SPE 75228
Evaluating Crude Oils by SARA Analysis
Tianguang Fan SPE, Jianxin Wang SPE, and Jill S. Buckley SPE/New Mexico Tech
Copyright 2002, Society of Petroleum Engineers Inc.
This paper was prepared for presentation at the SPE/DOE Improved Oil Recovery Symposium
held in Tulsa, Oklahoma, 1317 April 2002.
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Abstract
The effectiveness of some improved oil recovery schemes can
depend on the composition of the target oil. Crude oils can be
described compositionally by a number of methods. SARA
analysis divides crude oil components according to their po-
larizability and polarity using a family of related analytical
techniques. Problems arise because several of the analytical
techniques in use do not produce identical results, although the
users of the data rarely distinguish between them, assuming
that SARA fraction values generated by any of the common
techniques are essentially interchangeable. We examine this
assumption for three SARA analysis methods: gravity-driven
chromatographic separation, thin layer chromatography
(TLC), and high pressure liquid chromatography (HPLC).
Results for a suite of six crude oil samples show that a signifi-
cant volume of volatile material that contains both saturates
and aromatics is lost in the TLC analysis. Application of
SARA fraction data to assessment of asphaltene stability is
demonstrated.
Introduction
Analysis of the composition of crude oils can be endlessly
complex; the amount of detail collected should be dictated by
the application for which the data is needed. One simple
analysis scheme is to divide an oil into its saturate, aromatic,
resin, and asphaltene (SARA) fractions. The saturate fraction
consists of nonpolar material including linear, branched, and
cyclic saturated hydrocarbons. Aromatics, which contain one
or more aromatic rings, are more polarizable. The remaining
two fractions, resins and asphaltenes, have polar substituents.
The distinction between the two is that asphaltenes are insolu-
ble in an excess of heptane (or pentane) whereas resins are
miscible with heptane (or pentane). This classification system
is useful because it identifies the fractions of the oil that per-
tain to asphaltene stability and thus should be useful in identi-
fying oils with the potential for asphaltene problems.
SARA analysis began with the work of Jewell et al.1
Three main approaches have been used to separate crude oils
and other hydrocarbon materials into SARA fractions. A clay-
gel adsorption chromatography method is the basis of ASTM
D2007. This method requires a fairly large oil sample, is time
consuming and difficult to automate, and requires large quan-
tities of solvents.
Improved methods fall into two groups. In the first group
are high pressure liquid chromatographic (HPLC) methods,
first introduced by Suatoni and Swab.2 Early HPLC tech-
niques used silica or alumina columns to separate lighter pe-
troleum fractions. The development in preparation of bonded
phase of HPLC columnsespecially NH2-bonded materials
made it practical to separate heavier fractions of petroleum
samples.3-7 HPLC techniques are faster, more reproducible,
and more readily automated than the ASTM column tech-
nique. In both cases, however, it is necessary to remove the
asphaltene fraction before proceeding with the chromatogra-
phy. Asphaltenes are either irreversibly adsorbed or precipi-
tated during the saturate elution step and quantitative recovery
cannot be achieved.8
The fastest separation method uses thin-layer chromatog-
raphy (TLC) with quartz rods that are coated with sintered
silica particles. Unlike column and HPLC techniques, asphal-
tenes need not be separated from other crude oil components
before chromatographic analysis. A popular technology
known as the Iatroscan that combines TLC with flame ioniza-
tion detection (TLC-FID) was first applied by Suzuki9 to
automate quantitative SARA separations, a method which has
since been used extensively.10-11 Barman12 compared SARA
analyses of heavy hydrocarbon distillates by the clay-gel and
TLC-FID methods. TLC-FID uses very small amounts of
sample. SARA fractions in a crude oil sample are often well
resolved using established development procedures and quan-
titative results are obtained by the measurement of peak areas,
assuming that each SARA fraction has an identical FID re-
sponse factor.
Comparisons of SARA fraction measurements by different
techniques, usually from different laboratories, can show large
differences. To some extent these differences might be real
caused by the use of different samples. In this work identical
samples were examined by several different techniques to il-
2 T.G. FAN, J.X. WANG, J.S. BUCKLEY SPE 75228

