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ARTICLE INFO
Article ID: 04-12-01-0003
Copyright © 2019
SAE International
doi:10.4271/04-12-01-0003

Identification and Quantification

of Phosphate Ester-Based Hydraulic
Fluid in Jet Fuel
Diana Stamker Gertopski, Konstantin Tartakovsky, and Moshe Rabaev, Israeli Air Force, Israel

Abstract History
Received: 26 Sep 2018
Phosphate ester-based hydraulic fluids are commonly used in aviation, due to their fire-resistant Revised: 19 Dec 2018
properties. However, contamination of jet fuel with hydraulic fluid may cause serious engine failure, Accepted: 22 Jan 2019
hot corrosion of metals, and swelling of elastomer and polymer seals. Identifying and quantifying e-Available: 13 Mar 2019
hydraulic fluids in jet fuels using chromatography is challenging since common hydraulic fluids, such
as ExxonMobil™ HyJet™ V and Skydrol™ LD-4, are composed of tri-butyl phosphate, the main peak Keywords
of which overlaps with peaks from jet fuels in chromatograms. In this work, three techniques to Jet fuel, Hydraulic fluid,
separate and differentiate the jet fuel peaks from the tri-butyl phosphate peaks were developed. Organophosphate,
Two methods are based on a solid phase extraction (SPE) procedure followed by identification and ExxonMobil™ HyJet™ V,
quantification, which is carried out using a gas chromatograph equipped with a mass spectrometer Skydrol™ LD-4, Solid phase
or a flame ionization detector. The third technique is single-staged, where the separation and analysis extraction method
are carried out by a gas chromatograph equipped with a polar column and a mass spectrometer.
Lowest level of detection reached was 0.1 ppm of tri-butyl phosphate in jet fuel, 10 times lower than Citation
the limitations. Linearity was achieved in all analysis methods up to contamination of 100 ppm. Stamker Gertopski, D.,
Tartakovsky, K., and
Rabaev, M., “Identification
and Quantification of
Phosphate Ester-Based
Hydraulic Fluid in Jet Fuel,”
SAE Int. J. Fuels Lubr.
12(1):43–49, 2019,
doi:10.4271/04-12-01-0003.

