Article Summary:

The 5200 Trivector Analyzer is rapidly becoming accepted as the industry standard for on-site oil analysis. It provides a comprehensive analysis including particle count with size distribution, detailed wear debris analysis, estimated water content, and dielectric; as well as ferrous, contaminant, and chemical indexes. Greatest interest so far has been from power, paper, and pharmaceutical industries. This OilView Newsletter explains the procedures for testing samples using the 5200 including best practices, methods for masking water for accurate particle counting of water contaminated oil samples, and for preparation of wear debris analysis filter patches. If you have questions or comments about this newsletter please respond by email to mailto:ray.garvey@compsys.com

Article Details:

5200 Test Procedure

The 5200 Trivector Analyzer has a simple 1-2-3 step operation yielding automatic chemistry, contamination, and wear measurements in about 5 minutes. When appropriate, a fourth step is added to extract particulate debris on filter patch(es) for detailed microscopic wear debris analysis. The diagram below outlines the testing sequence: Test 2, wear and contamination. Pour 1:1 diluted sample:solvent to top of taper in chamber, run test, and then flush/clean with solvent. Test 3, particle count contamination. Fill 30 ml syringe with diluted sample (1:1 to 1:99). Use optional water mask solvent. Degas to remove air and then run test. Test 1, chemistry. Fill 10 ml syringe with neat, undiluted oil. Insert syringe tip and inject into hole at bottom, run test, and then flush/clean with solvent.

Verify that the oils quickly dissolve into a clear liquid when mixed with the cleaning and diluting solvent you select. You must choose a different solvent if the oil and solvent mixture becomes either milky or layered indicating oil and solvent are immiscible.

WDA Patches Typically use 3 and/or 8 micron patches as needed to view wear debris from Test 2. Two patches may be stacked with the larger pore size patch on top.

Sampling

When collecting used oil samples, collect approximately 2/3 of a sample bottle of oil. This will be sufficient for running the digital viscometer test and all 5200 tests. Do not fill the bottle to the top. Full bottles are not easily mixed by hand shaking. If you need more oil for other tests, consider collecting a second sample bottle. Viscosity Use the OilView Digital Viscometer to measure the viscosity of the undiluted oil sample. You may want to test viscosity on all samples in the batch before beginning 5200 tests. Always run the viscosity test on the undiluted oil before the 5200 tests. Solvent Selection Before testing any oil samples, test that the cleaning solvent easily dissolves with that oil type. To test this, add equal amounts of oil and solvent to a clear bottle, shake, and watch. If the fluid comes clear in 10 or 15 seconds then you are okay to begin testing. If the mixture stays milky, cloudy, or separated into layers, STOP. Find another solvent that easily dissolves in that oil before testing it in the Trivector Analyzer. The table below provides a general guideline of solubility for different oil types. Table 1. Oil and Solvent Solubility; Y=Yes, N=No Fluid B Toluene Original Lamp Oil + Fluid B Original Lamp Oil or Kerosene Ultra Pure Lamp Oil Fluid C Hexane Fluid A

Note:
Both Toluene and Isopropyl Alcohol have flash points below room temperature. They require an explosion proof vacuum pump.

Oil Class Mineral Oil PAO Diester POE + PAG PAG PhE

2.12.4 2.1-2.4 3.4-4.3 4.6-4.8 6.6-7.3 6.0-7.1

Dielectric

Y Y Y Y N ?

