ASTM D483-04(2009)e1
(Test Method)Standard Test Method for Unsulfonated Residue of Petroleum Plant Spray Oils
Standard Test Method for Unsulfonated Residue of Petroleum Plant Spray Oils
SIGNIFICANCE AND USE
This test method is useful for distinguishing between oils that are adaptable to various types of spraying application, with a higher unsulfonated oil being required for leaf spraying as compared to dormant vegetation application.
SCOPE
1.1 This test method covers the determination of unsulfonated residue in plant spray oils of petroleum origin and applies only to the petroleum oil content. It provides a measure of the degree of refinement of plant spray oils by determining the extent to which the oil is attacked by 98.61 % sulfuric acid under closely standardized conditions. Since the relationship between unsulfonated residue and the actual composition of the oil is not known, this test method should be applied only for measuring the degree of refinement and not for the determination of aromatics or olefins, or both.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
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Designation: D483 − 04(Reapproved 2009)
Standard Test Method for
Unsulfonated Residue of Petroleum Plant Spray Oils
This standard is issued under the fixed designation D483; 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 (´) indicates an editorial change since the last revision or reapproval.
´ NOTE—Deleted informational inch-pound units to make solely SI standard editorially in July 2009.
1. Scope D4177 Practice for Automatic Sampling of Petroleum and
Petroleum Products
1.1 This test method covers the determination of unsul-
fonated residue in plant spray oils of petroleum origin and
3. Terminology
applies only to the petroleum oil content. It provides a measure
3.1 Definitions:
of the degree of refinement of plant spray oils by determining
3.1.1 unsulfonated residue, n— in oils, that portion of an oil
the extent to which the oil is attacked by 98.61 % sulfuric acid
remaining unsulfonated after treatment with concentrated sul-
under closely standardized conditions. Since the relationship
furic acid.
betweenunsulfonatedresidueandtheactualcompositionofthe
oil is not known, this test method should be applied only for
4. Summary of Test Method
measuring the degree of refinement and not for the determina-
tion of aromatics or olefins, or both.
4.1 A measured volume of sample is shaken with 98.61 %
sulfuric acid at 100°C in a Babcock bottle, shaking mechani-
1.2 The values stated in SI units are to be regarded as
cally for 10 s at 10-min intervals. The volume not absorbed by
standard. No other units of measurement are included in this
the acid is a measure of the unsulfonated residue in the sample.
standard.
1.3 This standard does not purport to address all of the
5. Significance and Use
safety concerns, if any, associated with its use. It is the
5.1 This test method is useful for distinguishing between
responsibility of the user of this standard to establish appro-
oils that are adaptable to various types of spraying application,
priate safety and health practices and determine the applica-
with a higher unsulfonated oil being required for leaf spraying
bility of regulatory limitations prior to use.
as compared to dormant vegetation application.
2. Referenced Documents
6. Apparatus
2.1 ASTM Standards:
6.1 Sulfonation Flask—The flask is shown in Fig.A1.1 and
D1193 Specification for Reagent Water
described in Annex A1.
D1250 Guide for Use of the Petroleum Measurement Tables
D1298 Test Method for Density, Relative Density (Specific 6.2 Meniscus Viewing Lens, focusing type, consisting of
Gravity), or API Gravity of Crude Petroleum and Liquid eyepiece and objective to facilitate reading the meniscus with
Petroleum Products by Hydrometer Method a minimum of parallax, is recommended.
D4052 Test Method for Density, Relative Density, and API
6.3 Water Baths— Two water baths maintained at 25 6
Gravity of Liquids by Digital Density Meter
0.5°C and 99.5 to 100°C, and conforming to the requirements
D4057 Practice for Manual Sampling of Petroleum and
prescribed in Annex A1.
Petroleum Products
6.4 Shaking Machine— The exact design described in the
appendix is required for uniform control of shaking and
precision results. Hand shaking is permissible if technique is
This test method is under the jurisdiction of ASTM Committee D02 on
developed to correlate results by machine shaking.
Petroleum Products and Lubricantsand is the direct responsibility of Subcommittee
D02.06 on Analysis of Lubricants.