luminate the strengths and weaknesses of each and to develop
a standard method. An improved HPLC technique is de-
scribed and the results are applied to the problem of predicting
asphaltene stability, which has implications for many oil re-
covery processes both through the possibility of deposition
and the potential for alteration of wettability.
Experimental Materials and Methods
Crude Oils. Six medium-gravity, dead crude oils, varying in
API gravity from 22.6 to 37.2, were used in this study. Se-
lected physical and chemical properties are shown in Table 1.
Densities were measured using a Mettler/Paar DMA 40 with a
circulating water bath for temperature control. API gravities
were calculated from measured densities. Average molecular
weight (MW) was determined by freezing point depression
(Precision Systems Cryoscope 5009). Kinematic viscosities
were measured in Cannon-Fenske viscometers and converted
to absolute viscosity units. The amounts of asphaltene
precipitated by n-heptane (1 g oil:40 ml heptane) ranged from
1.3 to 8.7%. Refractive index (RI) was measured with an
Index Instruments GPR11-37 automatic refractometer. PRI is
the RI of a mixture of oil and the least amount of heptane in
which asphaltene aggregates can be observed microscopically
(320X). The difference between RI of the oil sample and PRI
is a measure of asphaltene stability.13 Among these samples,
C-LH-99 had the most stable asphaltenes. Three of the oils (C-
R-00, S-Ven-39, and Tensleep-99) contained aphaltene aggre-
gates in the samples as received. In SQ-95 crystalline waxes
can be observed using crossed polar microscopy at ambient
conditions.
gel in hot toluene. Volatile components lost during the proc-
ess were calculated by weight difference.
TLC-FID. An MK-5 Iatroscan (Iatron Labs Inc., Tokyo),
equipped with a flame ionization detector (FID), interfaced
with a Model 203 PeakSimple data system (SRI Instrument),
was used to scan silica-coated quartz rods (Chromarod-SIII,
Iatron Laboratories). The rods were 15.2-cm long and 1.0-mm
in diameter with a uniform coating of 5.0-m silica particles
(pore diameter 60 ). The FID detector was operated with a
pure grade hydrogen flow rate of 160 ml/min, an air flow rate
of 2.0 L/min supplied by a pump and a scan speed of 60s/scan.
Crude oil samples were dissolved in HPLC grade di-
chloromethane (DCM) at a concentration of 20 mg/mL. A 1
L repeating syringe (Alltech Associate, Inc.) was used to
spot 10 to 20 g of sample on freshly activated rods. Devel-
opment steps included exposure to HPLC grade hexane for 30
min, HPLC grade toluene for 10 min, and a 95:5 mixture of
DCM and methanol for 4 min. The rods were dried in air for 3
min between solvent exposures. A typical chromatogram is
shown in Fig. 1 for S-Ven-39. Evaporative losses during the
development steps were evaluated by tests of similarly treated
preparative thin layer chromatography plates for which
changes in weight could be measured and by comparison of
peak sizes for undeveloped rods.

