ASTM D483-04(2018)
(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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
General Information
Relations
Standards Content (Sample)
This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D483 − 04 (Reapproved 2018)
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 D4052 Test Method for Density, Relative Density, and API
Gravity of Liquids by Digital Density Meter
1.1 This test method covers the determination of unsul-
D4057 Practice for Manual Sampling of Petroleum and
fonated residue in plant spray oils of petroleum origin and
Petroleum Products
applies only to the petroleum oil content. It provides a measure
D4177 Practice for Automatic Sampling of Petroleum and
of the degree of refinement of plant spray oils by determining
Petroleum Products
the extent to which the oil is attacked by 98.61 % sulfuric acid
under closely standardized conditions. Since the relationship
3. Terminology
betweenunsulfonatedresidueandtheactualcompositionofthe
oil is not known, this test method should be applied only for 3.1 Definitions:
measuring the degree of refinement and not for the determina-
3.1.1 unsulfonated residue, n— in oils, that portion of an oil
tion of aromatics or olefins, or both.
remaining unsulfonated after treatment with concentrated sul-
furic acid.
1.2 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this
4. Summary of Test Method
standard.
1.3 This standard does not purport to address all of the
4.1 A measured volume of sample is shaken with 98.61 %
safety concerns, if any, associated with its use. It is the
sulfuric acid at 100 °C in a Babcock bottle, shaking mechani-
responsibility of the user of this standard to establish appro-
cally for 10 s at 10 min intervals. The volume not absorbed by
priate safety, health, and environmental practices and deter-
the acid is a measure of the unsulfonated residue in the sample.
mine the applicability of regulatory limitations prior to use.
1.4 This international standard was developed in accor-
5. Significance and Use
dance with internationally recognized principles on standard-
5.1 This test method is useful for distinguishing between
ization established in the Decision on Principles for the
oils that are adaptable to various types of spraying application,
Development of International Standards, Guides and Recom-
with a higher unsulfonated oil being required for leaf spraying
mendations issued by the World Trade Organization Technical
as compared to dormant vegetation application.
Barriers to Trade (TBT) Committee.
6. Apparatus
2. Referenced Documents
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
6.2 Meniscus Viewing Lens, focusing type, consisting of
D1298 Test Method for Density, Relative Density, or API
eyepiece and objective to facilitate reading the meniscus with
Gravity of Crude Petroleum and Liquid Petroleum Prod-
a minimum of parallax, is recommended.
ucts by Hydrometer Method
6.3 Water Baths—Two water baths maintained at 25 °C 6
0.5 °C and 99.5 °C to 100 °C, and conforming to the require-
This test method is under the jurisdiction of ASTM Committee D02 on ments prescribed in Annex A1.
Petroleum Products, Liquid Fuels, and Lubricantsand is the direct responsibility of
Subcommittee D02.06 on Analysis of Liquid Fuels and Lubricants. 6.4 Shaking Machine—The exact design described in the
Current edition approved Oct. 1, 2018. Published November 2018. Originally
appendix is required for uniform control of shaking and
approved in 1961. Last previous edition approved in 2014 as D483 – 04 (2014).
precision results. Hand shaking is permissible if technique is
DOI: 10.1520/D0483-04R18.
2 developed to correlate results by machine shaking.
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
6.5 Centrifuge—A centrifuge as described in Annex A1 is
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. recommended.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D483 − 04 (2018)
7. Reagents cles⁄min was used in the manual shaking tests in the coopera-
tive program on the reference oil; however, an individual
7.1 Purity of Reagents—Reagent grade chemicals shall be
operator’s calibrated rate can differ appreciably from 300 cy-
used in all tests. Unless otherwise indicated, it is intended that
cles⁄min.
all reagents shall conform to the specifications of the Commit-
tee onAnalytical Reagents of theAmerican Chemical Society,
10. Sampling
where such specifications are available. Other grades may be
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 Adjust the temperature of the boiling water bath to
7.2 Fuming Sulfuric Acid (approximately 15 % free SO ).
99.5 °C to 100 °C and keep it in this temperature range
(Warning—See 7.3 and7.4.)
