Group Title: Citrus Station mimeo report -Florida Citrus Experiment Station ; 60-3
Title: Physicochemical procedure to determine method of extraction and origin of coldpressed orange oil
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 Material Information
Title: Physicochemical procedure to determine method of extraction and origin of coldpressed orange oil
Series Title: Citrus Station mimeo report
Physical Description: 4 leaves : ; 28 cm.
Language: English
Creator: Kesterson, J. W
Hendrickson, Rudolph
Edwards, G. J
Citrus Experiment Station (Lake Alfred, Fla.)
Florida Citrus Commission
Publisher: Florida Citrus Experiment Station :
Florida Citrus Commission
Place of Publication: Lake Alfred FL
Publication Date: 1959
Subject: Orange oil -- Florida   ( lcsh )
Genre: government publication (state, provincial, terriorial, dependent)   ( marcgt )
bibliography   ( marcgt )
non-fiction   ( marcgt )
Bibliography: Includes bibliographical references (leaf 4).
Statement of Responsibility: J.W. Kesterson, R. Hendrickson and G.J. Edwards.
General Note: Caption title.
General Note: "September 16, 1959."
 Record Information
Bibliographic ID: UF00072392
Volume ID: VID00001
Source Institution: University of Florida
Rights Management: All rights reserved by the source institution and holding location.
Resource Identifier: oclc - 74846249

Full Text

Citrus Station Mimeo Report 60-3
September 16, 1959

Physicochemical Procedure to Determine Method of Extraction
and Origin of Coldpressed Orange Oil

J. W. Kesterson, R. Hendrickson and G. J. Edwards

Examination of the physicochemical properties of coldpressed orange
oils have revealed differences in the ultraviolet spectra and in the
evaporative residues of the oils that reflect the geographical source of
the oil and the method by which it was extracted. Taken together these
tests offer a quick and accurate means by which the method of extraction
and geographical origin may be determined. It is anticipated that the
method will be useful to the Essential Oil Industry.


Coldpressed orange oil samples were secured from commercial plants
that utilize the screw press, Pipkin roll, and FMC In-Line extractors pre-
viously described by Kesterson and Hendrickson (2, 3). The samples obtained
by the screw press and FMC In-Line extractor processes were taken from
30,000-pound lots of oil, which approximates the amount of oil recovered
from 220,000 field boxes of fruit. The total quantity of oil from which
the Pipkin roll samples were taken is unknown but the samples were typical
of oil obtained by this process. Oil samples used in this study were of
excellent quality and representative of pure coldpressed orange oil pro-
duced in Florida.

Evaporative residues were determined in accordance with the procedures
given by Guenther (1). Ultraviolet absorption data were secured in accor-
dance with the procedure of Sale, et al. (4). A Beckman Model DU quarts
spectrophotometer with hydrogen lamp attachment and a dilution of 0.25 g.
oil in 100 ml. of 95 percent ethanol were used. The orange oil samples
were evaluated in a 10 mm. silica-absorption cell.

Experimental Results

The spectrophotometric analyses and evaporative residues for screw
press, FMC In-Line extractor, Pipkin roll and California orange oils are
shown in Table 1. Since our analyses of coldpressed California orange oil
were,unfortunately, limited to a few samples, we obtained data from com-
mercial analyses of 27 lots of California oil for comparison; these commer-
cial analyses were of samples collected over a period from 1953 to 1958.
The data are summarized in Table 2.

Florida Citrus Experiment Station
and Florida Citrus Commission, Lake Alfred, Florida
933 9/16/59 FWW

Discussion of Results

Orange oil samples used in this study were produced from early season,
mid-season and late season fruit. Early season oil was produced from mix-
tures of Hamlin and Parson Brown fruit. The mid-season oil was produced
primarily from Pineapple oranges and the late season oil from Valencia
fruit. Data presented in Table 1 show that, for any one process, the
variety of fruit from which the oil was made seemed to have no direct
relationship to CD values.

The physical and chemical characteristics such as specific gravity,
refractive index and optical rotation of the original oils and 10 percent
distillates, and aldehyde content were determined for the screw press,
FMC In-Line extractor and Pipkin roll oils. These values are not reported
since they were similar to previously reported (2, 3) analyses.

The California orange oils used were commercial samples and repre-
sent different bulkings of oil. We have no means of ascertaining when the
oils were produced or by what method they were manufactured. It is con-
ceivable that these bulkings contained both early and late production oil
as well as blends of oil made by different processing methods. Different
processes might possibly give oils with different values for CD and evapo-
rative residue but our analyses were for blended oils and there is no way
to determine the effect of this variable. The data in Table 2 are in
agreement with those obtained for the California oils (Table 1). There
is a slight difference in the point at which the peak absorptions occurred.
This difference could be due to the instrument or operator involved in
making the determination and is considered to be of no consequence.

On the basis of data presented (Tables 1 and 2) it seems logical that
the following criteria could be used as a basis to identify and characterize
coldpressed orange oils:

Type oil CD Evaporative residue

California 0.10 to 0.20 not significant


Screw Press 0.20 to 0.40 below 2 %

FMC 0.20 to 0.40 above 2 %

Pipkin roll 0.40 to 0.60 not significant

On the basis of CD and peak absorption values, it would be impos-
sible to distinguish between FMC and screw press oil. However, in con-
sideration of the values for evaporative residue presented in Table 1
it is an easy matter to distinguish between these two types of oil.

