tribologik lubricant handling and analysis presentation
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LUBRICANTS HANDLING AND
ANALYSIS
Training Session, June 2013
Moussa ZIDOUNE, PhD ChemistLaboratory Director
Agenda
Fundamentals of lubrication
Functions of lubricant
Lube oil properties
Oil sampling
Storage and handling of oils
Oil analysis
Application
Reports and Interpretation
Conclusion
Tribology
• Is the study of the interactions of sliding surfaces that includes three subjects: Friction, Lubrication and Wear.
• It’s science and technology of the interactions between surfaces moving relative to each other.
FrictionFriction is defined as the resisting force to the relative Motion of two contacting bodies.
1) Static Friction : Is the friction that exists between two stationary objects and the force required to set them in motion.
2) Dynamic friction : The friction that exists between two surfaces in relative motion.
1- Solid friction- Sliding surfaces in direct contact- Independent of overall surface area
2- Fluid friction: - Describes friction that occurs between molecules of
liquid (lubricated friction, fluid separate two solid surfaces).
3- Skin friction
- The force resisting the motion of solid body through fluid Varies with speed and area (shear stress).
Types of friction
Wear
• Wear is the rubbing away of metal surfaces due to mechanical action.
• Abrasive wear• Corrosive wear• Fatigue wear• Erosive wear• Cavitation wear• Adhesive wear
1986, Canada’s friction losses are in the neighbourhoodof 5 Billion dollars*
Today’s technology allows recovery of 35% of those losses.
The benefits are :• Longer machine life cycles• Less energy consumption• Less materials consumed• Safer operating conditions
*1986 NRC report : A strategy for tribology in Canada
Cost of Friction
Lubrication
• Lubrication is the process, or technique employed to reduce wear of one or both surfaces in close proximity, and moving relative to each other, interposing a substance between the two surfaces called lubricant
• Lubrication describes the reduction of wear.
What is Oil?
• 85% of the oil is “Base Oil”.• About 15% is the additives.
• This is what makes a hydraulic oil different from an engine, gear, transmission and compressor oil.
Mineral Oils: products of the distillation of crude petroleum, consisting of hydrocarbon chains: Paraffinic Naphtenic Aromatic
Synthetic Oils: oils made by chemical synthesis: Polyalphaolefins (PAO) Polyglycols (PAG) Ester oils Silicones Phosphate esters
Semi-synthetic: blends of mineral oils with synthetic base oils
Vegetable Oils: made of soja, corn, castor, canola, cotton seed Animal lubricants : Produced from the animals fat.
Base Oils – General Classification
Biodegradability Oils: is the chemical breakdown of materials by living organisms in the environment to carbon dixide and water
Primary biodegradability is the measure of the product loss without measuring degree of the biodegradability
Readily biodegradable when more than 60 % of the oil is converted to carbon dioxide in 28 days
Base Oils – General Classification
Classification of Lubricants by Additives
Additives are substances formulated for the improvement of the anti-friction, chemical and physical properties of base oils (mineral, synthetic, vegetable or animal), which results in enhancing the lubricant performance and extending the useful life of equipments.
Additives can make up to 30% of the lubricant.
Friction modifiers
Anti-wear
Extreme pressure (EP)
Anti-rust and corrosion inhibitors
Anti-oxidants
Detergents
Dispersants
Pour point depressants
Viscosity index enhancers
Anti-foaming agents
Classification of additives by application
•
Prevent seizure conditions caused by direct metal-to-metal contact between the parts under high loads
- Graphite- Molybdenum disulfides- Boron nitride (BN)- Polytetrafluoroethylene (PTFE)
Friction modifiers
•
Prevent direct metal-to-metal contact between the machine parts
- Zinc dithiophosphate (ZDP)
- Zinc dialkyldithiophosphate (ZDDP);
- Tricresylphosphate (TCP).
Anti-wear additives
Friction modifiers reduce coefficient of friction, resulting in less fuel consumption when the oil film is broken down.
- Chlorinated paraffins;- Sulphurized fats;- Esters;- Zinc dialkyldithiophosphate (ZDDP);- Molybdenum disulfide
Extreme pressure (EP) additives
Form a barrier film on the substrate surface reducing the corrosion rate and attack of oxygen, water and other chemically active substances.
- Alkaline compounds;
- Organic acids;
- Esters;
- Amino-acid derivatives.
•
Rust and corrosion inhibitors
Mineral oils react with oxygen of air forming organic acids.
The oxidation reaction products cause increase of the oil viscosity, formation of sludge and varnish, corrosion of metallic parts and foaming.- Zinc dithiophosphate (ZDP);- Alkyl sulfides;- Aromatic sulfides;- Aromatic amines;- Hindered phenols.
Anti-oxidants
Neutralize strong acids.
Form a film on the part surface preventing high temperature deposition of sludge and varnish.
- Phenolates, Sulphonates and phosphonates, such as calcium (Ca), magnesium (Mg), sodium (Na) or Ba (barium)
Detergents
Improvers keep the viscosity at acceptable levels, which provide stable oil film even at increased temperatures
- Viscosity improvers are widely used in multigrade oils
- Acrylate polymers.
•
Viscosity index improvers
Foaming not only enhances oil oxidation but also decreases lubrication effect causing oil starvation.- Dimethylsilicones (dimethylsiloxanes)
Anti-foaming agents
Keep the foreign particles (sludge and varnish, dirt, products of oxidation, water) present in a lubricant in a dispersed form.
- Polyisobutylene
Dispersants
Depressants inhibit formation and agglomeration of wax particles, keeping the lubricant fluid at low temperatures.
- Co-polymers of polyalkyl methacrylates
Pour point depressants
Engine oils
Gear oils
Hydraulic oils
Compressor oils
Transformer oils (insulating oils)
Turbine oils
Cutting fluids (coolants)
Grease (bearings)
Classification of Lubricants by application
Engine
Gearbox
Hydraulic
Compresor
Functions of engine oil: Provision of stable oil film between sliding
surfaces
Provision of reliable engine operation in a wide temperature range.
