InfraCal TOG/TPH Analyzers InfraCal TOG/TPH Analyzers for for

Oil and Grease MeasurementsOil and Grease Measurements

www.WilksIR.com

Portable Field or Lab AnalyzerPortable Field or Lab Analyzer

Results in < 30 secondsResults in < 30 seconds

Rugged and Easy to UseRugged and Easy to Use

Over 2000 in use worldwide todayOver 2000 in use worldwide today

Off shore oil rigsOff shore oil rigs

RefineriesRefineries

Industrial WastewaterIndustrial Wastewater

Metal Parts CleaningMetal Parts Cleaning

Monitoring Using an Offsite LabMonitoring Using an Offsite Lab

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Delayed ResultsDelayed Results

Typical commercial laboratory turn around - two Typical commercial laboratory turn around - two days to two weeksdays to two weeks

In-house hexane/gravimetric—several hoursIn-house hexane/gravimetric—several hours

Results in the discharge of effluent above Results in the discharge of effluent above regulatory limit for extended timeregulatory limit for extended time

Add costs in time and dollars Add costs in time and dollars

Monitoring Using an Offsite LabMonitoring Using an Offsite Lab

Non ComplianceNon Compliance

The sooner the industry or regulating agency The sooner the industry or regulating agency can detect non compliancecan detect non compliance

The sooner the problem can be correctedThe sooner the problem can be corrected

What is needed:What is needed:

A quick, accurate and simple A quick, accurate and simple

field and/or in-plant analysis:field and/or in-plant analysis:

Available with the Available with the

InfraCal TOG/TPH AnalyzerInfraCal TOG/TPH Analyzer

Two different models available Two different models available depending on desired measurement depending on desired measurement

range and extraction solventrange and extraction solvent

Model CVH Model CVH Model HATR-T2Model HATR-T2

  CVH HATR-T2 Minimum Detection Limit 2 ppm 8 ppm

Solvent Perchloroethylene, Freon, S-316

hexane, pentane, Vertrel MCA

Component Measured Measures all hydrocarbons Measures hydrocarbons with a boiling point higher than the solvent—volatile hydrocarbons will be evaporated along with the solvent.

Instrument Repeatability +/- 1 ppm +/- 2 ppm

Other Solvents are heavier than water and require a seperatory

funnel or inverted vial with a septa cap to collect a solvent

sample.

Solvents are lighter than water and solvent sample can be collected from the

top of the container.

Acidify sample to pH of 2Acidify sample to pH of 2

Add 10 ml solvent to 100ml sample (10 to 1 ratio)Add 10 ml solvent to 100ml sample (10 to 1 ratio)

Shake for 2 minutesShake for 2 minutes

A portion of the solvent is A portion of the solvent is presented to the analyzer for presented to the analyzer for analysisanalysis

Measuring Oil in Water withMeasuring Oil in Water withthe InfraCal TOG/TPH Analyzerthe InfraCal TOG/TPH Analyzer

Basic Measurement ConceptBasic Measurement Concept

Infrared Analysis:Infrared Analysis:

Hydrocarbons have a characteristic Hydrocarbons have a characteristic absorbance in the infrared region:absorbance in the infrared region:

2930 cm-2930 cm-11 or 3.4 microns or 3.4 microns

Spectrum of a hydrocarbon (red)Spectrum of a hydrocarbon (red)

Overlaid with a 3.4 micron filter (black)Overlaid with a 3.4 micron filter (black)

Infrared AbsorbanceInfrared Absorbance

The amount of energy absorbedThe amount of energy absorbed is proportional to the amount ofis proportional to the amount of

oil/grease in the sample: oil/grease in the sample:

A higher oil and grease concentration A higher oil and grease concentration has a higher infrared absorbancehas a higher infrared absorbance

A lower oil and grease concentration A lower oil and grease concentration has a lower infrared absorbancehas a lower infrared absorbance

The Measurement of Oil using The Measurement of Oil using HexaneHexane

Model HATR-T2Model HATR-T2

The hexane evaporates leaving an The hexane evaporates leaving an oil film on the crystaloil film on the crystal

Oil Film

ATR crystal Source

Dual Detector

Filters (Ir / Ia) A = log (I r / I a )

Infrared light (source) is focused on the Infrared light (source) is focused on the end of the crystalend of the crystal

Oil Film

ATR Crystal

Source Dual Detector

Filters (Ir / Ia)

A = log (I r / I a )