Y Y Y Y N N

Y Y Y Y N Y

Y Y Y Y Y Y

Y Y Y Y Y Y

Y Y Y Y N N

Y Y Y Y N Y

N N Y Y N Y

Most industrial lubricants Synthetic Hydrocarbon Diester Polyol Ester + Polyalkylene Glycol Polyalkylene Glycol Phosphate Ester

Software Test Setup The software provides instructions and the hardware flashes appropriate LEDs to automatically lead the user through the test sequence. However, before pressing the Start button to begin testing, check the following: 1Select the correct sample on the database tree. If the sample is not there, then add the sample to the correct Area, Equipment, and Point. 2Normally all three 5200 tests are run by default. If some tests are not required for a particular sample, then un-check the test-enable boxes next to the test icons for the nonrequired tests. 3When diluting by weight using the scale, make sure the scale-enable checkbox is checked. Also, select the additional dilution for Test 3 as needed. You will be directed to the scale at the appropriate time during the test. 4Press the Start button in the software. This will initiate the testing sequence. Now simply follow the instructions and the flashing LED. Test 1, Chemistry Use this test to accurately measure the dielectric of the neat, undiluted oil sample, and generate the chemical index. You may also use this test to establish a reference dielectric for a new reference sample on the Ref DB tree. 1Thoroughly shake the sample bottle to get a homogeneous mixture. 2Use a clean, 10 ml syringe, and extract 10 ml of the neat oil from the sample bottle. Be careful to NOT pull air pockets into the syringe. Air will cause a false, low measurement. 3Place the tip of the syringe into the hole at the bottom of the Test 1 chamber and squirt the sample into the instrument. Leave the syringe in place for now. This will prevent any air bubbles from being sucked into the sensor. |Note To obtain more accurate results for high dielectric oils, first prime the sensor with 5 to 10 ml of the undiluted sample. 4Press the button next to the flashing Test 1 LED. The test will take approximately 5 seconds. The LED will change to solid red after the results have been automatically read and saved to the database. 5When the LED changes to a flashing yellow color, this means that it is time to clean Test 1. This may occur immediately after Test 1, if it is the only test in the sequence, or at some later time if other tests are being run. 6Flush Test 1. Remove and discard the syringe. Use the foot pedal to run the vacuum pump to evacuate the oil from the Test 1 chamber. You may push thick oils out of the sensor using a syringe filled with solvent.

7Clean Test 1. Pour lamp oil or other solvent into the chamber to flush out the oil. Do this for 5 to 10 seconds, and then, without pouring any additional solvent, just vacuum air through the chamber to dry it. 8Perform a clean check. Press the Test 1 button next to the flashing yellow LED, and the software will take a reading. If not sufficiently clean, you may try vacuuming more air and pressing the button again. If this fails, then clean by flushing with more solvent and vacuuming air, then repeat the clean check. 9When the chamber is sufficiently clean, you will be directed to the next test to clean, or to wait for Test 2 to complete. Test 2, Wear and Contamination Use this test to detect water and metal debris that settle out of the oil onto the sensor at the bottom of the chamber. The patented, time-resolved dielectric measurement is sensitive to water, iron, and other metal particles in the oil. All oil samples are diluted approximately 1:1 with solvent (see Table 1) before filling the Test 2 chamber with approximately 20 ml of diluted oil. Dilution reduces the viscosity of industrial oils having a viscosity range of 32 to 680 cSt down to a very low range of 10 to 20 cSt. This allows the particles to settle during the test time. Dilution also makes cleaning easy and cross-contamination unlikely. |Note If subsequent Test 3 particle counting is to be run on the sample, then the representative particle count for the diluent must be saved first using the Calibrate / Test 3 Diluent/Clean Fluid Calibration procedure described later in this chapter. After completing any required, undiluted oil tests (for example, viscosity and Test 1 chemistry tests), follow these Test 2 procedures: 1Determine which dilution method will be used, either the volumetric or weighing method as described later. If weighing, then enable the scale and the software will guide you through the process. Otherwise, disable the scale and enter the volumes into the software. 2Dilute the sample approximately 1:1 in its original sample bottle, using the appropriate solvent (see Solvent Selection information above). 3Replace the lid on the sample bottle and shake vigorously until the Test 2 LED flashes green indicating the sample may be added. 4Open the bottle and pour the diluted oil sample into the Test 2 chamber up to the top of the tapered cone this takes approximately 20 ml. The sensor will automatically detect the fluid, start the test by itself, and stop flashing the LED. |Note High dielectric oils such as PAGs or Phosphate Esters require priming of the sensor grid. The software will check the Test 1 dielectric and the reference dielectric. If either value is above a threshold, the software will prompt the user to prime the Test 2 sensor grid with a few ml of the diluted sample. After

