Test distillation apparatus

Fig, 135). Recently, test distillation apparatus (Fig. 237) for amounts of 200 to 500 ml has increasingly been used. It contains a short packed column and allows initial operation at an infinite reflux ratio in order to determine the bubble point exactly. 

Oxidation, (i) Dissolve 5 g. of potassium dichromate in 20 ml. of dil. H2SO4 in a 100 ml. bolt-head flask. Cool and add 1 ml. of methanol. Fit the flask with a reflux water-condenser and warm gently a vigorous reaction soon occurs and the solution turns green. The characteristic pungent odour of formaldehyde is usually detected at this stage. Continue to heat for 3 minutes and then fit the flask with a knee-tube (Fig. 59, p. 100) and distil off a few ml. Test the distillate with blue litmus-paper to show that it is definitely acid. Then apply Test 3 p. 350) for formic acid. (The reflux-distillation apparatus (Fig. 38, p. 63) can conveniently be used for this test.)... 

Sodium -toluenesulfonate, 3, 37, 38 Splitting C C linkage, 4, 39 Splitting C Hg linkage, 7, 19 Stabilizer, 8, 56 Stannous chloride, 8, 96 Starch-iodide test 3, 7 79, 8, 42, 80 Steam distillation apparatus, 2, 0 Steam distillation, reduced pressure, 5, 80... 

A sample of the readily peroxidisable allyl ether, tested with a peroxide test strip gave a negative test result, so was charged into a distillation apparatus, but there was a detonation during distillation. It was recommended that an additional test (potassium iodide-acetic acid) should be used unless it is certain that the test strips will give a positive result with a particular peroxide-containing liquid. 

To a stirred suspension of 1.9 g orthocarbamoyl cinnamamide in 50 ml methanol add 26 ml 0.77 N NaOCl and heat in a distillation apparatus at 40° for 2 hours, or until no more indole is distilled off (can use the indole tests described earlier). Extract the distillate with CHCI3 and dry, evaporate in vacuum (or steam distill the solvent) to get about 45% indole. 

Extraction and Concentration. Five 5-gram units of each ground extrudate were placed into five micro-Kjeldahl flasks. Fifty ml of 80°C deionized water were added to each flask, the flask connected to the distillation apparatus and 40 ml of distillate collected in a screwcap test tube. Eight ml of freshly... 

Arsenic Assemble the special distillation apparatus as shown in Fig. 13 under Arsenic Limit Test, Appendix IIIB. 

Place a drop of the alkaline test solution in the distillation apparatus of Fig. 11.59 and evaporate to dryness. Add 5 drops concentrated sulphuric acid and 5 drops pure methanol, stopper the apparatus, and heat to 80°C in a water bath. Collect the methyl borate which distils over in a micro porcelain crucible, waxed on the inside, and containing about 1 ml reagent. A black precipitate forms. For very small amounts of borate it is best to add a few drops of benzidine acetate solution and thus to detect the traces of manganese dioxide by the... 

Traces of fluoride can be separated from aqueous solutions by extraction with triethylchlorsilane in m-xylene The conditions were optimized and co-precipitation (for enrichment) reactions were tested Adsorption on hydroxyl apatite was found most suitable. From acidified solutions of biological materials fluoride was selectively extracted with a solution of trimethylchlorsilane in benzeneOrganic material or blood was destroyed by heating with hydrochloric acid and hydrogen peroxide in a closed distilling apparatus. The resulting distillates were extracted by triethylchlorsilane in tetrachloroethylene ... 

Rapid removal of the product from the reaction mixture is essential to the success of this preparation. The steam-distillation assembly should be sturdily constructed, with all parts except the distilling flask in place at the time the reaction is started. To ensure the proper fitting of the distilling flask it is convenient to construct the distillation apparatus with the flask in place and, after testing of the apparatus, to remove the flask and incorporate it into the reaction assembly. 

Fig. 39. Semimicro distillation apparatus for distilling directly from an ordinary eight- or six-inch test tube...

A simple distillation apparatus consisting of a 10-ml round-bottom microflask with a 4-cm neck fitted with a one-hole rubber stopper is fabricated. The latter supports a glass tube drawn out at one end to approximately 0.4 mm inside diameter on the receiver end. The tube is bent so that it will extend to the bottom of a 50-ml volumetric flask. Absorption measurements are made with matched l-cm Corex cells, or equivalent, using a prism spectrophotometer. Any final pH adjustments on the test solution are made with a pH meter. 

