ASTM D483-00

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An American National Standard
Designation:D483–00
Standard Test Method for
Unsulfonated Residue of Petroleum Plant Spray Oils
This standard is issued under the fixed designation D 483; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope 3. Terminology
1.1 This test method covers the determination of unsul- 3.1 Definition:
fonated residue in plant spray oils of petroleum origin and 3.1.1 unsulfonated residue, n— in oils, that portion of an oil
applies only to the petroleum oil content. It provides a measure remaining unsulfonated after treatment with concentrated sul-
of the degree of refinement of plant spray oils by determining furic acid.
the extent to which the oil is attacked by 98.61 % sulfuric acid
4. Summary of Test Method
under closely standardized conditions. Since the relationship
betweenunsulfonatedresidueandtheactualcompositionofthe 4.1 A measured volume of sample is shaken with 98.61 %
sulfuric acid at 100°C in a Babcock bottle, shaking mechani-
oil is not known, this test method should be applied only for
measuring the degree of refinement and not for the determina- cally for 10 s at 10-min intervals. The volume not absorbed by
the acid is a measure of the unsulfonated residue in the sample.
tion of aromatics or olefins, or both.
1.2 The values stated in SI units are to be regarded as the
5. Significance and Use
standard.
5.1 This test method is useful for distinguishing between
1.3 This standard does not purport to address all of the
oils that are adaptable to various types of spraying application,
safety concerns, if any, associated with its use. It is the
with a higher unsulfonated oil being required for leaf spraying
responsibility of the user of this standard to establish appro-
as compared to dormant vegetation application.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
6. Apparatus
2. Referenced Documents
6.1 Sulfonation Flask—The flask is shown in Fig.A1.1 and
described in Annex A1.
2.1 ASTM Standards:
6.2 Meniscus Viewing Lens, focusing type, consisting of
D 1193 Specification for Reagent Water
eyepiece and objective to facilitate reading the meniscus with
D 1250 Guide for Petroleum Measurement Tables
a minimum of parallax, is recommended.
D 1298 Test Method for Density, Relative Density (Specific
6.3 Water Baths— Two water baths maintained at 25 6
Gravity), or API Gravity of Crude Petroleum and Liquid
0.5°C and 99.5 to 100°C, and conforming to the requirements
Petroleum Products by Hydrometer Method
prescribed in Annex A1.
D 4052 Test Method for Density and Relative Density of
6.4 Shaking Machine— The exact design described in the
Liquids by Digital Density Meter
appendix is required for uniform control of shaking and
D 4057 Practice for Manual Sampling of Petroleum and
precision results. Hand shaking is permissible if technique is
Petroleum Products
developed to correlate results by machine shaking.
D 4177 Practice for Automatic Sampling of Petroleum and
6.5 Centrifuge—A centrifuge as described in Annex A1 is
Petroleum Products
recommended.
7. Reagents
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricantsand is the direct responsibility of Subcommittee
7.1 Purity of Reagents—Reagent grade chemicals shall be
D02.06on Analysis of Lubricants.
used in all tests. Unless otherwise indicated, it is intended that
Current edition approved Dec. 10, 2000. Published January 2001. Originally
published as D 483 – 61 T. Last previous edition D 483 – 97.
all reagents shall conform to the specifications of the Commit-
Annual Book of ASTM Standards, Vol 11.01.
tee onAnalytical Reagents of theAmerican Chemical Society,
Annual Book of ASTM Standards, Vol 05.01.
Annual Book of ASTM Standards, Vol 05.02.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D483–00
where such specifications are available. Other grades may be test. Adjust the shaker rate and check it before and after each
used, provided it is first ascertained that the reagent is of test to make sure that the rate does not deviate more than 610
sufficiently high purity to permit its use without lessening the cycles/min from the rate established by calibration.
accuracy of the determination. (Warning—When hand shaking, protect the face with a safety
7.2 Fuming Sulfuric Acid (approximately 15 % free mask and point the Babcock bottle away from other personnel.
SO ).Warning—See Notes 1 and 2. Protect hands by wearing suitable safety gloves.)
