InfraCal™ TOG/TPH Analyzer Solvent Selection Guide
Since the Montreal Protocol banned the production of Freon-113, the search has been on to find a suitable replacement solvent for measuring total oil and grease (TOG) and total petroleum hydrocarbon (TPH) levels in water and soil using infrared analysis. Wilks Enterprise has studied potential candidates for Freon replacement and have found several that are usable. Their characteristics, along with those of Freon-113 are described in the following chart. Please note, there are other infrared transmitting solvents that can be used for TOG/TPH analyses.
SOLVENTS
Freon-113 A volatile CFC compound previously specified for EPA Methods 413.2 and 418.1. While its manufacture has been discontinued, its use had been extended by the EPA until 2003 and it is readily available in many parts of the world. Since it is heavier than water, the solvent still after extraction will be on the bottom. Because of its infrared transparency, it can be used with a 10mm cuvette cell. Freon is ideal for applications requiring the measurement of light ends, as well as, the heavier components in water and soil samples.

Perchloroethylene A moderately volatile non-hydrocarbon solvent that that is being used as a replacement for Freon-113. Many grades are stabilized with hydrocarbons that make them unsuitable for TOG and TPH analysis. Hydrocarbon-free grades are available which make them usable for analysis by IR transmission methods. Since its heavier than water, the solvent after extraction will be on the bottom. Presently accepted as a Freon replacement in the UK. The perchloroethylene must be a spectroscopic grade that has not been stabilized with any hydrocarbon compound.

AK-225 A volatile HCFC solvent that nevertheless has low ozone depletion efficiency. It can be used as a replacement solvent for Freon-113. However, because of absorption in the C-H region, it has lower sensitivity than Freon-113 but is still usable for analysis by transmission methods. AK-225 is heavier than water and, therefore, the solvent after extraction will be on the bottom. At the lower concentration ranges, some method of moisture removal such as sodium sulfate may be required.

S-316 A proprietary, non-hydrocarbon solvent said by its manufacture to be environmentally safe. Since S-316 is heavier than water, the solvent after extraction will be on the bottom. Because of its transparency in the C-H region, it can be used with a 10mm cuvette. Approves S-316 as a replacement solvent for Freon. ASTM Standard Test Method D 7066-04.

Hexane A volatile hydrocarbon that is specified for EPA Method 1664. Because it is a hydrocarbon, it must be evaporated prior to making the infrared measurement to determine TOG or TPH levels in a sample, which takes approximately 3 - 5 minutes. Since hexane is lighter than water, the solvent, after extraction will rest on top, making it easy to deliver a measured amount of extract to the sample platform or plate with a 50 microliter auto pipette without losing any of the sample.

Pentane A volatile hydrocarbon preferred in Scandinavian countries over Hexane. Similar in performance and use to hexane although it has a lower boiling point and therefore will retain more of the low boiling point components. Pentane is lighter than water and like hexane will rest on top after the extraction.

Vertrel MCA A volatile HFC solvent that has been used primarily as a replacement solvent for Freon in cleaning operations. Because of its hydrocarbon absorption, like hexane, it must be evaporated prior to making the infrared measurement to determine TOG or TPH levels. Vertrel MCA is a suitable solvent to use instead of hexane. Vertrel MCA has no ozone depleting potential, is non-flammable and has low toxicity. As Vertrel MCA is heavier than water, the solvent after extraction will rest on the bottom. A microliter glass pipette can be used when preparing a sample; however, because of the weight of Vertrel, the extract should be delivered to the sample platform or plate with a 50 microliter syringe, rather than a pipette for analysis.

Solvent for Extraction Process
Freon-113PerchloroethyleneAK-225S-316HexanePentaneVertrel
Recommended Grade Purity99+%99+%
hydrocarbon
free
99+%N/A95+%95+%MCA
Extraction Efficiency91%87%88%98%98%98%95%
Infrared MethodTransmissionTransmissionTransmissionTransmissionATR/ EvaporationATR/ EvaporationATR/ Evaporation
Boiling Point
(0C)
4812154134693639
Recommended Drying
Time (minutes)
N/AN/AN/AN/A3:00-5:00*3:00-5:00*3:00-5:00*
% Usable Energy at C-H Band89812880000
Includes/Loses Volatile
Components
IncludesIncludesIncludesIncludesLosesLosesLoses
Recommended InfraCal
Model(s)
CVHCVHCVHCVHHATR-T2, CHHATR-T2, CHHATR-T2, CH
Useful Range (ppm) (1)(3)
Water
10:1 extraction ratio
CVH 2-1000CVH 2-1000CVH 2-1000CVH 2-1000HATR-T2 4-1000
CH 40-2000
HATR-T2 4-1000
CH 40-2000
HATR-T2 4-1000
CH 40-2000
Useful Range (ppm) (2)(3)
Soil
1:2 extraction ratio
CVH 3-5000CVH 3-5000CVH 3-5000CVH 3-5000HATR-T 20-5000
CH 200-5000+
HATR-T 20-5000
CH 200-5000+
HATR-T 20-5000
CH 200-5000+
Approved or Screening MethodApproved
EPA
413.2/418.1
Screening
Equivalent to
EPA 413.2/418.1
Screening
Equivalent to
EPA 413.2/418.1
Approved ASTM
Method D 7066-04
Screening
Equivalent to
EPA 413.2/418.1
Screening
Corelates to
EPA 1664
Screening
Correlates to
EPA 1664
Screening
Correlates to
EPA 1664
Average Analysis Time including extraction (minutes)10-1510-1510-1510-1510-1510-1510-15
(1) Based on an extraction ratio of 10 parts of water to one part solvent (10:1 ratio).
(2) Based on an extraction ratio of one part soil to two parts of solvent (1:2 ratio). Higher levels of TPH can be sampled by increasing the raio of solvent to soil.
(3) The useful measurement range is based on the average operator's sample handling skill level to obtain reproducible data. Lower minimum detectable levels may be achieved if the operator has a high degree of sample handling expertise.
N/A = Not Applicable * Recommended time for use on off-shore oil platforms is 5 minutes
Solvent Selection Guide (pdf).
WILKS ENTERPRISE, Inc. InfraCal

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