Florida Citrus Experiment and Florida Citrus Commission
Lake Alfred, Florida 933a 9/16/59 FWW

Table 1. Spectrophotometric analyses and evaporative residue
values for coldpressed orange oils.

0.25 g
U. V. Spectrum 330 mu log E 100 mi.
FMC ~In-Line H
Screw Press xtractor Pi kin roll California

Evap. Evap. Evap. Evap.
CD Peak Res. CD Peak Res. CD Peak Res. CD Peak Res.
% % % %

1956-57 Season

0.34 0.56 1.52 0.25 0.47 2.49 -

0.26 0.44 1.59 0.29 0.51 1.96

0.25 0.44 1.74 0.28 0.42 2.29 -- -

0.30 0.52 1.72 0.23 0.44 2.78 0.42 0.68 1.79 -- --

1957-58 Season

0.22 0.40 1.35 -- 0.45 0.72 1.74 -- -- -
-,.-- ,-.-- -- I -I- "'------ --- *--- ---*"-
0.21 0.39 1.20 0.22 0.43 2.95 0.45 0.69 1.29 -- -- --

0.28 0.49 1.50 0.30 0.53 2.42 0.53 0.85 2.8

0.28 0.50 1.85 0.24 0.45 2.52 0.45 0.72 1.72 0.14 0.32 2.80

1958-59 Season

0.35 0.62 1.70 0.27 0.51 2.40 0.42 0.68 1.57 0.14 0.34 3.32

S0.24 0.44 1.87 0.27 0.52 2.81 0.46 0.74 1.92 0,16 0.37 3.78

0.28 0.483 1.83 0.34 0.58 2.56 0.50 0.79 1.53 0.13 0.32 3.90
--.-- --j-- --- -- -- .-- -- -----------
0.29 0.50 1.88 0.39 0.671 3.35 0.52 0.82 1.61 0.14 0.35 4.00

Max. 0.35 0.62 1.88 0.39 0.67 3.35 0.53 0.85 2.48 0.16 0.37 4.00

Min. 0.21 0.39 1.20 0.22 0.43 1.96 0.42 0.68 1.29 0.13 0.32 2.80

Avg. 0.28 0.48 1.65 0.28 0.51 2.59 0.47 0.74 1.74 0.14 0.34 3.56

Florida Citrus Experiment Station and
Florida Citrus Commission, Lake Alfred, Florida
931 8/15/59 FWW

Table 2. Summary of 27 spectrophotometric analyses of California
coldpressed orange oils by commercial companies.

U. V. Spectrum Mu log E 652

CD Peak Mu

Maximum 0.20 0.43 329

Minimum 0.11 0.27 328

Average 0.16 0.36 329

Florida Citrus Experiment Station and
Florida Citrus Commission, Lake Alfred, Florida
931 8/15/59 FWW

The evaporative residue for screw press oil in general never exceeds 2.0
percent; whereas the evaporative residue for FMC extractor oil is always
greater than 2.0 percent. There may be some instances in which residues
for the screw press oil would be higher than 2.0 percent and conversely
the residue for FMC oil would be lower than 2.0 percent. However, on
the basis of our findings, from a three-year study, this would be the
exception rather than the rule.

It is an easy matter to distingu*4id ipkin roll oil from screw
press and FMC extractor oil solely on the basis of CD values. The Pipkin
roll oil has an average CD value of 0.417 which is almost twice that of
0.28 for the screw press and FMC oil.

Califoinia orange oil has average OC values of 0.14 and 0.16 on the
basis of data presented in Tables 1 and 29i; hese average values of 0,14
and 0.16 are approximately one-half of 0.28 kbr the FMC and screw press
oil, and approximately one-third of 0.47 for the Pipkin roll oil. Thus
California oil can be distinguished from all three types of Florida oil
on the basib of CGD ale alone.


A physicoch cal method has been developed whereby coldpressed
Florida orange oil'can be distinguished from coldpressed California orange
oil. This methodihas the further advantage of being able to show by what
manufacturing procedure Florida oils have been produced.

Florida Citrus Experiment Station
and Florida Citrus Comissalon
Lake Alfred, Florida
9336 9/16/5 FWW


Literature Cited

1. Guenther, E. The Essential Oils. 1: 427. 1948. D. Van Nostrand
Co., Inc.

2. Kesterson, J. W. and R. Hendrickson.
production of citrus oils in Florida.
67:2: 35-38. 1956.

Two commercial methods for the
Amer. Perf. and Aromatics

3. Kesterson, J. W. and R. Hendrickson. Essential oils from Florida
citrus. Univ. of Fla. Agr. Exp. Sta. Tech. Bul. 521: 1-70. 1953.

4. Sale, J. W., et al. Analysis of lemon oil. Jour. Assoc. Offic. Agr.
Cheaists 36:1: 112-119. 1953.

Florida Citrus Experiment Station
and Florida Citrus Commission
Lake Alfred, Florida
933c 9/16/59 FWW

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