Oil Viscosity - How It's Measured and Reported According to the Society of Tribologists and Lubrication Engineers (STLE),

viscosity is one of an oils most important physical properties. It is often one of the first parameters measured by most oil analysis labs because of its importance to oil condition and lubrication. But what do we really mean when we talk about an oils viscosity? A lubricating oils viscosity is typically measured and defined in two ways, either based on its kinematic viscosity or its absolute (dynamic) viscosity. While the descriptions may seem similar, there are important distinctions between the two. An oils kinematic viscosity is defined as its resistance to flow and shear due to gravity. Imagine filling a beaker with turbine oil and another with a thick gear oil. Which one will flow faster from the beaker if it is tipped on its side? The turbine oil will flow faster because the relative flow rates are governed by the oils kinematic viscosity. Now lets consider absolute viscosity. To measure absolute viscosity, insert a metal rod into the same two beakers. Use the rod to stir the oil, and then measure the force required to stir each oil at the same rate. The force required to stir the gear oil will be greater than the force required to stir the turbine oil. Based on this observation, it might be tempting to say that the gear oil requires more force to stir because it has a higher viscosity than the turbine oil. However, it is the oils resistance to flow and shear due to internal friction that is being measured in this example, so it is more correct to say that the gear oil has a higher absolute viscosity than the turbine oil because more force is required to stir the gear oil. For Newtonian fluids, absolute and kinematic viscosity are related by the oils specific gravity. However, for other oils, such as those containing polymeric viscosity index (VI) improvers, or heavily contaminated or degraded fluids, this relationship

does not hold true, and can lead to errors if we are not aware of the differences between absolute and kinematic viscosity. For a more detailed discussion on absolute versus kinematic viscosity, refer to the article Understanding Absolute and Kinematic Viscosity by Drew Troyer. Capillary Tube Viscometer Test Method The most common method of determining kinematic viscosity in the lab utilizes the capillary tube viscometer (Figure 1). In this method, the oil sample is placed into a glass capillary U-tube and the sample is drawn through the tube using suction until it reaches the start position indicated on the tubes side. The suction is then released, allowing the sample to flow back through the tube under gravity. The narrow capillary section of the tube controls the oils flow rate; more viscous grades of oil take longer Figure 1. Capillary Tube Viscometer

to flow than thinner grades of oil. This procedure is described in ASTM D445 and ISO 3104. Because the flow-rate is governed by resistance of the oil flowing under gravity through the capillary tube, this test actually measures an oils kinematic viscosity. The viscosity is typically reported in centistokes (cSt), equivalent to mm2/s in SI units, and is calculated from the time it takes oil to flow from the starting point to the stopping point using a calibration constant supplied for each tube. In most commercial oil analysis labs, the capillary tube viscometer method described in ASTM D445 (ISO 3104) is modified and automated using a number of commercially available automatic viscometers. When used correctly, these viscometers are capable of reproducing a similar level of accuracy produced by the capillary tube manual viscometer method.

Stating an oils viscosity is meaningless unless the temperature at which the viscosity was measured is defined. Typically, the viscosity is reported at one of two temperatures, either 40C (100F) or 100C (212F). For most industrial oils, it is common to measure kinematic viscosity at 40C because this is the basis for the ISO viscosity grading system (ISO 3448). Likewise, most engine oils are typically measured at 100C because the SAE engine oil classification system (SAE J300) is referenced to the kinematic viscosity at 100C (Table 1). Additionally, 100C reduces the rise of measurement interference for engine oil soot contamination.

Rotary Viscometer Test Method A less common method of determining an oils viscosity utilizes a rotary viscometer. In this test method, the oil is placed in a glass tube, housed in an insulated block at a fixed temperature (Figure 2). A metal spindle is then rotated in the oil at a fixed rpm, and the torque required to rotate the spindle is measured. Based on the internal resistance to rotation provided by the shear stress of the oil, the oils absolute viscosity can be determined. Figure 2. Rotary Viscometer ASTM D2983. While less common than kinematic viscosity, absolute viscosity and the Brookfield viscometer are used in formulating engine oils. For example, the W designation, which is used to denote oils that are suitable for use at colder temperatures, is based in part on the Brookfield viscosity at various temperatures (Table 2). Based on SAE J300, a multigrade engine oil that is designated as SAE 15W-40 must therefore conform to the kinematic viscosity limits at elevated temperatures according to Table 1 and the minimum requirements for cold cranking as shown in Table 2. Viscosity Index One other important property of an oil is viscosity index (VI). The viscosity index is a unitless number, used to indicate the temperature dependence of an oils kinematic viscosity. It is based on comparing the kinematic viscosity of the test oil at 40C, with the kinematic viscosity of two reference oils - one of which has a VI of 0, the other with a VI of 100 (Figure 3) - each having the same viscosity at 100C as the test oil. Absolute viscosity is reported in centipoise (cP), equivalent to mPas in SI units. This method is commonly referred to as the Brookfield method and is described in

Tables for calculating VI from the measured kinematic viscosity of an oil at 40C and 100C are referenced in ASTM D2270.