Rust/corrosion protection of the engine parts
Cleaning sludge from the engine parts
Sealing piston ring - cylinder gap
Prevention of foaming
Cooling the engine parts
Engine Oils
Hydraulic Oils
Characteristics and properties Thermal and chemical stability Low compressibility Hydraulic stability Good lubrication Low foaming Emulsion capacity
Benefits of Oil Analysis
Reduction in maintenance costs Reduction in unscheduled downtime Reduction in unscheduled maintenance Reduction in machine power consumption Effective maintenance scheduling Improved equipment reliability. Elimination of arbitrary oil changes Minimization of installation errors. Increase in equipment availability Reduction in disposal cost Verifies correct lubricant in place ,
• Work till it fails• Preventative Maintenance• Predictive Maintenance• Pro-Active Maintenance
1900 1940 1970 1990 2009
Laboratory Tribologik®
LaboratoryHuman Verification
VERIFIED REPORTS ARE SENT BY EMAIL AND ACCESSED ON
TRIBOLOGIK SECURE SITE
ACCESS 24 / 7
CONSTANTLY UPDATE AND TRACK YOUR
CURRENT EQUIPMENT
Oil analysis is like a blood test
=Prognosis
RecommendationLogical Conclusion
=
Doctor Tribologik
• 1st Time: Doctor: Acquire basic personal information• 1st Time: Tribologik®: Complete equipment profile• 2nd Time: Doctor: Comparison of previous results• 2nd Time: Tribologik®: Comparison of previous results• 3rd Time: Doctor : Trending but limited to doctors knowledge• 3rd Time: Tribologik®: Trending with each report building on previous one
Limited knowledgeContaining over 1500
conclusions based upon tens of thousand of
possibilities from 75 years of professional knowledge
• Past failure modes• Historical data• Clients comments• Critical equipment status• Duty cycle• Oil supplier data sheet• Industry guidelines for oil tests
Criteria for Determining Type of Analysis
• Storage and dispensing equipment must be contaminant free
• Use proper labeling for all containers with color code label or tag.
• Date all lubricant storage• Store the oil in the designated room (in-doors)• Use clean sealed plastic container (not galvanized)• Use one container per lubricant type• Keep containers closed when not in use• Determine if prefiltration is req’d before adding oil• Use lube filter cart where applicable
Lube Dispensing
Properties relatively unaffected by sample locations are:
• Viscosity• Neutralization number• FTIR (InfraRed spectroscopy)
Properties that are sample location sensitive:
• Particle count• Moisture levels• Wear levels
QUESTIONS
LUBRICANTS SAMPLING
Training Session, June 2013
Moussa ZIDOUNE, Ph. D., ChemistLaboratory Director
Agenda
• Guidelines• Where to take the Samples• Sampling Materials• Sampling Procedures• Post-Sampling Procedures• Sources of Interference
• The importance of proper sampling is critical.
• Poor samples lead to poor results(false plus or minus)
• Poor results lead to poor decisions!!!
• Know what you want to sample• Correct sampling procedures
– Vacuum pump – Mini – valve– Syringe
• Representative sample• Quantity to be collected: 100 ml
Sampling Procedure Guidelines
Sampling Procedure Guidelines
• Sample only under normal operating conditions• Sample from live zones• Sample at specific components upstream &
downstream• Sample at correct frequency
– On run time– Or calendar time– Root cause failure analysis
• Record hours to time the data
• Install sampling hardware to ensure consistent sample location
• Flush sample ports effectively to obtain a live sample
• Use documented procedures to maintain accuracy• Use clean bottles and tubing• Send sample to lab ASAP
Sampling Procedure Guidelines
Don’t sample• When the systems are cold• From the bottom of the machine
Where to take the samples
• Proper sampling location• Correct machine identification.• Correct test point location.
– From the middle of the machine, tank– From the same point in the tank or sump to ensure good
trending of data.– From turbulent zones
• When the systems are running and warm• Flush sample ports effectively to obtain a live sample
Materials required :• A sample bottle that is capped and
placed in a sealed ziplock baggy and only removed for sampling
• A coil of ¼” poly tubing in a ziplock baggy
• Bottle labels• Knife to cut tubing• Tube weighting materials• Dip stick & tie wraps
Materials required:• A suitable vacuum pump enclosed in a
zip lock baggy prior to and after use• A wrench to open the port• A container for collecting flushing fluid
Probe Sampling Valve (XK Series)
Push Button Sampling Valve (XPM Series)
Disposable Probe Tube Cap (XKR Series)
Sampling Accessories
Sampling Accessory Kit
Drop Tube Sampling Method
• Drop tube sampling is one of the most common methods of sampling static tanks.
• Engines are commonly sampled by this method
• A vampire pump is attached to specimen bottle and a new piece of poly tubing
Drop Tube Sampling Method
Vampire/Vacuum Pump Set-up
1. Order100 ml plastic bottles from PMC
2. Use 1/4 inch (6,5 mm), new poly tubing. Order from PMC
3. Cut it at an angle, long enough so that it can reach the bottom of the sump or reservoir, or approximately 6 inches (15 cm) longer than the oil dipstick.
Vampire/Vacuum Pump Set-up4. Insert the tubing through
the hole in the knob of the vacuum pump and let it extend about 1 inch (2,5 cm) into the sampling bottle.
5. Tighten the knob. Uncap the bottle and screw it into the pump. Make sure it is seated properly.
Vampire Pump
Use pump handle to drain oil in a slow pumping action until sample bottle is almost full. Do not fill completely as this could cause overflow and contaminate pump.
Never reuse the same tubing
Vampire Pump Maintenance
All components of pump should be cleaned at least every 3-5 samples in order to reduce chances of contamination
Existing Sampling Valve
. Locate already existing sampling valve on machine.
Oil sampling Procedure
Oil Sampling Procedure from Gearbox
• Draw sample during normal operation or within 10 minutes of shutdown.
• Check the lube level prior to sampling to confirm it is at the required level
• Watch the lube level during sampling to ensure that lubrication starvation is avoided, especially on small sumps
• Allow oil to flow for a few seconds to ensure proper representative sample.
• Place bottle below valve and open to allow flow of oil into bottle.
Sampling Procedure
• Remove plug or cover to the fill port, vent, breather or other opening through which the sample will be drawn.
