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T110 METHODS OF SAMPLING AND TESTING

Standard Method of Test for

Moisture or Volatile Distillates in Bituminous Paving Mixtures

AASHTO DESIGNATION: T 110-941


(ASTM DESIGNATION: D 1461-85)

1. SCOPE receiver shall be ground off at an angle of require adaptors for connection to the
30 degrees from the vertical axis of the metal still.
condenser or otherwise configured to fit 4.3.2 For determination of the volatile
1.1 This method is intended for the the receiver. For mixtures with very
determination, by direct measurement, of fractions of the bitumen, the receiver
volatile solvents, it may be necessary to shall conform to the dimensions shown in
moisture or volatile fractions of the supplement this water-cooled condenser
bitumen in bituminous paving mixtures. Figure 5.
with a second water-cooled condenser of
1.2 The values stated in SI units are to be approximately the same dimensions. 4.4 Solvent-For general use, an aromatic
regarded as the standard. solvent is preferred, since it has high
solvency and dispersing power for most
1.3 This standard may involve hazardous bituminous materials. Xylene. or a blend
materials, operations and equipment. This of 20 percent toluene and 80 percent
standard does not purport to address all xylene, is recommended. For asphalts
of the safety problems associated with its and similar petroleum products, a
use. It is the responsibility of whoever petroleum distillate, 5 percent boiling
uses this standard to consult and establish between 90 and 100° C (194 and 212° F),
appropriate safety and health practices and 90 percent distilling below 210° C
and determine the applicability of (410° F), may be used. For coal tar.
regulatory limitations prior to use. water-gas tar, and similar materials, the
aromatic solvent must be used.
2. REFERENCED DOCUMENTS 4.5 Heating Device-Any satisfactory
source of heat that will be capable of
maintaining a rate of distillation of 85 to
2.1 AASHTO Standard: NOTE-All dimensions in millimeters. 95 drops per minute.
T 168 Sampling Bituminous Paving
Mixtures
5. SAMPLING

3. SIGNIFICANCE AND USE


5.1 Sampling shall be carried out in
accordance with the procedures set forth
3.1 This method is used for determining in Method T 168.
either the amount of moisture or the
5.2 The sample shall be representative of
amount of volatile petroleum distillates in
the material and shall be of such size as
bituminous paving mixtures.
practical to fill the container in which it is
transported to the laboratory. For
4. APPARATUS duplicate test, a 2 liter (½, gal) friction
top tin pail full of material would be
satisfactory.
4.1 Metal Still-A vertical cylindrical still,
as illustrated in Figure 7, having a faced FIGURE 1 Receivers (Style A)
flange at the top to which the head is 6. TEST SPECIMEN AND SAMPLE
tightly attached by means of a clamp. The
head shall be of metal, and shall be 4.3 Receiver of well-annealed glass, of
6.1 Thoroughly mix the sample and
provided with a tubulation 25.4 mm (I one of the following types depending
weigh out an amount estimated to show a
in.) in inside diameter. upon the purpose of the test:
percentage of moisture or diluent within
4.3.1 For determination of water in the capacity of the receiver calibration.
NOTE 1-Still diameters of up to 127 mm (5") bituminous paving mixtures, a glass Keep the remainder of the sample in its
may be used if required to accommodate larger receiver of 10 or 25 mL capacity shall be tightly covered container. The weighed
samples. used. The receiver shall be graduated in sample should be, preferably, not less
0.1 mL divisions with a ± 0.05 mL than 500 g for normal mixtures.
maximum error below 1 mL and in 0.2 Thoroughly break up this sample to avoid
4.2 Condenser, of the water cooled reflux
mL divisions with a ± 0.1 mL maximum large lumps, and place it in the still.
glass-tube type, having a condenser
error above 1 mL as specified in Table I
jacket not less than 400 stun (15 ¾, in.)
and Figures 1. 2, 3. and 4. Receivers with
long with an inner tube 9.5 to 12.7 mm
tapered or ball bottom vapor tube ends
(3/8 to ½, in.) in outside diameter. The
end of the condenser inserted in the

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T110 METHODS OF SAMPLING AND TESTING

TABLE 1 Description of Receivers

Description
Size of Smallest Scale Scale Error
Style Top of Graduated Bottom of Bottom of Vapor Figure Range, mL
Receiver, mL Division, mL Max, mL
Tube Graduated Tube Tube
0 to 1.0 0.1 0.05
A § joint conical § joint 1 10 Over 1.0 to10.0 0.2 0.1
B § joint conical § joint 2 0 to 1.0 0.1 0.05
C § joint conical plain 3 25 Over 1.0 to 25 0.2 0.1
D plain conical plain 4 5 0 to 5.0 0.1 0.05
E § joint round § joint 5 10 0 to 10.0 0.1 0.1

