Laboratory Safety

• Read SDS/MSDS before

using any
Reagent/Chemical
 Laboratory Safety
• Wear appropriate Personal
Protective Equipment (PPE)
 Laboratory Analysis of
Item 612 Reflective Thermoplastic
Stripping Materials (Solid Form)

• Also called thermoplastic traffic paint

 References used
• D.O. NO 103, Series of 2013
• Glass beads - AASHTO M 247 (Standard
Specification for Glass Beads Used in Pavement
Markings)
• Thermoplastic traffic paint - AASHTO M 249
 Minimum Testing Requirement

• 10 kg of Reflectorized Thermoplastic Paint for every 100

Bags or Fraction Thereof
 Gradation (Uncoated Premix Glass Beads)
• AASHTO M-247 Type 1 - shall be known as a Standard Gradation
• AASHTO T 346 - Method A - ASTM D1214 - Hand Sieve Method
- Method B - AASHTO PP 74 - Computerized Optical Method

Sieve Mass Sieve Mass Sieve Mass

Designation % Designation % Designation %
mm US Passing mm US Passing mm US Passing
1.18 No. 16 100 0.710 No. 25 - 0.300 No. 50 15-35
1.00 No. 18 - 0.600 No. 30 75-95 0.180 No. 80 0-5
0.850 No. 20 95-100 0.425 No. 40 - 0.150 No. 100 0-5
 ASTM D1214 - Standard Test Method for
Sieve Analysis of Glass Spheres
Apparatus
• Balance - sensitive to 50 milligrams or 0.05 gram
• 200 mm or 8 inch in diameter; and conforming to ASTM E11;
• 1.18 (#16); 1.00 mm (#18); 0.850 mm (#20); 0.710 mm
(#25), 0.600 mm (#30), 0.425 mm (#40), 0.300 mm (#50),
0.180 mm (#80) and 0.150 mm (#100) Sieves
• Oven capable of maintaining a temperature of 105 to 110 °C
 ASTM D1214 - Standard Test Method for
Sieve Analysis of Glass Spheres
Dry the specimen to Stack the sieves on
Take 50 g laboratory substantially constant top of each other in
sample by quartering weight at a the order of
or riffle sampling temperature of 105 decreasing size of
to 110 °C opening from the top
to the bottom

Place a pan at the Weigh 50 g of the

bottom of the stack to dried glass spheres to
catch any glass beads
that pass through the the nearest 0.1g and Next Slide
0.150 mm or US No. place on the 1.18 mm
100 Sieve or US No. 16 Sieve
 ASTM D1214 - Standard Test Method for
Sieve Analysis of Glass Spheres

Cover the 1.18 mm or Slightly incline the set of sieves. Gently strike the
US No. 16 Sieve to side about 150 times per minute against the palm of
prevent loss of your hand. Turn the sieve every 25 strokes about
sample during sieving one sixth of a revolution in the same direction

Continue the operation Before weighing the

until not more than 0.05 material passing
g passes through the through the sieve, tap Next Slide
sieve in 1 minute of the side of the sieve
continuous sieving with the brush handle
 ASTM D1214 - Standard Test Method for
Sieve Analysis of Glass Spheres
Remove the cover of Invert the sieve over
the sieve and transfer a piece of glazed
Label and weigh a the glass beads
clean empty container remaining on the white paper (glossy
sieve to the pre- paper or glossy
weighed container photo paper)

Add the material

Clean the wire cloth collected at the
by brushing the glazed white paper Next Slide
to the glass beads
underside removed from the
sieve.
 ASTM D1214 - Standard Test Method for
Sieve Analysis of Glass Spheres

Weigh the portion of Do this for all of the Calculate the weight
the specimen retained sieves using separate and the percent of
on the sieve to the containers for each glass beads passing
nearest 0.1 g sieve. each of the sieves

Take note that when using a set of sieves at the same Reported the total
time, the total weight of beads passing through a specific percent passing each
sieve should include the mass of beads that pass through sieve to the nearest 0.5
the sieves having sizes of opening smaller than the size %
of opening of the sieve being reported.
Calculation using a set of sieves at the same time
Sieve Designation Mass of Glass Mass
mm US Beads Retained % Passing
1.18 No. 16 j (a + b + c + d + e + f + g + h + i) / k
1.00 No. 18 i (a + b + c + d + e + f + g + h) / k
0.850 No. 20 h (a + b + c + d + e + f + g) / k
0.710 No. 25 g (a + b + c + d + e + f) / k
0.600 No. 30 f (a + b + c + d + e) / k
0.425 No. 40 e (a + b + c + d) / k
0.300 No. 50 d (a + b + c) / k
0.180 No. 80 c (a + b) / k
0.150 No. 100 b a/k
Pan a N/A
k=a+b+c+d+e+f+g+h+i+j
 Roundness (Uncoated Premix Glass Beads)

• AASHTO T 346 Section 6

• Method A - ASTM D1155
• Method B - AASHTO PP74 - Computerized Optical
Method
• The beads shall have minimum of 90 percent true sphere
(D.O. No. 103, Series of 2013)
 ASTM D1155 - Standard Test Method for
Roundness of Glass Spheres
Apparatus
• Electrical Feeder-Vibrator, upon which is mounted a smooth glass
panel, 152.4 mm (6 in.) wide and 381 mm (15 in.) long
• Hinged Base, supporting the vibrator and panel in such a manner
that the angle of slope of the glass panel with the horizontal may
be varied and fixed in any predetermined position
• Vibrator—Means of varying the amplitude or strength of the
vibrations transmitted to the glass panel, at a fixed frequency of 60
impulses per second.
 ASTM D1155 - Standard Test Method for
Roundness of Glass Spheres
Apparatus
• Feeding Device or Pan, affixed to the glass panel in such a manner
that the selected sample of glass may be evenly dropped at a
uniform rate upon the glass panel, from various heights above the
panel and at various points on the slope
• Collecting Pans or Containers, at either end of the sloping panel, in
which to collect the spheres and irregular particles.
• Digital Level, approximately 30 to 60 cm (12 to 24 in.) in length
• 300-μm (No. 50) sieve conforming to ASTM E11
ASTM D1155 - Standard Test Method for
Roundness of Glass Spheres
Apparatus
 ASTM D1155 - Standard Test Method for
Roundness of Glass Spheres - Procedure A
Take approximately Set aside in separate
50 g laboratory Sieve through a 300- containers the retained
glass beads and glass
sample by quartering μm (No. 50) sieve beads that passed
or mechanical splitter through the sieve

set the decimal angle

of the roundometer
Level the glass panel plate to the 300-μm Next Slide
(50 U.S. Sieve) setting
of 2.3 degrees using
a digital level
 ASTM D1155 - Standard Test Method for
Roundness of Glass Spheres - Procedure A
Affix the feed hopper
to the side of the Place retained glass
panel at the upper beads in the feed start the vibrator
one-third point of the pan
slope

Set the vibrator amplitude control at such a position

that irregular particles on the upper half of the Next Slide
panel will move slowly up the slope, while the true
spheres roll down.
 ASTM D1155 - Standard Test Method for
Roundness of Glass Spheres - Procedure A
Feed slowly, at such a
rate that no When the glass panel Stop feeding until
“bunching up” or is well covered with separation of true
flooding of spheres spheres spheres has occurred
on the panel occurs.

