Typical commercial laboratory turn around - two days to two weeks In-house hexane/gravimetric several hours Results in the discharge of effluent

Transcription

1 On-site Oil and Grease Measurements in under a Minute Sandy Rintoul Wilks Enterprise, Inc. IPEC Booth #3 srintoul@wilksir.com

2 Portable Field or Lab Analyzer Results in < 1 minute Rugged and Easy to Use Over 2200 in use worldwide today

3 Off shore oil rigs Refineries Industrial Wastewater TPH in Soil Remediation

4 Monitoring Using an Offsite Lab = Delayed Results

5 Monitoring Using an Offsite Lab Typical commercial laboratory turn around - two days to two weeks In-house hexane/gravimetric several hours Results in the discharge of effluent above regulatory limit for extended time Or puts equipment on hold at a remediation site Add costs in time and dollars

6 Non Compliance The sooner the industry or regulating agency can detect non compliance The sooner the problem can be corrected

7 What is needed: A quick, accurate and simple field and/or in-plant analysis: Available with the Portable Infrared Analyzers

8 Basic Measurement Concept Infrared Analysis: Hydrocarbons have a characteristic absorbance in the infrared region: 2930 cm- 1 or 3.4 microns

9 Basic Measurement Concept Infrared Analysis: Filter based infrared analyzers use a filter to select this wavelength 2930 cm- 1 or 3.4 microns

10 Spectrum of a hydrocarbon (red) Overlaid with a 3.4 micron filter (black)

11 Infrared Absorbance The amount of energy absorbed is proportional to the amount of oil/grease in the sample: A higher oil and grease concentration has a higher infrared absorbance A lower oil and grease concentration has a lower infrared absorbance

12 Solvent Extraction/Infrared Analysis Water Add 10 ml solvent to 100ml sample (10 to 1 ratio) Shake for 2 minutes A portion of the solvent is presented to the analyzer for analysis

13 Solvent Extraction/Infrared Analysis Soil Add 10 ml solvent to 10 grams soil (1 to 1 ratio) Shake for 2 minutes Filter A portion of the solvent is presented to the analyzer for analysis

14 Two different sample systems available depending on desired measurement range and extraction solvent Model CVH Model HATR-T2T2

15 Solvent CVH Perchloroethylene, Freon, S-316 HATR-T2 hexane, pentane, Vertrel MCA Minimum Detection Limit 2 ppm 8 ppm Component Measured Measures all hydrocarbons Instrument Repeatability +/- 2 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. Measures hydrocarbons with a boiling point higher than the solvent volatile hydrocarbons will be evaporated along with the solvent. Solvents are lighter than water and solvent sample can be collected from the top of the container.

16 The Measurement of Oil using Hexane, Pentane, Vertrel MCA Model HATR-T2T2

17 The hexane evaporates leaving an oil film on the crystal Oil Film Source ATR crystal A = log (I r / I a ) Filters (I r / I a ) Dual Detector

18 Infrared light (source) is focused on the end of the crystal Oil Film Source ATR Crystal A = log (I r / I a ) Filters (I r / I a) Dual Detector

19 The infrared light reflects off the surface of the crystal Oil Film Source ATR Crystal A = log (I r / I a ) Filters (I r / I a ) Dual Detector

20 At each reflection, the infrared light penetrates into the oil film and is absorbed by the oil at 2930cm -1 Infrared light Sample Oil Film

21 The infrared light is focused on to a detector containing a 2930cm - 1 filter Oil Film Source ATR crystal Filters (I r / I a ) Dual A = log (I r / I ) a Detector

22 Preset timer allows hexane to evaporate After timer countdown Value is displayed

23 Cleaning the Trough Crystal Add enough solvent to cover crystal Wipe the crystal

24 Analysis Procedure The whole analysis, from sample collection to final result, takes under 15 minutes An operator with minimal training can do the analysis

25 Measurement Range Hexane extraction Soil mg/kg * Water ppm* * the upper limit can be extended by dilution

26 Repeatability of the Hexane/Infrared Method Repeated runs on same sample: + 02 Independent applications of sample: + 03

27 The Measurement of Oil using S-316 or Perchloroethylene Model CVH

28 ASTM Infrared Oil and Grease Method to replace Freon/IR Method ASTM Method D7066: Standard Test Method for dimer/trimer of chlorotrifluoroethylene (S-316) Recoverable Oil and Grease and Nonpolar Material by Infrared Determination

29 ASTM Method D Uses a transmission cell - Model CVH Measures volatile constituents

30 The Measurement of IR Absorption of an Oil Sample with a Cuvette Sample Filters (I R / I A ) Source Detectors A = log I R / I A

31 Cuvette is filled with solvent extract

32 Cuvette is placed in the analyzer After 15 seconds, Oil and Grease value is displayed

33 Measurement Range S-316 or Perchloroethylene: Soil: mg/kg Water: ppm* * the upper limit can be extended by dilution

34 Repeatability of the S-316 or perc/infrared Method Repeated runs on same sample: + 02 Independent applications of sample: + 03

35 Comparing Different Analytical Procedures

36 Oil and Grease Not a unique chemical entity A mixture of chemical species that vary from source to source It is defined by the analytical procedure, ie: infrared, gravimetric, GC/FID

37 Comparing Different Analytical Infrared Gravimetric Procedures Gas Chromatograph/Flame Ionization Detector (GC/FID) Ultraviolet Each method measures different physical properties

38 Technology Infrared Gravimetry GC/FID Ultraviolet What is Measured All analytes removed from the samples by the extraction solvent that contain a C-H stretching absorption All analytes removed from the sample by the extraction solvent that are not volatilized All analytes removed from the sample by the extraction solvent that can be chromatographed and that respond to the detector Aromatics only What is Not Measured Very polar organics Volatiles Very polar or involatile compounds depending on choice of column, temperature program, time, etc. Aliphatics

39 Note: Ultraviolet (UV) measures only the aromatic hydrocarbons in a water sample. If the aromatic/ aliphatic ratio changes, the reading will not be correct. Infrared measure both the aromatic and the aliphatic hydrocarbons.

40 Comparison of Hexane/Infrared and Meat Packing Plant Hexane/Gravimetric Infrared Gravimetric Sample 1 67 ppm 70 ppm Sample After Grease Trap at a Restaurant Sample Sample Sample Sample Sample

41 Same Samples, Three Different Laboratories InfraCal Wilks InfraCal Lab 1 Lab 2 Lab 3 Customer <5

42 Using this simple and quick infrared procedure, operators of a pretreatment system can: Quickly and easily assess their system s efficiency Take samples before and after treatment Change their system s parameters and immediately test the results of their changes See how their system functions under heavy loads Avoid discharging effluent that is above the regulatory limit

43 Using this simple and quick infrared procedure, operators at a remediation site: Quickly determine the limits of contamination Avoid putting excavation equipment on hold while waiting for lab results Reduce laboratory cost by sending less samples to lab

44 Advantages of Filter Based Infrared Analyzers No moving parts Rugged and portable Easy to operate Can be battery operated for on-site analysis Sandy Rintoul Wilks Enterprise, Inc. IPEC Booth #3