• Cut the tube at 45 degree angles on both ends to an acceptable length.
• Place one end of the plastic tube into the vacuum pump such that at least one-half inch will protrude into the bottle cavity.
• Secure the tube into the pump head such that a proper seal is achieved. Thread the flushing bottle tightly onto the vacuum pump.
Sampling Procedure
• Direct the other end of the tube into the machine compartment opening to a measured distance that is halfway into the tank or sump.
• With the tube inserted into the tank, actuate the pump to vacuum out approximately 8 ounces of oil (200 ml) into the flushing bottle in order to adequately flush the tube of pre-existing debris.
• Once the flush is complete, remove the flushing bottle.
Sampling Procedure
• Remove the bottle cap from the sample bottle without opening the plastic bag.
• Tighten the bottle sufficiently to accomplish an air-tight seal
• Actuate the pump to draw the sample into the bottle while keeping the sample bottle in an upright position.
• Fill the sample bottle to level of 100 ml (3 oz)
Sampling Procedure
• Once the bottle has been filled, unthread it from the vacuum pump.
• Without opening the plastic bag, thread the cap back onto the bottle securely.
• Remove the tube from the tank or sump.• Remove the bottle from the zip-lock bag. • Securely reattach the cap or vent breather to the tank or sump.• Remove the plastic tube from vacuum pump.• Dispose of the plastic tubing. DO NOT REUSE.• Return the vacuum pump to its zip-lock bag to avoid
contamination.• Dispose of the flushing fluid properly.
Post- Sampling Procedure
• Complete or verify all required documentation to accompany the sample, including the following:– If preprinted labels are used, be sure the
correct label is affixed to the correct bottle.– Note any abnormalities associated with the
sampling procedure.– Note any abnormalities associated with the
machine, filter or operating conditions.
Post- Sampling Procedure - Documentation
• If the sample is being tested onsite, refer to testing procedures and analyze immediately.
• If the sample is being sent to a lab for testing, appropriately package the bottle for shipment.
• Ship the bottle to the lab as soon as possible.
Post- Sampling ProcedurePackaging/Shipping
- Picking up bottom sediment and water- Contaminating the sample during handling- Contamination of the plastic tubing.· Contamination from the vacuum pump.
Potential Sources of Interference - Contamination
· Failure to ensure that the sample is drawn from the same point each time due to variable distance into the tank or sump.
· Failure to ensure that the machine is sampled during operation each time, or
· Failure to ensure that the machine is sampled within the same delay after shutdown, each time.
Potential Sources of InterferenceNon-Consistent Procedures
QUESTIONS
Training Session, June 2013
OIL TEST METHODS
Moussa ZIDOUNE, Ph. D., ChemistLaboratory Director
Oil Analysis allows detection of:
Dirt and dust Water Glycol Fuel Soot Sulfates and nitrates Particles
Inductively Coupled Plasma (ICP) Direct Reading Ferrography (DR) Analytical Ferrography (AF) Filter Debris Analysis (PT)
Contamination Degradation of the oil by:
Kinematic viscosity (VIS) Oxidation (FTIR) Acid number (AN) Base number (BN) Wear
SP – Spectroscopy VIS – Viscosity FTIR – Infrared Analysis
TAN – Total Acid Number TBN – Total Base Number
PC – Particle count DR – Direct reading AF – Analytical Ferrography
FU- Fuel FP – Flash Point FIRE – Fire Point
GYL – Glycol Water -Tests
VCT – Varnish Test RULER COPPER CORROSION
Machine and Lubricant Condition
MACHINERY
AFDRPC
LUBRICANTS
FTIR VISTAN TBNWater, FU
SP
PCDR
SP - Analytical SpectroscopyDetects 22 elements (Particles <6 microns in size)
Wear Metals
Contamination- Boron, Sodium, Silicium, Potassium, Aluminum
Additives - Calcium, Phosphorus, Zinc, Magnesium, Barium
• Aluminum • Barium • Boron • Cadmium • Calcium • Chrome • Copper • Iron • Lead • Magnesium • Manganese • Molybdenum • Nickel • Potassium • Phosphorous • Silicium • Silver • Sodium • Tin • Titanium • Vanadium • Zinc
VIS - Viscosity
Measures the resistance to flow
Measured in centiStokes (cSt)
40 ◦C and/or 100 ◦C
Affected by: Oxidation Contamination
Change oil if the limit is > 20%, and Monitor trend if > 10%!
Viscosity is the most significant property of a lubricating oil
PdM Procedure on Oil Handling and Analysis
• Viscosity Index is a unitless• number used to indicate the effect of Temperature
on an oil.
• Higher VI= Less effect by temperatures• Multigrade oil has higher VI than monograde
Viscosity Index
FTIR – Infrared Analysis
Fingerprint of the lubricant
Soot Level Oil Degradation
Oxidation Nitrates Sulfates
Contamination Glycol Water Fuel
Additives Level Mineral or Synthetic Base Oil Wavelength (cm-1)
Ab
sor b
ance
Water & glycol
Thickening Oil Degradation Products
New oil
Oxidation
4000
3500
3000
2500
2000
1500
1000
Total Acid Number(TAN) Total Base Number (TBN), ASTM D974 & ASTM D4739
TAN indicates oil oxidation or contamination by an acidic product. Acid number increases with oxidation Recommended for all industrial equipment
TBN measures the alkaline content of oil. Abnormal reduction indicates reduced acid neutralizing capacity. Recommended for engines
Effects of Water on Oil
Causes hydrolysis and oxidation
Generates acids
Thickening
Varnish and sludge
Contributes to foaming and emulsion
Effects of Water Contamination on the Machine
Water accelerates machine deterioration
Corrosion: water in oil confers their maximum destruction potential to acids
Loss of lubricating film, cavitation, lower filtration capacity and blocks valves.
Bearing wear due to water contamination
Hot Plate Test - Semi-quantitative FTIR (infrared) - Qualitative Spectroscopy – Indicative Karl Fischer – Coulometric titration -
Quantitative Distillation, ASTM D95 - Quantitative
Water Detection Methods
The hot plate test is very effective in detecting water in quantities equal to or higher than 0.1% (1000 ppm or more).