Figure 3. Determination of Viscosity Index (VI) Figure 3 shows that an oil that has a smaller change in kinematic viscosity with temperature will have a higher VI than an oil with a greater viscosity change across the same temperature range. For most paraffinic, solvent-refined mineral-based industrial oils, typical VIs fall in the range of 90 to 105. However, many highly refined mineral oils, synthetics and VI improved oils have VIs that will exceed 100. In fact, PAO-type synthetic oils typically have VIs in the range 130 to 150. Viscosity Monitoring and Trending Monitoring and trending viscosity is perhaps one of the most important components of any oil analysis program. Even small changes in viscosity can be magnified at operating temperatures to the extent that an oil is no longer able to provide adequate lubrication. Typical industrial oil limits are set at 5 percent for caution, and 10

percent for critical, although severe- duty applications and extremely critical systems should have even tighter targets. A significant reduction in viscosity can result in:

Loss of oil film causing excessive wear Increased mechanical friction causing excessive energy consumption n Heat generation due to mechanical friction n Internal or external leakage

Increased sensitivity to particle con- tamination due to reduced oil film Oil film failure at high temperatures, high loads or during start-ups or coastdowns.

Likewise, too high a viscosity can cause:

Excessive heat generation resulting in oil oxidation, sludge and varnish buildup

Gaseous cavitation due to inadequate oil flow to pumps and bearings Lubrication starvation due to inadequate oil flow Oil whip in journal bearings Excess energy consumption to over- come fluid friction Poor air detrainment or demulsibility Poor cold-start pumpability.

Whenever a significant change in viscosity is observed, the root cause of the problem should always be investigated and corrected. Changes in viscosity can be the result of a change in the base oil chemistry (a change in the oils molecular structure), or due to an ingressed contaminant (Table 3).

Viscosity changes may require additional tests, such as: acid number (AN) or Fourier transform infrared spectroscopy (FTIR), to confirm incipient oxidation; contaminant testing to identify signs of water, soot or glycol ingress; or other less commonly used tests, such as the ultracentrifuge test or gas chromatography (GC), to identify a change in the base oil chemistry. Viscosity is an important physical property that must be monitored and controlled carefully because of its impact on the oil and the oils impact on equipment life. Whether measuring viscosity onsite using one of many onsite oil analysis instruments capable of determining viscosity changes accurately, or whether sending samples routinely to an outside lab, it is important to learn how viscosity is determined, and how changes can impact equipment reliability. A proactive approach must be taken to determine the condition of the equipments lifeblood - the oil!

Many factors need to be considered when devising meaningful viscosity tests for adhesives and sealants.

Most people in the adhesives and sealants industry are aware of viscosity and realize that it characterizes the way a material will flow. More technically speaking, viscosity refers to a materials resistance to flow; it can be measured in various ways, depending on the nature of the application. An evaluation of how the material is being processed in manufacturing or how the end user will try to apply it is the basis for determining the type of viscosity test that should be performed.

Measuring Caulk Viscosity

Imagine a caulk gun. The squeezing force required to expel the material out of the nozzle is important to know. If the caulk is not sufficiently viscous, too much will come out and some will be wasted. In addition, the caulk that does come out probably wont hold its position on the substrate. Should the caulk be too viscous, it may not come out at all. In either case, the material is rejected and the customer is unhappy. Quality control (QC) in manufacturing requires that a test method be established to predict this type of problem before it happens. The way to simulate the guns squeezing action on the caulk is through an extrusion test. An instrument called a texture analyzerwith an extrusion cell-is ideally suited for this type of test. This type of instrument, also sometimes called a universal tester, essentially applies compression or tension to a material. In this case, the instrument simulates the process of pushing the material through a tube and out of the nozzle. During this type of test, the extrusion cell is filled with the sample material. A small circular opening in the bottom of the cell represents the nozzle diameter through which the caulk material will be expelled. A disc-shaped plunger is brought down into contact with the material in the top of the cell. The test method is to move the plunger at a defined speed down into the cell. The material is expelled out of the opening in the cell bottom. A load sensor in the instrument monitors the resistive force experienced by the plunger as it pushes downward into the material. The key data recorded is the force as a function of time and distance, which provides a complete characterization of the squeezing action required to extrude the caulk out of the gun. Technically speaking, this type of instrument is not a viscometer, but it nonetheless gives