Brush or scrape all

Stop the vibrator after particles remaining on
all true spheres have
rolled down the slope the panel into the Next Slide
into the sphere pan upper pan containing
the irregular particles
 ASTM D1155 - Standard Test Method for
Roundness of Glass Spheres - Procedure A
Repeat the placing of retained glass beads in the
feed pan procedure up to the brush or scrape all
particles remaining on the panel into the upper pan
containing the irregular particles until all retained
glass beads have been separated

Using the true spheres collected, repeat the placing

of glass beads in the feed pan procedure up to the
brush or scrape all particles remaining on the panel Next Slide
into the upper pan containing the irregular
particles
 ASTM D1155 - Standard Test Method for
Roundness of Glass Spheres - Procedure A
Using the irregular particles collected in the first Examine the separated
separation, repeat the placing of glass beads in the spheres and irregular
feed pan procedure up to the brush or scrape all particles under a 20-
particles remaining on the panel into the upper pan diameter magnifying
containing the irregular particles glass

Determine the total

Repeat the reruns until weights of the true
satisfactory separation Next Slide
is obtained spheres and of the
irregular particles
 ASTM D1155 - Standard Test Method for
Roundness of Glass Spheres - Procedure A
Run the glass beads that passed through the 300-μm Determine the total
(No. 50) sieve through the same process only weights of the true
changing the decimal angle of the roundometer spheres and of the
plate to 3.9 degrees using a digital level. irregular particles

Calculate the percent of true spheres in the total specimen from the total weight of true
spheres obtained from the retained glass beads and glass beads that passed through the
sieve, using as 100 % the total weight of true spheres plus irregular particles collected in
the test
 ASTM D1155 - Standard Test Method for
Roundness of Glass Spheres - Procedure A

• Percent true sphere =

• a = weight of true spheres from the glass beads retained at 300-μm (No. 50) sieve
• b = weight of true spheres from glass beads that passed through the 300-μm (No. 50)
sieve
• c = weight of irregular particles from the glass beads retained at 300-μm (No. 50) sieve
• d = weight of irregular particles from glass beads that passed through the 300-μm (No.
50) sieve
 ASTM D1155 - Standard Test Method for
Roundness of Glass Spheres - Procedure B

• Uses 600-μm (No. 30), 425-μm (No. 40), 300-μm (No. 50), and (No. 70)
instead of just 300-μm (No. 50) sieve.
• Same procedure except the decimal angle of the roundometer plate and
number of reruns shall be as follows:
Passing Sieve Retained on Sieve Decimal Angle Number of Reruns
600-μm (No. 30) 1.1 until satisfactory separation
600-μm (No. 30) 425-μm 1.5 4
425-μm (No. 40) 300-μm 2.3 4
300-μm (No. 50) 212-μm 3.1 5
212-μm (No. 70) 3.9 5
 ASTM D1155 - Standard Test Method for
Roundness of Glass Spheres - Procedure B

• Percent true sphere =

total weight of true spheres from all size groups

total weight of true spheres from all size groups +
total weight of irregular particles from all size groups
 Refractive Index

• AASHTO T 346 Section 7

• Liquid immersion method (ASTM C1648 - Standard Guide
for Choosing a Method for Determining the Index of
Refraction and Dispersion of Glass - Becke Line Method or
equivalent) at a temperature of 25 ± 5°C
• The beads shall have a refractive index of 1.50–1.55
(D.O. No. 103, Series of 2013)
 ASTM C1648 - Becke Line Method
Apparatus and Materials
• Microscope - Use a microscope having a total magnification of
at least 80× that has a sub-stage condenser with a variable-
aperture iris diaphragm. (A 10× objective lens and a 10×
ocular are very satisfactory)
• Microscope Slides and Cover Glasses - Use standard glass
microscope slides, 1×3-inch, 1-mm thick, and microscope
cover glasses, 18 mm (preferred) or 22 mm2 and 0.35-mm
thick (#1 ½).
 ASTM C1648 - Becke Line Method
Apparatus and Materials
• Bandpass Filters - Narrow spectral bandpass filters, about 1-nm FWHM
(full width at half maximum transmittance), should be used
(measurement with white light reduces the accuracy of a result). These
can be commercial interference filters. Owing to the bandwidth of about
10 nm, the wavelengths of the transmittance maxima of the filters need
not fall at exactly the wavelengths of the spectral lines that are specified
for determining dispersion-numbers. For the Abbe ν-value, standard
interference filters with nominal peak wavelengths of 490 nm, 590 nm,
and 650 nm or 660 nm would work well. The filter should be mounted
close to the substage condenser assembly. This will avoid focusing dirt or
surface defects of the filter onto the plane of the specimen.
 ASTM C1648 - Becke Line Method
Apparatus and Materials
• Calibrated Immersion Oils - Sets of calibrated index oils are available with
indices over the range 1.300 to 2.31. Partial sets, by preset groupings or
by custom selections, can be purchased according to particular need. The
label of each bottle has the index for the sodium D-line at 25°C,
standardized to 2×10-4, the temperature coefficient of index, and the
indices for the hydrogen C and F-lines. Liquids with indices above 1.70
require special handling, as taught by the manufacturer. The oils are
supplied in 7.4-cc (1⁄4 fl oz) bottles; the caps have small glass rods for
transfer of fluid by the drop. The refractive indices of the oils depend on
their temperature; therefore, store the oils at room temperature and
measure the temperature at the time of testing. Temperature-corrections
of the indices of the oils must be made. Note: Toxic
 ASTM C1648 - Becke Line Method
Apparatus and Materials
• Calibrated Immersion Oils - Sets of calibrated index oils are
available with indices over the range 1.460 to 1.640 (adjusted
based on the DPWH refractive index requirement of 1.50–1.55).
The label of each bottle has the index for the sodium D-line at
25°C, standardized to 2×10-4, the temperature coefficient of index,
and the indices for the hydrogen C and F-lines. Supplied in 7.4-cc
(¼ fl oz) bottles; the caps have small glass rods for transfer of fluid
by the drop. Store the oils at room temperature and measure the
temperature at the time of testing. Temperature-corrections of the
indices of the oils must be made.
 ASTM C1648 - Becke Line Method
Apparatus and Materials
• Mortar and Pestle – A small mortar and pestle of agate or of a
hard ceramic is used to prepare the specimens for observation.
• Thermometer - A thermometer that is sensitive and accurate
to 0.5°C is needed
• Alcohol - for cleaning glass samples, no grade required
• 100-mesh and 170-mesh sieves conforming to ASTM E11
 ASTM C1648 - Becke Line Method
Place the glass
sample into the Collect the glass beads
mortar and crush it by Pass the samples that pass through a
pressing down with through 100-mesh 100-mesh sieve but are
and 170-mesh sieves retained by a 170-
the pestle using a mesh sieve
rocking motion

Transfer about 10 glass Three piles can be

beads to the placed on a slide, Next Slide
microscope slide using a spaced about 20-mm
spatula with a small tip apart
 ASTM C1648 - Becke Line Method
Spread the particles
over an area about Lay a cover slip on the spread and dispense 1
10-mm diameter and to 3 drops of a calibrated index oil by touching
remove any the tip of the rod to the edge of the cover slip
exceptionally large and the surface of the slide
particles