Results: 0.0%, 0.1%, 1.0%, 2.0%, 5%
Hot Plate Detection Method
0.0%, 0.1% 1.0% 2.0%
FTIR Detection Method
Water & glycol
Degradation Products (nitrate-sulfate)
Oil Thickening
New Oil
3.5
3.0
2.5
2.0
1.5
1.0
0.5
4000 3500 3000 2500 2000 1500 1000
Wavelength (cm-1)
Ab
sorb
ance
Oxidation
Spectroscopy
Presence of boron, B
Presence of sodium, Na
Presence of potassium, K
Distillation MethodCooler
condensor
Water
Heating plate
Quantitative Method for High Concentration (5% -100%)
Applicable when and where water contamination level is critical and must be kept very low.
Both equipment and oil can accept a certain amount of water
Result is given in percent (ex: 0.1% = 1000 ppm).
KF - Karl Fisher ASTM D4928/D6304/D1744
Antifreeze
Glycol and water are the main constituents (50%/50%) of antifreeze or coolant liquids.
Ethylene Glycol (High heat transfer)
Propylene Glycol (More toxic, less popular)
Additives: borates, molybdates, silicates, nitrates, potassium ...etc
Glycol Contamination
Effects of Glycol
Oil thickening, change in viscosity Emulsion and gels, dispersion Acid formation Precipitation of additives Lower oil debit Filter degradation Bad lubrification
Glycol Detection Methods
FTIR DetectionDegradation Products
(nitrate-sulfate)
Oil Thickening
New Oil oxydation
3.5
3.0
2.5
2.0
1.5
1.0
0.5
4000 3500 3000 2500 2000 1500 1000
Wave length (cm-1)
Abs
orba
nce
Water & glycol
Detection by Spectroscopy
Presence of Boron, B
Presence of sodium, Na
Presence of potassium, K
Presence of silicium, Si
Detection by ASTM D2982 Method Colorimetric method
HCl solution is added to oil to oxidize glycol
The reaction produces aldehyde
Aldehyde reacts alternatively with a reactant, producing a positive color change from colorless to pink / to purple
The darker the color, the more glycol there is
Results: 0.01%, 0.05% and 1 %
Detection by GC ASTM D4291 Method
This method is the most precise, although more expensive and more time consuming than others.
The most widely used GC procedure is ASTM 4291.
First you must extract glycol
Extract is then injected into the GC where polar components are separated and detected on a chromatogram.
1. Fuel Dilution ASTM D3828
2. FTIR Detection
3. Detection by Flash Point
4. GC, ASTM D Detection is the most precise and most expensive method. The most currently used GC method is ASTM 3524
Fuel Contamination
FU - percent of unburned diesel or gasoline present in engine. It’s most destructive contaminant of the oil.
FP - Temperature at which the lubricant flashes when exposed to an open flame
FIRE - Temperature at which the lubricant continues to burn when exposed to an open flame
FP – Flash Point ASTM D92 FIRE – Fire Point ASTM D92
CLP - Temperature at which crystals of paraffin wax precipitate from solution to obstruct filtration systems.
PP - Temperature at which the fuel or oil is not moving (immobilized) once at an angle of 90 degrees to a horizontal surface.
CLP – Cloud Point ASTM D97 PP – Pour Point ASTM D2500
This test is performed using an automatic laser light particle counting instrument. A laser light beam is shown through a constant flow rate stream of oil. As particles entrained in the oil pass through the light beam, the attenuation of the transmitted light as seen by a sensor is measured versus time. Using the The number of counts for given size ranges are then classified according to an ISO 4406 Standard.
PC – Particle Count
Recommended on all pieces of equipment requiring filtration
Cleanliness level expressed in ISO 4406 (1999) or NAS 1638 codes
Dimensions (-) and quantity of the particles Water particles are also counted Evaporation may be used to eliminate part of this
water for a better particle counting.
PC – Particle Count
27/23/13 4 -
6 -
14 -
ISO 4406:1999
Particles by ml
More than Up to Scale
160,000 320,000 25
80,000 160,000 24
40,000 80,000 23
20,000 40,000 22
10,000 20,000 21
5,000 10,000 20
2,500 5,000 19
1,300 2,500 18
640 1,300 17
320 640 16
160 320 15
80 160 14
40 80 13
20 40 12
10 20 11
5 10 10
2.5 5 9
1.3 2.5 8
0.64 1.3 7
ISO 4406 NAS 1638
23/21/18 12
22/20/18 --
22/20/17 11
22/20/16 --
21/19/16 10
20/18/15 9
19/17/14 8
18/16/13 7
17/15/12 6
16/14/12 --
16/14/11 5
15/13/10 4
14/12/9 3
13/11/8 2
12/10/8 --
12/10/7 1
12/10/6 --
Comparison between ISO 4406 & NAS 1638 Cleanliness codes
DR – Direct Reading
Recommended for gearboxes, differentials and screw compressors
Detects metallic, non–metallic particles, contaminants included
Indicates changes in wear rate and severity
Quantitative Ferrography
AF – Analytical Ferrography In-depth DR
Type of wear
Detection of large particles
Degradation products by
oxidation in suspension
Recommended systematically
when particles are detected
When Spectroscopy, Direct Read Ferrography, or Particle Count Analysis indicates there is a wear or contamination problem, a ferrogram slide is made and the particles microscopically examined. Wear modes, wear severity, and contaminants can then be identified visually.
Wear Particles - Debris
By abrasion Copper Alloy Slicing
Red OxidesBlack Oxides
Particle Quantifier Index, PQ
Sensitive Magnetometer - measures the mass of ferrous debris in the sample – in PQ index.
The PQ index test is quantitative
Recommended for engine oils
Analex PQA
When iron is high and PQ is low ~> small particles
When iron and PQ are high ~> small particles
When PQ is high and iron is low ~> large particles
Interpretation of PQ results
Copper Corrosion ASTM D130
• The copper strip corrosion test is designed to assess therelative degree of corrosivity of a petroleum product due toactive sulfur compounds.
• The Copper Corrosion test is a widely used oil analysis method for gearbox, turbine and hydraulic lubricants.
