% Apiezon on Embacel followed by sublimation in vacua. 

Phenyl 4-tolylcarbonate [13183-20-5] Apiezon on Embacel, and sublimed in vacuo. 

If s-l,2-divinylcyclobutane is desired, it can be isolated in 7—8% yield from the reaction mixture by preparative gas chromatography with the Beckman Megachrom instrument, using columns packed with Apiezon J. 

Non-polar hydrocarbon-type liquid phases, e.g. paraffin oil(Nujol), squalane, Apiezon L grease and silicone-gum rubber the latter is used for high-temperature work (upper limit 400°C). 

Gas chromatography on a 200 cm. by 0.6 cm. column packed with 10% Apiezon L on Chromosorb W (AW, DMCS) using a flame-detector instrument, at a 40 ml./minute helium carrier gas flow rate, gives a trace peak at 9.9 minutes (diphenylmethane), a major peak at 11.7 minutes (1,1-diphenylethane), and a trace peak at 15.4 minutes (1.1-diphenylethanol) when the oven is held at 190° for 10 minutes and then programmed at 10°/minute to 290°. 

Numerous stationary phases were investigated by Callahan et al. [135] but only OV-101 separated C14 5-sultone from the C14 unsaturated-y/2-chloro-y-sultone combination and also separated these from other components present in the sample. Apiezon L separated all three sultones of interest but other components in the neutral oil interfered with the C14 unsaturated y-sultone. Additional stationary phases were found which will separate these sultones, but again, interfering components preclude their use for neutral oil analysis. 

Commercially available Apiezon greases are usually orange colored prior to cleanup and colorless afterwards. Exhaustive hydrogenation can be used to saturate aromatic and olefinic groups to produce a more stable product, Apiezon MB, having properties more typical of a saturated hydrocar]x>n phase [18].. ... 

Fig. 5. Scanning electron microscopy picture of a tungsten tip coated with Apiezon wax. Only the foremost 10 pm of the tip or less remain uncoated.

Boylan and Tripp [76] determined hydrocarbons in seawater extracts of crude oil and crude oil fractions. Samples of polluted seawater and the aqueous phases of simulated samples (prepared by agitation of oil-kerosene mixtures and unpolluted seawater to various degrees) were extracted with pentane. Each extract was subjected to gas chromatography on a column (8 ft x 0.06 in) packed with 0.2% of Apiezon L on glass beads (80-100 mesh) and temperatures programmed from 60 °C to 220 °C at 4°C per minute. The components were identified by means of ultraviolet and mass spectra. Polar aromatic compounds in the samples were extracted with methanol-dichlorome-thane (1 3). 

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