Place the slide on the

Close the iris
stage of the microscope diaphragm Next Slide
appreciably
 ASTM C1648 - Becke Line Method
Bring a particle into
focus and adjust the iris
diagram and the focus a
until the boundary
between particle and
oil is sharp (c)

Note the darkness and

breadth of the particle-
oil boundary for
estimating a small or a a Next Slide
large change of index
for the next oil
 ASTM C1648 - Becke Line Method
Repeat these
Raise the focal plane of the microscope above the observations for several
plane of the particle while observing the formation particles and act
of the bright Becke line and its motion into one according to the
medium, whether glass or oil indication of the
majority

Next, choose an oil with index closer to that of

the glass. Repeat the procedure until a match is
achieved (glass fragment will seem to Next Slide
disappear in the oil) or until the 2 closest
(bracketing) oils are found.
 ASTM C1648 - Becke Line Method
If desired to have an Estimate the index by interpolating between the
estimate of the indices of the bracketing oils using relative contrasts
dispersion of the glass,
repeat with bandpass of the boundary when the particle is in focus. The
filters for the C and F- estimate can be as good as one-fourth of the step
lines. of index between the two oils.

The estimate must also

be whether to assign Multiply the difference between 25°C and the
the exact index of 1 oil temperature of the oil (that is, room temperature) by
(for a close match) or to the temperature coefficient of index-variation and
assign the value of the add (algebraically) to obtain the correct index
nearest quarter-step.
 Sampling - AASTO T 250 Section 3
Quartering Method
Apparatus and Materials
• 1.2-by-1.2-m (4-by-4-ft) section of cardboard, smooth wood, or
metal;
• Metal scooping pan;
• Metal splitting device; and
• Unlined 3.8-L (1-gal) cans.
 Sampling - AASTO T 250 Section 3
Quartering Method
Place the 1.2-by-1.2-
m (4-by-4-ft) section Place the 20-kg Using the metal scoop,
mix the material,
of cardboard, smooth sample onto the breaking up any large
wood or metal on a sample area lumps
level section of floor

Shape the pile of Take the metal

thermoplastic into as splitting device and
high a pile as possible, center it over the Next Slide
forming a symmetrical apex of the
inverted cone thermoplastic
 Sampling - AASTO T 250 Section 3
Quartering Method
Take the material The 2 remaining quarters are
Lower the device onto from any 2 to be mixed and split in the
the material, thus opposing quarters same manner as explained
splitting it into four and return it to above, rotating between the
quarter sections the thermoplastic 2 quarters that are retained
bag at the end of each step

Label the outside of

Repeat the process Retain the final 2 the 3.8-L (1-gal)
2 more times or opposing quarters as a sample can with the
until you decrease part of the composite laboratory number,
the mass of each sample and place in the
quarter to 1.25 kg color and type of
unlined 3.8-L (1-gal) can. material
 Sampling - AASTO T 250 Section 3
Splitter Method
Apparatus and Materials
• 1:1 Splitter with pans; and
• Unlined 3.8-L (1-gal) can.
 Sampling - AASTO T 250 Section 3
Splitter Method
Place the 20 kg Place a pan
sample into one of Empty the contents in
the pans and place underneath each of the top pan such that
on top of the 1:1 the two discharge the material passes
sections of the splitter through the splitter
splitter

Take each half and split Split the two

individually to form remaining pans
quarters. Return two Next Slide
opposing pans, or individually to form
quarters, to the bag quarters
 Sampling - AASTO T 250 Section 3
Splitter Method
Repeat the above This splitting procedure
procedure by splitting is performed two times
the two opposing pans or until you decrease
while returning the the mass of each
others to the bag quarter to 1.25 kg

Label the outside of the

Placing the final quarters 3.8-L (1-gal) sample can
into the sample container with the laboratory
number, color and type
of material
 Sampling - AASTO T 250 Section 3
Thieving Method
Apparatus and Materials
• 5-cm (2-in.) ID metal pipe approximately 1 m (3 ft) long;
• Unlined 3.8-L (1-gal) cans.
 Sampling - AASTO T 250 Section 3
Thieving Method
Carefully cut the bag Insert the sample pipe
Place the bag at the top or bottom into the bag and push
containing the 20 kg to allow the pipe to through the
sample on a flat be inserted into the
thermoplastic material
surface through the entire
bag. length of the bag.

Carefully remove the Repeat the process, Label the outside of

pipe and empty the pushing the pipe the 3.8-L (1-gal)
thermoplastic material through a different sample can with the
that is retained in the area of the sample bag laboratory number,
pipe into the unlined until an ~2.5-kg sample color and type of
3.8-L (1-gal) can. has been obtained. material
 Sample Meltdown and Preparation
AASTO T 250 Section 4
Apparatus and Materials
• A stainless steel 4000-mL beaker, 15-cm (6-in.) diameter by 23 cm (9
in.) high, such as a Volrath No. 84000 or equivalent such as an unlined
metal 3.8-L (1-gal) can.
• Suitable heating mantle, such as a Glas-Col heating mantle, Model
TM620 or equivalent.
• Temperature indicator-controller, such as an Omega Engineering
Model 400JF or equivalent.
 Sample Meltdown and Preparation
AASTO T 250 Section 4
Apparatus and Materials
• Thermocouple, such as an Omega Engineering No. TJ36-ICSS-
116G-12 with 1.6-mm (1/16-in.) 304SS sheath, or equivalent.
• Air powered variable speed mixer, such as a Lightning Model 30
with two Lightning A310 stainless steel impellers or similar
equipment.
• Aluminum lid to cover the top of the stainless steel 4000-mL
beaker with slot to clear the air motor agitator shaft and
thermocouple.
 Sample Meltdown and Preparation
AASTO T 250 Section 4
Apparatus and Materials
• Stainless steel ladle with pouring spout, 60-mL (2-oz) capacity.
• Tachometer to measure shaft speed of mixer.
• Copper or stainless steel tubing approximately 3 mm (1/8 in.)
and 25 cm (10 in.) long.
• Porcelain dish, 150 mL.
• Crucibles, 30 mL.
• Glass beaker, 2 L.
Sample Meltdown
and Preparation

AASTO T 250
Section 4

Apparatus Set-up

Detail A
 Sample Meltdown and Preparation
AASTO T 250 Section 4
Wire the heating Mount the controller- Make a test melt to set
mantle power cord to indicators in a panel the proportional band
the temperature that can be wall and other adjustments
indicator controller mounted to keep the to give a controlled
per manufacturer’s unit away from heat, temperature of 218 ±
instructions. dirt, and vibrations 1°C

Change about one-half

the granular sample Turn on the power to
into the appropriate
container and place in the mantle and Next Slide
the heating mantle and controller
attach the stirring shaft
 Sample Meltdown and Preparation
AASTO T 250 Section 4
As the thermoplastic Note: The entire Start the variable-
melts down, add the composite sample speed air agitator
remainder of the from the sampling when plastic has
procedure should be softened sufficiently to
sample melted mix

Maintain temperature Remove the

Continue to mix and at 218 ± 1°C for the thermoplastic sample
heat until temperature number of hours that using a 60-mL (2-oz)
reaches 218°C and the the specific test method ladle and prepare
sample is homogeneous requires before getting samples or run tests as
melted sample required
 Specific Gravity