• This oil analysis method will detect the corrosive effects of a lubricant on copper alloys.
• A polished copper strip is immersed in 30mL of sample at elevated temperature, 50 °C or 100° C, depending on the type of gazoline, grease or oil tested, for a period of three hours.
• At the end of this period, the copper strip is cleaned and examined for evidence of degradation.
Procedure
• Results are rated by comparing the stains on the copper strip to the ASTM color-match scale from 1A to 4C.
• The rating of 1A is given for appearance of freshly polished copper.
• 1B indicates slight tarnish• 4C being the worst,corroded,
blackened, and pitted coupon.
Varnish ?
• Varnish is a thin, oil-insoluble layer of oil-degradation residues and by-products that develops over time on the internal surfaces of lubricated equipment. This can even occur on well-maintained machines with clean lubricants.
• Oxidation• Thermal Degradation
Causes
• Air, Heat, water; contamination, radiation, additive degradation, etc.
Factors
How to Measure Varnish?
• Varnish formation potential is measured by : quantitative spectrophotometric analysis (QSA)
• Contaminant, sub-product evaluation method based on the extraction by disssolution of insoluble contaminants, through a membrane, measured in CIE_dE, on a scale of 1 to 100.
• The higher CIE_dE is, the higher the proportion of varnish in the oil.
What makes this testing different?
QSA testing protocol was designed to isolate, identify and measure the specific degradation by-products responsible for the formation of sludge and varnish.
QSA does not use traditional oil analysis methods or instruments. Because nonone of these can detect the varnish.
Why traditional methods cannot detect varnish ?
Analytical Methods
Effective Points Ineffective Points
ICP Spectrometer
Since the metal particles act as the catalyst in oxidation process, observing the concentration tendency of metal elements, such as, Cu, Zn etc. can help to get the idea of the oxidation improving.
The by-products responsible for varnish are often non-metallic (the elements: C, H, N, O) and therefore cannot be directly identified or measured using this method.
FTIR
FTIR analysis often can indicate the presence of oxidation by-products. 1630 cm-1 (N=O) or 1714 cm-1 (C=O) peak in the infrared spectrum incraease over time, this is an indication of varnish build up.
The data produced is difficult to quantifying the varnish potential of a lubricant when used alone.
Why traditional methods cannot detect varnish ?
Viscosity 40°C
The oil viscosity can increase from hydrocarbon chain polymerization which is a useful indicator that degradation is occurring.
The varnish typically occurs before a meaningful change in viscosity, therefore, varnish cannot be determined from changes in viscosity alone.
TAN
TAN measures the lubricant’s acidic constituents.
TAN cannot measure directly all forms of varnish. Some of the by-products are nonacidic. And varnish can begin well ahead of a change in TAN.
ISO Particle Count
Varnish soft contaminants are insoluble in the oil, it would seem that ISO reading will be increase with the varnish potential improving.
In fact, the vast majority of soft contaminants are typically less than 1μ which is under the limit of the ISO particle count test.
Varnish Results
MONITOR MARGINAL CRITICALNORMAL
CIE_dE Results on a 1 – 100 scale
< 15 15 ~ 30 30 ~ 40 > 40
Photo of membrane
Each report includes the QSA, a severity scale that depicts where the result lies between normal, marginal
and critical, a digital image of the separated contaminants, and a written interpretation of the
laboratory results.
How is the information is reported?
The RulerTest Remaining Useful Life of the Lubricant
• The Remaining Useful Life Evaluation Routine (RULER®) test can determine the remaining useful life of used oil by comparing its anti-oxidative concentration (oxidation inhibitors) with those of new oil.
• The RULER is an oil analysis technology to measure the resistance to oxidation of high performance lubricants and greases, used in critical equipment operating on a continuous basis such as turbines, aircraft engines, pumps and compressors
Oxidation is the source of oil acidity which in turn is the source of rust and corrosion.
The role of antioxidant additives is crucial to counter lubricant acidification, it is therefore critical to prevent corrosion of the equipment.
Water in hydraulic and steam turbines is the primary cause of corrosion, it is therefore of prime importance to make sure that the level of antioxidants is at all times sufficient to protect these critical equipments against rust and corrosion.
Measuring the Level of Antioxydants with the Ruler
• The Ruler ® test allows comparing the concentration of antioxidants in the oil currently used in your equipment with its reference oil at any time. We consider the reference oil as 100 % of Amine and phenol.
• The RULER® oil analysis technology can be used to prolong oil change intervals by replacing the antioxidant additives when required.
• It can also be used to quantify the levels of antioxidants in oils at the time of receipt, or in tanks, or a method to detect sudden additive depletion rate indicating abnormal operating condition.
Action!!
