Designation: D3800M 11

Standard Test Method for

Density of High-Modulus Fibers1
This standard is issued under the fixed designation D3800M; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon () indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the U.S. Department of Defense.

1. Scope E177 Practice for Use of the Terms Precision and Bias in
1.1 This test method covers the determination of the density ASTM Test Methods
of high-modulus fibers and is applicable to both continuous and
discontinuous fibers. 3. Terminology
1.2 The values stated in SI units are to be regarded as 3.1 DefinitionsTerminology D3878 defines terms relating
standard. No other units of measurement are included in this to composite materials. Terminology E12 defines terms relating
standard. to density. Practice E177 defines terms relating to statistics. In
the event of a conflict between terms, Terminology D3878 shall
1.3 This standard may involve hazardous materials,
have precedence over other standards.
operations, and equipment. This standard does not purport to
address all of the safety concerns, if any, associated with its 3.2 Symbols:
use. It is the responsibility of the user of this standard to 3.2.1 sdensity of standard
establish appropriate safety and health practices and deter- 3.2.2 ldensity of liquid
mine the applicability of regulatory limitations prior to use. 3.2.3 fdensity of fiber
See Section 9 for additional information.
3.2.4 mfdensity of the measured fiber containing sizing
2. Referenced Documents 3.2.5 mldensity of the measured liquid containing surfac-
2.1 ASTM Standards:2 tant
D891 Test Methods for Specific Gravity, Apparent, of Liquid 3.2.6 surdensity of surfactant
Industrial Chemicals 3.2.7 szdensity of sizing
D1505 Test Method for Density of Plastics by the Density- 3.2.8 wdensity of water
Gradient Technique
D3878 Terminology for Composite Materials 3.2.9 sstandard deviation
D5229/D5229M Test Method for Moisture Absorption Prop- 3.2.10 M1weight of suspension wire in air
erties and Equilibrium Conditioning of Polymer Matrix 3.2.11 M2weight of suspension wire in liquid (to immer-
Composite Materials sion point)
D6308 Guide for Identification of Composite Materials in
3.2.12 M3weight of suspension wire plus item whose
Computerized Material Property Databases (Withdrawn
density is to be determined (in air)
1999)3
E12 Terminology Relating to Density and Specific Gravity 3.2.13 M4weight of suspension wire plus item whose
of Solids, Liquids, and Gases (Withdrawn 1996)3 density is to be determined (in liquid)
3.2.14 M3 M1weight of item for density to be deter-
mined in air
1
This test method is under the jurisdiction of ASTM Committee D30 on 3.2.15 M4 M2weight of item for density to be deter-
Composite Materials and is the direct responsibility of Subcommittee D30.03 on
Constituent/Precursor Properties.
mined in liquid
Current edition approved Aug. 1, 2011. Published September 2011. Originally
approved in 1979. Last previous edition approved in 2010 as D3800 99 (2010). 4. Summary of Test Method
DOI: 10.1520/D3800M-11.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 4.1 Procedure ABuoyancy (Archimedes) Method:
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM 4.1.1 The sample is weighed in air and weighed in a liquid
Standards volume information, refer to the standards Document Summary page on
that will thoroughly wet the sample and is of a lower density.
the ASTM website.
3
The last approved version of this historical standard is referenced on 4.1.2 The difference in weight of the sample in the two
www.astm.org. media is the buoyancy force. This force is converted to sample

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 D3800M 11
volume by dividing it by the liquid density. The sample weight 6.1.5 Effect of Surfactant DensityThe addition of a sur-
in air divided by the sample volume equals the sample density. factant to a liquid may produce bias if not considered. The
effect may be shown by the following equation:
4.2 Procedure BSink-Float Technique:
4.2.1 The sample is placed in a container containing a liquid ~ 100 2 x ! l 1x ~ sur!
ml 5 (2)
that will thoroughly wet the sample and is of a lower density. 100
A liquid of higher density than the sample and miscible with where
the first liquid is then added slowly to the container under
x = mass of surfactant as a percentage of total mass of the
constant gentle mixing until the sample is suspended in the
measured liquid.
mixture.
4.2.2 The density of the resulting mixed liquid is deter- 6.2 (Method A):
mined using either a hydrometer or a pycnometer. The density 6.2.1 Immersion PointThe distance the sample is lowered
of the sample is equal to the density of the liquid in which the into the liquid and the overall liquid level should be the same
sample is suspended. throughout determinations for Procedure A. This may be done
by putting a line for the desired liquid level on the outside of
4.3 Procedure CFor an alternative method, which may be the container. The sample size should be within a few grams
used, see Test Method D1505. from one sample to another.

