ASTM D483-04(2014)
(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
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.
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 2014)
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.
1. Scope 3. Terminology
1.1 This test method covers the determination of unsul- 3.1 Definitions:
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
under closely standardized conditions. Since the relationship
4. Summary of Test Method
betweenunsulfonatedresidueandtheactualcompositionofthe
4.1 A measured volume of sample is shaken with 98.61 %
oil is not known, this test method should be applied only for
sulfuric acid at 100°C in a Babcock bottle, shaking mechani-
measuring the degree of refinement and not for the determina-
cally for 10 s at 10-min intervals. The volume not absorbed by
tion of aromatics or olefins, or both.
the acid is a measure of the unsulfonated residue in the sample.
1.2 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this
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
2.1 ASTM Standards:
described in Annex A1.
D1193 Specification for Reagent Water
6.2 Meniscus Viewing Lens, focusing type, consisting of
D1250 Guide for Use of the Petroleum Measurement Tables
eyepiece and objective to facilitate reading the meniscus with
D1298 Test Method for Density, Relative Density, or API
a minimum of parallax, is recommended.
Gravity of Crude Petroleum and Liquid Petroleum Prod-
ucts by Hydrometer Method
6.3 Water Baths— Two water baths maintained at 25 6
D4052 Test Method for Density, Relative Density, and API
0.5°C and 99.5 to 100°C, and conforming to the requirements
Gravity of Liquids by Digital Density Meter
prescribed in Annex A1.
D4057 Practice for Manual Sampling of Petroleum and
6.4 Shaking Machine— The exact design described in the
Petroleum Products
appendix is required for uniform control of shaking and
D4177 Practice for Automatic Sampling of Petroleum and
Petroleum Products 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
This test method is under the jurisdiction of ASTM Committee D02 on
recommended.
Petroleum Products, Liquid Fuels, and Lubricantsand is the direct responsibility of
Subcommittee D02.06 on Analysis of Lubricants.
CurrenteditionapprovedMay1,2014.PublishedJuly2014.Originallyapproved
7. Reagents
ε01
in 1961. Last previous edition approved in 2009 as D483 – 04 (2009) . DOI:
10.1520/D0483-04R14.
7.1 Purity of Reagents—Reagent grade chemicals shall be
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
used in all tests. Unless otherwise indicated, it is intended that
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
all reagents shall conform to the specifications of the Commit-
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. tee onAnalytical Reagents of theAmerican Chemical Society,
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D483 − 04 (2014)
where such specifications are available. Other grades may be 10. Sampling
used, provided it is first ascertained that the reagent is of
10.1 Obtain a sample for this test method using Practices
sufficiently high purity to permit its use without lessening the
D4057 or D4177.
accuracy of the determination.
7.1.1 Commercially prepared solutions may be used when 11. Procedure
they meet or exceed the specifications set in 7.1.
11.1 Adjustthetemperatureoftheboilingwaterbathto99.5
to 100°C and keep it in this temperature range throughout the
7.2 Fuming Sulfuric Acid (approximately 15 % free SO ).
(Warning—See 7.3 and7.4.) test. Adjust the shaker rate and check it before and after each
test to make sure that the rate does not deviate more than
7.3 Sulfuric Acid (98.61 %)—Prepare by blending reagent-
610 cycles⁄min from the rate established by calibration.
gradefumingandconcentratedsulfuricacidstoaconcentration
(Warning—When hand shaking, protect the face with a safety
of 98.61 6 0.1 % H SO as determined by titration.
2 4
mask and point the Babcock bottle away from other personnel.
(Warning—Corrosive. Health hazard. Oxidizer.) (Warning—
Protect hands by wearing suitable safety gloves.)
While preparing the reagent, protect the face with a safety
mask and place the flask in a tray.) NOTE 1—If hand shaking is used, shake the sulfonation flask by
grasping the neck between the thumb and index finger and swinging the
7.4 Sulfuric Acid (sp gr 1.84, approximately 95 %)—
flask through an arc of approximately 20° so that the bottom of the flask
Concentrated sulfuric acid (H SO ). (Warning—Corrosive.
passes through a distance of 64 to 89 mm. Shake at the rate established by
2 4
calibration within a tolerance of 610 cycles/min.
Health hazard. Oxidizer.).
11.2 Using Test Methods D1298 or D4052, determine the
8. Reference Spray Oil
density at 25°C in grams per millilitre by means of data
obtained from Vol VIII and Vol XI/XII of the Petroleum
8.1 Test results for unsulfonated residue are highly depen-
Measurement Tables. (See Guide D1250.)
dent upon rate of shaking. A reference spray oil has been
calibrated for unsulfonated residue by a group of cooperating
11.3 Weigh into a clean, dry sulfonation flask the equivalent
laboratories using both machine and hand shaking. Instructions of 4.9 to 5.1 mLof the sample at 25°C, weighed to the nearest
are given in Section 8 for using this reference oil as a guide to
0.005 g, adding the oil to the flask by pipet, and taking care to
ensure that the rate of shaking is correct. deposit as little oil as possible on the neck of the flask. From
the weight of the sample, calculate its volume at 25°C.
