LAAN-A-FT-E082

Application Spectrophotometric Analysis

News
Quantitative Analysis of Oil and Grease in Water
Using FTIR Based on ASTM D7575
No. A544
The discharge of oil and grease into water environments <Contents of ClearShot Extraction Package>
such as oceans and rivers is a water quality control issue • ClearShotTM Extraction Technology cartridges
since it may lead to environmental problems including (ClearShot extractors)
adverse effects on ecological systems and malodor. • ClearShot Holding Card
A measurement method described in JIS K 0102 "Testing • Calibration Standard Devices (CSD) Set
Methods for Industrial Wastewater"*1 that involves • Drying System
determining the quantity of n-Hexane extract is one
method for quantifying oil and grease in water. However,
there are issues with this method including the necessity „ Calibration Curve Creation
of cumbersome pretreatment and the long time required After measuring the background with a new ClearShot
until results are obtained. extractor, the seven calibration standard devices (CSD) for
This article introduces a quantitative analysis method for calibration curve creation were measured using the
oil and grease in water that employs FTIR based on the transmittance mode. A calibration curve was created by
ASTM D7575 standard.*2 ASTM standards are set and setting a baseline between 2990 cm-1 and 2800 cm-1 in the
published by ASTM International, which is the world's obtained infrared spectra and determining the heights of
largest international standardization and standards- the top peaks from the baseline at 2920 cm-1. Table 1 lists
setting organization. ASTM D7575 enables quantitation of the measurement conditions, Fig. 2 shows an enlarged
oil and grease in water with a simple measurement view of peaks around 2920 cm-1 of the standard samples,
method that utilizes the absorption band of CH groups, and Fig. 3 shows the calibration curve and lists the
thereby eliminating the need for solvent extraction. standard sample concentrations.
R. Fuji Table 1 Measurement Conditions

„ Overview of Testing Based on ASTM D7575 Instrument

Resolution
:
:
IRTracer-100
4 cm-1
Testing was performed using the ClearShot Extraction Accumulation : (BKG) 200 times, (sample) 64 times
Package*3 manufactured by Orono Spectral Solutions, Inc., Apodization function : SqrTriangle
shown in Fig. 1. The measurement instrument, testing Detector : DLATGS
equipment, reagents used, and contents of the ClearShot
CSD1
Extraction Package are listed below. CSD2
1.2
CSD3
Abs CSD4
1.0
CSD5
CSD6
CSD7
0.8

0.6

0.4

0.2

0.0
ClearShot Extraction Package
3100 3080 3060 3040 3020 3000 2980 2960 2940 2920 2900 2880 2860 2840 2820 2800 2780 2760 2740 2720
<Measurement Instrument and Testing Equipment> cm-1

• Fourier transform infrared spectrophotometer Enlarged View of Peaks Around 2920 cm-1
• 1 L glass sample collection bottle
• Ultrasonic cleaner capable of heating to 40 °C and Sample Absorbance
Concentration
[ppm]
accommodating the 1 L glass sample collection bottle Height

• 10 mL syringe CSD1 0.0020 0.73

• 10 mL and 1 mL measuring pipets CSD2 0.026 4.54

• 100 mL measuring flask CSD3 0.096 15.23

<Reagents Used> CSD4 0.28 40.56

• 12.1 M hydrochloric acid CSD5 0.60 87.57
r=1.0
(The following items are for recovery rate verification.) CSD6 0.87 127.55
• Ion exchange water
CSD7 1.2 168.70
• Acetone
• Hexadecane Calibration Curve and Standard Sample Concentrations
• Stearic acid
Application No. A544
News