ISSN: 1946-3952
e-ISSN: 1946-3960

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44 Stamker Gertopski et al. / SAE Int. J. Fuels Lubr. / Volume 12, Issue 1, 2019
1. Introduction
T
he hydraulic pumping system of the aircraft is
immersed in the jet fuel tanks, which are operated by
a hydraulic fluid. Any slight leaking failure in the
system, which results in higher pressure of the hydraulic fluid
than that of the surrounding fuel, can cause serious contami-
nation of the fuel in the tanks. Hydraulic fluids used in
aviation hydraulic systems contain a variety of compounds
based on phosphate esters. These compounds play a significant
role in fire resistance [1, 2, 3] but may also cause hot corrosion
of turbine and metal bearings [4, 5, 6, 7]; damage composite
parts [8, 9]; damage of corrosion inhibitor coatings, which are
widely used in the aircraft industry [10, 11]; and swelling of
polymer seals. Contamination of jet fuel with hydraulic fluid
may endanger operating seals and engine parts, which are
made of materials that are incompatible with phosphate
compounds, in turn causing serious engine failure. Due to
the corrosive effect of phosphate esters on cobalt, the level of
phosphate ester contamination must not exceed 1 ppm of
hydraulic f luid in engines manufactured using cobalt-
containing alloys and must be less than 10 ppm in engines
manufactured without cobalt alloys [12].
A multitude of chromatographic methods for the identi-
fication and quantification of hydraulic fluids [13, 14] and
organophosphate [15, 16] contaminations in turbine engine
oil, occupational air [17], human plasma [18], soil [19], water
[20], and human urine [21] have been reported in recent years.
Moreover, a chemical multisensory device as a detector for
hydraulic oil contamination in air was developed [22].
Methods for monitoring the quality of hydraulic fluids using
acid-base indicators and chromatography have also been
developed [23, 24]. However, despite the danger of hydraulic
fluid contamination in jet fuel, only scarce methods for the
identification and quantification of the contamination have
been reported. One such method was described by Spila et al.
[25] and another in a patent by Werner et al. [12]. The two
methods refer to a contamination caused by Skydrol hydraulic
fluid. The presence of tri-butyl phosphate in jet fuel may
be  tested using other analytical techniques, for example,
inductively coupled plasma atomic emission spectroscopy
(ICP-AES), but the detection limit is too low [26]. Another
possible method uses a pulse flame photometric detector
(PFPD) coupled with a gas chromatograph, which is very
sensitive to many elements including phosphorous [27].
The Israeli Air Force (IAF) uses both brands of hydraulic
fluid-ExxonMobil™ HyJet™ V and Skydrol™ LD-4 (Exxon and
Skydrol). Quantification and identification of Skydrol can
be  performed according to its dibutyl phenyl phosphate
component, as described by Spila et al. A similar analysis of
the second fluid - Exxon - cannot be performed in the same
way, since it does not contain dibutyl phenyl phosphate.
Measuring the concentration of both Skydrol and Exxon can
be carried out through analysis of their tri-butyl phosphate
compound, which exists in both fluids. The mass spectrum
of tri-butyl phosphate shows a main peak at 99 m/z that was
considered nonsignificant for analysis because of the
interference of peaks originating from the matrix of hydro-
carbons. Failures of the hydraulic system in air refueling jets
have led to contamination of the jet fuel. Together with the
use of hydraulic fluid mixtures in the IAF, this has revealed
a need for a universal method for identification and quanti-
fication of both hydraulic fluids in jet fuel. The lower detection
limit of the methods developed had to be  at least 1 ppm
according to the policy of IAF and engine manufactures,
though the specific limitation has not been proven yet [28].
The main goal of the present work was to develop a simple
and reliable analysis method for the detection of contamination
by either hydraulic fluid or a mixture of both in jet fuels at a
concentration of at least 1 ppm using mass spectrometry (MS)
or flame ionization detector (FID). Tri-butyl phosphate, a
compound common in both Skydrol and Exxon, was separated
from the matrix of jet fuel hydrocarbons using three methods
presented herein. Two separation methods were developed by
using solid phase extraction (SPE) columns. The use of SPE
technique resulted in isolation of the 99 m/z signal originating
from both hydraulic fluids, so that identification and quantifica-
tion was carried out using a gas chromatograph equipped with
a mass spectrometer (GC-MS) or by GC-FID. The third method
is based on gas chromatographic separation and was carried
out by a GC equipped with a polar column and MS analysis.
2. Experimental
The SPE-GC-MS/FID methods were comprised of a separation
stage that was carried out by an SPE technique followed by
injection into a gas chromatograph where the analysis was
performed by an MS or FID detector. The gas chromato-
graphic separation method (GC-MS) was carried out in one
stage by injecting the sample without any prior procedure.
The gas chromatographic separation was performed by a polar
column and analysis was carried out by an MS detector.
2.1. Reagents
Commercial products were used in the preparation of the
standard solutions: ExxonMobil™ HyJet™ V (ExxonMobil),
Skydrol LD-4 (Solutia Inc.), hexane (anhydrous, 95%, Sigma-
Aldrich), methanol (HPLC grade 99.9%, Sigma Aldrich), jet
fuel JP8, and Strata® FL-PR Florisil SPE columns (170 μm, 80
Å, 500 mg/6 mL).
2.2. Instruments
2.2.1. GC-MS Method A Varian 450-GC gas chromato-
graph was equipped with a DB-WAX (30 m, 0.25  mm ID,
0.25 μm df) column. The MS analysis was carried out by a
Varian 300 MS system.
2.2.2. SPE-GC-MS/FID Methods The apparatus used
for GC-MS analysis was comprised of a Varian 450-GC gas
chromatograph equipped with a Rxi®-5 ms (Crossbond® 5%
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Stamker Gertopski et al. / SAE Int. J. Fuels Lubr. / Volume 12, Issue 1, 2019 45