Table 1. Crude Oil Sample Properties

density RI n-C7
Oil API MW PRI
at 20C at 20C asph
3
(g/cm ) (g/mol) (%)
A-95 25.2 0.8956 236 1.5128 1.4513 8.7
C-LH-99 22.6 0.9161 268 1.5137 1.4231 2.8 Figure 1. TLC-FID chromatogram of S-Ven-39.
C-R-00 31.3 0.8673 235 1.4851 1.4444 1.9
S-Ven-39 28.8 0.8795 240 1.4976 1.4465 5.8 HPLC. The HPLC chromatographic separation system con-
SQ-95 37.2 0.8409 213 1.4769 1.4223 1.3
sisted of a Model 110A pump (Beckman), an R401 differential
refractometer (Waters), a U6K universal injector (Waters), a
Tensleep-99 31.1 0.8685 270 1.4906 ~1.44 4.1
Model 7040 high pressure switching valve (Rheodyne), and a
Waters 486 UV detector (Millipore). Analog signals from the
ASTM Column Separation. Each of the crude oils was test- RI detector were interfaced to a Model 203 PeakSimple data
ing using the full ASTM-recommended procedure (ASTM acquisition system (SRI Instrument). Two 3.9300 mm
D2007-93) using n-hexane to separate the asphaltenes. The Bondapak NH 2 columns (Waters) were used in series for
ASTM procedure is a chromatographic separation of the non- chromatographic separation of crude oil. The UV detector
asphaltic oil components through two columns: an Attapulgite was operated at a wavelength of 254 nm to monitor elution of
clay-packed column adsorbs the resins and a second column each fraction.
packed with activated silica gel separates aromatics from the Selectivity of the columns was tested using mixtures of
saturate fraction. A 50:50 mixture of toluene and acetone is known compounds. Mixtures of n-decane (C10), n-tridecane
used to recover the resin fraction from the clay packing. The (C13), n-pentadecane (C15), and n-octadecane (C18) in hexane
aromatics can be recovered by Soxhlet extraction of the silica eluted as a single peak, as did hexane solutions of toluene and
1,3diisopropylbenzene (DIPB). Hexane solutions of a single-
SPE 75228 EVALUATING CRUDE OILS BY SARA ANALYSIS 3

ring aromatic, DIPB, with a two-ring compound, 1- filtration through an 0.22 m filter, dried and weighed. Sev-
methylnaphthalene (1-MN) eluted as two well-resolved peaks. eral 0.5 ml aliquots of the maltene/hexane mixture were in-
Mixtures of the hexane solutions of DIPB, 1-MN, and C15 jected onto the HPLC columns, using a gas tight HPLC sy-
eluted as three distinct peaks (Fig. 2). ringe (HAMILTON).
methylnaphthalene Saturates and aromatics were eluted with hexane at a flow
rate of 1.5 ml/min. A typical chromatogram is shown in Fig.
3. The amounts of saturates and aromatics were calculated
diisopropylbenzene
from calibration factors measured with known compounds
(Table 2).
n-pentadecane
Table 2. RI Detector Calibration
Signal
Class Hydrocarbon
(area/mg)
saturates n-heptadecane 4,647
1-ring aromatics DIPB 7,088
2-ring aromatics 1-MN 12,517
Figure 2. Separation of paraffins from single-ring and double-ring 3-ring aromatics phenanthrene 16,022
aromatics.
Resins were strongly adsorbed and did not elute with hex-
ane. A 30% (v/v) dichloromethane/hexane backflush was
saturates used to elute the resins accumulated from at least three repli-
aromatics: cate injections to ensure that sufficient resins could be col-
single ring lected for accurate gravimetric determinations of the amount
of resin remaining after solvent evaporation.
The principal improvements in the HPLC method de-
scribed here over previously proposed HPLC techniques in-
clude:
the use of NH2-bonded columns,
2 rings analysis of the maltenes without solvent evaporation,
3 rings thus avoiding the uncertainties due to evaporation of
0.10 0.20 0.30 0.40 0.50 0.60 0.70 0.80 0.90 1