• AASHTO T 250 Section 16 - Specific Gravity

• ASTM D792 - Standard Test Methods for Density and
Specific Gravity (Relative Density) of Plastics by
Displacement - Method A [Test Method A for Testing Solid
Plastics in Water (Specimens 1 to 50 g)]
• S.G.max = 2.15 (D.O. No. 103, Series of 2013) (for white
and yellow)
ASTM D792 Method A - Density and Specific Gravity
(Relative Density) of Plastics by Displacement
Apparatus and Materials
• Analytical Balance - precision of 0.1 mg or better for materials
having densities less than 1.00 g/cm3 and sample weights less than
10 grams. Shall be equipped with a stationary support for the
immersion vessel above the balance pan (“pan straddle”).
• Digital Balance - precision of 1 mg or better for other materials and
sample weights (Analytical balances comply with this requirment).
Shall be equipped with a stationary support for the immersion
vessel above the balance pan (“pan straddle”)
ASTM D792 Method A - Density and Specific Gravity
(Relative Density) of Plastics by Displacement
Apparatus and Materials
• Sample Holder - corrosion-resistant (for example, wire, gemholder, etc.).
• Sinker - A sinker for use with specimens of plastics that have specific gravities
less than 1.00. The sinker shall: (1) be corrosion-resistant; (2) have a specific
gravity of not less than 7.0; (3) have smooth surfaces and a regular shape; and
(4) be slightly heavier than necessary to sink the specimen. The sinker shall
have an opening to facilitate attachment to the specimen and sample holder.
• Immersion Vessel - A beaker or other wide-mouthed vessel for holding the
water and immersed specimen.
• Thermometer - A thermometer readable to 0.1°C or better.
 ASTM D792 Method A - Density and Specific Gravity
(Relative Density) of Plastics by Displacement
Make a test specimen Test specimen shall be a single piece with a size and
from the molten shape that fits the testing apparatus, a volume of not
thermoplastic after less than 1 cm3 and its surface and edges smooth.
heating for 4 hours The thickness of the specimen shall be at least 1 mm
(AASHTO T250 for each 1 g of weight. (1 to 5 g is convenient)
Section 16)

Prepare the testing

The specimen shall be apparatus setup
free from oil, grease,
and other foreign based on Next Slide
matter. manufacturer’s
recommendation
 ASTM D792 Method A - Density and Specific Gravity
(Relative Density) of Plastics by Displacement
Weigh the specimen
Measure and record in air (refer to Refer to manufacturer’s
the water “Apparatus and instruction manual on
temperature Materials” for the how to use the testing
appropriate balance apparatus
to use)

If necessary, attach to the balance a piece of fine wire

sufficiently long to reach from the hook above the pan to
the support for the immersion vessel. Attach the specimen
to the wire such that it is suspended about 25 mm above Next Slide
the vessel support. [mass of the specimen, a = (mass
ofspecimen + wire, in air) − (mass of wire in air)]
 ASTM D792 Method A - Density and Specific Gravity
(Relative Density) of Plastics by Displacement
Mount the immersion vessel on the support, and Remove any bubbles
completely immerse the suspended specimen adhering to the
specimen, sample
(and sinkers, if used) in water at a temperature holder, or sinker, by
of 23 ± 2°C. The vessel must not touch sample rubbing them with a
holder or specimen wire.

Pay particular attention to holes in the specimen

and sinker. If the bubbles are not removed by
this method or if bubbles are continuously Next Slide
formed (as from dissolved gases), the use of
vacuum is recommended
 ASTM D792 Method A - Density and Specific Gravity
(Relative Density) of Plastics by Displacement
Determine the mass of Record this apparent
mass as b (the mass of Weigh rapidly in
the suspended specimen the specimen, sinker, if order to minimize
using the same balance
as the one used in used, and the partially absorption of water
weighing in air immersed wire in by the specimen.
liquid).

Weigh the sample

holder (and sinker, if Record this weight as
used) in water with w (mass of the Make two specimens
immersion to the same sample holder in per sample
depth as used in the liquid)
previous step
ASTM D792 Method A - Density and Specific Gravity
(Relative Density) of Plastics by Displacement
Calculations

• sp gr 23/23°C =
• = apparent mass of specimen in air
• = apparent mass of specimen completely immersed and of
the wire partially immersed in liquid
 Composition - Resin - Binder

• AAHTO T 250 Section 5 - Binder Content

• ASTM D4797 - Standard Test Methods for Gravimetric
Analysis of White and Yellow Thermoplastic Pavement
Marking
• Bindermin = 18.0 (D.O. No. 103, Series of 2013) (for
white and yellow)
 ASTM D4797 - Binder Composition
Apparatus and Reagents

• Balance - analytical, capable of weighing to 0.1 mg or better

• Crucibles - 30+ mL, porcelain or aluminum pan
• Desiccator with dessicant
• Furnace - Muffle, capable of maintaining 540°C
• Hot Plate or Heating Mantle - capable of heating a can of
thermoplastic to 218°C
 ASTM D4797 - Binder Composition
Apparatus and Reagents

• Sieve, 3 in., 45-μm (No. 325) (metal)

• Buchner Funnel
• Vacuum Flask and Rubber Hose
• Vacuum Pump
• Oven capable of reaching 218°C
• Microwave Oven
 ASTM D4797 - Binder Composition
Apparatus and Reagents

• 400 mL Beaker or acid proof container

• Magnetic Stirring Bar
• Magnetic Stirring Plate
• Spatula
• Hydrochloric Acid - Concentrated
 ASTM D4797 - Binder Composition
Take sample during Flow the sample out
the first hour after the Patties approximately 3
entire sample on a smooth clean mm (⅛ in.) thick are
becomes molten non-stick surface and usually easy to break
(AAHTO T 250 allow it to cool to up specimens for the
room temperature. described analysis.
Section 5)

Break the specimen into The binder test can

small pieces and weigh be done on samples
to the nearest 0.1 mg
into a weighed crucible as small as 10 g Next Slide
that is at least twice the (0.353 g) and be
volume of specimen. effective
 ASTM D4797 - Binder Composition
Cover the crucible and
Larger samples can supply place into a muffle furnace
preheated to 540°C and
more glass beads for ash for 1 hour or until no
evaluation later if required carbonaceous material
remains

Remove the crucible with Weigh the

the ashed remains of the crucible and ash
specimen and place into
a desiccator and cool to to the nearest 0.1
room temperature. mg
 ASTM D4797 - Binder Composition
Calculations
• D = (1 – (S ⁄ W)) x 100
• D = percent binder
• S = ashed weight of thermoplastic specimen, g, (crucible +
• ash wt.) – crucible wt.
• W = weight of thermoplastic specimen, g, (crucible +
thermoplastic specimen) – crucible wt.
 Composition - Glass Reflectorizing Sphere - Glass
Beads
• AAHTO T 250 Section 6 – Glass Beads Content
• ASTM D4797 - Standard Test Methods for Gravimetric
Analysis of White and Yellow Thermoplastic Pavement
Marking
• Glass Beads = 30-40 (D.O. No. 103, Series of 2013)
 ASTM D4797 - Glass Beads Composition
Apparatus and Reagents