7.3 Sulfuric Acid (98.61 %)—Prepare (Warning—
NOTE 1—If hand shaking is used, shake the sulfonation flask by
Corrosive. Health hazard. Oxidizer.) (Warning—While pre-
grasping the neck between the thumb and index finger and swinging the
paring the reagent, protect the face with a safety mask and
flask through an arc of approximately 20° so that the bottom of the flask
placetheflaskinatray.)byblendingreagent-gradefumingand passes through a distance of 64 to 89 mm (2.5 to 3.5 in.). Shake at the rate
established by calibration within a tolerance of 610 cycles/min.
concentratedsulfuricacidstoaconcentrationof98.61 60.1 %
H SO as determined by titration.
2 4 11.2 Using Test Methods D 1298 or D 4052, determine the
7.4 Sulfuric Acid (sp gr 1.84, approximately 95 %)—
density at 25°C in grams per millilitre by means of data
Concentrated sulfuric acid (H SO ). (Warning—Corrosive.
2 4 obtained from Vol VIII and Vol XI/XII of the Petroleum
Health hazard. Oxidizer.).
Measurement Tables. (See Guide D 1250.)
11.3 Weigh into a clean, dry sulfonation flask the equivalent
8. Reference Spray Oil
of 4.9 to 5.1 mL of the sample at 25°C, weighed to the nearest
8.1 Test results for unsulfonated residue are highly depen-
0.005 g, adding the oil to the flask by pipet, and taking care to
dent upon rate of shaking. A reference spray oil has been
deposit as little oil as possible on the neck of the flask. From
calibrated for unsulfonated residue by a group of cooperating
the weight of the sample, calculate its volume at 25°C.
laboratories using both machine and hand shaking. Instructions
11.4 Slowly introduce 20 6 0.5 mL of H SO (98.61 %)
2 4
are given in Section 8 for using this reference oil as a guide to
into the flask in such a way that oil adhering to the neck of the
ensure that the rate of shaking is correct.
flask will be washed down.Transfer the flask to the carrier, and
suspend the carrier in the boiling water bath, with the flask
9. Calibration
immersed to a point between the 0 and 10 marks, noting the
9.1 Machine Shaking Rate—A rate of 425 cycles/min was
time when this is done. Close the cover of the bath, and direct
used in the cooperative work to establish the unsulfonated
a gentle stream of air across the top of the flask to blow away
residue of the reference spray oil. There are small variations in
any steam arising from the opening.
severity of shaking between individual machines, even when
11.5 After the flask has been in the bath for 10 6 1 min,
they are newly built and of the same make; and these
remove the carrier and install it, with minimum delay, on the
differences can increase with use. Consequently, each labora-
shaker. While wearing a face shield, shake for 10 61satthe
tory shall run occasional tests on the reference spray oil. If an
rate established in the calibration with the reference spray oil.
unsulfonated residue is found which differs by more than
(Warning—Certain samples of low unsulfonated residue can
60.4 % from the established value, the rate of shaking shall be
foam excessively when shaken. Stop the shaker when the foam
adjusted accordingly. A faster rate tends to give a lower
rises in the neck of the flask, and shake intermittently but at the
unsulfonated residue, and vice versa.
specified rate. Substitute the counter for the timer and shake a
9.2 Hand Shaking Rate—Each operator shall standardize
total number of cycles equal to one-sixth of the number
his technique of shaking so as to obtain the established value
representing the established rate in cycles per minute, even
(within 6 0.4 %) on the reference spray oil. A rate of 300
though it requires more than 10 s for example, if the rate is 425
cycles/min was used in the manual shaking tests in the
cycles/min, shake 71 cycles.) After shaking, return the carrier
cooperative program on the reference oil; however, an indi-
to the bath as quickly as possible. Repeat the shaking at 10 6
vidual operator’s calibrated rate can differ appreciably from
1 min intervals for a total of six shaking periods, so that an
300 cycles/min.
hour has elapsed between the time of placing the flask in the
bath, and the removal for the final shaking.
10. Sampling
11.6 After the final shaking, cool to approximately room
10.1 Obtain a sample for this test method using Practices D
temperature, and add sufficient H SO (95 %) to raise the oil
2 4
4057 or D 4177.
into the neck of the flask nearly to the top graduation. Place the
flask in the centrifuge, balancing as necessary, and centrifuge
11. Procedure
for 10 min at a speed calculated by
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