ASTM D4423-00
(Test Method)Standard Test Method for Determination of Carbonyls In C4 Hydrocarbons
Standard Test Method for Determination of Carbonyls In C<sub>4</sub> Hydrocarbons
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 1.2, as found in polymerization-grade 1,3-butadiene.
1.4 The values stated in SI units are to be regarded as the standard.
1.5 This standard does not purport to address all of the safety problems, 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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An American National Standard
Designation:D4423–00
Standard Test Method for
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Determination of Carbonyls In C Hydrocarbons
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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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope 4. Significance and Use
1.1 This test method covers the determination of carbonyls 4.1 The determination of the carbonyl content of
(ketones and aldehydes) in C hydrocarbons. This test method polymerization-grade1,3-butadieneisnecessary,sinceinsome
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was tested on polymerization-grade 1,3-butadiene. polymerization reactions, the presence of carbonyls in excess
1.2 The applicable range for this test method is 0 to 50 over some specified amount can have a deleterious effect upon
mg/kg carbonyls calculated as acetaldehyde. the polymer properties or the reaction itself, or both.
1.3 Other C hydrocarbons and their mixtures besides
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5. Apparatus
polymerization-grade 1,3-butadiene could be tested using this
5.1 Bunsen Valves—Adeviceconstructedsothatwhenused
same test method. However, the precision section of this test
method covers only carbonyls in applicable range as listed in with an Erlenmeyer flask, the sample vapors can exit the flask
while protecting the flask’s liquid contents. See Fig. 1 for
1.2, as found in polymerization-grade 1,3-butadiene.
1.4 The values stated in SI units are to be regarded as the details.
5.2 Cooling Coil—Prepare a cooling coil by winding about
standard.
1.5 This standard does not purport to address all of the 10 to 15 cm of seamless copper tubing (about 6-mm diameter)
on a short length of pipe (about 1.5 to 2.0-cm diameter),
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- allowing sufficient length of tubing at the end of the coil to
connect it to the sample source. Attach a valve at a point that
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. would not extend more than 8 cm above the surface of the
cooling bath liquid. To the valve, attacha6to8cm length
2. Referenced Documents
piece of tubing bent downward so that the hydrocarbon liquid
2.1 ASTM Standards: can be directed into the receiving container.
D484 Specification for Hydrocarbon Dry Cleaning Sol- 5.3 Dewar Flask—The Dewar flask must be of sufficient
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vents volume to completely immerse the main portion of the cooling
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D1193 Specification for Reagent Water coil except for the extremities necessary for receiving and
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E1 Specification for ASTM Thermometers delivering the sample through the coil.
5.4 Erlenmeyer Flasks. 250-mL capacity.
3. Summary of Test Method
5.5 Volumetric Flasks. 1-L capacity. These flasks should be
3.1 A measured amount of sample is added to an alcoholic Class A glassware.
hydroxylamine hydrochloride solution that has been adjusted
5.6 Graduated Cylinders—100-mL capacity, glass cylin-
to a given coloration using either alcoholic acid or base. The ders, graduated in 1 or 2-mL divisions.
carbonyls will react with the hydroxylamine hydrochloride
5.7 Microburets.2.00or5.00-mLcapacity.Themicroburets
releasing an equivalent amount of hydrochloric acid which is should be ClassAglassware with 0.01 or 0.02-mLdivisions or
thenback-titratedtotheoriginalcoloration.Ablankcontaining
less. It is advisable to have the buret’s tip end equipped with a
only methanol and sample is titrated and the sample’s results syringe needle to dispense very small drops of titrant.
are calculated using the blank adjustment. Results are reported
5.8 Sample Cylinders—These should be of sufficient vol-
as milligrams per kilogram carbonyls as acetaldehyde. ume to give the required amount of sample for testing.
Stainlesssteelcylindersequippedwithneedlevalvesshouldbe
used. It is suggested that a 500-mL-capacity cylinder be the
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This test method is under the jurisdiction of ASTM Committee D02 on
minumum size to be used for butadiene.
PetroleumProductsandLubricantsandisthedirectresponsibilityofSubcommittee
5.9 Thermometer—For observing temperatures
D02.D0.04 on C Hydrocarbons.
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Current edition approved Dec. 10, 2000. Published January 2001. Originally below−45°C. The Low Cloud and Pour Point Thermometer,
published as D4423–84. Last previous edition D4423–91(1996).
conforming to the requirements for ASTM Thermometer 6C,
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Discontinued; see 1983 Annual Book of ASTM Standards, Vol. 05.01.
asprescribedinSpecificationE1,issatisfactory.Thermometer
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Annual Book of ASTM Standards, Vol 11.01
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6C has a range from−80 to+20°C.
Annual Book of ASTM Standards, Vol 14.03.
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