• Balance - analytical, capable of weighing to 0.1 mg or better

• Crucibles - 30+ mL, porcelain or aluminum pan
• Desiccator with dessicant
• Furnace - Muffle, capable of maintaining 540°C
• Hot Plate or Heating Mantle - capable of heating a can of
thermoplastic to 218°C
 ASTM D4797 - Glass Beads Composition
Apparatus and Reagents

• Sieve, 3 in., 45-μm (No. 325) (metal)

• Buchner Funnel
• Vacuum Flask and Rubber Hose
• Vacuum Pump
• Oven capable of reaching 218°C
• Microwave Oven
 ASTM D4797 - Glass Beads Composition
Apparatus and Reagents

• 2-L Beaker or acid proof container

• Magnetic Stirring Bar
• Magnetic Stirring Plate
• Spatula
• Hydrochloric Acid - Concentrated
 ASTM D4797 - Glass Beads Composition
Take sample during Flow the sample out
the first hour after the Patties approximately 3
entire sample on a smooth clean mm (⅛ in.) thick are
becomes molten non-stick surface and usually easy to break
(AAHTO T 250 allow it to cool to up specimens for the
room temperature. described analysis.
Section 6)

Break the specimen into The binder test can

small pieces and weigh be done on samples
to the nearest 0.1 mg
into a weighed crucible as small as 10 g Next Slide
that is at least twice the (0.353 g) and be
volume of specimen. effective
 ASTM D4797 - Glass Beads Composition
Larger samples can Cover the crucible and Remove the crucible
supply more glass place into a muffle with the ashed remains
furnace preheated to of the specimen and
beads for 540°C and ash for 1 hour place into a desiccator
evaluation later if or until no carbonaceous and cool to room
required material remains temperature.

Weigh the crucible Transfer the ash to a

and ash to 0.1 mg 2-L beaker or other
acid-proof container Next Slide
and calculate the and with minimal
percent ash. pressure
 ASTM D4797 - Glass Beads Composition
Break apart the Stir occasionally
ashed specimen Place in vented hood
without crushing the and add to the ash until most of the
retroreflective
~250 to 750 mL of effervescence has
1+1 HCL ceased
optics.

Immediately dilute the contents with as

much water as possible to allow the
glass beads to settle. Decant the water Next Slide
and particulate carefully so as not to
loose glass beads
 ASTM D4797 - Glass Beads Composition
If all the ash residue has not gone Continue adding
into solution, reintroduce HCL solution HCL or diluting with
and stir using magnetic stirring bar water and
and magnetic stirrer or stirring with decanting until the
a spatula water is clear.

Transfer the residue Wash with enough

into a weighed 3-in. cold water to remove
45-μm (No. 325) sieve
any residue. Repeat Next Slide
or a Buchner funnel
acid washing until the
with filter paper glass beads appear
clean
ASTM D4797 - Glass Beads Composition

If using sieve, dry the sides and the bottom of the sieve
with a paper towel and dry for 1 hour in a gravity oven
preheated to 100°C. If using buchner funnel, use vacuum
to evacuate the water and then dry the glass beads
containing-filters in a oven or microwave oven.

Place in a desiccator Weigh the

and cool to room sieve/filter and glass
temperature. beads to 0.1 mg
 ASTM D4797 - Glass Beads Composition
Calculations

• % Glass Beads = R/W x 100

• R = weight of glass beads after acid wash (g)
(not including sieve/filter weight)
• W = original weight of thermoplastic specimen
(g) (not including crucible weight)
 Composition - Pigment - Titanium dioxide

• ASTM D1394 - Standard Test Methods for Chemical

Analysis of White Titanium Pigments - Total Titanium by
the Jones Reductor Method
• ASTM D4764 - Standard Test Method for Determination
by X-ray Fluorescence Spectroscopy of Titanium Dioxide
Content in Paint
 Composition - Pigment - Titanium dioxide

• Titanium dioxidemin= 10.0 (only for white) (D.O. No. 103,

Series of 2013)
• Only for White thermoplastic paint
• For yellow thermoplastic paint - Amount of Yellow
Pigment, calcium carbonate, and inert fillers shall be at
the option of the manufacturer, providing all other
requirements of AASHTO M 249-12 are met.
 ASTM D1394 - Total Titanium by the Jones Reductor
Method
Appartus
• Jones Reductor - having a zinc column at least 450 mm in length, and 19 mm in
diameter. The filtering pad must be tight enough to hold all the particles of
amalgamated zinc resting on it, and made of glass-wool supported by platinum
gauze or a perforated porcelain plate. Use the least amount (0.1 to 1.0 %) of
mercury that will enable satisfactory control of hydrogen evolution, since heavy
amalgamation tends to reduce the rate of reaction. Prepare the amalgam by
washing 20-mesh zinc for 1 min in enough 1 N HCl to cover it, adding the
proper amount of 0.25 M mercuric nitrate or chloride solution, and stirring
rapidly for 3 min. Decant the solution and wash the amalgam with water and
store under water to which a few drops of HCl have been added. After using,
keep the reductor filled with water when not in use, in order that basic salts will
not be formed and clog it.
 ASTM D1394 - Total Titanium by the Jones Reductor
Method
Appartus
• Weighing bottle and cap
• Desiccator with desiccant
• 250 mL chemical and heat-resistant glass beaker
• Chemical and heat-resistant reagent bottles
 ASTM D1394 - Total Titanium by the Jones Reductor
Method
Reagents
• Ammonium Hydroxide (sp gr 0.90) - Concentrated ammonium hydroxide
(NH4OH)
• Ammonium Sulfate ((NH4)2SO4)
• Carbon Steel or Iron - Pure iron or plain carbon steel
• Ferric Sulfate Solution (1 mL = 0.02 g Fe) - Dissolve 20 g of iron or carbon steel
in a slight excess of HCl, oxidize with approximately 12 mL of HNO3, add about
80 mL of H2SO4, and heat to dense white fumes. Cool, dilute with water to 1 L,
digest on a steam bath until sulfates are dissolved, and filter if necessary. To
oxidize any ferrous iron that may be present, add 0.1 N KMnO4 solution until a
faint pink color persists for 5 min. Ferric ammonium sulfate
(FeNH4(SO4)2•12H2O) may also be used to prepare this solution
 ASTM D1394 - Total Titanium by the Jones Reductor
Method
Reagents
• Hydrochloric Acid (sp gr 1.19) - Concentrated hydrochloric acid
(HCl)
• Iron or Carbon Steel - Pure iron or plain carbon steel.
• Nitric Acid (sp gr 1.42) - Concentrated nitric acid (HNO3).
• Sodium Oxalate - National Institute of Standards and
Technology standard reference material No. 40 of sodium
oxalate (Na2C2O4).
 ASTM D1394 - Total Titanium by the Jones Reductor
Method
Reagents
• Potassium Permanganate, Standard Reference Material (0.1 N, 1 mL = 0.008 g
TiO2) - Dissolve 3.16 g of KMnO4 in water and dilute to 1 L. Let stand 8 to 14
days, siphon off the clear solution (or filter through sintered glass, medium
porosity), and standardize against the National Bureau of Standards standard
sample No. 40 of sodium oxalate (Na2C2O4) as follows: In a 400-mL beaker
dissolve 250 to 300 mg Na2C2O4 in 250 mL of hot water (80 to 90°C) and add
15 mL of H2SO4(1+1). Titrate at once with the KMnO4 solution, stirring the
liquid vigorously and continuously. The KMnO4 solution must not be added more
rapidly than 10 to 15 mL/min, and the last 0.5 to 1 mL must be added dropwise
with particular care to allow each drop to be fully decolorized before the next is
introduced. (Continued at next slide)
 ASTM D1394 - Total Titanium by the Jones Reductor
Method
Reagents
The solution shall not be below 60°C by the time the end point has been
reached. (More rapid cooling may be prevented by allowing the beaker to
stand on a small hot plate during the titration. The use of a small type
thermometer as a stirring rod is most convenient.) Keep the KMnO4 solution
in a glass-stoppered bottle painted black to keep out light or in a brown
glass bottle stored in a dark place. Calculate the TiO2 equivalent in grams of
TiO2 per mL of the KMnO4 solution as follows:
TiO2 equivalent = (W /1.192)/V
W = Na2C2O4 used, g, and
V = KMnO4 solution required for the titration, mL
 ASTM D1394 - Total Titanium by the Jones Reductor
Method
Reagents
• Sulfuric Acid (sp gr 1.84) - Concentrated sulfuric acid (H2SO4)
• Sulfuric Acid (1+1) - Carefully mix 1 volume of H2SO4 (sp gr
1.84) into 1 volume of water with rapid stirring.
• Sulfuric Acid (1+19)—Carefully mix 1 volume of H2SO4 into 19
volumes of water with rapid stirring.
 ASTM D1394 - Total Titanium by the Jones Reductor
Method
Determine the dry Weight to 0.1 mg Dry the specimen in
weight of a 300 to 350 mg of the opened
weighing bottle and the sample to be weighing bottle for
cap to 0.1 mg analyzed into the 2 hours at 105 to
weighing bottle 110°C