a measure of the caulks viscosity. The output parameter is the force required to extrude the caulk. This correlates to how much work the user will perform to get the caulk out of the gun. It is crucial to select a test method that correctly characterizes what is happening to the material. Since many adhesive and sealant materials are applied from a gun of some type, the texture analyzer becomes a relevant tool to perform the tests.

Shear Rate
One key concept that is often not understood is that a materials viscosity is not a single point measurement; it typically depends on a number of factors. Take the previous example of the caulk. The speed at which the plunger pushes into the material will have a direct effect on the force resistance that is measured. The faster the plunger moves into the caulk, the higher the force that will be measured. Therefore, the rate of shearing action on the caulk is greater and may result in different viscosity values. The primary challenge to understanding viscosity is to recognize that shear rate plays a key role in determining the resistance to flow. As previously stated, it is necessary to think about how the material will be processed or handled when in use. The shearing action is what should be analyzed in order to arrive at a relevant test method for measuring viscosity. For liquid glues, the use of a rotational viscometer running at different speeds simulates what is happening to the material when stored in a bottle or applied to a substrate. The shearing action of the glue sloshing around in the bottle is relatively low, while the application process for placing the glue can be rather high. Once the glue is applied, the shearing action is again pretty low, because only gravity is causing it to spread out farther. This assessment of how the glue is used leads to the selection of the appropriate viscometer.

Dynamic Viscosity
Rotational viscometers are perhaps the most popular tool for measuring viscosity. The spindle, when inserted into the test material, rotates at various discrete speeds, thereby shearing the material at precise shear rates. The viscometer measures the amount of torque resistance imparted by the material against the rotating spindle at each speed. The torque measurement is quantified as the shear stress acting on that portion of the spindle surface that is immersed in the material. The measured parameter (torque) and the control parameter (spindle speed) are combined into an equation that defines dynamic viscosity as the ratio of shear stress to shear rate:

Dynamic Viscosity = Shear Stress Shear Rate Centipoise (cP) is the unit of measurement most often used in North and South America to quantify rotational viscosity; the milli-Pascal second (mPa.s) is typically used outside the Americas (1 cP = 1 mPa.s). This one-for-one equivalency minimizes potential problems when comparing data between multinational manufacturing plants. Distilled water is the benchmark reference for comparing the viscosity of all other materials. The National Institute of Standards and Technology (NIST) specifies that the viscosity of water is 1cP when measured with a capillary viscometer at 20

Shear Rate
The choice of shear rate is determined by analyzing how the material is processed. Imagine that the material is sandwiched between two plates separated by a fixed distance. If the bottom plate is kept stationary and the top plate moves at a defined velocity, then the shear rate is the ratio of the moving plate velocity (V) to the distance separating the plates (X):

Shear Rate = V X The reciprocal second (s-1) is the unit of measurement for shear rate. This approach to quantifying shear rate assumes that the fluid behaves in a uniform (laminar) way, as shown by the arrows in Figure 2. The layers of molecules in the material remain together in the same plane and slide over each other in such a way that the closer they are to the moving plate, the faster each layer moves. The relevant shear rate(s) for an application can easily be computed by applying the above equation. When placing adhesive on a substrate with a scraper, the substrate and the scraper represent the two plates. To lay down a bead of adhesive 1 mm thick in an automated operation where the substrate is moving at 50 cm/sec, the shear rate is 500 sec-1. This becomes one of the shear rates that should be used in a QC test.

Figure 3. Flow Curves for Viscosity vs. Shear Rate

Flow Behavior
With the above concept concerning relevant shear rates in mind, it is possible to see more clearly that viscosity may not be a single number for a given material. The idea is to test a material with a viscometer at different rotational speeds (i.e., different shear rates) and see what viscosity values are measured. The most common flow behavior is called pseudoplastic (or shear thinning), where a materials viscosity decreases with increasing shear rate. Figure 3 is a rheogram that illustrates the behavior for a liquid adhesive tested at relatively low shear rates. Most adhesive and sealant materials exhibit pseudoplastic behavior; for example, autobody fillers are highly viscous materials with obvious pseudoplastic flow. Figure 4 shows that the apparent viscosity decreases dramatically as the shear rate increases to 100 s-1, then decreases more gradually above that shear rate.