NOTE-All dimensions in millimeters. FIGURE 2 Receivers (Style B)

7. PROCEDURE FOR at 15 minute intervals show no increase to 10 minutes after the heat has been
DETERMINATION OF MOISTURE in the amount of water being condensed, applied and will drip from the condenser
except that in no case shall distillation at the rate of 85 to 95 drops per minute.
continue for more than 1.5 hours. In case the sample contains a large
7.1 After the sample has been placed in amount of very volatile solvent it may be
the still, add 200 mL of the solvent and 7.4 Allow the contents of the receiver to
reach room temperature and read the necessary to add a second watercooled
quickly stir it into the sample. condenser above the first one or to reduce
volume of water in the receiver to the
7.2 Assemble the components of the nearest scale division. Record the volume the rate of distillation somewhat to
apparatus as. illustrated in Figure 6, of water and calculate in percentage by prevent escape of the solvent.
choosing the receiver in accordance with mass of sample taken as described in 8.3 Continue distillation until three
the expected water content of the sample Section 9.1. successive readings of the upper and
and making all connections vapor and lower levels of the diluent at 15 minute
liquid tight. Insert a gasket of heavy intervals show no increase in the quantity
paper, moistened with water, between the 8. PROCEDURE FOR being collected. Then remove the source
still body and cover. The condenser tube DETERMINATION OF of heat and allow the apparatus to stand
and receiver must be chemically clean to VOLATILE DISTILLATES for 0.5 hour to permit the solvent to cool
assure free drainage of water into the and separate.
bottom of the trap. Insert a loose cotton
plug in the top of the condenser to 8.1 After the sample has been placed in 8.4 Record the volume of diluent in the
prevent condensation of atmospheric the still, add 350 mL of water and receiver to the nearest scale division and
moisture inside it. Circulate cold water approximately 3 g of sodium carbonate calculate in percentage by mass of
through the jacket of the condenser. (Na,CO3), and quickly stir into the sample taken as described in Section 9.2.
sample. Firmly attach the still cover and Use the specific gravity of the diluent at
7.3 Apply heat at such a rate that assemble the receiver and condenser in 25° C (75° F).
refluxing will start within 5 to 10 the manner prescribed in Section 7.2,
minutes, after the heat has been applied except that the gasket is moistened with a
and the condensed solvent will drip into solvent and the trap used shall be the NOTE 2-Assume specific gravity of diluent
the receiver at a rate of 85 to 95 drops per based on knowledge of diluent type or values
dilution trap specified in Section 4.3.2. in range of 0.85 to 0.90. This only defines
minute. Continue the distillation until
three successive readings of the receiver 8.2 Apply heat at such a rate that the volatiles that are obtained at the maximum test
water and solvent will begin to reflux in 5 temperature.
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T110 METHODS OF SAMPLING AND TESTING

9. CALCULATION 10.1 Report the moisture content as 11.1.2 Reproducibility-The results


mass percent water content in accordance submitted by each of two laboratories
with Section 9.1. should be considered suspect if they
9.1 Calculate the moisture content as
follows: 10.2 Report the volatile distillates as differ by more than the following
the mass percent diluent content in amounts:
A
Water, % = x 100 accordance with Section 9.2. Water Collected
B 0 - 1.0 ML 0.2 mL
where: 1.1 - 25 mL 0.2 mL or 10% of the mean,
11. PRECISION whichever is greater
A = Volume of water in receiver
11.2 Precision for Determination of
B = Mass of sample
11.1 Precision for Determination of Volatile Distillates-The precision of this
9.2 Calculate the volatile distillate as Moisture-The following criteria should method is obtained by statistical
follows: be used for judging the acceptability of examination or interlaboratory test results
CxD results (95 percent probability) when us- . as follows:
Diluent, % = x 100 ing the 10 mL or 25 mL receivers.
E 11.2.1 Repeatability-Duplicate
where: 11.1.1 Repeatability-Duplicate determinationsof volatile distillates by
determinations of water by the same the same operator should be considered
C = Volume of dilute in receive operator should be considered suspect if suspect if they differ by more than 0.6
D = Sp. G. of dilute at 25° C they differ by more than the following volume percent.
E = Mass of sample. amounts: 11.2.2 Reproducibility-The results
submitted by each of two laboratories
Water Collected should be considered suspect if they
10. REPORT
0 - 1.0 mL 0.1 ML differ by more thanl.4 volume percent.
1.1 - 25 mL 0.1 mL or 2% of the mean,
whichever is greater
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T110 METHODS OF SAMPLING AND TESTING

FIGURE 5 Apparatus for Determining Volatile Distillates

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T110 METHODS OF SAMPLING AND TESTING

1
Similar but not identical to ASTM D1461-85. Receiver details are more clearly illustrated in ASTM D1461, D123, and D322.

169

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