The infrared light reflects offThe infrared light reflects off the surface of the crystal the surface of the crystal

Oil Film

ATR Crystal Source

Dual Detector

Filters (Ir / Ia)

A = log (I r / I a )

At each reflection, the infrared light At each reflection, the infrared light penetrates into the oil film and is absorbed penetrates into the oil film and is absorbed

by the oil at 2930cmby the oil at 2930cm-1-1

Sample

Internal Reflectance Element (IRE)Source

DualDetector

Filters (Ir / Ia)

A = log (Ir / Ia)

Oil Film

Infrared light

The infrared light is focused on to The infrared light is focused on to a detector containing a a detector containing a

2930cm2930cm-1-1 filter filter

Oil Film

ATR crystal Source

Dual Detector

Filters (Ir / Ia)

A = log (I r / I a )

A higher oil and grease concentration A higher oil and grease concentration has a higher infrared absorbancehas a higher infrared absorbance

A lower oil and grease concentration A lower oil and grease concentration has a lower infrared absorbancehas a lower infrared absorbance

Preset timer allows Preset timer allows hexane to evaporatehexane to evaporate

After timer After timer countdown and 15 countdown and 15 second run timesecond run time

Value is displayedValue is displayed

Cleaning the Trough CrystalCleaning the Trough Crystal

Add enough solvent Add enough solvent to cover crystalto cover crystal

Wipe slowly across Wipe slowly across the crystalthe crystal

Analysis ProcedureAnalysis Procedure

The whole analysis, from sample The whole analysis, from sample collection to final result, takes under 15 collection to final result, takes under 15 minutesminutes

An operator with minimal training can An operator with minimal training can do the analysisdo the analysis

Measurement RangeMeasurement Range

Hexane extraction: 10- 300 ppmHexane extraction: 10- 300 ppm**

** the upper limit can be extended by dilutionthe upper limit can be extended by dilution

Repeated runs on same sample: Repeated runs on same sample: ++ 01 01

Independent applications of sample: Independent applications of sample: ++ 02 02

Independently prepared samples: Independently prepared samples: ++0303**

* * Repeatability is dependent on how carefully the Repeatability is dependent on how carefully the analyst does the extractionanalyst does the extraction

Repeatability of the Hexane/Infrared Repeatability of the Hexane/Infrared MethodMethod

The Measurement of Oil using The Measurement of Oil using S-316 or PerchloroethyleneS-316 or Perchloroethylene

Model CVHModel CVH

ASTM Infrared Oil and Grease Method to ASTM Infrared Oil and Grease Method to replace Freon/IR Methodreplace Freon/IR Method

ASTM Method D7066-04:ASTM Method D7066-04:

Standard Test Method for dimer/trimer of Standard Test Method for dimer/trimer of chlorotrifluoroethylene (S-316) chlorotrifluoroethylene (S-316) Recoverable Oil and Grease and Nonpolar Recoverable Oil and Grease and Nonpolar Material by Infrared DeterminationMaterial by Infrared Determination

ASTM Method D 7066-04ASTM Method D 7066-04

Uses a transmission cell - Model CVHUses a transmission cell - Model CVH

Measures volatile constituentsMeasures volatile constituents

The Measurement of IR Absorption ofThe Measurement of IR Absorption ofan Oil Sample with a Cuvettean Oil Sample with a Cuvette

A = log IR / IA

Filters (IR / IA )Sample

Source Detectors

InfraRed light passes through the cuvette filled with solvent from the sample extract

A = log IR / IA

Filters (IR / IA )Sample

Source Detectors

The amount of IR energy absorbed by the sample correlates to the concentration of

oil and grease in the sample

The infrared light is focused on to The infrared light is focused on to a detector containing a a detector containing a

2930cm2930cm-1-1 filter filter

Cuvette is filled with Cuvette is filled with solvent extractsolvent extract

Cuvette is placed in the analyzerCuvette is placed in the analyzer

After 30 seconds,After 30 seconds,Oil and Grease value is displayedOil and Grease value is displayed

Measurement RangeMeasurement Range

S-316 or Perchloroethylene:S-316 or Perchloroethylene: 2 -300 2 -300

ppmppm**

** the upper limit can be extended by dilutionthe upper limit can be extended by dilution

Repeatability of the Repeatability of the S-316 or perc/Infrared MethodS-316 or perc/Infrared Method

