Use - This method is not intended as a substitute for experimental measurements of heat of combustion.
Instead, by establishing a correlation of application to other hydrocarbon distillates and hydrocarbons, the
methodology can be used in determining heat combustion.
PART B - D-95 STANDARD TEST PROCEDURE FOR WATER IN
PETROLEUM PRODUCTS AND BITUMINOUS MATERIALS BY DISTILLATION
Requirements and Warnings.
Xylene/Toluene Warning. Flammable. Vapor harmful. Keep away from heat, sparks, and open flame.
Keep container closed. Use with adequate ventilation. Avoid breathing of vapor or spray mist. Avoid
prolonged or repeated contact with skin.
Naphtha Warning. Extremely flammable. Harmful if inhaled. Vapors may cause flash fire. Keep away
from heat, sparks, and open flame. Keep container closed. Use with adequate ventilation. Avoid a
build-up of vapors and eliminate all sources of ignition, especially non explosion-proof electrical
apparatus and heaters. Avoid prolonged breathing of vapors or spray mist. Avoid prolonged or repeated
skin contact.
Environmental precautions for this test method are to clean up all spills immediately. Dispose of
hazardous materials and hazardous waste in accordance with (IAW) laboratory standard operating
procedure (SOP). Report all hazardous material and hazardous waste spills immediately. Be familiar
with and know the location of material safety data sheets (MSDS) for all hazardous materials present in
the workplace.
Apparatus for this test method includes a glass or metal still, a heater, a reflux condenser, and a
graduated glass trap.
Sampling requirement for this test: the size of the test portion should be based on the expected water
content of the sample, such that the water yield does not exceed the capacity of the trap.
Testing procedure.
Measure a suitable amount of sample to an accuracy of 1% and transfer it to the still.
Measure ordinary liquid samples in a graduated cylinder of an appropriate size. Rinse the material
adhering to the cylinder with one 50-ml and two 25-ml portions of the solvent-carrier liquid. Drain the
cylinder thoroughly after the sample transfer and each rinsing.
Weigh solid of viscous materials directly into the still and add 100 ml of the selected solvent-carrier
liquid. In cases of material with a low-water content when large samples must be used, a solvent-carrier
liquid volume in excess of 100 ml may be necessary.
Glass beads or other boiling aids may be added if necessary to reduce bumping.
Assemble the components of the apparatus, choosing the trap in accordance with the expected water
content of the sample and making all connections vapor- and liquid-tight. If a metal still with a
removable cover is used, insert a gasket of heavy paper, moistened with solvent, between the still body
and the cover. The condenser tube and trap must be chemically clean to assure free drainage of water
into the bottom of the trap. Insert a loose cotton plug in the top of the condenser to prevent
condensation of atmospheric moisture inside it. Circulate cold water through the jacket of the condenser.
Apply heat to the still, adjusting the rate of boiling so that condensed distillate discharges from the
condenser at the rate of 2 to 3 drops per second. If the metal still is used, start heating with the ring
burner about 76 ml (3 in.) above the bottom of the still and gradually lower the burner as the distillation
proceeds. Continue distillation until no water is visible in any part of the apparatus except in the trap and
the volume of water in the trap remains constant for 5 minutes. If there is a persistent ring of water in the
condenser tube, carefully increase the rate of distillation or cut off the condenser water for a few minutes.
When the evolution of water is complete, allow the trap and contents to cool to room temperature.
Dislodge any drops of water adhering to the sides of the trap with a glass rod or other suitable means and
transfer them to the water layer. Read the volume of the water in the trap to the nearest scale division.
Calculation and reporting procedures. Calculate the water in the sample, as weight or volume
present, in accordance with the basis on which the sample was taken, as follows:
Water, %= V/W x 100
where:
V = volume of water in trap and
1-3
QM 5181
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