6.5 Centrifuge—A centrifuge as described in Annex A1 is
Current edition approved April 15, 2009. Published July 2009. Originally
recommended.
approved in 1961. Last previous edition approved in 2004 as D483–04. DOI:
10.1520/D0483-04R09E01.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 7. Reagents
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
7.1 Purity of Reagents—Reagent grade chemicals shall be
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. used in all tests. Unless otherwise indicated, it is intended that
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
´1
D483 − 04 (2009)
all reagents shall conform to the specifications of the Commit- 10. Sampling
tee onAnalytical Reagents of theAmerican Chemical Society,
10.1 Obtain a sample for this test method using Practices
where such specifications are available. Other grades may be
D4057 or D4177.
used, provided it is first ascertained that the reagent is of
sufficiently high purity to permit its use without lessening the
11. Procedure
accuracy of the determination.
11.1 Adjustthetemperatureoftheboilingwaterbathto99.5
7.1.1 Commercially prepared solutions may be used when
to 100°C and keep it in this temperature range throughout the
they meet or exceed the specifications set in 7.1.
test. Adjust the shaker rate and check it before and after each
7.2 Fuming Sulfuric Acid (approximately 15 % free SO ). (
test to make sure that the rate does not deviate more than 610
Warning—See 7.3 and 7.4.)
cycles/min from the rate established by calibration.
(Warning—When hand shaking, protect the face with a safety
7.3 Sulfuric Acid (98.61 %)—Prepare by blending reagent-
mask and point the Babcock bottle away from other personnel.
gradefumingandconcentratedsulfuricacidstoaconcentration
Protect hands by wearing suitable safety gloves.)
of 98.61 6 0.1 % H SO as determined by titration. (
2 4
Warning—Corrosive. Health hazard. Oxidizer.) ( Warning—
NOTE 1—If hand shaking is used, shake the sulfonation flask by
While preparing the reagent, protect the face with a safety grasping the neck between the thumb and index finger and swinging the
flask through an arc of approximately 20° so that the bottom of the flask
mask and place the flask in a tray.)
passes through a distance of 64 to 89 mm. Shake at the rate established by
7.4 Sulfuric Acid (sp gr 1.84, approximately 95 %)—
calibration within a tolerance of 610 cycles/min.
Concentrated sulfuric acid (H SO ). (Warning—Corrosive.
2 4
11.2 Using Test Methods D1298 or D4052, determine the
Health hazard. Oxidizer.).
density at 25°C in grams per millilitre by means of data
obtained from Vol VIII and Vol XI/XII of the Petroleum
8. Reference Spray Oil
Measurement Tables. (See Guide D1250.)
8.1 Test results for unsulfonated residue are highly depen-
11.3 Weigh into a clean, dry sulfonation flask the equivalent
dent upon rate of shaking. A reference spray oil has been
of 4.9 to 5.1 mLof the sample at 25°C, weighed to the nearest
calibrated for unsulfonated residue by a group of cooperating
0.005 g, adding the oil to the flask by pipet, and taking care to
laboratoriesusingbothmachineandhandshaking.Instructions
deposit as little oil as possible on the neck of the flask. From
are given in Section 8 for using this reference oil as a guide to
the weight of the sample, calculate its volume at 25°C.
ensure that the rate of shaking is correct.
11.4 Slowly introduce 20 6 0.5 mL of H SO (98.61 %)
2 4
9. Calibration
into the flask in such a way that oil adhering to the neck of the
flaskwillbewasheddown.Transfertheflasktothecarrier,and
9.1 Machine Shaking Rate—A rate of 425 cycles/min was
used in the cooperative work to establish the unsulfonated suspend the carrier in the boiling water bath, with the flask
immersed to a point between the 0 and 10 marks, noting the
residue of the reference spray oil. There are small variations in
severity of shaking between individual machines, even when time when this is done. Close the cover of the bath, and direct
a gentle stream of air across the top of the flask to blow away
they are newly built and of the same make; and these
differences can increase with use. Consequently, each labora- any steam arising from the opening.
tory shall run occasional tests on the reference spray oil. If an
11.5 After the flask has been in the bath for 10 6 1 min,
unsulfonated residue is found which differs by more than
remove the carrier and install it, with minimum delay, on the
60.4 % from the established value, the rate of shaking shall be
shaker. While wearing a face shield, shake for 10 61satthe
adjusted accordingly. A faster rate tends to give a lower
rate established in the calibration with the reference spray oil.
unsulfonated residue, and vice versa.