9. Calibration
11.4 Slowly introduce 20 6 0.5 mL of H SO (98.61 %)
2 4
into the flask in such a way that oil adhering to the neck of the
9.1 Machine Shaking Rate—A rate of 425 cycles/min was
flask will be washed down.Transfer the flask to thecarrier,and
used in the cooperative work to establish the unsulfonated
residue of the reference spray oil. There are small variations in suspend the carrier in the boiling water bath, with the flask
immersed to a point between the 0 and 10 marks, noting the
severity of shaking between individual machines, even when
they are newly built and of the same make; and these 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
differences can increase with use. Consequently, each labora-
tory shall run occasional tests on the reference spray oil. If an any steam arising from the opening.
unsulfonated residue is found which differs by more than
11.5 After the flask has been in the bath for 10 6 1 min,
60.4 % from the established value, the rate of shaking shall be
remove the carrier and install it, with minimum delay, on the
adjusted accordingly. A faster rate tends to give a lower
shaker. While wearing a face shield, shake for 10 61satthe
unsulfonated residue, and vice versa.
rate established in the calibration with the reference spray oil.
(Warning —Certain samples of low unsulfonated residue can
9.2 Hand Shaking Rate—Eachoperatorshallstandardizehis
foam excessively when shaken. Stop the shaker when the foam
technique of shaking so as to obtain the established value
rises in the neck of the flask, and shake intermittently but at the
(within 6 0.4 %) on the reference spray oil. A rate of
specified rate. Substitute the counter for the timer and shake a
300 cycles⁄min was used in the manual shaking tests in the
total number of cycles equal to one-sixth of the number
cooperative program on the reference oil; however, an indi-
representing the established rate in cycles per minute, even
vidual operator’s calibrated rate can differ appreciably from
though it requires more than 10 s for example, if the rate is
300 cycles/min.
425 cycles⁄min, shake 71 cycles.) After shaking, return the
carrier 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
Reagent Chemicals, American Chemical Society Specifications, American
an hour has elapsed between the time of placingtheflaskinthe
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 for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pha
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM 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
Designation: D483 − 04 (Reapproved 2009) D483 − 04 (Reapproved 2014)
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.
ε 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
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.
2. Referenced Documents
2.1 ASTM Standards:
D1193 Specification for Reagent Water
D1250 Guide for Use of the Petroleum Measurement Tables
D1298 Test Method for Density, Relative Density, or API Gravity of Crude Petroleum and Liquid Petroleum Products by
Hydrometer Method
D4052 Test Method for Density, Relative Density, and API Gravity of Liquids by Digital Density Meter
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D4177 Practice for Automatic Sampling of Petroleum and Petroleum Products
3. Terminology
3.1 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 A measured 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 Products, Liquid Fuels, and Lubricantsand is the direct responsibility of
Subcommittee D02.06 on Analysis of Lubricants.
Current edition approved April 15, 2009May 1, 2014. Published July 2009July 2014. Originally approved in 1961. Last previous edition approved in 20042009 as
ε01
D483D483 – 04 (2009) –04. DOI: 10.1520/D0483-04R09E01.10.1520/D0483-04R14.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
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
D483 − 04 (2014)
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 Water Baths— Two water baths maintained at 25 6 0.5°C and 99.5 to 100°C, and conforming to the requirements prescribed
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 7.3 and7.4.)
7.3 Sulfuric Acid (98.61 %)—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. (Warning—Corrosive. Health hazard. Oxidizer.) (Warning—While preparing
2 4
the reagent, protect the face with a safety mask and place the flask in a tray.)
7.4 Sulfuric Acid (sp gr 1.84, approximately 95 %)—Concentrated sulfuric acid (H SO ). (Warning—Corrosive. Health hazard.
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
of the reference spray oil. There are small variations in severity of shaking between individual machines, even when they are newly
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 300300 cycles cycles/min ⁄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 D4057 or D4177.
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 610610 cycles
cycles/min ⁄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. Shake at the rate established by calibration within
a tolerance of 610 cycles/min.
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.
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 to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee,
which you may attend.
D483 − 04 (2014)
11.2 Using Test Methods D1298 or D4052, 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 D1250.)
11.3 Weigh into a clean, dry sulfonation flask the equivalent of 4.9 to 5.1 mL of the sample at 25°C, weighed to the nearest 0.005
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 with the reference spray oil. (Warning
—Certain s
...
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