Viscosity Measurement

So Easy, Yet So Difficult

by Janet L. Lane and Kenneth O. Henderson

Viscosity is a measure of a fluid’s resistance to flow. It is one of the

most important properties of a fluid and plays a very prominent role in
the petroleum industry. The viscosity of a crude oil affects our ability to
pump it out of the ground; the viscosity and volatility of a fuel affect
how easy it is to atomize in the fuel injector; the viscosity of a lubricant
affects its ability to protect an engine. It is an important measurement
characteristic in the food, paint, polymer coating, and other industries
where flow is a critical product or use characteristic.

Small changes in viscosity can have a dramatic impact on the

properties of petroleum fluids. The criticality of kinematic viscosity
measurement prompted the petroleum industry to develop a very
precise method, first published in 1937, ASTM D 445, Test Method for
Kinematic Viscosity of Transparent and Opaque Liquids. The term
“kinematic” simply means that the measurement is made while fluid is
flowing under the force of gravity. It is determined by measuring the
time it takes for a volume of fluid to flow under gravity through a
calibrated glass capillary viscometer.

Although it sounds very simple, achieving the high accuracy and

precision required by the industry is an extremely formidable task.
There are many factors that affect the precision of this test method.

In economic terms, an error of 1 percent product viscosity that causes

a blend adjustment can easily result in increasing product cost by a
penny a gallon. For a large lubricant manufacturer, this can amount to
$1,000,000 in lost revenue per year. If this is a 10 percent reduction in
profits, then it is equivalent to throwing away 10 percent of your
paycheck.

Temperature

As the saying goes, “The most important factor affecting the value of a
home is location, location, location.” In terms of viscosity
measurements, “The most important factor affecting the quality of a
viscosity measurement is temperature, temperature, temperature.”

Temperature control is the single most important parameter for

obtaining accurate and precise kinematic viscosity measurements. This
is especially true for petroleum products as their rate of viscosity
change per unit temperature is significantly greater than other
products. Thus a slight variation in temperature can have a very large
effect on the viscosity of a fluid. The bath temperature for the most
common measurements, 40°C and 100°C, must be controlled to within
+/- 0.02°C. That is an extremely tight window and great care must be
taken to achieve this control.

There are a number of factors that impact the temperature:

• Use the specified thermometer or other temperature-sensing device

having the specified accuracy and meeting the test method
requirements. Reading a thermometer to 0.01°C accurately can be
extremely difficult, so the use of a magnifying lens is recommended.
The thermometer must be immersed in the bath at the correct depth. It
must be calibrated at least yearly to +/- 0.02°C. In addition, the
thermometer ice point should be determined every six months and the
correction factor applied. The procedure for calibrating thermometers is
quite involved and is described in ASTM E 77, Test Method for the
Inspection and Verification of Thermometers. Since temperature
control is such an important parameter, the use of two thermometers
per bath is recommended.
• Bath temperature uniformity and stability are other important
parameters. The entire length of the viscometer must be maintained at
the appropriate temperature. The type of circulator used, the age of the
bath fluid and the bath fluid viscosity impact temperature uniformity.
The circulator and the viscosity of the bath fluid need to be balanced to
provide a uniform temperature throughout the bath. The bath fluid
needs to be changed well before it begins to discolor, as the
discoloration usually indicates the fluid has oxidized and the viscosity
probably has increased. The bath should not be located near a draft,
such as in a fume hood, which usually causes excessive temperature
gradients in the bath. Temperature stability will be negatively impacted
if a second viscometer is added to the test bath during the same time
that another adjacent viscometer is being used for a measurement.
• There needs to be sufficient illumination of the sample in the tube
while in the bath to ensure consistent visual detection of the meniscus
crossing the timing lines. Care needs to be taken that this lighting
device does not affect the bath temperature control and stability.

These temperature requirements cannot be taken lightly since slight

variations in temperature can cause dramatic changes in viscosity for
certain types of petroleum products.

Viscometers

Fully annealed, low-expansion borosilicate glass shall be used for the

construction of all viscometers. There are a number of factors to
consider when choosing which viscometer size to use to analyze a
sample. First, the viscometer must be calibrated to calculate viscosity.
The procedure is described in ASTM D 446, Specification and
Operating Instructions for Glass Capillary Kinematic Viscometers.
Viscosity standards are used to determine the viscometer constant.
Although a single standard is sufficient to obtain a constant, the use of
two standards covering the capillary range yields a more robust
calibration constant. Viscosity standards have an expiration date and
should not be used beyond that date. Calibrated viscometers can be
purchased with constants at appropriate temperatures. Since the
viscometer constant varies as a function of temperature for certain
types of viscometers, it is important to calculate the viscometer
constant for the temperature at which the sample is being analyzed.
Viscometer constants should be verified at least yearly.

The size of the viscometer must be chosen such that the flow time is at
least 200 seconds for manual determinations, otherwise eye-hand
coordination will become a significant factor. The operator waits for the
meniscus of the fluid to pass the timing lines and uses a clock or
stopwatch to measure the flow time. Flow times over 200 seconds are
required to eliminate possible operator variation.