evacuating the priming fluid with the vacuum system, add 20 ml of the diluted, shaken sample and push the button to start the test manually. 5This test will take approximately four minutes to complete. If you are also running Test 3, then you will be directed on to start that test while Test 2 is running. After Test 3 finishes, you will be prompted to clean Test 1 if necessary. 6 When the LED changes to a flashing yellow color, this means that Test 2 is finished and it is time to clean. Before cleaning, examine the Test 2 and Test 3 results to see if wear debris analysis filter patches should be made. 7If you wish to prepare filter patches, make them at this time, following the procedure outlined later in this chapter for making WDA filter patches. 8 Clean Test 2. Pour lamp oil or other solvent into the chamber to flush out the sample. Do this for 5 to 10 seconds, and then, without pouring any additional solvent, just vacuum air through the chamber to dry it. Use a cotton-tipped swab to gently wipe the surface of the grid to dry off most of the solvent. |Caution! Never touch the Test 2 sensor grid with a hard object! Doing so may permanently damage the sensor. 9Perform a clean check. Press the Test 2 button next to the flashing yellow LED, and the software will take a reading. If not sufficiently clean, you may try further drying and press the button again. If this fails, then clean by flushing with more solvent and vacuuming air, then repeat the clean check. Manual Clean Check Tests 1 and 2 include a manual clean check button (the C button on the display next to the test icon) that may be used before starting a test to make sure the sensor has been left clean. This will perform a short test and display the dielectric value of the clean sensor. A dry sensor will have a dielectric close to 1.00. However, a slightly wet sensor could read 1.20 or higher. The software will display a message indicating the pass/fail status.
Test 3 Water-Masking

Tests 2 & 3 diluting solvent Used oil sample

Test 3, Particle Counts Use this test to count particles and determine particle size distributions in eight different size ranges. This is a laser optical particle counter. Air bubbles and water droplets can cause false counts. Air bubbles are eliminated in the vacuum degassing step. Water

droplets are eliminated using water-masking solvent (method protected by US Patent 6,064,480 issued to CSI; see Table 2, Particle Counting Water Masking Options below). All samples are diluted for this test from 1:1 to 1:99 (sample:solvent). Most mineral oil samples are diluted 1:1, just like for Test 2, so there is no additional dilution after Test 2. However, second and even third dilutions are performed for three reasons: 1) If the oil has a milky or cloudy visual appearance due to water contamination then the patented water-masking solvent is added to turn the solution clear before particle counting, 2) If the oil has high particulate contamination then it may require high dilution ratios to keep from exceeding the count rates for the laser sensor. If you can see particles in the oil, then the sample will require extra dilution; and 3) If the oil is extremely dark in color then additional dilution may be required. The OilView software accounts for dilution ratios and back-calculates to report the particle counts for an undiluted sample. In order to do this, representative particle counts for both the standard diluent and the water-masking solvent (when used) must be saved ahead of time. See the Test 3 Diluent/Clean Fluid Calibration section later in this chapter for the procedures for saving diluent counts. The following table summarizes the water masking solvent options (see U. S. Patent 6,064,480):

Table 2. Patented Particle Counting Water Masking Options Solvents Available from chemical supplyDOWANOL DPnB* (**Fp 205F) Available from chemical supplyIsopropyl Alcohol (Fp 54F) Available from chemical supplyToluene (Fp 50F)

Ratio (Diluted sample to masking fluid)***

Note:
Both Toluene and Isopropyl Alcohol have flash points below room temperature. They require an explosion proof vacuum pump.

Water Mas king Solv ent Mixt ure

Application

Mask 1 Mask 2 Mask 3

100% 75% 25% 25% 75%

Add until clear 1:2 1:2

Particle count with water-in-oil Particle count with water-in-oil Particle counting diluent for water-glycol hydraulics

*Use this URL for product information: http://www.dow.com/dowanol/nam/products/dpnb.htm **These solvent blends are added to the already diluted 1:1 sample from Test 2. * **Fp = Flashpoint.

