Cassia flask

Ten c.c. of the oil containing cineol are mixed in a cassia flask of 100 c.c. capacity with so much 50 per cent, resorcinol solution that the flask is filled to about four-fifths. The mixture is shaken thoroughly... 

Assay Mix 50.0 mL of sample with 500 mg of tartaric acid, shake for 5 min, and filter. Dry the filtered oil over anhydrous sodium sulfate, and then pipet 10.0 mL of the clear, treated oil into a 150-mL cassia flask. Add 75 mL of a 30% solution of sodium bisulfite, stopper the flask, and shake until a semisolid to solid sodium bisulfite addition product has formed. Allow the mixture to stand at room temperature for 5 min, then loosen the stopper, and immerse the flask in a water bath heated to between 85° and 90°. Maintain the water bath at this temperature, shaking the flask occasionally, until the addition product dissolves, and then continue heating and intermittently shaking for another 30 min. When the liquids have separated completely, add enough 30% sodium bisulfite solution to raise the lower level of the oily layer within the graduated portion of the flask s neck. Calculate the percentage, by volume, of the citral by the formula... 

Pipet a 10-mL sample into a 100-mL cassia flask fitted with a stopper, and add 50 mL of a freshly prepared 30 in 100 solution of sodium sulfite. Add 2 drops of phenolphthalein TS, and neutralize with 50% (by volume) acetic acid solution. Heat the mixture in a boiling water bath, and shake the flask repeatedly, neutralizing the mixture from time to time by the addition of a few drops of the 50% acetic acid solution, stoppering the flask to prevent loss of volatile material. After no coloration appears upon the addition of a few more drops of phenolphthalein TS and heating for 15 min, cool to room temperature. When the liquids have separated completely, add sufficient sodium sulfite solution to raise the lower level of the oily layer within the graduated portion of the neck of the flask. Calculate the percentage, by volume, of the aldehyde or ketone by the equation... 

Pipet 10 mL of the oil, which has been subjected to any treatment specified in the monograph, into a 100-mL cassia flask, add 75 mL of 1 A potassium hydroxide, and shake vigorously for 5 min to ensure complete extraction of the phenol by the alkali solution. Allow the mixture to stand for about 30 min, then add sufficient 1 A potassium hydroxide to raise the oily layer into the graduated portion of the flask, stopper the flask, and allow it to stand overnight. Read the volume of insoluble oil to 0.05 mL. Calculate the percentage, by volume, of phenols by the equation... 

Assay Mix 50.0 mL of the sample with 500 mg of tartaric acid, shake for 5 min, and filter. Dry the filtered oil over anhydrous sodium sulfate, and then pipet 10.0 mL of the clear, treated oil into a 150-mL cassia flask. 

If a pycnometer was used, determine its volume from 1% — and the density dg of pure water at 25°C (0.997044 g cm % If a Cassia flask was used, carry out this volume calculation for both fillings with water and compare your results with the direct volume readings Vg and m. If necessary devise a calibration procedure that can be applied to correct the Cassia volume readings obtained on the solutions. 

Calculate solution using Eq. (17) for pycnometer data or Eq. (16) for Cassia flask data. Plot tp versus Vm. Determine the slope dcf)ldy[m and the intercept at w = 0 from the best straight line through these data points. This should be done with a linear least-squares fitting procedure. 

Pycnometer (approximately 70 mL) with wire loop for hanging in bath or Cassia flask one or two 200-mL volumetric flasks 100-mL pipette, and 50-mL pipette if a Cassia flask is used pipetting bulb 250-mL Erlenmeyer flask one 250- and one 100-mL beaker large weighing bottle short-stem funnel spatula filter paper and gum-rubber tube (1 to 2 ft long) if an Ostwald-Sprengel pycnometer is used. 

Constant-temperature bath set at 25°C bath hardware for holding flasks and pycnometer reagent-grade sodium chloride (35 g of solid or 200 mL of solution of an accurately known concentration, 50 g or 285 mL if a Cassia flask is used) acetone to be used for rinsing cleaning solution. 

Densities of reaction mixtures of lactic acid and methanol have also been investigated. Troupe and Kobe [12] used a calibrated thin-walled lOOmL cassia flask to determine the densities of methanol/lactic acid mixtures. An equation based on this calibration was derived for the relationship between true and apparent densities of the reaction mixtures ... 

Ten c.c. of the oil containing cineol are mixed in a cassia flask of 100 c.c. capacity with so much 50 per cent, resorcinol solution that the flask is filled for about four-fifths. The mixture is shaken thoroughly for five minutes, and the oil portions which have not entered into reaction are brought into the neck of the flask by adding resorcinol solution, and their volume determined. By subtracting the volume from 10 the cineol-content of the oil is obtained, which is then expressed in per cent, by volume by multiplication with 10. 

Five to 10 c.c. of the oil are shaken in a Hirschsohn fiask, as used for cassia oil analysis, with a 5 per cent, solution of caustic soda, until absorption is complete, and the unabsorbed oil driven into the neck cf the flask by more of the solution and its volume read off. The difference between the original amount of oil used and the unabsorbed portion may be taken as phenols. Strictly speaking, this method gives a volume percentage, which can be converted into a weight percentage if the specific gravities of the two portions of the oil be known. 

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