diphenyl 95% dimethylpolysiloxane, 30 m, 0.25 mm ID, 0.25 flow, 1.5 mL/min; oven, initial temperature 100°C for 1 min,
μm df) column. The MS analysis was carried out in a Varian heating to 230°C with rate 10°C/min; MS single-ion count-
300 MS system. The apparatus used for the GC-FID analysis ing, 99 m/z; liner type, with quartz wool.
was composed of a gas chromatograph and a Rxi®-5 ms col-
umn as described above. The analysis was carried out by an 2.4.2. SPE-GC-MS Method GC-MS analysis was car-
FID detector. ried out under the following conditions: injection volume,
0.5 μL; injector, split/splitless (type 1177); injector tempera-
ture, 240°C; split ratio, 1:20; carrier gas, helium; column
2.3. Procedure flow, 1.5 mL/min; oven, initial temperature 100°C for 1 min,
heating to 230°C with rate 10°C/min; MS single-ion count-
The stock solution was prepared by adding 0.08 mL of ing, 99 m/z; liner type, with quartz wool.
hydraulic f luid (Exxon/Skydrol) to 80 mL of jet fuel.
Preparation of standard solutions was done by dilution of 2.4.3. SPE-GC-FID Method GC-FID analysis was car-
stock solution in jet fuel. Dilution was done according to the ried out under the conditions: injection volume, 1 μL; injector,
desired concentrations of standard solutions. split/splitless (type 1177); injector temperature, 240°C; make-
up flow, 28 mL/min; hydrogen flow, 45 mL/min; air flow, 300
2.3.1. GC-MS Method The sample and the standard so- mL/min; column flow, 1.5 mL/min; detector temperature,
lutions were injected to the GC-MS without any preparation. 240°C. Oven, initial temperature 100°C for 1 min, heating to
230°C with rate 10°C/min; liner type, with quartz wool.
2.3.2. SPE-GC-MS/FID Methods Each standard so-
lution was treated using the SPE technique: the SPE column
was loaded with 20 mL of standard solution, 15 mL of hexane
loaded in the column to extract jet fuel leftovers, and 2 mL of
methanol used to extract the polar phosphate fraction from
3. Results and Discussion
the SPE column. The methanol fraction containing the phos-
Both hydraulic fluids and jet fuel were separately injected to
phate ester was analyzed by 1 μL that was injected into the
the GC-MS to examine their composition. Figure 1 shows that
GS-MS or into the GC-FID system.
ion 99 m/z is common to both hydraulic fluids and originates
from tri-butyl phosphate. Ion 99 m/z is inseparable from the
saturated aliphatic ion fraction originating from the non-
2.4. System Conditions contaminated jet fuel (Figure 2).
Following the detection of ion peak 99 m/z in both
2.4.1. GC-MS Method GC-MS analysis was carried out hydraulic fluids and jet fuel chromatograms, three methods
under the following conditions: injection volume, 1 μL; in- for the identification of hydraulic fluid contamination in jet
jector, split/splitless (type 1177); injector temperature, 240°C; fuel were developed: GC-MS with polar column method,
splitless injection for 2 min; carrier gas, helium; column SPE-GC-MS method, and SPE-GC-FID method.

 FIGURE 1   Chromatogram of Exxon and Skydrol. Ion 99 m/z indicated.

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46 Stamker Gertopski et al. / SAE Int. J. Fuels Lubr. / Volume 12, Issue 1, 2019
 FIGURE 2   Chromatogram of ion 99 m/z in Skydrol and in uncontaminated jet fuel.
3.1. GC-MS with Polar Column
Method
The separation of ion 99 m/z originating from tri-butyl phos-
phate from the matrix of hydrocarbon peaks was achieved by
using a DB-WAX column. It is evident that ion 99 m/z was
not present in the chromatogram of uncontaminated jet fuel,
but the former could be detected in the standard solutions
beginning with 10 ppm of hydraulic fluid in jet fuel (Figure 3).
The calibration curve in the range of 10-100 ppm of hydraulic
fluid showed a linear relationship (y = 2562958x + 5531704,
R 2 = 0.997). The limit of detection of hydraulic fluid contami-
nation in jet fuel was 5 ppm.
3.2. SPE-GC-MS Method
In this separation method, the tri-butyl phosphate compound
was separated from the jet fuel before the chromatographic
analysis was performed. The separation was carried out by
SPE that was performed according to the procedure described
(Section 2.3.2). Solid extraction concentrates the sample and
separates the jet fuel from the hydraulic fluid.
After separation, the methanol fraction containing the
phosphate was analyzed by GC-MS. The chromatogram of the
methanol showed a peak of ion 99 m/z. In the chromatogram
of the jet fuel fraction, no peaks of ion 99 m/z were observed
(Figure 4), indicating no traces of tri-butyl phosphate were left
in the jet fuel after SPE. Quantification and identification of the
contamination showed a lowest detection limit of 0.5 ppm of
contamination in jet fuel. The calibration curve at a range
of 0.5-100 ppm of hydraulic fluid showed a linear relationship
(y = 2592269x + 3549189, R 2 = 0.997). The limit of detection of
hydraulic fluid contamination in jet fuel was 0.1 ppm.
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3.3. SPE-GC-FID Method
The other analysis method was based on GC-FID. Following
the separation step described above, the methanol fraction
containing the phosphate was analyzed by GC-FID. The chro-
matogram of the methanol showed a peak in retention time
of 5.3 min, while the chromatogram of the jet fuel that passed
the SPE column did not contain this peak, again indicating
that no traces of tri-butyl phosphate were left in the jet fuel
after SPE. The SPE-GC-FID method showed the same detec-
tion limit as the SPE-GC-MS method, at 0.1 ppm of contami-
nation in jet fuel. The calibration curve at a range of 0.5-100
ppm of hydraulic fluid showed a linear relationship (y =
20903x + 551, R 2 = 0.998).
The quantification of contamination in all three methods
mentioned above was based on the detection of the tri-butyl
phosphate reagent that was separated from the jet fuel
matrix. These quantification methods are not specific for
only one type of hydraulic fluid contamination, unlike the
methods described by Spila et al. and Werner et al., which
were proven only for Skydrol. The GC-MS method is a single-
step method, with no need for any sample preparation,
unlike the method described in the patent of Werner et al.
This method may be used when determination of massive
concentrations of contamination is needed or for contamina-
tion detection in jet fuel used in engines not manufactured
using cobalt metals. The SPE-GC-FID and SPE-GC-MS
methods provided a better limit of detection of the contami-
nants, lower than in the method described by Spila et al. The
SPE-GC-FID method allowed the use of more accessible
equipment, since GC-FID is more common than GC-MS or
GC-FPD, which were used in the article and in the patent
mentioned above (Table 1).
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 FIGURE 3   Chromatogram (10.5-10.9 min) of uncontaminated jet fuel and standard solutions of hydraulic fluid in jet fuel. Ion 99
m/z was indicated only in standard solutions and not in uncontaminated jet fuel. GC-MS with polar column method.