Figure 4. Viscosity vs. Shear Rate in an Autobody Filler

A related issue that affects measured viscosity values is the length of time the shearing action is applied to the material. When a material is sheared at a constant rate and the measured viscosity decreases with time, the flow behavior is called thixotropic. Many adhesive and sealant materials exhibit thixotropic behavior; it is important to consider whether the viscosity recovers to its original value once the shearing action stops, and whether this type of behavior is wanted or expected. Once the bead of glue has been placed on the substrate, does the viscosity recover so that the material holds its shape and doesnt spread out like water on a flat surface? Temperature is yet another parameter to consider when measuring viscosity. As temperature increases, most materials exhibit a decrease in viscosity. Therefore, the temperature at which the QC check is performed should be defined in order to ensure consistent results. When new adhesives or sealants are formulated, it is customary to perform a temperature profile test. The material is tested at a constant shear rate while the temperature cycles between a minimum and maximum value. The resulting graph provides QC with a reference chart for expected viscosity values at different temperatures.

Figure 5. Yield Stress Flow Curve for Floor Adhesive at Room Temperature

Yield Stress
Some users may wish to apply an adhesive to a particular area and have it stay put (hold its position) until pushed with a blade or trowel. Perhaps a second piece is then pressed into place on the adhesive layer. Flooring adhesive is an example of this type of application. The property corresponding to that behavior is called yield stress and it represents the amount of applied force at which a solid material begins to flow like a liquid. The yield strain is the degree of sample deformation that results from the applied yield stress. These two values appear on a stress-strain curve at the yield point. One easy method for testing the yield stress of adhesive/sealant materials is to use a rotational viscometer running at a very low speed (e.g., 0.01-1 rpm). The instrument uses a vane spindle immersed in the material and running at a constant speed. The calibrated spring inside the viscometer winds up, applying increasing force to the vane spindle, but the sample resists moving. The sample then begins to deform slightly, until its structure breaks down and it starts to flow. The measured torque value is converted into a stress value (in Pascals or dyne-cm), and this defines the yield stress for the material. Figure 5 shows the type of flow curves that can be generated when measuring yield stress with a viscometer. In this case, the instrument is specifically configured to measure yield stress and present the data in the appropriate scientific units for this parameter. Four curves show good repeatability for the yield stress of this particular material. The test is easy to run and typically takes less than one minute. The controlled stress rheometer is an alternative instrument for measuring yield stress. If the quantity of material available for testing is limited, the cone/plate system is the best choice. Practically speaking, the cone/plate system is also ideal if temperature control is required; the time required to bring the sample to temperature is minimized when using cone/plate. The test method is to run a shear ramp in which increasing torque is applied to the spindle until it begins to rotate. The torque value where the rotation of the spindle commences is the yield stress. Controlled stress rheometers are more expensive instruments than benchtop viscometers. If the budget allows for the controlled stress rheometer, this is the preferred approach, because the instrument can also perform the viscosity flow curve test and check for pseudoplastic behavior, thixotropy, and recovery of material after being sheared.

Figure 6. Cure Test Data for Epoxy Material

Curing Test
One final thought on viscosity testing applies to materials like epoxies, where viscosity builds with time as the adhesive gains strength. The objective is to know the endpoint of the reaction (i.e., the final strength of the epoxy and how long it takes to get there). A curing algorithm can be used with a standard digital viscometer that is equipped with a special program that enables the instrument to change speeds automatically. The viscometer measures viscosity continuously as the spindle rotates initially at a high speed (e.g., 50 or 100 rpm). When the measured torque reaches 95% of capacity, the viscometer downshifts its speed by an order of magnitude and the test continues without interruption. This process repeats itself several times while the viscometer continues to report the increasing viscosity value of the epoxy (see Figure 6). At the conclusion of the test, the final viscosity value and the time needed to reach it are reported.

Summary
Many factors must be considered when devising meaningful viscosity tests for adhesives and sealants. Careful thought regarding how the material is processed in manufacturing or applied by the end user will result in specifying tests that are more relevant for an effective QC program. If they are not sure about the best approach to take, adhesives and sealants manufacturers should contact an instrument manufacturer and review the test plan with them. Instrument manufacturers are the experts on getting the most out of their equipment and can help ensure that the most appropriate tests are run for a given application.