throughout the test. Adjust the shaker rate and check it before
7.3 Sulfuric Acid (98.61 %)—Prepare by blending reagent-
and after each test to make sure that the rate does not deviate
gradefumingandconcentratedsulfuricacidstoaconcentration more than 610 cycles⁄min from the rate established by cali-
of 98.61 % 6 0.1 % H SO as determined by titration.
bration. (Warning—When hand shaking, protect the face with
2 4
(Warning—Corrosive. Health hazard. Oxidizer.) (Warning— a safety mask and point the Babcock bottle away from other
While preparing the reagent, protect the face with a safety
personnel. Protect hands by wearing suitable safety gloves.)
mask and place the flask in a tray.)
NOTE 1—If hand shaking is used, shake the sulfonation flask by
7.4 Sulfuric Acid (sp gr 1.84, approximately 95 %)—
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
Concentrated sulfuric acid (H SO ). (Warning—Corrosive.
2 4
passes through a distance of 64 mm to 89 mm. Shake at the rate
Health hazard. Oxidizer.).
established by calibration within a tolerance of 610 cycles/min.
8. Reference Spray Oil
11.2 Using Test Methods D1298 or D4052, determine the
density at 25 °C in grams per millilitre by means of data
8.1 Test results for unsulfonated residue are highly depen-
obtained from Vol VIII and Vol XI/XII of the Petroleum
dent upon rate of shaking. A reference spray oil has been
Measurement Tables. (See Guide D1250.)
calibrated for unsulfonated residue by a group of cooperating
laboratories using both machine and hand shaking. Instructions
11.3 Weigh into a clean, dry sulfonation flask the equivalent
are given in Section 8 for using this reference oil as a guide to
of 4.9 mL to 5.1 mL of the sample at 25 °C, weighed to the
ensure that the rate of shaking is correct.
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.
9. Calibration
From the weight of the sample, calculate its volume at 25 °C.
9.1 Machine Shaking Rate—A rate of 425 cycles⁄min was
11.4 Slowlyintroduce20 mL 60.5 mLofH SO (98.61 %)
2 4
used in the cooperative work to establish the unsulfonated
into the flask in such a way that oil adhering to the neck of the
residue of the reference spray oil. There are small variations in
flask will be washed down.Transfer the flask to thecarrier,and
severity of shaking between individual machines, even when
suspend the carrier in the boiling water bath, with the flask
they are newly built and of the same make; and these
immersed to a point between the 0 and 10 marks, noting the
differences can increase with use. Consequently, each labora-
time when this is done. Close the cover of the bath, and direct
tory shall run occasional tests on the reference spray oil. If an
a gentle stream of air across the top of the flask to blow away
unsulfonated residue is found which differs by more than
any steam arising from the opening.
60.4 % from the established value, the rate of shaking shall be
adjusted accordingly. A faster rate tends to give a lower 11.5 Aftertheflaskhasbeeninthebathfor10 min 61 min,
unsulfonated residue, and vice versa. remove the carrier and install it, with minimum delay, on the
shaker.While wearing a face shield, shake for 10 s 6 1 s at the
9.2 Hand Shaking Rate—Eachoperatorshallstandardizehis
rate established in the calibration with the reference spray oil.
technique of shaking so as to obtain the established value
(Warning—Certain samples of low unsulfonated residue can
(within 60.4 %) on the reference spray oil. A rate of 300 cy-
foam excessively when shaken. Stop the shaker when the foam
rises in the neck of the flask, and shake intermittently but at the
3 specified rate. Substitute the counter for the timer and shake a
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For Suggestions on the testing of reagents not
total number of cycles equal to one-sixth of the number
listed by the American Chemical Society, see Annual Standards for Laboratory
representing the established rate in cycles per minute, even
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
though it requires more than 10 s for example, if the rate is
and National Formulary, U.S. Pharm
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.