Change oil if viscosity is - 20% of initial value
Change oil if fuel has been detected and low viscosity
Change oil if glycol has been detected
Action !! Filter oil if code ISO is higher than recommended
Inspect machine if wear is severe
Proceed to AF test if volume of large particles is high
Eliminate the source of water infiltration
Monitor color and odor of oil, oxidation index
Eliminate varnish if detected
QUESTIONS
Test Packages
Moussa ZIDOUNE, Ph. D., ChemistLaboratory Director
Training Session, June 2013
ENGINES
SP ICP SPECTROMETRIC ANALYSIS ASTM D5185
FTIR FOURIER TRANSFORM INFRARED ANALYSIS JOAP
MOBFTV VIS100 VISCOSITY 100 ◦C ASTM D445 100ml MONTHLY
FU FUEL DILUTION ASTM D3828
HP CRACKLE TEST PMC
COPOF COLOR,ODOR,CLARITY,PRECIPITATE,FOAM PMC
SP ICP SPECTROMETRIC ANALYSIS ASTM D5185
FTIR FOURIER TRANSFORM INFRARED ANALYSIS JOAP
VIS100 VISCOSITY 100 ◦C ASTM D445
MOBPLUS TBN TOTAL BASE NUMBER ASTM D4739 100ml MONTHLY
FU FUEL DILUTION ASTM D3828
HP CRACKLE TEST PMC
COPOF COLOR,ODOR,CLARITY,PRECIPITATE,FOAM PMC
SP ICP SPECTROMETRIC ANALYSIS ASTM D5185
FTIR FOURIER TRANSFORM INFRARED ANALYSIS JOAP
VIS40 VISCOSITY 40 ◦C ASTM D445
VIS100 VISCOSITY 100 ◦C ASTM D445
MENGP VI VISCOSITY INDEX (VIS40+VIS100) ASTM D2270 100ml MONTHLY
GCF GAS CHROMATOGRAPHY ANALYZE FUEL ASTM D3524, ASTM D3525
PQ PARTICLE QUANTIFIER INDEX PMC
HP CRACKLE TEST PMC
COPOF COLOR,ODOR,CLARITY,PRECIPITATE,FOAM PMC
HYDRAULIC FLUIDHydraulic pump, Turbines
TESTING PACKAGE
CODE CODE DESCRIPTION METHOD
SAMPLE VOLUME
REQ. CALENDAR
SP ICP SPECTROMETRIC ANALYSIS ASTM D5185
FTIR FOURIER TRANSFORM INFRARED ANALYSIS JOAP
VIS40 VISCOSITY 40 ◦C ASTM D445
PRAN PC PARTICLE COUNTING ISO 4406 100ml MONTHLY
COPOF COLOR,ODOR,CLARITY,PRECIPITATE,FOAM PMC
TESTING PACKAGE
CODE CODE DESCRIPTION METHOD
SAMPLE VOLUME
REQ. CALENDAR
SP ICP SPECTROMETRIC ANALYSIS ASTM D5185
FTIR FOURIER TRANSFORM INFRARED ANALYSIS JOAP
VIS40 VISCOSITY 40 ◦C ASTM D445
PRANP PC PARTICLE COUNTING ISO 4406 100ml MONTHLY
TAN TOTAL ACID NUMBER ASTM D974,ASTM D664
KF KARL FISCHER WATER TEST ASTM D4928
COPOF COLOR,ODOR,CLARITY,PRECIPITATE,FOAM PMC
GEARBOX, DIFFERENTIAL & COMPRESSOR
TESTING PACKAGE
CODE CODE DESCRIPTION METHOD
SAMPLE VOLUME
REQ. CALENDAR
SP ICP SPECTROMETRIC ANALYSIS ASTM D5185
FTIR FOURIER TRANSFORM INFRARED ANALYSIS JOAP
DROT VIS40 VISCOSITY 40 ◦C ASTM D445 100ml MONTHLY
DR DIRECT READING PMC
COPOF COLOR,ODOR,CLARITY,PRECIPITATE,FOAM PMC
SP ICP SPECTROMETRIC ANALYSIS ASTM D5185
FTIR FOURIER TRANSFORM INFRARED ANALYSIS JOAP
VIS40 VISCOSITY 40 ◦C ASTM D445
DROTP DR DIRECT READING PMC 100ml MONTHLY
KF KARL FISCHER WATER TEST ASTM D4928
TAN TOTAL ACID NUMBER ASTM D974,ASTM D664
COPOF COLOR,ODOR,CLARITY,PRECIPITATE,FOAM PMC
COMPRESSOR Axial compressor ,Centrifuge compressor
TESTING PACKAGE CODE CODE DESCRIPTION METHOD SAMPLE VOLUME REQ. CALENDAR
SP ICP SPECTROMETRIC ANALYSIS ASTM D5185
BROA FTIR FOURIER TRANSFORM INFRARED ANALYSIS JOAP 100ml MONTHLY
VIS40 VISCOSITY 40 ◦C ASTM D445
COP COLOR,ODOR,CLARITY,PRECIPITATE,FOAM PMC
SP ICP SPECTROMETRIC ANALYSIS ASTM D5185
FTIR FOURIER TRANSFORM INFRARED ANALYSIS JOAP
BROAP VIS40 VISCOSITY 40 ◦C ASTM D445 100ml MONTHLY
KF KARL FISHER WATER TEST ASTM D4928
TAN TOTAL ACID NUMBER ASTM D974,ASTM D664
COP COLOR,ODOR,CLARITY,PRECIPITATE,FOAM PMC
SP ICP SPECTROMETRIC ANALYSIS ASTM D5185
VIS40 VISCOSITY 40 ◦C ASTM D445
RRF KF KARL FISHER WATER TEST ASTM D4928 100ml MONTHLY
(HVAC UNIT) TAN TOTAL ACID NUMBER ASTM D974,ASTM D664
COP COLOR,ODOR,CLARITY,PRECIPITATE,FOAM PMC
TRANSMISSIONAutomatic transmission, Constant Mesh transmission, Hydrostatic transmission,
Planetary transmission, Manual transmission, Semi-Automatic transmission,
TESTING PACKAGE CODE CODE DESCRIPTION METHOD SAMPLE VOLUME REQ. CALENDAR
SP ICP SPECTROMETRIC ANALYSIS ASTM D5185
MOBFT FTIR FOURIER TRANSFORM INFRARED ANALYSIS JOAP 100ml MONTHLY
FU FUEL DETECTION ASTM D3828
HP CRACKLE TEST PMC
COP COLOR,ODOR,CLARITY,PRECIPITATE,FOAM PMC
SP ICP SPECTROMETRIC ANALYSIS ASTM D5185
FTIR FOURIER TRANSFORM INFRARED ANALYSIS JOAP
MOBT VIS40 VISCOSITY 40 ◦C (MOBT PACKAGE) ASTM D445
OR VIS100 VISCOSITY 100 ◦C (MOBFTV PACKAGE) ASTM D445 100ml MONTHLY
MOBFTV FU FUEL DILUTION ASTM D3828
HP CRACKLE TEST PMC
COP COLOR,ODOR,CLARITY,PRECIPITATE,FOAM PMC
SP ICP SPECTROMETRIC ANALYSIS ASTM D5185
FTIR FOURIER TRANSFORM INFRARED ANALYSIS JOAP