Follow these steps to obtain Test 3 particle counts on the sample: 1Visually inspect the undiluted sample to decide if additional dilution (beyond 1:1 needed for Test 2) is needed. If diluting for high contamination or dark oils, then use the same solvent as for Test 2 (refer to the Oil and Solvent Solubility Table). If diluting

because the sample is cloudy or milky from water contamination then use the watermasking solvent. You must make this decision before starting the test. If necessary, select the Additional Dilution checkbox on the display next to the last bottle icon. Double-click the last bottle icon to toggle the selection between the standard diluent and masking solution for additional dilution. The bottle icon will display half blue when the water masking solvent has been selected. 2When using the scale, the software will prompt you for re-weighing after filling Test 2 if additional dilution has been selected. If not using the scale, you must type in the relative volumes to give the correct dilution ratios. 3Shake the diluted oil sample to thoroughly mix the solvent and re-suspend the particles. 4Open a new syringe package and extract 30 ml of diluted sample from the bottle. 5Fully extend the syringe plunger to create an air gap, until the plunger hits the built-in stop. 6Insert the syringe spacer to hold the plunger out, and place the tip of the syringe into the degassing port (located on the left side at the top of the Test 3 column). 7Turn the valve on the 5200 to the degas position pointing up. 8Use the foot pedal to run the vacuum pump so that any air bubbles in the oil can be removed from the syringe. This will take from 15 seconds up to a minute depending upon the viscosity of the dilution. For thicker dilutions, you will be able to see a wave of bubbles rise to the top. 9Push the Test 3 button once next to the flashing yellow LED to tell the software that degassing is complete. After a second, the LED will start flashing green. 10Remove the syringe from the vacuum port and remove the spacer. With the tip of the syringe pointing up, slowly push in the plunger to remove the air pocket and return the plunger to about 30 ml. 11Insert the tip of the syringe into the Test 3 test port and clip the body in place. 12Press the Test 3 button next to the flashing green LED. The LED should stop flashing, and the stepper motor arm will come down and drive the syringe plunger at a constant rate. The first 10 ml pushed through the syringe is flush volume, the next 15 ml are counted as the fluid goes through the laser sensor, and approximately 5 ml are left in the syringe at the end and can be discarded. 13At the end of the test, the Test 3 LED will change from green to red indicating that the data has been automatically saved to the database. The motor will reverse and return the arm to the top, home position. |Note Test 3 itself is not cleaned because the initial 10 ml of the diluted sample is used to flush the laser detector. Additional cleaning should be performed at the end of the day by manually squirting a syringe full of solvent into the Test 3 input port. Manual cleaning should also be used after testing a very dirty sample or between dissimilar fluid batches. 14Remove and discard the used syringe. The syringe has been contaminated on both the inside and outside and will contaminate the next sample if re-used.

5200 Results
The 5200 results are broken down by the three tests. The main results from the three tests are also summarized on the main test screen. Test 1 Chemistry Dielectric The dielectric of the oil is a basic property and changes with oxidation, nitration, and moisture content. Different oil types have different dielectrics as well. The Test 1 sensor measures the dielectric of a small volume of the sample between two electrical plates. Chemical Index The chemical index is a measure of the change in dielectric of the used oil sample relative to the reference oil. This indicates a chemical change in the oil, water in the oil, or a mixture of different oil types. The chemical index is scaled such that a 0.10 dielectric change produces a chemical index value of 10 which is an alarm status for most oils. A reference oil with known dielectric must be assigned in order to calculate the chemical index. Test 2 Wear / Contamination The Test 2 sensor measures dielectric properties of contaminants in the oil. The Test 2 sensor uses gravity and an electromagnetic field to concentrate and move particles on the surface of the sensor grid during the test. See the Test 2 Plot example later to better illustrate the following indices. Contamination Index This index is based upon the change in apparent dielectric resulting from non-ferrous contaminants settling onto the sensor grid over the test time. Water has the largest effect on the contamination index, but other non-ferrous metals affect it as well. The contamination index is calculated by scaling the total dielectric change during the test. Non-Ferrous Index This index is the same as the Contamination Index. Ferrous 1 Index This index is a measure of the delta dielectric resulting from the ferrous particles standing up and lying down on the sensor grid. An internal electromagnet changes states during the first part of Test 2 to produce this effect. Ferrous 2 Index During the second part of Test 2, a different electromagnetic field sequence is used to sweep the settled iron outside of the sensing area. The resulting change in dielectric is scaled to give the Ferrous 2 Index.