5. Significance and Use 7. Apparatus

5.1 Fiber density is useful in the evaluation of new materials 7.1 General:
at the research and development level and is one of the material 7.1.1 Thermometer, capable of reading the test temperature
properties normally given in fiber specifications. during the test to 0.1C.
7.1.2 AgitatorStirrer or mixing propeller capable of
5.2 Fiber density is used to determine fiber strength and slowly agitating solution without test interference.
modulus both of a fiber bundle and an individual filament.
These properties are based on load or modulus slope over an 7.2 Procedure A:
effective area. Fiber density may be used with lineal mass of 7.2.1 Balance, analytical, capable of weighing to 0.0001 g,
the fiber to give an approximation of effective tow area. Tow adapted for suspension weighing.
area divided by the average number of filaments in a tow gives 7.2.2 Balance Stand, depending on the type of balance used;
an approximation of the effective area of an individual fila- two recommended stands are shown in Figs. 1 and 2.
ment. 7.2.3 Laboratory Jack, heavy-duty precision.
7.2.4 Suspension Wire, nickel or stainless steel, approxi-
5.3 Fiber density is used as a constituent property when mately 0.4 mm in diameter, cut and shaped to match the system
determining reinforcement volume and void volume based on used.
reinforcement mass and laminate density. 7.2.5 Vacuum Desiccator (with Pump)An airtight con-
tainer in which a low vacuum (less than 75 kPa [560 Torr]) can
6. Interferences be maintained.
6.1 General (All Methods): 7.2.6 Density StandardA solid piece of borosilicate glass
6.1.1 TemperatureThe temperature of the liquid shall (density approximately 2.2 g/mL) of known density to four
remain constant within a tolerance of 61C, since liquid significant figures as determined by water immersion.4 A NIST
density changes with temperature. standard of this type (SRM 1825) is recommended.
7.2.7 Vacuum Pump or Aspirator, used to provide vacuum-
6.1.2 Sample Wetting (Entrapped Air)Since this test
to-vacuum desiccator.
method is very dependent on buoyancy, any entrapped air in
7.2.8 Container, glass or other transparent container resis-
the sample will change the measured density and not give a
tant to a liquid medium is recommended.
true material density. Ensure visually that the sample does not
7.2.9 Immersion LiquidThe liquid used shall not dissolve
contain entrapped air bubbles.
or otherwise affect the specimen, but should wet it and have a
6.1.3 Homogenous MixtureThe density of the liquid shall
specific gravity less than that of the specimen.5 The specific
be uniform, through suitable agitation.
gravity of the immersion liquid shall be determined shortly
6.1.4 Removal of SizingA bias will exist if sizing is not before and after each use.
removed. In this case, the measured fiber density is a combi-
nation of the density of the fiber and the sizing. The following 7.3 Procedure B:
equation may be used to calculate the effect of the sizing on the 7.3.1 Container, glass or other transparent container resis-
density of the material. tant to liquids used is recommended.
7.3.2 Immersion LiquidsSee Notes 1 and 2. One liquid
~ 100 2 x ! f 1x ~ sz! should have a density less than the fiber, and the other greater,
mf 5 (1)
100

where 4
A No. 19 Pyrex glass stopper with a 3.175-mm diameter hole bored through
x = mass of sizing as a percentage of the total mass of the the top for suspension purposes has proved satisfactory.
5
One suitable surfactant to use with water is Triton X manufactured by Rohm
measured fiber.
and Haas, Philadelphia, PA.

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 D3800M 11

FIG. 1 Density Apparatus (Alternative)

so when mixed they have the same density as the fiber. Two Place the cap over the side arm, wipe the outside carefully, and weigh the
suitable liquids are trichloroethylene and dibromomethane filled bottle again to the nearest 0.2 mg. Empty the pycnometer, dry, and
then fill and weigh with the other liquid in the same manner as was done
(having densities of 1.464 and 2.477 g/mL). Both of these with the water. Calculate the specific gravity at 23C of the liquid, f , as
liquids pose hazards (see Section 8). follows:
7.3.3 Hydrometer, capable of reading liquid density.
l 5 ~b 2 e!/~w 2 e! (3)
7.4 Procedure CUse the apparatus described in Test
Method D1505. where:
e = apparent weight of empty pycnometer,
NOTE 1Standard deionized or distilled water need not be measured, w = apparent weight of pycnometer filled with water at 23C, and
but can be taken as a value from standard tables.6 For the determination b = apparent weight of pycnometer filled with liquid at 23C.
of the specific gravity of the liquid, the use of a standard plummet of If a constant-temperature bath is available, a pycnometer without a
known volume (Note 3) or Test Method A, C, or D of Test Methods D891, thermometer may be used.
using the modifications required to give specific gravity at 23C is NOTE 2One standard, which has been found satisfactory for this
recommended. One suggested procedure is the following: If a constant purpose, is the Reimann Thermometer Plummet. These are normally
temperature water bath is not available, determine the weight of the clean, calibrated for measurements at temperatures other than 23/23C, so that
dry pycnometer with the thermometer to the nearest 0.1 mg on an recalibration is necessary for the purpose of these test methods. Calibra-
analytical balance. Fill the pycnometer with water cooler than 23C. Insert tions at intervals of one week are recommended.
the thermometer stopper causing excess water to be expelled through the
side arm. Permit the filled bottle to warm in air until the thermometer
reads 23C. Remove the drop of water at the tip of the side arm with a bit 8. Reagents
of filter paper, taking care not to draw any liquid from within the capillary. 8.1 Purity of ReagentsAs a minimum, a technical grade
reagent is required to provide accurate results. However, when
6
One such reference is in CRC Handbook of Chemistry and Physics, CRC Press resolving disputes or performing subsequent analysis of extract
Inc., Boca Raton, FL. or residue, a reagent grade reagent shall be used. Unless

