ASTM D4423-00(2006)
(Test Method)Standard Test Method for Determination of Carbonyls In C4 Hydrocarbons
Standard Test Method for Determination of Carbonyls In C<inf>4</inf> Hydrocarbons
SIGNIFICANCE AND USE
The determination of the carbonyl content of polymerization-grade 1,3-butadiene is necessary, since in some polymerization reactions, the presence of carbonyls in excess over some specified amount can have a deleterious effect upon the polymer properties or the reaction itself, or both.
SCOPE
1.1 This test method covers the determination of carbonyls (ketones and aldehydes) in C4 hydrocarbons. This test method was tested on polymerization-grade 1,3-butadiene.
1.2 The applicable range for this test method is 0 to 50 mg/kg carbonyls calculated as acetaldehyde.
1.3 Other C4 hydrocarbons and their mixtures besides polymerization-grade 1,3-butadiene could be tested using this same test method. However, the precision section of this test method covers only carbonyls in applicable range as listed in , as found in polymerization-grade 1,3-butadiene.
1.4 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
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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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:D4423–00 (Reapproved 2006)
Standard Test Method for
Determination of Carbonyls In C Hydrocarbons
This standard is issued under the fixed designation D4423; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope releasing an equivalent amount of hydrochloric acid which is
thenback-titratedtotheoriginalcoloration.Ablankcontaining
1.1 This test method covers the determination of carbonyls
only methanol and sample is titrated and the sample’s results
(ketones and aldehydes) in C hydrocarbons. This test method
are calculated using the blank adjustment. Results are reported
was tested on polymerization-grade 1,3-butadiene.
as milligrams per kilogram carbonyls as acetaldehyde.
1.2 The applicable range for this test method is 0 to
50mg/kg carbonyls calculated as acetaldehyde.
4. Significance and Use
1.3 Other C hydrocarbons and their mixtures besides
4.1 The determination of the carbonyl content of
polymerization-grade 1,3-butadiene could be tested using this
polymerization-grade1,3-butadieneisnecessary,sinceinsome
same test method. However, the precision section of this test
polymerization reactions, the presence of carbonyls in excess
method covers only carbonyls in applicable range as listed in
over some specified amount can have a deleterious effect upon
1.2, as found in polymerization-grade 1,3-butadiene.
the polymer properties or the reaction itself, or both.
1.4 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this
5. Apparatus
standard.
5.1 Bunsen Valves—Adeviceconstructedsothatwhenused
1.5 This standard does not purport to address all of the
with an Erlenmeyer flask, the sample vapors can exit the flask
safety concerns, if any, associated with its use. It is the
while protecting the flask’s liquid contents. See Fig. 1 for
responsibility of the user of this standard to establish appro-
details.
priate safety and health practices and determine the applica-
5.2 Cooling Coil—Prepare a cooling coil by winding about
bility of regulatory limitations prior to use.
10 to 15 cm of seamless copper tubing (about 6-mm diameter)
2. Referenced Documents on a short length of pipe (about 1.5 to 2.0-cm diameter),
2 allowing sufficient length of tubing at the end of the coil to
2.1 ASTM Standards:
connect it to the sample source. Attach a valve at a point that
D484 Specification for Hydrocarbon Dry Cleaning Sol-
3 would not extend more than 8 cm above the surface of the
vents
cooling bath liquid. To the valve, attacha6to8cm length
D1193 Specification for Reagent Water
piece of tubing bent downward so that the hydrocarbon liquid
E1 Specification for ASTM Liquid-in-Glass Thermometers
can be directed into the receiving container.
3. Summary of Test Method 5.3 Dewar Flask—The Dewar flask must be of sufficient
volume to completely immerse the main portion of the cooling
3.1 A measured amount of sample is added to an alcoholic
coil except for the extremities necessary for receiving and
hydroxylamine hydrochloride solution that has been adjusted
delivering the sample through the coil.
to a given coloration using either alcoholic acid or base. The
5.4 Erlenmeyer Flasks, 250-mL capacity.
carbonyls will react with the hydroxylamine hydrochloride
5.5 Volumetric Flasks, 1-L capacity. These flasks should be
Class A glassware.