some of the more volatile material along with the sol-

Figure 3. HPLC separation of C-R-00 maltenes. vent, and
gravimetric quantification of the amount of resins
One ml of crude oil was weighed and dissolved in 40 ml of eluted by backflushing the columns.
hexane in an open-top screw cap vial with a Teflon/silicon
septum. After 48 hours, a sample of maltenes dissolved in Results and Discussion
hexane was withdrawn through a 0.2 m PTFE syringe filter. The SARA fractions measured by these three techniques are
The withdrawn maltene solution was sealed in a 5-ml crimp- summarized in Table 3 and Fig. 4. The results of the ASTM
top glass vial with an aluminum seal and PTFE/silicon sep- method provide a baseline against which other SARA separa-
tum. The precipitated asphaltenes were recovered by tion methods can be compared.
Table 3. SARA Fractions by Three Methods
Oil Method Volatiles (wt%) Saturates (wt%) Aromatics (wt%) Resins (wt%) n-C6 Asphaltenes (wt%)
ASTM 6.7 46.2 19.7 18.6 8.8
A-95 HPLC 0 51.0 20.5 19.7 8.8
TLC-FID 53.3 13.8 12.4 13.4 7.1
ASTM 10.3 38.8 23.6 23.9 3.4
C-LH-99 HPLC 0 49.4 21.5 25.6 3.4
TLC-FID 54.3 12.5 15.3 13.5 4.4
ASTM 2.4 68.7 17.4 9.9 1.6
C-R-00 HPLC 0 70.6 16.4 11.4 1.6
TLC-FID 37.5 38.0 12.1 9.2 3.2
ASTM 16.3 47.0 19.4 14.7 2.6
SQ-95 HPLC 0 65.2 18.3 13.9 2.6
TLC-FID 61.5 17.3 10.2 9.1 1.9
ASTM 6.3 45.6 27.8 14.2 6.1
S-Ven-39 HPLC 0 51.1 28.3 14.5 6.1
TLC-FID 47.5 17.2 10.5 14.5 10.4
ASTM 3.2 59.0 22.9 11.7 3.2
Tensleep-99 HPLC 0 64.0 19.8 12.9 3.2
TLC-FID 39.6 26.5 18.8 8.1 6.9
4 T.G. FAN, J.X. WANG, J.S. BUCKLEY SPE 75228

75 75
(a) A-95 (b) C-LH-99

50 50

ASTM HPLC TLC-FID ASTM HPLC TLC-FID

25 25

0 0
Volatiles Saturates Aromatics Resins Asphaltenes Volatiles Saturates Aromatics Resins Asphaltenes

75 75
(c) C-R-00 (d) S-Ven-39

50 50

ASTM HPLC TLC-FID ASTM HPLC TLC-FID

25 25

0 0
Volatiles Saturates Aromatics Resins Asphaltenes Volatiles Saturates Aromatics Resins Asphaltenes

75 75
(e) SQ-95 (f) Tensleep-99

50 50

ASTM HPLC TLC-FID ASTM HPLC TLC-FID

25 25

0 0
Volatiles Saturates Aromatics Resins Asphaltenes Volatiles Saturates Aromatics Resins Asphaltenes