(Warning —Certain samples of low unsulfonated residue can
foam excessively when shaken. Stop the shaker when the foam
9.2 Hand Shaking Rate—Eachoperatorshallstandardizehis
rises in the neck of the flask, and shake intermittently but at the
technique of shaking so as to obtain the established value
specified rate. Substitute the counter for the timer and shake a
(within 6 0.4 %) on the reference spray oil. A rate of 300
total number of cycles equal to one-sixth of the number
cycles/min was used in the manual shaking tests in the
representing the established rate in cycles per minute, even
cooperative program on the reference oil; however, an indi-
vidual operator’s calibrated rate can differ appreciably from though it requires more than 10 s for example, if the rate is 425
cycles/min, shake 71 cycles.) After shaking, return the carrier
300 cycles/min.
to the bath as quickly as possible. Repeat the shaking at 10 6
1 min intervals for a total of six shaking periods, so that an
Reagent Chemicals, American Chemical Society Specifications, American
hour has elapsed between the time of placing the flask in the
Chemical Society, Washington, DC. For Suggestions on the testing of reagents not
bath, and the removal for the final shaking.
listed by the American Chemical Society, see Annual Standards f
...
This document is not anASTM standard and is intended only to provide the user of anASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
´1
An American National Standard Designation: D 483 – 04 (Reapproved 2009)
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 (´) indicates an editorial change since the last revision or reapproval.
´ NOTE—Deleted informational inch-pound units to make solely SI standard editorially in July 2009.
1. Scope
1.1 This test method covers the determination of unsulfonated residue in plant spray oils of petroleum origin and applies only
tothepetroleumoilcontent.Itprovidesameasureofthedegreeofrefinementofplantsprayoilsbydeterminingtheextenttowhich
the oil is attacked by 98.61 % sulfuric acid under closely standardized conditions. Since the relationship between unsulfonated
residue and the actual composition of the oil is not known, this test method should be applied only for measuring the degree of
refinement and not for the determination of aromatics or olefins, or both.
1.2The values stated in SI units are to be regarded as the standard.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory
limitations prior to use.
2. Referenced Documents
2.1 ASTM Standards:
D 1193 Specification for Reagent Water
D 1250 Guide for Use of the Petroleum Measurement Tables
D 1298 Test Method for Density, Relative Density (Specific Gravity), orAPI Gravity of Crude Petroleum and Liquid Petroleum
Products by Hydrometer Method
D 4052 Test Method for Density and Relative Density of Liquids by Digital Density Meter
D 4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D 4177 Practice for Automatic Sampling of Petroleum and Petroleum Products
3. Terminology
3.1 Definition: Definitions:
3.1.1 unsulfonated residue, n— in oils, that portion of an oil remaining unsulfonated after treatment with concentrated sulfuric
acid.
4. Summary of Test Method
4.1 Ameasured volume of sample is shaken with 98.61 % sulfuric acid at 100°C in a Babcock bottle, shaking mechanically for
10 s at 10-min intervals. The volume not absorbed by the acid is a measure of the unsulfonated residue in the sample.
5. Significance and Use
5.1 This test method is useful for distinguishing between oils that are adaptable to various types of spraying application, with
a higher unsulfonated oil being required for leaf spraying as compared to dormant vegetation application.
6. Apparatus
6.1 Sulfonation Flask—The flask is shown in Fig. A1.1 and described in Annex A1.
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products and Lubricants and is the direct responsibility of Subcommittee D02.06 on
Analysis of Lubricants.
Current edition approved Dec. 10, 2000. Published January 2001. Originally published as D483–61T. Last previous edition D483–97.
Current edition approved April 15, 2009. Published July 2009. Originally approved in 1961. Last previous edition approved in 2004 as D 483–04.
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
, Vol 11.01.volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
´1
D483–04 (2009)
6.2 Meniscus Viewing Lens, focusing type, consisting of eyepiece and objective to facilitate reading the meniscus with a
minimum of parallax, is recommended.
6.3 WaterBaths—Twowaterbathsmaintainedat25 60.5°Cand99.5to100°C,andconformingtotherequirementsprescribed
in Annex A1.
6.4 Shaking Machine— The exact design described in the appendix is required for uniform control of shaking and precision
results. Hand shaking is permissible if technique is developed to correlate results by machine shaking.
6.5 Centrifuge—A centrifuge as described in Annex A1 is recommended.
7. Reagents
7.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where
such specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high
purity to permit its use without lessening the accuracy of the determination.
7.1.1 Commercially prepared solutions may be used when they meet or exceed the specifications set in 7.1.
7.2 Fuming Sulfuric Acid (approximately 15 % free SO ).). ( Warning—See Notes 1 and 2.
7.3—See 7.3 and 7.4.)
