ASTM D1023-52(1976)

Method of Test for Separation of Residue from Butadiene (Withdrawn 1983)

General Information

• Status: Withdrawn
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.D0.02 - Ethylene

Standards Content (Sample)

AMERICAN socrA'lPMtSfP~NG MATERIALS
1916 RACE ST., PHILADELPHIA 3, PA.
A .Reprint lrom Copyrighted A.S.T.M. Publications
Standard Method of Test for
1 2
SEPARATION OF RESIDUE FROM BUTADIENE •
APPROVED AS
AMERICAN STANDARD
BY THE AMERICAN STANDARDS ASSOCIATION
· ASA NO.: Zll.75•1952
UDC 665.52:620.1
REAFFIRMED 1960
ASTM Designation: - D 1023-52 (t\'lt)
ADOPTED, 1952.
This Standard of the American Society for Testing Materials is issued under
the fixed designation D 1023; the final number indicates the year of original
adoption as standard or, in the case of revision, the year of last revision.
Scope Outline of Method
1. This method of test describes a 2. The sample is distilled throu~ a
procedure for the separation of polymer­ small, simply designed fractionating
ization grade or recycle butadiene into a column with rapid throughput and slight
distillate consisting of butadiene to­ reflux (Fig. 1). The overhead vapors are
gether with c6 and lighter hydrocarbons, condensed for use in analyses requiring
and a residue containing butadiene dimer samples free from dimer, styrene, and
(4-vinyl-1-cyclohexene), nonvolatile mat­ nonvolatile matter. The residue is further
te!, and styrene if present. purified for analyses for dimer or styrene,
or both.
NOTE 1.-If the butadiene sample is to be
analyzed only for dimer or styrene, or both, so
NOTE 2.-The separation is sufficiently quan.
that it is unnecessary to collect the distillate,
titative so that the distillate may be used in
use the distillation procedure of ASTM Method
analyses, such as those for butadiene and C
D 1024; Test for Butadiene Dimer and Styrene
hydrocarbons, in which dimer, nonvolatile mat­
in Butadiene Concentrates.•
ter, and styrene interfere. However, the residue
must be further purified to remove traces of Ci
and c6 hydrocarbons before its analysis for
Under the etandardization procedure of the
dimer or styrene, or both.
Society, this method is under the jurisdiction of
the ASTM Committee D-2 on Petroleum Prod­
ucts and Lubricants.
Apparatus
I This method is an adaptation of one de­
veloped and cooperatively tested by the Buta­
3. (a) Fractionating Column, vacuum­
diene Producer's Committee on Specifications
jacketed and packed with i-in. glass
and Methods of Analyses of the Office of Rubber
Reserve. It appears in the Butadiene Labora­ helices, constructed as detailed in Fig. 1.
tory Manual, Office of Rubber Reserve, as
(b) Distillation Flask, flat-bottomed,
Method No. 2.1.56.2.
125-ml capacity, with 24/40 standard
• Prior to adoption as standard, this method
was published as tentative from 1949 to 1952.
taper ground-glass joint.
Published first as information in Proceedings,
(c) Receiver, as shown in Fig. 1.
Arn. Soc. Testing Mats., Vol. 48, p. 309 (1948).
(d) Graduated Cylinder, capacity of
'1959 Supplement to Book of ASTM Stand-
ards, Part 7. 517
518 TEST FOR RESIDUE SEPARATION FROM BUTADIENE (D 1023 -52)
50 ml, graduated in 0.5-ml subdivisions,
Provide a drying tube filled with CaCl1
and accurate to 0.24 ml. at the opening to the air.
(e) Water Bath.-A 1000-ml beaker.
(h) Thermometer, having a range of
A
ORY IC£
CONDENSER
CHROME I.
WIRE WHORL.
CHLOROFORM TRAP
21 MM. 0.0.
£VACUAT£0
JACKET RECEIVER
CHROME!.
WIRE WHORL
I
I
l!>I A NICHAOMI
I
WIRE SPRING
I
I
2.4/40 STANOAAO
I
TAPER JOINT
I
I
I
I
I
f
I
I I
FIG. 1.-Assembly of Distillation Apparatus.
(f) Dry Ice-Acetone Bath.-A wide­
-40 to 50 C, graduated in 1 C intervals,
mouth, 1-qt Dewar fl.ask.
and mercury-filled.
(g) Chloro
...