Figure 4. Comparison of SARA fractions determined by the ASTM method, by the improved HPLC method, and by TLC-FID.
SPE 75228 EVALUATING CRUDE OILS BY SARA ANALYSIS
The ASTM method also produces fractions of sufficient
volume to permit measurements of fraction properties, such as
RI, as shown in Fig. 5. RI of each oil is the volume-weighted
average of RI of each fraction. For the non-polar species that
dominate in a crude oil, RI is related to solubility parameters
and thus to solvent quality for asphaltenes. The low RI satu-
rate fractions are poor asphaltene solvents whereas the high RI
aromatics and resins are good solvents for asphaltenes.
1.65
Oil
Saturates
Aromatics
1.60
Resins
1.55
RI
1.50
1.45
1.40
1.35
A-95 C-LH-99 C-R-00 S-Ven-39 SQ-95 Tensleep-99
Figure 5. RI of oils and their saturate, aromatic, and resin frac-
tions.
TLC-FID vs. ASTM. Summation of the volatile and saturate
amounts from the TLC-FID method would significantly over-
estimate the saturate fraction and underestimate the amount of
aromatics. Ignoring the volatilization and simply reporting the
relative amounts of the four peaks would lead to even greater
divergence from the ASTM results. Only by separating all of
the volatile material up to some fairly high boiling point
(Karlsen and Larter10 measured losses of approximately 50%
of n-C14 which boils at 253.5C, whereas the loss of n-C16
which boils at 286.8C was negligible) and analyzing that
fraction separately, then combining the two sets of data would
one be able to apply the TLC-FID technique to medium grav-
ity oil samples with any confidence, but the advantage of rapid
analysisthe main reason for using this techniquewould be
lost. Apportioning the high molecular weight polar materials
between resins and asphaltenes, which is always based, rather
arbitrarily, on solvency, inevitably will vary from the ASTM
and HPLC methods as well since the solvents used are not
identical. On the basis of these comparisons, the TLC-FID
technique cannot be recommended for routine SARA analysis
of medium gravity oils.
HPLC vs. ASTM. Differences between the improved HPLC
SARA fractions and those measured by the ASTM-
recommended method were mainly in the volatile and saturate
fractions. There were no losses to evaporation in the HPLC
technique, unlike the ASTM method in which there were some
losses (during evaporation of the solvent after removal of the
asphaltenes and in the various fraction recovery and solvent
evaporation processes). However, if all of the volatile mate-
5
rial lost in the ASTM measurements was assumed to belong to
the saturate fraction, the comparisons between saturates, aro-
matics, and resins determined by the ASTM and HPLC meth-
ods was quite close. (Note that the amounts of asphaltenes
given for the ASTM and HPLC methods are from the same
measurements.) The major differences between the two tech-
niques are the amounts of time, sample, and solvent required.
For both techniques there is a two day period required for
separation of the asphaltenes. Beyond that, however, the
HPLC technique requires only about one hour per sample
compared to at least 20 hours for the ASTM separation. One g
of oil is adequate to give the same accuracy by the HPLC
technique as the 10 g required by the ASTM test. The solvent
requirements are on the order of 300 ml and 2 L per sample
for the HPLC and ASTM tests, respectively.
SARA Fractions and Asphaltene Stability. The proportions
of each of the SARA fractions in a crude oil are related to the
stability of asphaltenes in that oil. Carbognani and Espidel14
demonstrated that reservoirs with asphaltene problems were
not primarily those with large amounts of asphaltene in the oil,
but those with high saturate fractions. Leontaritis15 recom-
mended using the ratio of resins to asphaltenes as an indicator
of asphaltene stability, based on the hypothesis that resins con-
fer asphaltene stability by peptizing (or coating) asphaltenes.
Evidence is lacking to support either that hypothesis or the
utility of any specific ratio of resins to asphaltenes as an indi-
cator of asphaltene stability. Similarly, Por16 (cited by Aso-
maning and Watkinson17) defined a colloidal instability index
as the ratio of (asphaltenes+ saturates) to (resins+asphaltenes).
As with the resin to asphaltene ratio, this index certainly
should show some correlation with asphaltene stability, but no
critical or definitive cut-off value can be expected.
Both of these indices rely on an arbitrary differentiation
between asphaltenes and resins that is an analytical conven-
ience that does not correspond to a clear chemical distinction.
Recent studies have shown (1) that asphaltene stability can be
quantified by and predicted from measurements of the RI at
the onset of asphaltene precipitation, PRI,18 (2) that broader
distributions of asphaltenes are more stable than narrower
ones, and (3) that resins confer stability by broadening the
range of asphaltene properties.19 PRI for precipitation caused
by addition of n-C7 ranges from 1.4223 to 1.4513 RI units for
the oils in this study. For a larger sample of oils, the average
n-C7 PRI was 1.44 with a standard deviation of 0.02. One way
to use the SARA fraction data to assess asphaltene stability
would be to estimate a value of RI from the volume fractions
and compare that number to the expected onset for heptane (or
other alkanes, which are related to the heptane onset value18).
The accuracy of the calculated value of RI can be evalu-
ated by examining the correlation between SARA fraction
data (acquired using the improved HPLC technique) and
measured values of oil RI, as shown in Fig. 6 for a set of RI
and SARA data for 67 crude oils. The aromatic fraction has
little or no influence on RIoil whereas the saturates correlate
negatively (Fig. 6a) and the resins and asphaltenes (Fig. 6b)
are positively correlated with RIoil.
6 T.G. FAN, J.X. WANG, J.S. BUCKLEY SPE 75228

The resins plus the asphaltenes show a better correlation

1.56
with RIoil than either resins or asphaltenes alone (Fig. 6c).
y = -319x + 539
1.54 2
R = 0.6
While it would not be possible to calculate accurate RI values,
given the degree of scatter, SARA fractions could be used to
1.52 make a preliminary estimate of RIoil and an evaluation of as-
phaltene stability. Based on the data for these 67 oils, the fol-
1.50 lowing empirical formula has been developed:
RI