7.3 Sulfuric Acid (98.61 %)—Prepare (Warning —Corrosive. Health hazard. Oxidizer.) (Warning —While preparing the
reagent, protect the face with a safety mask and place the flask in a tray.) by blending reagent-grade fuming and concentrated
sulfuricacidstoaconcentrationof98.61 60.1%H
—Prepare by blending reagent-grade fuming and concentrated sulfuric acids to a concentration of 98.61
6 0.1 % H SO as determined by titration.
7.4as determined by titration. ( Warning—Corrosive. Health hazard. Oxidizer.) ( Warning—While preparing the reagent,
protect the face with a safety mask and place the flask in a tray.)
7.4 SulfuricAcid(spgr1.84,approximately95 %)—Concentratedsulfuricacid(H SO ).(Warning—Corrosive.Healthhazard.
2 4
Oxidizer.).
8. Reference Spray Oil
8.1 Test results for unsulfonated residue are highly dependent upon rate of shaking. A reference spray oil has been calibrated
for unsulfonated residue by a group of cooperating laboratories using both machine and hand shaking. Instructions are given in
Section 8 for using this reference oil as a guide to ensure that the rate of shaking is correct.
9. Calibration
9.1 Machine Shaking Rate—A rate of 425 cycles/min was used in the cooperative work to establish the unsulfonated residue
ofthereferencesprayoil.Therearesmallvariationsinseverityofshakingbetweenindividualmachines,evenwhentheyarenewly
built and of the same make; and these differences can increase with use. Consequently, each laboratory shall run occasional tests
on the reference spray oil. If an unsulfonated residue is found which differs by more than 60.4 % from the established value, the
rate of shaking shall be adjusted accordingly. A faster rate tends to give a lower unsulfonated residue, and vice versa.
9.2 Hand Shaking Rate—Each operator shall standardize his technique of shaking so as to obtain the established value (within
6 0.4 %) on the reference spray oil. A rate of 300 cycles/min was used in the manual shaking tests in the cooperative program
on the reference oil; however, an individual operator’s calibrated rate can differ appreciably from 300 cycles/min.
10. Sampling
10.1 Obtain a sample for this test method using Practices D 4057 or D 4177.
11. Procedure
11.1 Adjust the temperature of the boiling water bath to 99.5 to 100°C and keep it in this temperature range throughout the test.
Adjust the shaker rate and check it before and after each test to make sure that the rate does not deviate more than 610 cycles/min
from the rate established by calibration. (Warning—When hand shaking, protect the face with a safety mask and point the
Babcock bottle away from other personnel. Protect hands by wearing suitable safety gloves.)
NOTE 1—If hand shaking is used, shake the sulfonation flask by grasping the neck between the thumb and index finger and swinging the flask through
an arc of approximately 20° so that the bottom of the flask passes through a distance of 64 to 89 mm (2.5 to 3.5 in.). mm. Shake at the rate established
by calibration within a tolerance of 610 cycles/min.
Annual Book of ASTM Standards, Vol 05.01.Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For
Suggestions on the testing of reagents not listed by the American Chemical Society, see Annual Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and
the United States Pharmacopeia and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.
Annual Book of ASTM Standards, Vol 05.02.
The reference spray oil may be obtained from R. E. Carroll, Inc., P.O. Box 5806, 1570 North Olden Ave., Trenton, NJ 08638. If you are aware of alternative suppliers,
please provide this information toASTM International Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee,
which you may attend.
´1
D483–04 (2009)
11.2 Using Test Methods D 1298 or D 4052, determine the density at 25°C in grams per millilitre by means of data obtained
from Vol VIII and Vol XI/XII of the Petroleum Measurement Tables. (See Guide D 1250.)
11.3 Weighintoaclean,drysulfonationflasktheequivalentof4.9to5.1mLofthesampleat25°C,weighedtothenearest0.005
g, adding the oil to the flask by pipet, and taking care to deposit as little oil as possible on the neck of the flask. From the weight
of the sample, calculate its volume at 25°C.
11.4 Slowly introduce 20 6 0.5 mL of H SO (98.61 %) into the flask in such a way that oil adhering to the neck of the flask
2 4
will be washed down. Transfer the flask to the carrier, and suspend the carrier in the boiling water bath, with the flask immersed
to a point between the 0 and 10 marks, noting the time when this is done. Close the cover of the bath, and direct a gentle stream
of air across the top of the flask to blow away any steam arising from the opening.
11.5 After the flask has been in the bath for 10 6 1 min, remove the carrier and install it, with minimum delay, on the shaker.
While wearing a face shield, shake for 10 6 1 s at the rate established in the calibration
...
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