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This standard has been approved for use by agencies of the Department of Defense.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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TABLE 1 Dimensions and Sizes of Traps
Description Small-
Size of est Scale
Style Top of Bottom of Bottom of Figure Trap, Range, mL Scale Error
Graduated Graduated Vapor mL Division, max, mL
Tube Tube Tube mL
0 to 1.0 0.1 0.05
A $ joint conical $ joint 7 10 over 1.0 to 10.0 0.2 0.1
should be preferably not less than 500 g for normal mixtures. 7.2 Assemble the components of the apparatus as illustrated
Thoroughly break up this sample to avoid larger lumps, and in Fig. 6, choosing the trap in accordance with the expected
place it in the still. water content of the sample and making all connections vapor
and liquid tight. Insert a gasket of heavy paper, moistened with
7. Procedure for Determination of Moisture water between the still body and cover. The condenser tube and
7.1 After the sample has been placed in the still, add 200 mL trap must be chemically clean to assure free drainage of water
of the solvent and quickly stir it into the sample. into the bottom of the trap. Insert a loose cotton plug in the tip
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of the condensor to prevent condensation of atmospheric and will drip from the condenser at the rate of 85 to 95 drops
moisture inside it. Circulate cold water through the jacket of per minute. In case the sample contains a large amount of very
the condenser. volatile solvent, it may be necessary to add a second water-
7.3 Apply heat at such a rate that refluxing will start within cooled condenser above the first one or to reduce the rate of
5 to 10 min after the heat has been applied and the condenser distillation somewhat to prevent escape of the solvent.
solvent will drip into the trap at a rate of 85 to 95 drops/min. 8.3 Continue distillation until three successive readings of
Continue the distillation until three successive readings of the the upper and lower levels of the diluent at 15-min intervals
trap at 15-min intervals show no increase in the amount of show no increase in the quantity being collected. Then remove
water being condensed, except that in no case shall distillation the source of heat and allow the trap and contents to reach
continue for more than 11⁄2 h. room temperature. Allow the trap to stand a minimum of 1⁄2h to
7.4 Allow the contents of the trap to reach room temperature permit the solvent to separate.
and read the volume of water in the trap to the nearest scale 8.4 Record the volume of diluent in the trap to the nearest
division. Record the volume of water and calculate in weight scale division and calculate in weight percent as described in
percent as described in 9.1. 9.2. Use the specific gravity of the diluent at 25°C (77°F).
8. Procedure for Determination of Volatile Distillates 9. Calculation
8.1 After the sample has been placed in the still, add 350 mL 9.1 Calculate the moisture content as follows:
of water and approximately 3 g of sodium carbonate (Na2CO 3)
and quickly stir into the sample. Firmly attach the still cover volume of water in trap
Water, % 5 weight of sample 3 100 (1)
and assemble the trap and condenser in the manner prescribed
in 7.2, except that the gasket is moistened with solvent and the 9.2 Calculate the volatile distillate as follows:
trap used shall be the dilution trap specified in 4.3.2. ~volume diluent in trap! ~sp gr diluent at 25°C!
8.2 Apply heat at such a rate that the water and solvent will Diluent, % 5 weight of sample 3 100
begin to reflux in 5 to 10 min after the heat has been applied (2)
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