1.48
RI oil (S * 1.4452 + A * 1.4982 + (R + As) * 1.6624 )/100 (1)
1.46
Saturates
y = 9E-05x + 1.4923
where S is the wt% of saturates, A is the wt% of aromatics, R
1.44 2
R =0 Aromatics is the wt% resins, and As is the wt% asphaltenes. In Fig. 7
measured RI values are compared with those calculated from
1.42
Eq. 1.
0 10 20 30 40 50 60 70 80
%
1.56
(a) saturates and aromatics
1.54 67 oils
1.56
y = 95x - 139
2
R = 0.4 1.52
1.54

Calculated RI
1.50
1.52

1.50 1.48
RI

y = 221x - 316
1.48 2 1.46
R = 0.6

1.46 1.44

Asphaltenes
1.44 1.42
Resins
1.42 1.44 1.46 1.48 1.50 1.52 1.54 1.56
1.42 Measured RI
0 5 10 15 20 25 30 35 40
% Figure 7. Comparison of measured and calculated values of RIoil
with estimates based on SARA analyses.
(b) resins and asphaltenes
Predicted and measured asphaltene stability can be com-
1.56
pared by calculating a value of RI = RIoil - PRI using an aver-
1.54 age PRI = 1.44. Measured and calculated values of RI =
RIoil - PRI are shown in Fig. 8 for the original set of six oils.
1.52 Exact boundaries for the stable and unstable asphaltene re-
gions cannot be defined, but oils with RI < 0.04 or 0.05 may
1.50
be problem oils whereas those with RI > 0.06 are more likely
RI

1.48
y = 317x - 455 to have stable asphaltenes.18 These boundaries are indicated
2
R = 0.7 by the shaded areas in Fig. 8. For two of the oils the measured
1.46 RI indicates that the asphaltenes are likely to be stable, one
Resins+Asphaltenes appears in the unstable region and the remaining three are in
1.44
the borderline region. Assessments of five of the six oils are
1.42
the same for the estimates based on the SARA fraction data.
0 10 20 30 40 50 In only one case, indicated by the circled data point, does the
% oil appear to be more stable than it really is.

(c) resins plus asphaltenes

Figure 6. Correlations between amounts of various SARA frac-
tions and RI of the oils from which they were derived.
 SPE 75228
0.10
stable asphaltenes
0.09
0.08
RIcalculated
0.07
0.06
0.05
0.04
unstable
asphaltenes
0.03
0.03 0.04 0.05 0.06 0.07 0.08
RImeasured
Figure 8. Asphaltene stability estimates compared to measured
values. RI = RIoil - PRI where RIoil estimates are made on the basis
of SARA fraction data and Eq. 1 and PRI is taken to be 1.44 for the
purpose of estimation.
Conclusions
Measurements of SARA fractions are highly dependent
on methodology. Results of different methods may not be
comparable. Caution is needed in comparing results even
from similar methods.
The TLC-FID technique cannot be used for medium grav-
ity oils without considerable additional analysis to ac-
count for components that boil at temperatures up to
250C. The apportioning of high molecular weight, polar,
aromatic material into asphaltenes and resins will not cor-
respond to the ASTM method.
An efficient HPLC methodology was developed and
shown to correspond closely to the more time-consuming
ASTM-recommended method of SARA analysis.
SARA fraction data can be used to screen crude oils for
likely asphaltene stability by relating a calculated RI
based on the amounts of saturates, aromataics, and asphal-
tenes plus resins to the RI conditions at the onset of as-
phaltene instability.
Acknowledgements
This work was supported by the National Energy Technology
Laboratory (NETL) of the US DOE through contract DE-
AC26-99BC15204 and by support from industrial sponsors
including BP, Chevron, Gaz de France, IFP, Norsk Hydro, and
TotalFinaElf. Crude oils were provided by ARCO, Chevron,
Shell, and the University of Wyoming.
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