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 D3800M 11

FIG. 2 Density Apparatus (Alternative)

otherwise indicated, it is intended that the reagents conform to 9. Hazards

the specifications of the Committee on Analytical Reagents of 9.1 This test method should be used only by laboratory
the American Chemical Society where such specifications are workers with general training in the safe handling of chemi-
available.7 cals. A source of useful information is Prudent Practices in the
8.1.1 Water, H2O, (deionized or distilled and degassed), may Laboratory: Handling and Disposal of Chemicals, National
contain a wetting agent such as glycerin or surfactant. This is Academy Press, 1995, 448 pp., ISBN 0-309-05229-7.
the safest reagent found, and recommended for Procedure A. (WarningIn addition to other warnings, consult the appro-
NOTE 3Reagents in 8.1.2 8.1.6 should be used if water is found to priate material safety data sheet for each material used,
be unsatisfactory to accurately determine the density of the fiber. Other including reagent materials and test specimen materials, for
reagents are listed in order of known hazard or toxicity. specific recommendations on safety and handling.)
8.1.2 Acetone (2-Propanone), CH3CHOCH3.
8.1.3 Methanol (Methyl Alcohol), CH3OH. 10. Test Specimen
8.1.4 o-dichlorobenzene, CH 4 Cl 2 . (Warningo- 10.1 A minimum of three test specimens shall be tested for
dichlorobenzene has been identified as toxic and an irritant.) each sample.
8.1.5 Dibromomethane, CH2Br2. (WarningAs of the ap-
10.2 The test specimen weight shall be a minimum of 0.5 g.
proval date of this test method, dibromomethane was listed by
the International Agency for Research on Cancer in Group 2C 11. Calibration and Standardization
as toxic.)
11.1 All measuring equipment shall have certified calibra-
8.1.6 Trichloroethylene, CHClCCl2. (WarningAs of the
tions that are current at the time of use of the equipment. The
approval date of this test method, trichloroethylene was listed
calibration documentation shall be available for inspection.
by the International Agency for Research on Cancer in Group
2D as a cancer suspect agent and mutagen.) 12. Conditioning
12.1 Test Method D5229/D5229M may be used to deter-
7
mine equilibrium dryness of a fiber. In general, no special
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For Suggestions on the testing of reagents not conditioning is needed for carbon fiber, less than 1 h at 100C
listed by the American Chemical Society, see Annual Standards for Laboratory is needed for glass fibers, and approximately 4 h at 100C is
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia needed for aramid fibers.
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
MD. 12.2 Condition liquids to a test temperature, typically 23C.

