On-Site Measurement of Oil in

Water Using the InfraCal 2

AMETEK Spectro Scientific ©2021

What will be covered:
 Why do we measure for oil in water?
 Options for measuring oil in water
 What are the advantages of using a field
method?
 Measuring a sample with the InfraCal
 ATR-SP Specifications
 Calibrations
Why do we measure for TOG/TPH
and FOG?
 To stay within the regulatory limit
 . To avoid over-treatment of wastewater
 Recover any residual oil before disposal or
re-injection
 Maintain best environmentally conscientious
behavior
Lab-Based Methods for Oil in Water
 Gravimetric
 Common regulatory method (EPA 1664)

 Labor intensive, difficult

 GC-FID
 ISO 9377-2 approved

 Precise, provides info on hydrocarbon make-up

 Equipment is expensive and requires trained

personnel
Field-Based Methods for Oil in
Water
 UV Fluorescence
 Great for online systems

 Only detects aromatic components

 IR
 Can be both lab-based or field-based

 Portable and inexpensive

 Mainly measures aliphatic components

Why a field analyzer?
 Obtain an immediate on-site test result
to tune separator process
 For use in remote sites that require
portability
 To avoid regulatory fines
 Avoid lab delays

1-2 week lab delay can be costly!

InfraCal 2 – a well established field
tool
 The InfraCal has been an accepted
method for 25 years
 Thousands sold over the last few decades

 Compares with EPA 1664, ISO 9377-2, APHA 5520

 Complies with ASTM D7066

 Low cost and portable

 Requires minimal/no training
Analyzing a Sample
Simple 5 Step Process:

1. Sample collection
2. Solvent extraction
3. Separation
4. Deposit 60 ul on crystal
5. Take a reading
The Sampling Step
Objective: to obtain a representative sample
composition

Factors that can effect the representative nature of

the sample:
 Variability of the water stream
 Flow conditions/cleanliness the sample point
 The sample container
 Preservation of the sample
Sample Extraction

 Add 10 ml solvent to 100

ml sample (10:1 ratio)
 Shake for 2 minutes
 Hexane/oil separates to
top
 Break any emulsions, if
present
Separation of polar and non-polar
hydrocarbons

Solvent extraction

HEM/TOG/FOG

Petroleum hydrocarbons Animal/vegetable

Silica gel (non-polar materials) (polar materials)
treatment

SGT-HEM/TPH
ATR-SP Analyzer: Dispense sample on
analyzer
 Attenuated Total Reflection Method
 Hexane, Pentane, other volatile hydrocarbon solvents
 Dispense extraction 60μL onto crystal
 Evaporation: ~4 minutes
IR analysis for TOG/TPH/FOG
 Infrared spectroscopy has been used as a method
to look for TOG/TPH for more than 40 years
 Why? Hydrocarbons contain C-H bonds that absorb
infrared energy at 2930 cm-1
 IR is primarily counting aliphatic hydrocarbons

GREEN = IR spectrum
RED = InfraCal 2 filter band-pass
 ATR-SP – Important Parameters

ATR-SP
Range of measurement 0.3 – 2000 ppm
Solvent Hexane Pentane
Extraction Efficiency 98% 98%
Includes/Loses Volatiles Loses Loses
Estimated Cost (1 liter) $135 $105
Correlates to EPA 1664
Approved or Screening Method ASTM method under Correlates to EPA 1664
development
Range of Measurement
 The two standard ranges for the ATR-SP is 0-200 ppm with a
10:1 extraction or 0-2000 ppm with a 1:1 extraction.

 The ATR-SP can achieve and LOD of 0.3 ppm but this
requires strong technique.

 The ATR-SP can use a modified extraction/measurement

method that allows the instrument to measure up to 10% or
higher. This method requires either perchloroethylene or
S316 as the solvent rather than hexane and is typically used
for soil or drill cuttings analysis.
Solvent Choice
 Cost
 ATR-SP uses volatile solvents such as hexane and pentane. These
solvents tend to be easy to obtain both domestically and internationally
and are typically cheaper than traditional chlorofluorocarbon solvents.

 Toxicity
 In general, solvents for the ATR-SP are toxic but less toxic than
traditional chlorofluorocarbon solvents.

 Regional Preference
 Some regions of the world typically prefer one solvent over the other.
This can be based on availability or because it was the solvent of choice
for previous methods
Regulatory Method
 InfraCal ATR-SP is mainly used as a pre-compliance check rather than directly for
regulatory purposes.
 While trending with the regulatory method the InfraCal is being compared to is
most important, accuracy is important as well.
 No current ASTM method exists for the ATR-SP but one is in development.

 Gravimetric Regulatory Methods

 For customers using the InfraCal to compare to a gravimetric regulatory methods
such as EPA-1664, ATR-SP is a great choice.
 Both use the same solvent (hexane) and both require an evaporation. This
means neither method can measure volatile components making the correlation
stronger.

 Non-gravimetric Regulatory Methods

 ATR-SP can still be used to compare to non-gravimetric methods but differences
may be greater, especially if the sample contains significant amounts of volatile
hydrocarbons.
Additional Factors
 Sample Make-Up
 The ATR-SP cannot measure volatile hydrocarbons. Samples which contain significant
amounts of hydrocarbons are difficult to impossible to measure with the ATR-SP.
 The ATR-SP mainly measures aliphatic but not aromatic hydrocarbons. However, many
aromatic components contain branches that can still be measured by the ATR-SP so the
instrument will still se a response although it is weaker. Aromatic hydrocarbons are only
typically 10-20% of the chemical make-up.
 On rare occasions the ATR-SP struggles with samples with high amounts of fats. This has
to do with the crystal/oil interaction and a lot of times can be fixed.

 Ease of Use
 Generally, the ATR-SP requires little to no training for most users.
 While the ATR-SP is considered to have a good ease of use, this is relative to other
methods. The extraction, while simplified, is still a cumbersome and sometimes difficult
process.
ATR-SP Calibration Standards
 403-1044: For customers whose samples contain primarily
non-polar/petroleum hydrocarbons. Covers the range of 0-200 ppm
(10:1 extraction) or 0-2000 ppm (1:1 extraction).

 403-1072: For customers whose samples contain primarily FOG (fats,

oils, and grease). Covers the range of 0-200 ppm (10:1 extraction) or 0-
2000 ppm (1:1 extraction).

 403-1081: For customers whose samples contain primarly

non-polar/petroleum hydrocarbons and want a more precise calibration
below 10 ppm. Covers the range of 0-7.5 ppm (10:1 extraction).

 600-00149: For customers looking to measure % level oil in water/soil.

This is mainly used for testing soil or drill cuttings. The range covers
from 0.3-10% using a 1:1 extraction.
Questions?

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