VIS40 VISCOSITY 40 ◦C (MOBPT PACKAGE) ASTM D445
MOBPT VIS100 VISCOSITY 100 ◦C (MOBPLUS PACKAGE) ASTM D445
OR TAN TOTAL ACID NUMBER (MOBPT PACKAGE) ASTM D974,ASTM D664 100ml MONTHLY
MOBPLUS TBN TOTAL BASE NUMBER (MOBPLUS PACKAGE) ASTM D4739
FU FUEL DILUTION ASTM D3828
HP CRACKLE TEST PMC
COP COLOR,ODOR,CLARITY,PRECIPITATE,FOAM PMC
DIFFERENTIALLimited Slip differential, Locking differential, Open differential,
Posi-Traction Differential, Torsen differential
TESTING PACKAGE CODE CODE DESCRIPTION METHOD SAMPLE VOLUME REQ. CALENDAR
SP ICP SPECTROMETRIC ANALYSIS ASTM D5185
FTIR FOURIER TRANSFORM INFRARED ANALYSIS JOAP
DROT VIS40 VISCOSITY 40 ◦C ASTM D445 100ml MONTHLY
DR DIRECT READING PMC
COP COLOR,ODOR,CLARITY,PRECIPITATE,FOAM PMC
SP ICP SPECTROMETRIC ANALYSIS ASTM D5185
FTIR FOURIER TRANSFORM INFRARED ANALYSIS JOAP
VIS40 VISCOSITY 40 ◦C ASTM D445
DROTP DR DIRECT READING PMC 100ml MONTHLY
KF KARL FISHER WATER TEST ASTM D4928
TAN TOTAL ACID NUMBER ASTM D974,ASTM D664
COP COLOR,ODOR,CLARITY,PRECIPITATE,FOAM PMC
OPTIMIZATION STUDIES FOR OIL CHANGEOUT
Mobile Engine
Industrial Equipment
TESTING PACKAGE CODE CODE DESCRIPTION METHOD SAMPLE VOLUME REQ. CALENDAR
SP ICP SPECTROMETRIC ANALYSIS ASTM D5185
FTIR FOURIER TRANSFORM INFRARED ANALYSIS JOAP
VIS40 VISCOSITY 40 ◦C ASTM D445
OPT VIS100 VISCOSITY 100 ◦C ASTM D445 100ml ON DEMAND
TBN TOTAL BASE NUMBER ASTM D4739
VI VISCOSITY INDEX ASTM D2270
COP COLOR,ODOR,CLARITY,PRECIPITATE,FOAM PMC
TESTING PACKAGE CODE CODE DESCRIPTION METHOD SAMPLE VOLUME REQ. CALENDAR
SP ICP SPECTROMETRIC ANALYSIS ASTM D5185
FTIR FOURIER TRANSFORM INFRARED ANALYSIS JOAP
VIS40 VISCOSITY 40 ◦C ASTM D445
OST VIS100 VISCOSITY 100 ◦C ASTM D445 100ml ON DEMAND
TAN TOTAL ACID NUMBER ASTM D974,ASTM D664
VI VISCOSITY INDEX ASTM D2270
COP COLOR,ODOR,CLARITY,PRECIPITATE,FOAM PMC
GREASERoulements, Compresseurs, Différentiel,
Boîte à engrenages, Transmission, Turbine
TESTING PACKAGE
CODE CODE DESCRIPTION METHOD
SAMPLE VOLUME
REQ. CALENDAR
GRS GRS ICP SPECTROMETRIC ANALYSIS PMC 2g MONTHLY
GRSPQ GRS ICP SPECTROMETRIC ANALYSIS PMC 10g MONTHLY
PQ PARTICLE QUANTIFIER INDEX PMC
VARNISHCompresseurs, Boîtes à engrenages, Hydraulique, Turbines
TESTING PACKAGE
CODE CODE DESCRIPTION METHOD
SAMPLE VOLUME
REQ. CALENDAR
QSA QUANTITATIVE SPECTROPHOTOMETRIC ANALYSIS (QSA) PMC
VBT GAF GRAVIMETRIC ANALYSIS (FILTRATION) PMC 200 ml QUARTERLY
COPOF COLOR,ODOR,CLARITY,PRECIPITATE,FOAM PMC
Test Reports
Sample Report
Sample Report
Sample Report
Sample Report
Sample Report
Sample Report
QUESTIONS
GREASE ANALYSIS
Moussa ZIDOUNE, Ph. D., ChemistLaboratory Director
Training Session, June 2013
Grease is solid or semi solid lubricant made up of approximately 75 - 90% oil, 5 - 20% thickeners (SOAP) and 0 – 15% additives.
What is Grease ?
Grease-Base oils
• Base oil does the lubrication so Viscosity is critical
• Base oils are divided into : • mineral • synthetic
• The type and characteristics of the oil determine the basic properties of the grease.
• Common Thickeners are:
– Calcium
– Lithium
– Sodium
• Lithium base greases, refers to the thickening component.
• Oxidation inhibitors– Prolong the life of the grease.
• EP Agents– Guards against Scoring and Galling.
• Anti-Corrosion Agents.– Protect metal against attack from water, sulfidesor corrosive elements.
• Anti wear Agents.– Prevent abrasion and metal to metal contact.
Grease additives
• Grease is used to:
• Reduce friction and wear• Provide corrosion protection• Resist leakage, dripping and throw-off• Stays in place under conditions of application• Self sealing• Compatible with seals• Tolerate or repel moisture
Grease Function
GREASEBearings, Compressors, Differentials,
Gearbox, Transmissions, Turbines
TESTING PACKAGE
CODE CODE DESCRIPTION METHOD
SAMPLE VOLUME
REQ. CALENDAR
GRS GRS ICP SPECTROMETRIC ANALYSIS PMC 2g MONTHLY
GRSPQ GRS ICP SPECTROMETRIC ANALYSIS PMC 10g MONTHLY
PQ PARTICLE QUANTIFIER INDEX PMC
• GRS testing is an elemental Analysis by ICP (inductively coupled plasma) for monitoring small particles that can be present in used grease due to mechanical wear, grease contamination or additive depletion.
Wear metals include: iron, copper, lead, tin, chromium, aluminum, silver, nickel, magnesium, vanadium, titanium, cadmium and manganese.
Grease contaminants include: silicon, boron, aluminum, sodium, and potassium.