Cool in a desiccator, Calculate the dry

cap the bottle, and weight of the
weigh as rapidly as specimen and use in Next Slide
possible the actual
calculation
 ASTM D1394 - Total Titanium by the Jones Reductor
Method
Transfer the dried
specimen to a dry add 20 mL of H2SO4 Mix well and heat on a
hot plate until dense
250 mL chemical and (sp gr 1.84) and 7 to white fumes are
heat-resistant glass 8 g of (NH4)2SO4 evolved
beaker

Continue the heating over a strong flame until

solution is complete (usually requires not over 5 min
of boiling) or it is apparent that the residue is Next Slide
composed of SiO2 or siliceous matter. Caution should
be observed in visually examining this hot solution
 ASTM D1394 - Total Titanium by the Jones Reductor
Method
Cool the solution, dilute with 100 mL of water, Wash the insoluble
stir, heat carefully to boiling while stirring, let residue with cold
settle, filter through paper, and transfer the H2SO4 (1+19) until
precipitate completely to the paper titanium is removed

Dilute the filtrate to 200 Wash out the Jones

mL and add about 5 mL reductor with H2SO4
of NH4OH to lower the (1+19) and water, leaving
acidity to sufficient water in the Next Slide
approximately 10-15% reductor to fill to the
H2SO4 (by volume) upper level of the zinc
 ASTM D1394 - Total Titanium by the Jones Reductor
Method
These washings should Run 50 mL of H2SO4
Empty the receiver, (1+19) through the
require not more than and put in it 25 mL reductor at such a
1 or 2 drops of 0.1 N
KMnO4 solution to of ferric sulfate uniform rate as to
solution require 5 to 10 min for
obtain a pink color. passage

Follow this with the

titanium solution at
such a uniform rate as Wash out with 100 Next Slide
to require 10 min to mL of H2SO4 (1+19).
pass through the
reductor.
ASTM D1394 - Total Titanium by the Jones Reductor
Method
Run through about 100 Gradually release the
mL of water. Take care suction. Wash
that the reductor is thoroughly the glass
always filled with tube that was
solution or water to the immersed in the ferric
upper level of the zinc. sulfate solution

Remove the receiver, Run a blank

and titrate determination, using the
same reagents and
immediately with 0.1 redactor washing
N KMnO4 solution procedure
 ASTM D1394 - Total Titanium by the Jones Reductor
Method
Calculations

• TiO2, % =

• V1 = KMnO4 solution required for titration of specimen, mL

• B = KMnO4 solution required for titration of the blank, mL
• T = TiO2 equivalent of the KMnO4 solution, g/mL, and
• S = dried specimen, g.
 ASTM D4764 - % TiO2 by X-Ray Fluorescence
Spectroscopy Method
Appartus
• X-ray Fluorescence Spectrometer, suitable for measurement of
the baseline corrected intensity of the Kα lines of titanium and
of bromine. For spectrometers equipped with a tungsten or
chromium target and a lithium fluoride (200) analyzing crystal,
these lines are observed at 2θ angles of 86.09° and 29.97°,
respectively
• Paint Shaker
 ASTM D4764 - % TiO2 by X-Ray Fluorescence
Spectroscopy Method
Appartus
• Film Applicator, to produce a 75-μm (3-mil) wet film thickness
• Plastic Sheet,4with no interfering X-ray fluorescence peaks and
not attacked by paint solvent
• Perforated Suction Plate, or other flat surface
• Vials and caps, 20 mL
 ASTM D4764 - % TiO2 by X-Ray Fluorescence
Spectroscopy Method
Reagents
• ASTM D1193 Type II water
• 2-ethoxyethanol, purified grade.
• Tetraethylammonium Bromide, internal standard solution - Into a 100-mL
volumetric flask weigh approximately 10.80 g of tetraethylammonium
bromide (TEAB) to 1 mg. Dissolve the TEAB in 2-ethoxyethanol, fill the
flask to the mark with 2-ethoxyethanol, and mix thoroughly. (TEAB
dissolved in 2-ethoxyethanol can be used as an internal standard for both
water-reducible and solvent-reducible paint. However, water may be
substituted for 2-ethoxyethanol, if only water reducible paint is to be
analyzed.)
 ASTM D4764 - % TiO2 by X-Ray Fluorescence
Spectroscopy Method
Turn on the
spectrometer and Select spectrometer settings to permit
allow it to stabilize measurement of the intensity of the Kα peaks
thoroughly before of titanium & bromine (Check manufacturer’s
beginning collection instruction manual)
of results

Place the disk in the

specimen holder such
that the coated side of Refer to XRF Equipment
the sheet is turned Manual for Sample Next Slide
toward the incident X- preparation options
rays
 ASTM D4764 - % TiO2 by X-Ray Fluorescence
Spectroscopy Method
Record the background Check the spectra for the presence of
spectrum in the ranges of interfering peaks and select for each
the Kα peaks of titanium peak an angle for background
& bromine, including at measurement where interference is at a
least 10° on each side minimum

At the selected angles measure Determine the net

the background intensities and intensity, c/s, of each
the intensities of the Kα peaks peak by subtracting
of titanium and bromine in the background count
counts per second (c/s) from the peak count.
 ASTM D4764 - % TiO2 by X-Ray Fluorescence
Spectroscopy Method
Calculations
• Use the values of the standard paint of known TiO2 content to
calculate Kt, the reference intensity ratio of titanium relative to
bromine in the film, defined as:

