ASTM D1089-59(1978)

Method of Test for Carbonyl Content of Butadiene (Withdrawn 1983)

General Information

• Status: Withdrawn
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.D0.03 - Propylene

Standards Content (Sample)

AMERICAN SOCIETY FOR TESTING MATERIALS
1916 RACE ST., PHILADELPHIA 3, PA.
Reprinted from Copyrigh.ted 1959 Supplement to
Book of ASTM Standards, Part 7
APPROVED AS
AMERICAN STANDARD
BY THB AMERICAN STANDARDS ASSOCl\11P.$fi
1960
ASA no . Zif.SI l95J UDC sis.162:620.1
OBS SSl.12. &6.1
Standard Method oj Test for
1
CARBONYL CONTENT OF BUTADIENE
~ \l.,
ASTM Designation: D 1089-59
1
ADOPTED, 1953; REVISED, 1959.
This Standard of the American Society for Testing Materials is issued under
the fixed designation D 1089; the final number indicates the year of original
adoption as standard or, in the case of revision, the year of last revision.
Scope Apparatus
3. (a) Bottles, narrow-mouthed, 500-
1. This method is intended for the de­
ml. fitted with cork stoppers.
termination of the carbonyl content in
(b) Thermometer.-For observing tem­
liquid Cc hydrocarbons containing less
peratures below -45 C, the Low Cloud
than 2500 ppm. Acid or alkaline ma­
and Pour Thermometer, having a range
terials, if present, interfere and are de­
of -80 to 20 C or -112 to 70 F and con­
termined by a blank titration.
forming to the requirements for ther­
mometer 6 C or 6 F as prescribed in the
Outline of Method
3
ASTM Specifications E 1 is satisfactory.
(c) Bomb Rack for supporting the
2. A measured quantity of liquid Cc
hydrocarbon is added to a cork stoppered sample bomb in an upright position.
narrow-mouthed bottle containing aque­ (d) Copper Cooling Coil.-Prepare a
ous hydroxylamine hydrochloride rea­ cooling coil by winding 4 in. of l-in.
seamless copper tubing on a short length
gent and Stoddard solvent. The carbonyl
content is determined from the increase of !-in. pipe, allowing sufficient length of
in the acidity of the resulting solution tubing at the end of the coil to connect
by titrating with a standard base, using it to the sample source. Attach a i-in.
a pH meter to determine the end point. valve on the outlet at a point that would
not extend more than 3 in. above the
surface of the bath liquid. To the valve
1
Under the standardization procedure of the
attach a 3-in. piece of tubing bent for
Society, this method is under the jurisdiction of
the ASTM Committee D-2 on Petroleum Prod­
carrying the liquid into the required
ucts and Lubricants.
apparatus.
The method was derived from the one de­
(e) pH Meter, having an accuracy of
veloped and cooperatively tested by the Buta­
diene Producers' Committee on Specifications
plus or minus 0.05 pH units.
and Methods of Analysis of the Office of Rubber
(j) Burel, 10-ml. with 0.02-ml. divi­
Reserve which appears in the Butadiene Lab­
oratory Manual as method 2.1.5.1. sions.
2 Prior to its adoption as standard, this
(g) Buret, 50-m.I. with 0.1-ml. divi­
method was published as tentative from 1950 to
sions.
1953.
In 1959, a new Note 2 was added and the sec­
'Appears in this publication, see Contents in Numeric
tion on Precision was revised.
Sequence of ASTM Designations at front of book.
561

---------------------- Page: 1 ----------------------
562 TEST FOR CA.lil.BONYL CONTENT O!" BUTADIENE (D 1089)
·orously for 1 min. Transfer the contents ,
Reagents
of the bottle to a 500-ml. beaker and
4. (a) Stoddard Solvent, conforming to
wash the bottle with 75 ml. of distilled
4
A.S.T.M. Specifications D 484.
water catching the rinsings in the
(b) Hydroxylamine Hydrochloride Rea­
' . .
beaker. Place the beaker on the t1tratmg
gent (2 per cent).-Dissolve ~O g. ~f c . .P·
stand of the pH meter and titrate the
hydroxylamine hydrochloride m dIS­
'olution with standard 0.05 N NaOH to
tilled water and dilute to 1 liter.
an end point of pH 3.85. Stir the solution
NOTE 1.-Hydroxylamine hydrochloride solu­
continuously during the titration.
tions are known to cause dermatitis. Rubber
Non: 3.-Use a 100-ml. size &le when less
gloves should be worn whenever handling this
than 100 ppm. carbonyl content i11 present in the
substance and all contact of it with the skin
material being tested and a 50-ml. sample for
should be avoided.
higher concentrations.
(c) Sodium Hydroxide Solution (0.05
(b) Blank Determination for Hydroxyl­
N).
amine Hydrochloride Reagent and Stod­
(d) Sulfuric Acid Solution (0.05 N).
dard Solvent.-Add to a 500-ml. bottle
25 ml. of distilled water, 25 ml. of hy­
Test Sample
droxylamine hydrochloride reagent, and
5. Set the sample bomb in an upright
150 ml. of Stoddard solvent. Stopper the
position in the bomb rack. Place the cop­
bottle and shake it vigorously for 1 min.
per cooling coil in a dry ice-Stoddard
Transfer the contents of the bottle to a
solvent bath and connect the coil to the
500-ml. beaker and wash the bottle with
lower valve of the bomb. Purge the line
75 ml. of distilled water, catching the
with some of the sample before taking
rinsings in the beaker. Place the beaker
the sample to be tested. Cool a 100-ml.
on the titrating stand of the pH meter
graduated cylinder in
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