This test method is under the jurisdiction of ASTM Committee D02 on
5.6 Graduated Cylinders—100-mL capacity, glass cylin-
PetroleumProductsandLubricantsandisthedirectresponsibilityofSubcommittee
ders, graduated in 1 or 2-mL divisions.
D02.D0.04 on C Hydrocarbons.
5.7 Microburets,2.00or5.00-mLcapacity.Themicroburets
Current edition approved July 1, 2006. Published August 2006. Originally
approved in 1984. Last previous edition approved in 2000 as D4423–00. DOI:
shouldbeClassAglasswarewith0.01or0.02-mLdivisionsor
10.1520/D4423-00R06.
less. It is advisable to have the buret’s tip end equipped with a
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
syringe needle to dispense very small drops of titrant.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
5.8 Sample Cylinders—These should be of sufficient vol-
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
ume to give the required amount of sample for testing.
Withdrawn. The last approved version of this historical standard is referenced
Stainlesssteelcylindersequippedwithneedlevalvesshouldbe
on www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D4423–00 (2006)
(Warning—Corrosive. Can cause severe burns or blindness.
Evolution of heat produces a violent reaction or eruption upon
too rapid mixture with water.) Make to volume with methanol
in a 1-L volumetric flask. Standardize against a primary
standard, potassium acid phthalate.
6.6 Dry Ice (Carbon Dioxide Solid)—(Warning—
Extremely cold (−78.5°C). Liberates heavy gas which may
cause suffocation. Contact with skin causes burns or freezing,
or both. Vapors may react violently with hot magnesium or
aluminum alloys.)
6.7 Stoddard Solvent—Conforming to the specification
listed in Specification D484.(Warning—Combustible. Vapor
harmful.)
6.8 Thymol Blue Indicator—Dissolve0.04gofthymolblue
in 100 mL of anhydrous methanol. (Warning—Flammable.
Vaporharmful.Maybefatalorcauseblindnessifswallowedor
FIG. 1 Apparatus
inhaled. Cannot be made nonpoisonous.)
7. Preparation of Apparatus
used. It is suggested that a 500-mL-capacity cylinder be the
minumum size to be used for butadiene.
7.1 Dry Ice-Stoddard Solvent Bath—Add a sufficient quan-
5.9 Thermometer—For observing temperatures below
tity of Stoddard solvent into the Dewar flask to ensure that the
−45°C. The Low Cloud and Pour Point Thermometer, con-
cooling coil will be submerged in the liquid plus dry ice (solid
forming to the requirements for ASTM Thermometer 6C, as
CO ). (Warning—See 6.6 and 6.7.) Carefully add sufficient
prescribedinSpecificationE1,issatisfactory.Thermometer6C
dry ice to the Stoddard solvent to obtain a temperature of at
has a range from −80 to +20°C.
least −50°C. (Warning—Great care must be taken during this
step. Do not add the dry ice all at once, but in small pieces,
6. Reagents and Materials
especially at the beginning. Wear protective gloves and ad-
6.1 Purity of Reagents—Reagentgradechemicalsshouldbe
equateeyeprotectiontopreventanycontactwiththeextremely
used in all tests. Unless otherwise indicated, it is intended that
cold materials.) Attach the sample cylinder containing the
all reagents conform to the specifications of the Committee on
butadiene (Warning—Extremely flammable gas under pres-
Analytical Reagents of theAmerican Chemical Society where
sure. May form explosive peroxides upon exposure to air.
such specifications are available. Other grades may be used,
Harmful if inhaled. Irritating to eyes, skin, and mucous
provided it is first ascertained that the reagent is of sufficiently
membranes.) to the cooling coil and immerse the coil into the
high purity to permit its use without lessening the accuracy of
liquid. Support the sample cylinder in a cylinder rack or using
the determination.
a ring stand and appropriate clamps. Be sure the coil is
6.2 Purity of Water—Unlessotherwiseindicated,references
positioned so that the delive
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