• Kt = X = X
 ASTM D4764 - % TiO2 by X-Ray Fluorescence
Spectroscopy Method
Calculations
• = TEAB used in making film, g,
= TEAB used, g, × 2 mL⁄100 mL = TEAB used, g, × 1⁄50
• = TiO2 in film, g,
= paint used, g, × (%TiO2 in dry paint/100) × %nonvolatile matter/100,
= paint used, g, × % TiO2 in liquid paint/100,
= paint used, g, × weight fraction of TiO2 in liquid paint,
• = nonvolatile matter (from paint) in film, g,
= paint used, g, × % nonvolatile matter/100,
= paint used, g, × % weight fraction of nonvolatile matter,
• b = intensity of bromine peak, c/s, and
• t = intensity of titanium peak, c/s.
 ASTM D4764 - X-Ray Fluorescence Spectroscopy
Method
Calculations

• Kt = X X

• = paint used, g, and

• = weight fraction of TiO2 in liquid paint
• Calculate the mean of the Kt values obtained from the two
disks coated with the standard paint and use in the next
calculation
 ASTM D4764 - X-Ray Fluorescence Spectroscopy
Method
Calculations

• % TiO2 =
 Composition - Filler - Calcium carbonate and inert
fillers
• ASTM D4797 - Standard Test Methods for Gravimetric Analysis of White
and Yellow Thermoplastic Pavement Marking
• ash, n - the inorganic components of thermoplastic traffic marking including
the pigment, glass spheres, and filler.
• Calcium carbonate and inert fillersmax= 42.0 (only for white) (D.O. No. 103,
Series of 2013)
• Only for White thermoplastic paint
• For yellow thermoplastic paint - Amount of Yellow Pigment, calcium
carbonate, and inert fillers shall be at the option of the manufacturer,
providing all other requirements of AASHTO M 249-12 are met.
 ASTM D4797 - Calcium Carbonate and Inert Fillers
Composition
Calculations
• Ash = pigment, glass spheres, and filler
• Then, filler = ash – ( pigment + glass spheres)
• Pigment = % TiO2
• Glass spheres = % Glass Beads
• Ash = weight of ash after ignition at 540°C from the analysis
of glass beads or TiO2
Composition - Color - Daylight reflectance @ 45° - 0°

• Daylight reflectance @ 45° - 0°min= 75% for white, 45%

for yellow (D.O. No. 103, Series of 2013)
• To determine the settings that need to be entered in the
spectrophotometer or spectrocolorimeter, we refer to
AASHTO T 249 Section 4.3.1 - Color
Composition - Color - Daylight reflectance @ 45° - 0°
• White: Daytime Luminance factor, Y (%) at 45°/0° - geometry
and illuminant D65 using the 1931 CIE 2° standard observer
≥75. For highway use, the color shall match Federal Test
Standard No. 595b, Color 17886.
• Yellow: Daytime Luminance factor, Y (%) at 45°/0° - geometry
and illuminant D65 using the 1931 CIE 2° standard observer
≥45. For highway use, the color shall match Federal Test
Standard No. 595b - Color 13538.
Composition - Color - Daylight reflectance @ 45° - 0°

• AASHTO T 250 Section 8 - Reflectance, Color and

Yellowness Index
• ASTM D4960 - Standard Test Method for Evaluation of
Color for Thermoplastic Traffic Marking Materials
• ASTM E1349 - Standard Test Method for Reflectance
Factor and Color by Spectrophotometry Using
Bidirectional (45°:0° or 0°:45°) Geometry
 ASTM D4960 & E1349 - Daylight reflectance @ 45° - 0°
Make a test specimen Pour into a clean,
from the molten Allow to cool to room
thermoplastic after non-stick pan, to form temperature for at least
heating for 240 ± 5 an approximately 8- 30 minutes to negate
cm (3-in.) diameter the initial effects of
minutes (AASHTO disk thermochromism
M250 Section 8)

Select the largest

port available for Next Slide
spectrophotometer or
spectrocolorimeter
 ASTM D4960 & E1349 - Daylight reflectance @ 45° - 0°
Standardize or verify the calibration of the Adjust the settings to show
“zero setting of the reflectance scale”, detect Daytime Luminance
“wavelength scale” and “stray-light level”. factor, Y (%) at 45°/0° -
Refer to the specific spectrophotometer or geometry and illuminant D65
spectrocolorimeter instruction manual for the using the 1931 CIE 2°
method of standardization or verification. standard observer

Remove the patty from Take three more

readings without record the average
the non-stick pan and of 4 readings with a
read the color removing the patty
measurement values from the sample port 90 degree rotation
from the flat smooth between each
rotating it 90° reading
side between readings
 Drying time

• ASTM M 249 Section 4.3.2 - Drying Time

• Drying timemax= 2.0 minutes at 10 ± 2 °C or 10.0
minutes at 32 ± 2 °C (D.O. No. 103, Series of 2013)
 ASTM M 249 Section 4.3.2 - Drying Time

• When applied at a temperature range of 211 ± 7°C

and thickness of 3.2 to 4.8 mm (125 to 188 mils), the
material shall set to bear traffic in not more than 2 min
when the air temperature is 10 ± 2°C and not more than
10 min when the air temperature is 32 ± 2°C
 ASTM M 249 Section 4.3.2 - Drying Time

• When applied at a temperature range of 211 ± 7°C

(412.5 ± 12.5°F) and thickness of 3.2 to 4.8 mm (125 to
188 mils), the material shall set to bear traffic in not more
than 2 min when the air temperature is 10 ± 2°C (50 ±
3°F) and not more than 10 min when the air temperature
is 32 ± 2°C (90 ± 3°F).
 Composition - Cracking Resistance @ Low
Temperature
• AASHTO T 250 Section 12 - Low Temperature Stress
Resistance
• Cracking Resistance @ Low Temperature = no cracks
(D.O. No. 103, Series of 2013)
 AASHTO T 250 Section 12 - Cracking Resistance @
Low Temperature
Apparatus
• Concrete blocks, 305 by 305 by 76 mm (12 by 12 by 3 in.), primed
with primer recommended for use by the thermoplastic manufacturer
• 1.9-L (0.5-gal) cans with rims removed.
• Spatula.
• Drawdown blade, 10 cm (4 in.) by 125 mL.
• Cold box or freezer, capable of maintaining a temperature of –9.4
± 2.0°C for 24 h.
 AASHTO T 250 Section 12 - Cracking Resistance @
Low Temperature
Heat the drawdown blade at Take sample from the
218°C for one-half hour (Start molten thermoplastic
heating the drawdown blade after after heating for 240 ±
heating the molten thermoplastic 5 minutes (AASHTO T
for 210 minutes or 3.5 hours) 250 Section 12)

Pour the Draw down a 10-cm

thermoplastic into (4-in.) wide line on Next Slide
the heated the concrete block at
drawdown blade room temperature.
AASHTO T 250 Section 12 - Cracking Resistance @
Low Temperature
When the test At the end of 24 h,
specimen has cooled to remove and
room temperature,
place it in the cold box immediately inspect
or freezer for 24 h at the specimen for
-9.4 ± 2.0°C cracking

Inspect the specimen

from a distance of Any cracking shall
305 mm (12 in.) constitute failure
under diffuse of the test
lighting.
 Composition - Impact Resistance