Potassium dichromate and sulphuric acid (chromyl chloride test) assemble a small, preferably all-glass, distillation apparatus as shown in Fig. 4.1. Place 10 ml 2m sodium hydroxide in the recipient test-tube. The sample which contains chloride must be in solid form. Mix the sample thoroughly with about three times as much powdered potassium dichromate, and place the mixture in the distillation flask. Add an equal volume of concentrated sulphuric acid and warm the mixture gently." Deep-red vapours of chromyl chloride, Cr02Cl2, are formed. When reacting with the sodium hydroxide in the recipient tube, chromyl chloride is converted to chromate ions, resulting in a yellow solution. The presence of chromate can be verified by appropriate reactions (cf. Section 4.33). 

Coal liquids need to be refined to finished products such as jet fuels and diesel by hydrotreating and hydrocracking. Before GC-MS analysis of coal-derived JP-8 fuels, these fuels were first tested by separation into five distillate fractions using a fractional distillation apparatus. Table 32.9 lists the yields and boiling range of fractional distillation [33]. 

Apparatus A 10-mL. a 50-mL. and a 100-mL round-bottom flask, separatory funnel, ice-water bath. 13-mm x 120-mm test tube, apparatus for heating under reflux, simple distillation, magnetic stirring, steam distillation with internal steam generation. vacuum filtration, and flameless heating. 

Procedure. The distillation can be carried out in the apparatus described on page 40 (Fig. 8). A porcelain crucible, paraffined inside, serves as receiver and should contain about 1 ml of reagent solution. A drop of the test solution (plus a drop of alkali if the solution is acid) is placed in the distillation apparatus, and evaporated to dryness. Five drops of concentrated sulfuric acid and 5 drops of pure methyl alcohol are then added, and, after stoppering the apparatus, it is heated to about 80 C in a water-bath. The methyl borate distils into the receiver and undergoes saponification. The resulting alkali causes the formation of a black precipitate. For very small amounts, it is advisable to add a few drops of an acetic acid solution of benzidine to the micro crucible. Traces of manganese dioxide are revealed by the blue color (see page 301). 

Compounds of this class are readily identified by treating with dilute sulphuric acid and testing for sulphur dioxide. When this gas has been detected, heat a fresh sample of the original substance with dilute sodium carbonate solution in a small distillation apparatus, and pass the condensate into methanolic 2,4-dinitro-phenylhydrazine sulphate. The formation of an orange precipitate indicates the presence of an aldehyde or ketone. The precipitate may be collected, purified and used as a derivative. 

The vacuum distillation apparatus, shown schematically in Fig. 1, consists in part of the components described below plus others that appear in Fig. 1 but are not specified, either as to design or performance. Some of these parts are not essential for obtaining satisfactory results from the tests but are desirable components of the assembly for the purpose of promoting the efficient use of the apparatus and ease of its operation. Both manual and automatic versions of the... 

A9.2 Summary of Test Method—The sample is distilled in an automatic distillation apparatus that duplicates the distillation conditions described in the manual procedure. Data are obtained from which the initial boiling point (IBP), the final boiling point (FBP), and a distillation curve of atmospheric equivalent temperature (AET) versus volume can be obtained. 

Xylene (Warning—see Note 1), reagent grade. A solvent blank will be established by placing 400 mL of solvent in the distillation apparatus and testing as outlined in Section 10. The blank will be determined to the nearest 0.025 mL and used to correct the volume of water in the trap as in Section 11. 

Add a 500-mL crude oil test specimen to tared round bottom flask. Obtain and record the mass of the crude oil-filled flask to the nearest 0.1 g. Connect the flask to the distillation apparatus. Place the heating mantle around the flask, and support the heating mantle/flask from the bottom. Connect the heating mantle to the variacs. Turn on the variacs and start the distillation. During the distillation. 

A key result from a distillation test is the boiling point curve, that is, the boiling point of the oil fraction versus the fraction of oil vaporized. The initial boiling point (IBP) is defined as the temperature at which the first drop of hquid leaves the condenser tube of the distillation apparatus. The final boiling point or the end point (EP) is the highest temperature recorded in the test. 

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