Large Ferrous As the particles settle onto the grid and the electromagnet changes states, large ferrous particles or ferrous chains of particles will sometimes cause abrupt spikes in the data plot. The Large Ferrous indicator is a count of these spikes. Large Non-Ferrous Spikes which occur while the ferrous particles are standing up are treated as Large Non-Ferrous indicators. Water Droplets As water droplets settle onto the sensing grid, they cause abrupt changes in dielectric too. However, these changes last for at least a few test cycles, and are thus distinguishable from other contaminant spikes. Estimated % Water As mentioned before, water has the largest effect on the contaminant index. Water will settle onto the sensor grid differently for different oil types and additive levels. Water also affects the Test 1 Chemical Index. The Estimated % Water is calculated by applying different scaling factors to the contaminant and chemical indices for different oil additive levels. Test 3 Contamination Test 3 uses a laser-based particle counter to simultaneously count and size particles in eight different size ranges as the fluid is forced through the sensor at a constant flow rate. The particle count table shows the individual particle counts per milliliter for each of the size ranges from greater than 2 microns to greater than 100 microns based upon the ISO 4402 calibration method. ISO Code The ISO codes are reported based upon the ISO 4406:1987 ISO code table where each increment of one ISO Code represents approximately a doubling of actual particle counts. The three reported ISO codes represent >2 micron, >5 micron, and >15 micron particle counts. NAS Code The NAS code is from the NAS 1638 standard for classifying particle distributions. The NAS classification method looks at five size ranges from 5 micron up to >100 micron. The worst case size range dictates the resulting code.

Making WDA Patches

The wear debris filter patch maker is connected between the Test 2 chamber and the drain. Therefore, as the diluted oil sample is drained from the Test 2 chamber, it passes through the filter patch maker. To create a filter patch you must open the filter patch maker and insert a filter patch before cleaning the chamber using the vacuum pump. Refer to the illustrations below to see how the filter patches are assembled into the patch maker. You may use either one or two filter patches at a time.

Select the pore size (0.8 to 30.0 micron) for the filter patch based on the size distribution and total contamination results from Test 3. A few tests will quickly reveal what pore sizes tend to plug and which ones yield meaningful specimens. The goal is to produce WDA patches with particles distributed so they can be easily viewed with a microscope. This is also a good way to see if the high particle counts from Test 3 were caused by water. You can separate large particles from smaller particles using stacked filter patches. For example, if the sample is highly contaminated you may choose to use a 30 micron filter above a 10 micron filter. Keep in mind that the small pore size filter is most often the one that is plugged from excess contamination. If you wish to view ferrous and non-ferrous particles on separate patches, then use the sheathed magnet to extract ferrous particles from the Test 2 chamber before ever flushing the diluted sample through the filter patch(es). After removing the ferrous particles, you can flush the remaining particles to create the non-ferrous patch(es). Remove the non-ferrous patch(es) and insert new patch(es) for the ferrous particles. Then remove the magnet from the sheath, and rinse the ferrous particles off of the sheath into the empty Test 2 chamber with solvent. Flushing this time will create the ferrous patches. If you are unsure of the composition of the debris, you can send the filter patch to the CSI Trivector Lab for Scanning Electron Microscopic examination including Energy Dispersive X-ray elemental analysis.