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 D3800M 11
13. Procedure 13.2.4 Put the container with the sample and liquid into a
13.1 Procedure ABuoyancy (Archimedes) Method): vacuum desiccator and pull vacuum to approximately 10-mm
13.1.1 Equipment Assembly: Hg or until boiling of the solution begins. Hold vacuum for a
13.1.1.1 The assembly of the apparatus is shown in Fig. 1 or minimum of 2 min or until all trapped air on the fiber surface
Fig. 2. The balance stand must be firmly secured to a stable is removed.
surface with the balance resting on the stand directly over the 13.2.5 Remove the container from the vacuum desiccator
hole provided for the suspension system. Place the immersion and allow to equilibrate to room temperature. The sample
fluid container on the laboratory jack directly under the should be near the bottom of the container.
suspension hook. 13.2.6 Add small increments of the heavier liquid used to
13.1.1.2 To prevent stray air currents between the bottom of prepare the mixture in 8.2.1. After each addition, gently swirl
the balance and the top of the stand, it is advisable to shield this the contents of the container. Continue adding increments of
area. If excessive vibration is observed while weighing, vibra- the heavy liquid until the fiber sample is suspended at an
tion damping pads must be used. intermediate point.
13.1.2 Density Standard CalibrationFill the immersion 13.2.7 Wait 5 min. If the fiber sinks, repeat 13.2.6. If the
fluid container 34 to 78 full with freshly boiled water, which has fiber rises, repeat 13.2.6, but with a light liquid. If the fiber
reached equilibrium at room temperature. Place the container remains stationary proceed to 13.2.8.
on a collapsed laboratory jack and zero the balance. Attach the 13.2.8 Measure the density of the liquid with a hydrometer
suspension wire and weigh. Record as M1, g. Raise the that reads to the appropriate limits. For example, if the liquid
laboratory jack to the immersion point of the suspension wire has a density of 1.5 g/mL, use an hydrometer with a range from
and record the weight as M2, g. Rinse the wire with acetone and 1.4 to 1.6 g/mL. More accurate results can be obtained from
let air dry. Attach the wire plus glass standard and weigh. hydrometers having a narrow range. Read the hydrometer to
Record as M3, g. Again raise the jack to the immersion point two decimal places and interpolate the third decimal place. The
and weigh. Record as M4, g. Lower the jack, remove the hydrometer reading is the density of the fiber.
standard plus wire, and rinse them with acetone to dry.
Measure the temperature of the water to 0.1C and record the 14. Calculation (Procedure A)
water density at that temperature. 14.1 Density of Glass Standard, g/mL:
13.1.3 Immersion Fluid StandardizationFill the clean and
s 5 ~ M 3 2 M 1 ! w / ~~ M 3 2 M 1 ! 2 ~ M 4 2 M 2 !! (4)
dry fluid container 34 to 78 full with liquid (water with
surfactant, methanol, or 1,2 dichlorobenzene for example) and where: the liquid is water and the sample is the glass
allow to come to temperature equilibrium. Proceed by weigh- standard.
ing the suspension wire. Record as M1, g. Raise the laboratory The density of the standard should remain consistent to
jack to the immersion point of the suspension wire and record 60.0001 g/mL.
the weight as M2, g. Rinse the wire with acetone and let air dry.
14.2 Density of Immersion Liquid, g/mL:
Attach the wire plus glass standard and weigh. Record as M3,
g. Again raise the jack to the immersion point and weigh. l 5 s ~~ M 3 2 M 1 ! 2 ~ M 4 2 M 2 !! / ~ M 3 2 M 1 ! (5)
Record as M4, g. Remove wire and standard and rinse with where: the liquid is the test liquid and the sample is the glass
acetone. This step should be done at the beginning of each standard.
series of density determinations.
13.1.4 Yarn DensitySelect a suitable representative length 14.3 Density of Fiber Sample, g/mL:
of yarn, weighing at least 0.15 g. Wrap the sample (the end of f 5 ~ M 3 2 M 1 ! l / ~~ M 3 2 M 1 ! 2 ~ M 4 2 M 2 !! (6)
a small winding cone is suitable) and intertwine the ends of the
fiber tow or yarn to prevent unraveling. Proceed by weighing where: the liquid is the test liquid and the sample is the fiber.
the suspension wire. Record as M1, g. Raise the laboratory jack
to the immersion point of the suspension wire and record the 15. Report
weight as M2, g. Rinse the wire with acetone and let air dry. 15.1 Report the following information:
Attach the sample to the wire and weigh. Record as M3, g. 15.1.1 Reporting of items that are beyond the control of a
Remove the wire and soak in the liquid and vacuum degas. given test laboratory, such as material details shall be the
Reattach the sample and wire to the balance. Again raise the responsibility of the requestor.
jack to the immersion point and weigh. Record as M4, g. 15.1.2 Complete identification of the material in accordance
Remove wire and standard and rinse with acetone. with Guide D6308, including fiber type, surface treatment, and
13.2 Procedure BSink Float Technique: fiber manufacturer.
13.2.1 In a suitable container, prepare a mixture of two 15.1.3 This test method (D3800 and Procedures A through
miscible liquids that, when thoroughly mixed, will yield a C).
liquid with a density less than the density of the fiber to be 15.1.4 Complete test parameters including test temperature
tested. in degrees Celsius and immersion liquid(s) used.
13.2.2 Cut approximately 150 mm of material to be tested 15.1.5 Each measured density and average, g/mL. A mea-
and tie a loose overhand knot. sure of the degree of variation in the density such as standard
13.2.3 Put the sample into the solution prepared in 13.2.1. deviation.

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 D3800M 11
16. Precision and Bias 17. Keywords
16.1 PrecisionThe data required for the development of a 17.1 Archimedes method; buoyancy method; density; fiber
precision and bias statement is not available for this test density
method. Committee D30 is currently planning a round-robin
test for this test method to determine precision.

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