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 FIGURE 4   Chromatograms (8-14 min) of jet fuel fraction (red chromatogram) and methanol fraction (blue chromatogram) after
SPE of 11 ppm of hydraulic fluid in jet fuel. Ion 99 m/z was present only in the methanol fraction. SPE-GC-MS method.
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48 Stamker Gertopski et al. / SAE Int. J. Fuels Lubr. / Volume 12, Issue 1, 2019
TABLE 1  Accuracy data and results for all analysis methods discussed in the article.
GC-MS-method SPE-GC-MS method SPE-GC-FID method Spila et al. [25] Spila et al. [25]
Linearity range (ppm) 10-100 0.5-100
Linearity regression 0.997 0.997
Sensitivity (ppm) 5 0.1
RSD (%, 10-15 ppm)/intra-day 3.8 (n = 5) 0.2 (n = 4)
RSD (%, 10-15 ppm)/inter-day 6.1 (n = 2) 1.5 (n = 2)
Sample preparation needed No SPE procedure
Detection Exxon and Skydrol Exxon and Skydrol
4. Conclusions
Three straightforward methods for the identification and
quantification of jet fuel contamination by hydraulic fluids
were developed. Analysis was performed both by a gas chro-
matograph equipped with a mass spectrometer and a gas
chromatograph equipped with an FID. Lowest level of detec-
tion reached was 0.1 ppm of tri-butyl phosphate in jet fuel,
approximately ten times lower than the limit previously
reported. Linearity was achieved for all analysis methods up
to contamination of 100 ppm. The methods developed allow
testing by two different detectors, thus minimizing depen-
dency on a single instrument in the laboratory. In cases when
one only needs to determine whether sample contamination
is below/above a certain limit, a simple comparative test with
a standard of a given contamination can be obtained within
1 h using the one of the methods reported herein.
Utilizing the methods developed during proactive main-
tenance of aircrafts can be successful in preventing failure, in
which leakage detection is made possible before the problem
becomes severe. These methods may prevent serious engine
failure both in civil and military aircrafts.
This research opens a gate for further development of an
online monitoring method. In addition, a method for puri-
fying jet fuel from hydraulic f luid contamination may
be developed according to our finding that the SPE method
enables it.
Contact Information
Moshe Rabaev
Israeli Air Force
Depot 22, Materials Division, Fuel and Chemistry Department
rabaevm@gmail.com
Acknowledgement
The author and publisher would like to acknowledge that this
article is based on a presentation at The International
Association for Stability, Handling and Use of Liquid Fuels
(IASH), Rome, Italy, September 10-14, 2017.
GC-MS method GC-FPD method
0.5-100 5-100 5-100
0.998 0.997 0.998
0.1 2 2
1.4 (n = 8) 3.0 4.0
4.3 (n = 4) 5.1 6.8
SPE procedure No No
Exxon and Skydrol Skydrol Skydrol
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