Repeated runs on same sample: Repeated runs on same sample: ++ 01 01

Independent applications of sample: Independent applications of sample: ++ 01 01

Independently prepared samples: Independently prepared samples: ++0202**

* * Repeatability is dependent on how carefully the Repeatability is dependent on how carefully the analyst does the extractionanalyst does the extraction

Comparing Different Analytical Comparing Different Analytical ProceduresProcedures

Oil and GreaseOil and Grease

Not a unique chemical entity Not a unique chemical entity

A mixture of chemical species that vary A mixture of chemical species that vary from source to sourcefrom source to source

It is defined by the analytical procedure, It is defined by the analytical procedure, ie: infrared, gravimetric, GC/FIDie: infrared, gravimetric, GC/FID

Comparing Different Analytical Comparing Different Analytical ProceduresProcedures

InfraredInfrared

GravimetricGravimetric

Gas Chromatograph/Flame Gas Chromatograph/Flame Ionization Detector (GC/FID)Ionization Detector (GC/FID)

Ultra VioletUltra Violet

Each method measures different physical Each method measures different physical propertiesproperties

Technology Technology

InfraredInfraredAll analytes removed from All analytes removed from the samples by the the samples by the extraction solvent that extraction solvent that contain a C-H stretching contain a C-H stretching absorption.absorption.

All analytes removed from All analytes removed from the sample by the extraction the sample by the extraction solvent that are not solvent that are not volatilized.volatilized.

All analytes removed from All analytes removed from the sample by the extraction the sample by the extraction solvent that can be solvent that can be chromatographed and that chromatographed and that respond to the detector.respond to the detector.

Aromatics only

Very polar organics Very polar organics

VolatilesVolatiles

Very polar or involatile Very polar or involatile compounds depending compounds depending on choice of column, on choice of column, temperature program, temperature program, time, etc. time, etc.

Aliphahtics

GravimetryGravimetry

GC/FIDGC/FID

What is What is MeasuredMeasured

What is Not What is Not MeasuredMeasured

Ultra VioletUltra Violet

Note:Note:

Ultraviolet (UV) Ultraviolet (UV) measures only the aromatic measures only the aromatic hydrocarbons in a water sample. If the hydrocarbons in a water sample. If the aromatic/ aliphatic ratio changes, the aromatic/ aliphatic ratio changes, the reading will not be correct.reading will not be correct.

InfraredInfrared measure both the aromatic and the measure both the aromatic and the aliphatic hydrocarbons.aliphatic hydrocarbons.

Comparison of Hexane/Infrared and Comparison of Hexane/Infrared and Hexane/GravimetricHexane/Gravimetric

Meat Packing PlantMeat Packing Plant

Infrared Infrared GravimetricGravimetricSample 1Sample 1 67 ppm67 ppm 70 ppm70 ppmSample 2Sample 2 19901990 20202020

After Grease Trap at a RestaurantAfter Grease Trap at a Restaurant

Sample 1Sample 1 423423 415415Sample 2Sample 2 332332 300300Sample 3Sample 3 103103 130130Sample 4Sample 4 157157 170170Sample 5Sample 5 6767 7474

Same Samples, Same Samples, Three Different LaboratoriesThree Different Laboratories

InfraCal    InfraCal     InfraCal        InfraCal        Lab 1          Lab 1           Lab 2 Lab 2 Lab 3Lab 3Wilks         Wilks         CustomerCustomer  

51     51      49 49 67              23 67              23 5151  62           62              61               61             74               4374               43 4747  71           71              --               --              76               70 76               70 4949  63            63             53              53             66                 5566                 55 4040  3               3                1               1               14                714                7 <5<5  

Using this simple and quick infrared procedure, Using this simple and quick infrared procedure, operators of a pretreatment system can:operators of a pretreatment system can:

Quickly and easily assess their system’s Quickly and easily assess their system’s efficiency efficiency

Take samples before and after treatment Take samples before and after treatment

Change their system’s parameters and Change their system’s parameters and immediately test the results of their changesimmediately test the results of their changes

See how their system functions under heavy See how their system functions under heavy loads loads

Avoid discharging effluent that is above the Avoid discharging effluent that is above the regulatory limitregulatory limit

Oil and Grease Analysis with the Oil and Grease Analysis with the InfraCal TOG/TPH AnalyzersInfraCal TOG/TPH Analyzers

www.WilksIR.com

For questions or more information:For questions or more information:info@WilksIR.com info@WilksIR.com

203-855-9136203-855-9136