• AASHTO T 250 Section 14 - Impact Resistance

• ASTM D256, Method A - Standard Test Methods for
Determining the Izod Pendulum Impact Resistance of
Plastics - Cantilever Beam Test
• Impact Resistancemin= 115.0 mm•kg (D.O. No. 103, Series
of 2013)
 AASHTO T 250 Section 14 - Impact Resistance
Apparatus and Materials
• Molds, 25 by 25 by 150 mm (1 by 1 by 6 in.), for casting
impact specimens.
• Izod-type impact test apparatus with 0 to 2.82 J (0 to 25
in.-lb) scale.
 AASHTO T 250 Section 14 - Impact Resistance
Preheat the specimen molds for Take sample from the molten
approximately 1 h at 218°C (Start thermoplastic after heating for
heating the drawdown blade after 4 hours (AASHTO M 250
heating the molten thermoplastic for Section 14) and quickly fill the
180 minutes or 3 hours) heated molds

After cooling, Cut each sample

carefully disassemble into
the molds and approximately Next Slide
remove the solidified 76-mm (3-in.)
material long sections
 AASHTO T 250 Section 14 - Impact Resistance
At least 2 or more Estimate the
individual determinations of breaking energy for
impact resistance must be the specimen and
made on each sample to be select a pendulum of
tested suitable energy

Use the lightest standard Follow the

pendulum that is expected to manufacturer’s
break each specimen in the instructions to Next Slide
group with a loss of not more correct for windage
than 85 % of its energy and friction
 AASHTO T 250 Section 14 - Impact Resistance
If excessive friction Measure and Position the specimen
is indicated, the record the precisely so that it is
machine shall be dimensions of the rigidly, but not too
adjusted before molded sample tightly, clamped in the
starting a test vise

Pay special attention Release the Subtract the windage &

to ensure that the pendulum. Record friction correction from the
“impacted end” of the indicated indicated breaking
the specimen is breaking energy & energy, unless determined
projecting above the appearance of the automatically by the
vise. broken specimen system
 Composition - Softening Point

• AASHTO M249 Section 4.3.5 - Softening Point

• ASTM D36 - Standard Test Method for Softening Point of
Bitumen (Ring-and-Ball Apparatus)
• Softening Point = 102.5 ± 9.5°C (D.O. No. 103, Series
of 2013)
 ASTM D36 - Softening Point
Apparatus
• Rings - Two square-shouldered brass rings conforming to the
dimensions requirements of ASTM D36 Figure 1(a)
• Pouring Plate - A flat, smooth, brass plate approximately 50 by 75
mm [2 by 3 in.]
• Balls - Two steel balls, 9.5 mm [⅜ in.] in diameter, each having a
mass of 3.50 ± 0.05 g
• Ball-Centering Guides - Two brass guides for centering the steel
balls, one for each ring, conforming to the general shape and
dimensions of ASTM D36 Figure 1 (b)
 ASTM D36 - Softening Point
Apparatus
• Bath - A glass vessel, capable of being heated, not less than 85 mm in
inside diameter and not less than 120 mm in depth from the bottom of
the flare. (An 800-mL, low-form Griffin beaker of heat-resistant glass
meets this requirement)
• Ring Holder and Assembly - A brass holder designed to support the two
rings in a horizontal position, conforming to the shape and dimensions of
ASTM D36 Figure 1 (c), supported in the assembly illustrated in ASTM
D36 Figure 1 (d). The bottom of the shouldered rings in the ring holder
shall be 25 mm [1.0 in.] above the upper surface of the bottom plate,
and the lower surface of the bottom plate shall be 16 ± 3 mm [⅝ ± ⅛
in.] from the bottom of the bath.
 ASTM D36 - Softening Point
Apparatus and Reagents
• ASTM High Softening Point Thermometer - range from 30 to 200°C, and
conforming to ASTM E1 - Thermometer 16C; or any other thermometric
device of at least equal accuracy, capable of indicating temperature to
within 1°C and stable to within 1°C for the duration of the exposure.
• USP Glycerin (do not use water as the expected Softening Point is 102.5
± 9.5°C based on the specifications of D.O. No. 103, Series of 2013
which is way above the 80°C maximum to use water)
• Release agent - silicone oil or grease, a mixture of glycerin and dextrin,
talc, or china clay
 ASTM D36 - Softening Point

Take sample from the Assemble the apparatus in the laboratory hood with
molten thermoplastic the specimen rings, ball-centering guides, and
after heating for 240 thermometer in position, and fill the bath so that the
± 5 minutes (AASHTO liquid depth will be 105 ± 3 mm [4⅛ ± ⅛ in.] with
M249 Section 4.3.5) the apparatus in place.

Using forceps, place the two steel balls in the

bottom of the bath for at least 5 min so they will Next Slide
reach the same starting temperature as the rest
of the assembly.
 ASTM D36 - Softening Point
Place the bath in ice water, if necessary, or Again using forceps,
gently heat to establish and maintain the place a ball from
proper starting bath temperature for 15 min the bottom of the
with the apparatus in place. Take care not to bath in each ball-
contaminate the bath liquid. centering guide.

Heat the bath from

below so that the Protect the bath from
temperature indicated
by the thermometer drafts, using shields if Next Slide
rises at a uniform rate necessary.
of 5°C/min
 ASTM D36 - Softening Point
The maximum Reject any test in Record for each ring and ball
permissible which the rate of the temperature indicated by
variation for any 1- temperature rise the thermometer at the instant
min period after does not fall
the thermoplastic surrounding
the first 3 min shall the ball touches the bottom
be ± 0.5°C within these limits plate

Make no correction If the difference Report to the nearest

for the emergent between the two 0.5°C the mean of the
stem of the temperatures exceeds temperatures recorded
thermometer 1°C, repeat the test as the softening point
 Composition - Flowability

• AASHTO T 250 Section 11 - Flowability (Percent Residue)

• Flowabilitymax = 18% (White), 21% (Yellow) (D.O. No.
103, Series of 2013)
 AASHTO T 250 Section 11 - Flowability (Percent
Residue)
Apparatus and Materials
• Round, unlined steel 475-mL (1-pt) can with rim removed from the
inside
• Balance - 0.01 g readability and sensitivity, 0.02 g accuracy
• Holder for cans, allowing suspension of cans at a 45° angle with
point contact.
• Electric hotplate, capable of heating material to 218°C
• Glass stem thermometer -max temperature range of at least 218°C
 AASHTO T 250 Section 11 - Flowability (Percent
Residue)
Take weigh 400.0 ±
0.1 g from the molten Place the sample onto a
thermoplastic after Place in tared 475- hotplate that has been
heating for 240 ± 5 mL can set on the maximum
minutes (AASHTO temperature setting
M249 Section 11.2.1)

Stir using a glass stem

thermometer until the Avoid splashing
material reaches a material on the inside Next Slide
temperature of 218 ± of the can
1°C
 AASHTO T 250 Section 11 - Flowability (Percent
Residue)
Remove the can from Immediately suspend Allow the material to
the hotplate and the can at a 45- flow over the rim where
scrape the material degree angle in a the thermometer was
from the thermometer holder with point scraped until flow
on the rim of the can contact ceases

Record the mass of

Calculate the
each can plus residue flowability (percent
residue)
 Flowability (Percent Residue)
Calculation
Flowability (Percent Residue) = (A x B) x 100
400

A = mass of can plus residue

B = mass of can