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APP OilandGreaseinWaterbyMid-Infrared PDF
APP OilandGreaseinWaterbyMid-Infrared PDF
Infrared Spectroscopy
Author
Aniruddha Pisal
PerkinElmer, Inc.
Shelton, CT 06484 USA
Volumetric flasks 10, 25, 50 and 100 mL Absorbance measurements were performed using the
PerkinElmer Spectrum 400 FT-IR/NIR spectrometer
Eppendorf micropipette (PerkinElmer, Inc., Shelton, CT USA) in mid-IR mode. Other
Analytical balance instrument models such as the Spectrum 100 (pictured in
Figure 1), Spectrum 65 or Spectrum One can also be used.
Filter paper
The software used to acquire spectra was Spectrum version
Glass funnel 6.3. Spectra were collected in transmission mode using a
Glass wide mouth sample bottle 250 mL, with screw cap glass cell with 10 mm pathlength. Spectra were acquired
having a fluoropolymer liner over the range 32002700 cm-1 at 8 cm-1 resolution with
~1 minute acquisition time, and ratioed against a spectrum
Isooctane
of pure solvent. The peak maximum between 2945 and
Octanoic acid 2915 cm-1 was determined and used in the linear regression
Sodium sulfate described on Page 3. A linear baseline fit through the points
at 3100 and 2800 cm-1 was subtracted before measuring the
Tetrachloroethylene (ACS spectroscopy grade)
peak height.
Sulfuric acid
Water, ASTM type II
2
Table 1. Calibration Standards.
Standard Volume of Concentration Equivalent conc. in mg/L
number 5 mg/mL (mg/mL) of OG in a 250-mL water
stock sample extracted into a
diluted to 50-mL volume of solvent
10 mL
Std1 0.05 0.025 5
Std2 0.10 0.050 10
Std3 0.20 0.100 20
Std4 0.30 0.150 30
Std5 0.50 0.250 50
Std6 0.60 0.300 60 Figure 3. Plot of estimated vs. specified values for validation
samples. The dashed line represents perfect agreement: the
Std7 0.70 0.350 70
systematic deviation from this is due to the extraction efficiency
Std8 0.80 0.400 80 being around 93%.
Spike Recovery
Results and Discussion
Any analytical method involving an extraction step
Calibration and Validation is at risk of negative bias introduced by incomplete
Over the calibration range, excellent linearity and precision were extraction. In addition to the findings above,
observed (see Figures 2 and 3), with a correlation coefficient (R2) of recovery studies were performed. The spiking
0.9999 and a standard error of prediction (SEP) of 0.002 mg/mL being solution was prepared by mixing equal volumes
obtained for analysis of the extract, corresponding to 0.4 mg/L OG in of octanoic acid and isooctane in a volumetric
water with the present extraction procedure. flask. 15 L (12.0 mg) of this solution was spiked
into the water samples. Table 2 summarizes the
results. The recoveries are high but show some
variability with values ranging from 91 to 97
percent. This indicates that the solvent extraction
recovers nearly all of the OG and introduces only
a small negative bias to the reported result.
3
Detection Limit Conclusion
Since several sources of error in the calibration are proportional to the The PerkinElmer Spectrum series spectrometers
concentration, a calibration with a high upper limit will tend to have a can be utilized successfully for the determination
higher detection limit. Thus, a series of standards at lower concentra- of oil and grease in water samples. The method
tions were prepared (Table 3) and a low-concentration model devel- shows good linearity and precision, with a detection
oped (Figure 4). limit below 0.5 mg/L. Tetrachloroethylene was
found to be a suitable solvent for this analysis,
Table 3. Standards Used for the Detection-Limit Study. and has a much lower environmental impact than
the previously favored solvents such as CFC-113
Standard Concentration Equivalent conc. in mg/L of OG in a
number (mg/mL) 250-mL water sample extracted into and tetrachloromethane.
a 50-mL volume of solvent
DL1 0.002 0.4 References
1. ASTM D7066-04: Standard test method for
DL2 0.003 0.6
dimer/trimer of chlorotrifluoroethylene (S-316)
DL3 0.004 0.8 recoverable Oil and Grease and Nonpolar
DL4 0.005 1.0 material by Infrared determination, 2004.
PerkinElmer, Inc.
940 Winter Street
Waltham, MA 02451 USA
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