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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