ASTM D1024-59

Method of Test for Butadiene Dimer and Styrene in Butadiene Concentrates (Withdrawn 1969)

General Information

• Status: Withdrawn
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants

Standards Content (Sample)

Standard Method of Test for
BUTADIENE DIMER AND STYRENE IN BUTADIENE
1
CONCENTRATES ·'
ASTM Designation: D 1024 - 59
This Standard of the American Society for Testing and :Materials i5 issued under
the fixed designation D 1024; the number immediately following the designa­
tion 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.
The committee responsible for this standard has voted its withdrawal.]
In the absence of substantial rea.~ons that it should be continued,
[
the Society will approve withdrawal from publication in January, 1970.
Scope and Application Summary of Method
2. The butadiene sample, with chloro­
1. This method of test describes a pro­
form added as a chaser, is rapidly dis­
cedure for the determination of butadiene
tilled through a small, simple distillation
dimer (4-vinyl-1-cyclohexene) and sty­
column (Fig. l). The dimer and styrene
rene monomer in hutadiene concentrates.
are retained in the residue while the buta­
The method includes a distillation pro­
diene is completely expelled without
cedure for isolating the dimer, styrene,
being condensed. The bromine number
and nonvolatile matter before analysis.
of the residue is then determined by the
If determinations of butadicne and Ca
procedure described in former ASTM
hydrocarbons on a dimer-free sample are
Method D 1158 - 59 T, Bromine Nwn­
aiso desired, reference shall be made to
ber of Petroleum Distillates bv Color-In­
the distillation procedure described in 4
dicator Titration. In the ~bsence of
ASTM Method D 1023, Test for Separa­
styrene, the dimer content of the resi­
3
tion of Residue from Butadiene.
due is calculated directly from the bro·
mine number. When styrene is present, a
correction must be applied for its reac·
1
Under the standardisation procedure of the
Society, thia method ia under the jurisdfotion tion with bromine.
of the ASTM Committee D-2 on Petroleum
Definitions
Products and Lubricants. A !ht of members may
be found in the AST:\1 Year Book.
3. Buladiene Concentrates are mixtures
Current edition accepted Sept. 10, 1959.
of essentially C hydrocarbons containing
Originally issued 19-t9. Repla~~ D 1024 - 53.
4
In Hl59. the method wa.~ rewritten to indude
a minimum of 60 per cent by weight of
but11diene conceutratP.s cont.aining not less than
1,3-butadiene.
60 per c•mt of butadieue and to perm.it detection
of styrene &a well ae b11t.adiene dimer.
Interferences
11
This method is an adaptation of one de­
veloped and cooperatively tested by the Ruta­ 4·. The interference of inhibitor (p-ter­
diene Producers' Committee on Specifications
tiary butyl catecbol) and nonvolatile
and Method& of Analysis of the Office ol Rubber
Reserve. It appears iu the Butadieue Labora­
I Appears in this publication.
4
tory Manual, Office of Rubber Heserve, as
Dilmontinued, see 1964 Book of ASTJf
Method No. 2.1.lii.
Standard.!, Part 17.
228
42-7

---------------------- Page: 1 ----------------------
TEST FO.R BUTADIE!l."'E DIMER AND STYRENE IN BUTADIENE (D 1024) 229
(g) Separalory Funnels, 125-ml ca­
butacliene polymers is negligible. How­
ever acetylene dimers or polymers, if pacity.
present, may interfere. Ethyl benzene is
Purity of Reagents
not determined in this procedure.
6. (a) Reagent grade chemicals shall be
Apparatus
used in all tests. Unless otherwise indi­
5. (a) Fractionating Column, vacuum­ cated, it is intended that all reagents shall
jacketed and packed with j-in. glass conform to the specifications of the Com­
helices, constructed as detailed in Fig. 1. mittee on Analytical Reagents of the
(b) Distillation Flask, .fiat-bottom, American Chemical Society, where such
5
125-ml capacity, with a 24/40 standard­ specifications are avai!able. Other grades
taper ground-glass joint. may be used provided it is first ascer-
rn'
,-Female Joint
~~~""
~,.-·Gloss Rad
r\~·-·· 10 ml Graduate
·6 ml Merk
· Woter Bath
~
·-chromel Wire Whorl
··- (Roam Temperature)
l
256 A Nichrome · - ----12mm OD
Wire Spring . /
·----- .
24/40 Stando'd Toper
Chloroform Trap
Join\
Frc. 1.-Asscmbly of Dimer Distillation Apparatus.
tained that the reagent is of sufficiently
(c) Water Bath, a 1000-ml beaker.
(d) Bromination Flask, a 500-ml, glass­ high purity to permit its use without
stoppered, iodine number flask. lessening the accuracy of the determina­
(e) Thermometer, having a range of tion.
-40 to 50 C, graduated in 1 C intervals, (b) Unless otherwise indicated, refer-
and mercury-filled.
~ "Reagent Chemicals, American Chemical
4
Wlll!hini:ton, D. C. For suggestions on the tea~
for photometric measurements on liquids
ing of reagents net liated by the American
in the 280 to 285 mµ, wavelength range.
Chemical Society, see "Reagent Ch~mic&!a and
Standards," by Joseph Rosin,
...