Additives include: lithium, phosphorous, zinc, calcium, barium, boron, sodium, molybdenum, magnesium, silicon and aluminum.
Dropping point is the temperature at which thegrease starts to melt when heated.
A rule of thumb is to select 50 c belowthe dropping point.
Dropping point
Grease is rated by it’s penetration Rate using a standard cone
Dropped into the sample and measuring thepenetration in 10ths /millimeter.
This determines the NLGI consistency # On the tube: 000, 00 ,0 ,1 , 2 , 3, 4 , 5 , 6.
Cone Penetration
• Although many similar greases are compatible, assume they are not.
• Label all guns with tag/colour code• Grease points labeled (qty.&type)/colour
code• Electric motors: supply rebuilder with our
grease to ensure compatibility• Correct re-greasing procedure
Greasing Best Practices:
COOLANT ANALYSIS
Moussa ZIDOUNE, Ph. D., ChemistLaboratory Director
Training Session, June 2013
Agenda
• Engine coolant definition
• Benefit of coolant testing
• Coolant properties
• Coolant analysis
• Reports and Interpretation
• Conclusion
• An engine coolant is a heat transfer fluid designed to remove excess heat from an internal combustion engine.
• They usually consist of a mixture of water with ethylene glycol or propylene glycol.
What’s the Engine Coolant ?
Glycol and water are the main constituents (50%/50%) of antifreeze or coolant liquids.
Ethylene Glycol (High heat transfer)
Propylene Glycol (More toxic, less popular)
Additives: borates, molybdates, silicates, nitrates, potassium ...etc
What’s the Engine Coolant ?
Why Test your Coolant Fluid?
Most people don’t pay much attention to the condition of their cooling system… until it’s too late!
Yet, over 40% of all maintenance problems on diesel engines can be attributed to poor maintenance of the cooling system.
• Freezing liquids increase in volume (just like water) and acquire a rock solid physical force strong enough to crack hoses, radiators and even break engine metal (cylinder head or cylinder block) to waste.
• Antifreeze compounds decompose under high temperature, producing a corrosive acid in the cooling circuit.
• They are vulnerable to contamination by stain, oil.
Consequences of Coolant Degradation
• Prolongation of the useful life and reliability of the engine;
• Reduction of maintenance costs;
• Improved engine oil perfermance
• Optimize coolant drain intervals
• Indicate when coolant should be replaced
• Can give indications as to other engine problems early
Benefits of Coolant Analysis
• Clean coolant promotes cooler working temperatures
• Properly maintained coolant means fewer coolant changes.
• Determine safe fluid service life
• Identifies the wear of mechanism
• Identify maintenance problems before engine failre occurs
• Failure prevention;
Benefits of Coolant Analysis
• DEN - Density• COC - Conductivity • FRT - Freezing Point• BP - Boiling Point• GLYCP (%) - Glycol percentage • pH • CSP – Spectrometric Analysis• IC – Ion Chromatography
Recommended Coolant Tests
COC – ConductivityDEN - Density
• Conductivity : Measure the rate of the dissolved salts in the coolant.– The ability of the liquid to transmit electrical current.– When this value is high, the coolant should be
changed.
• Density : Describes the ratio of mass and volume of a liquid
- Density can help determine the composition of the cooling fluid.
FRT - Freezing PointBP - Boiling Point
Freezing Point -Temperature at which the coolant freeze
- Freeze point is dependent upon the concentration of antifreeze in an engine coolant.
Boiling Point - Temperature at which the coolant boil
- Boil Point is dependent upon the concentration of antifreeze in an engine coolant.
COP- Visual observation GLYCP - Glycol Percentage (%)
• COP - appearance, color, odor, deposits & foam
• GLYCP - Measure the percentage of Glycol present in the coolant by refrectometer.
- Concentration of 50/50 (glycol/water) is acceptable. Below -35 C a 60/40 mixture is recommended.
- Glycol concentration higher than 70 %, the freeze point is not improved and heat transfer capacity is reduced and additives may not be totally dissolved.
pH - Coolant
pH - Detemines whether the solution is acid, neutral or basic
The pH level of cooling fluid is measured to ensure a stable range between 7.5 and 11 to provide adequate corrosion protection.
An acidic pH will cause corrosion of ferrous components while a basic pH will cause corrosion of copper and aluminum components.
SP - Analytical Spectroscopy-Coolant
Detects 17 elements (Particles <6 microns in size)
Wear Metalsiron, copper, lead, tin, chromium, aluminum, silver, Zinc
and nickel.
Contamination- Silicium, Aluminium
Additives - Sodium, Boron, Sodium, Silicium, Potassium
• Aluminum • Boron • Calcium • Chrome • Copper • Iron • Lead • Magnesium • Molybdenum • Nickel • Potassium • Phosphorous • Silicium • Sodium • Tin • Titanium • Zinc
• Additives (nitrite & nitrate), which metal protecting inhibitors • Contaminants (chloride & sulfate), resulting from spring water or
air leaks.• Degradation Acids (glycolate, formate & oxalate), resulting from
the thermal breakdown of ethylene glycol
IC – Ion Chromatography
The ion chromatography test provides quantitative determination of common anions in coolant in the mg/L to low percent range in parts per million (ppm).
Recommended Coolant package
TESTING PACKAGE CODE CODE DESCRIPTION METHOD SAMPLE VOLUME REQ. CALENDAR
CSP ICP SPECTROMETRIC ANALYSIS PMC
DEN DENSITY OF GLYCOL ASTM D1298
FRT FREEZING POINT ASTM D1177
COOL PH pH MEASUREMENT ASTM D1287 600ml MONTHLY
COC CONDUCTIVITY OF COOLANT PMC
GLYCP GLYCOL PERCENTAGE PMC
TDS TOTAL DISSOLVED SOLIDS PMC
COP COLOR,ODOR,CLARITY,PRECIPITATE,FOAM PMC
SUPPLEMENTAL TESTS CODE DESCRIPTION METHOD SAMPLE VOLUME REQ. CALENDAR
BP BP BOILING POINT ASTM 1120 50ml MONTHLY
COOLANT REPORT EXPLANATION
QUESTIONS ?
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