It is obvious that a clean viscosity tube must be used for the analysis,
but what is actually meant by “clean”? The tube must be free from dust
or other particles and the fluid should clearly wet the surface of the
glass. Typically, several rinsings with a sample solvent such as
naphtha, followed by a drying solvent such as acetone and then a
purging with a dry, dust-free gas such as air or nitrogen, is sufficient.
The solvents should be free of any particles, so filtering is required.
The solvents also must be residue-free on drying. This is of particular
concern if commercial or practical grade solvents are used.
The residue of previous samples coating the inside of the viscometer
can be removed with a chromic acid (1) cleaning solution or a
nonchromium- containing, strongly oxidizing cleaning solution. (2)
Never use an alkaline liquid detergent or any cleaning solution with a
pH above 8.0 because they will actually change the dimensions of the
capillary by dissolving the glass walls and thus change the calibration
constant. These types of liquids are often found throughout an
analytical laboratory and can be used in other applications, but if one is
used to clean a tube, the tube will need to be re-calibrated. Another
way to change the calibration constant of the smallest size viscometers
significantly is to soak the tube overnight in boiling water. The tube
might be clean but it needs to be re-calibrated before its next use.

The tube must also be dry before using. The use of dry, dust-free air or
nitrogen is recommended.

When suspended in the temperature bath, the tube should be in the

specified vertical position, free from vibration, and at the specified
immersion depth. Follow the manufacturer’s instructions and those in
the test method.

Timing Device

The timing device must have an accuracy of within +/- 0.07 percent of
the reading and must be capable of taking readings within a
discrimination of 1 part in 2000 or 0.1 seconds for a 200-second flow
time. Care must be taken when using electrical timing devices because
alternating currents may not provide the required
accuracy. Timing devices should be checked against a National
Institute of Standards and Technology (NIST) reference or other
accepted timing reference on a regular basis. Yearly verification is
recommended.

Sample Handling

Filter samples if there are any visible particles present. This is

especially important when analyzing used oils. The sample should be
free of air. Allow samples to sit to disperse the entrained air if present.
Just as caustic cleaning fluids will change the calibration constant, the
same is true for caustic (high pH) samples. As the sample pH goes up,
the change in the constant increases more rapidly. The smaller the
capillary, the faster the constant changes. The tube may need
recalibration after a caustic sample is analyzed, although very caustic
samples are not found very often in the petroleum industry.

Samples must be equilibrated at the desired test temperature. Up to 30

minutes may be necessary and possibly longer with some materials.
Make two measurements of flow time for each sample. If the two
determinations of kinematic viscosity, calculated from the flow time
measurements, agree within the stated determinability limit for the
sample type tested, then report the average of the two determinations.
If the two determinations do not agree to within the stated
determinability, then the measurements must be repeated after an
investigation and correction of the possible causes. A dirty viscometer,
or incorrect bath temperature or equilibration time are possible culprits.

Automated Viscometers

Automated viscometers have been used for the determination of

kinematic viscosity by D 445 in the petroleum industry for over 30
years. They mimic the physical conditions, operations or processes of
the manual apparatus and must meet the precision specified by the
method.

All but one of the requirements discussed above equally apply to

automated instruments. The flow-time requirement of greater than 200
seconds was at one time relaxed for automated instruments. The
ASTM subcommittee responsible for this test method, D02.07 on Flow
Properties, is currently determining the minimum allowable flow time for
these automated instruments. If indeed the flow time requirement is
relaxed, then two additional requirements will come into play. First, the
calculation of the kinematic viscosity from the tube constant and flow
time might require an additional term, the kinetic energy correction
factor. This factor takes into account the energy that is imparted to
speed up the fluid as it passes from the reservoir to the capillary. This
correction is negligible for longer flow times. Second, the timing device
will need to maintain the 1-part-in-2000 resolution and detection
sensitivity.
Quality Control

A quality control sample should be used routinely to monitor the

measurement system and verify that results are within the precision of
the test method. Any sample that is similar in composition to samples
typically analyzed should be used. For details on using a quality control
system, see ASTM D 6299, Standard Practice for Applying Statistical
Quality Assurance Techniques to Evaluate Analytical Measurement
System Performance.

Interlaboratory Crosscheck Programs

ASTM’s Interlaboratory Crosscheck Programs provide participating

laboratories with a statistical quality assurance tool, enabling them to
compare their performance in the use of ASTM methods against other
laboratories worldwide. The kinematic viscosity measurement by ASTM
D 445 is included in most of the programs. Over 700 laboratories
participated in the 2003 testing, including over 45 percent participation
by laboratories outside the United States.

D 445 Online Tutorial

ASTM International offers a comprehensive, Web-based training

resource providing instruction on ASTM standards and other related
technical information. D 445 is one of those standards. The course for
D 445, 30-45 minutes in length, is a step-by-step overview of the test
method and can be used to enhance your current training procedures.

Summary

The Test Method for Kinematic Viscosity of Transparent and Opaque

Liquids is one of the most critical tests in the petroleum industry. It has
been used since 1937, yet the method is continually being improved.
The technique appears to be quite simple, yet many factors can affect
the precision of the measurement. Meeting all the requirements for
performing the test method will allow laboratories to meet or exceed
the stated precision.

Notes
1 Chromic acid is a health hazard and must be handled with
precaution. It is toxic, a recognized carcinogen, highly corrosive, and
potentially hazardous when in contact with organic materials.
2 Nonchromium-containing, strongly oxidizing cleaning solutions are
also highly corrosive and potentially hazardous when in contact with
organic materials