„ Checking Repeatability Table 3 Recovery Rate Verification Results

Repeatability of measurement was checked using Sample Absorbance Concentration [ppm]
standard sample CSD5. Table 2 shows the repeatability 1 0.28 41.22
measurement results obtained by two different methods: 2 0.25 37.65
(a) 10 consecutive measurements without removing the
3 0.29 42.09
cartridge inserted in the sample chamber and (b) 10
measurements by removing and then reinserting the 4 0.29 42.88
cartridge for each measurement. Fig. 4 shows the infrared
spectra obtained from the 10 consecutive measurements.
Variation between measurements was low and favorable
„ Quantitative Analysis of Oil and
Grease in Water
repeatability was obtained even with the method in which
the cartridge was removed. The procedure is described below.
<Sample Preparation>
Table 2 Repeatability ① Put the measurement sample into the glass sample
(a) 10 consecutive measurements without removing the sample collection bottle and adjust to pH 2 by adding the 12.1 M
(b) 10 measurements with removal of the sample
for each measurement
hydrochloric acid.
② Put the sample collection bottle into the ultrasonic cleaner
Measurement
Method
Number of
Measurements
Concentration
[ppm]
Standard
Deviation [ppm]
heated to 40 °C and leave it for 20 minutes.
(a) No removal 10 95.33 0.96 <Sample Measurement>
(b) With removal 10 94.63 0.99 ① Put about 12 mL of sample into the 10 mL syringe and let
0.70
it stand for a short while to allow any air bubbles within the
Abs
0.65
CSD5-1 sample to escape.
CSD5-2
0.60
CSD5-3
② Filter 10 mL of sample solution using a ClearShot extractor.
0.55
0.50 CSD5-4 Then dry the ClearShot extractor holding captured extract
0.45 CSD5-5 by blowing it with compressed air for a few minutes.
CSD5-6
③ Measure the background with a new ClearShot extractor
0.40
0.35 CSD5-7
0.30 CSD5-8 and then measure the infrared spectrum of the dried
0.25 CSD5-9 ClearShot extractor.
0.20
0.15
CSD5-10
④ Calculate the quantitative value using the created
0.10 calibration curve.
0.05
0.00 Quantitative analysis was performed on three samples by the
-0.05
above procedure. Table 4 shows the results.
3090 3050 3010 2970 2930 2890 2850 2810 2770 2730
cm-1

Infrared Spectra of Repeated Measurements Table 4 Measurement Conditions

(10 Consecutive Measurements) Sample Absorbance Concentration [ppm]

„ Verification of Recovery Rate 1

2
0.15
0.49
22.84
72.70
The procedure is described below.
<Sample Preparation> 3 0.79 115.14
① Put 400 mg ±4 mg of hexadecane and 400 mg ±4 mg of
stearic acid into the 100 mL measuring flask. „ Conclusion
② Add acetone to prepare a 1:1 solution of hexadecane and The analysis method for oil and grease in water based on
stearic acid. the ASTM D7575 standard allows simple and fast
③ Use the ion exchange water as a solvent to adjust the quantitation in the order of ppm without the need for
solution from step ② to a concentration of 40 ppm. solvent extraction. In this Application News, we confirmed
that by using Shimadzu's FTIR and the ClearShot Extraction
<Sample Measurement> Package manufactured by Orono Spectral Solutions, Inc.,
① Put about 12 mL of sample into the 10 mL syringe and let calibration curve creation, repeatability checking, recovery
it stand for a short while to allow any air bubbles within the rate verification, and actual quantitation of oil and grease
sample to escape. can be done easily based on the ASTM D7575 standard.
② Filter 10 mL of sample solution using a ClearShot extractor.
Then dry the ClearShot extractor holding captured extract References:
by blowing it with compressed air for a few minutes. *1 JIS K 0102 "Testing Methods for Industrial Wastewater"
③ Measure the background with a new ClearShot extractor *2 ASTM D-7575 -Standard Test Method for Solvent-Free Membrane
and then measure the infrared spectrum of the dried Recoverable Oil and Grease by Infrared Determination-
ClearShot extractor. *3 The ClearShot Extraction Package complies with the ASTM D7575 standard.
Clearshot Extraction Technology is a registered trademark of Orono
④ Calculate the quantitative value using the created Spectral Solutions, Inc.
calibration curve. http://www.ossmaine.com/
Table 3 lists the verification results of the recovery rates Caution 1) The ClearShot Extraction Package is not sold by Shimadzu. Please
obtained by the above procedure. By comparing the purchase it directly from Orono Spectral Solutions, Inc.
concentrations calculated from the absorbance values Caution 2) The cartridges included in the ClearShot Extraction Package
and the concentrations of the samples, we obtained cannot be fitted to the standard cassettes of the IRTracer-100 and
recovery rates between 94 % and 107 %. IRAffinity-1S. For details, contact your Shimadzu representative.

First Edition: Sep. 2017

For Research Use Only. Not for use in diagnostic procedure.

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