ASTM D2894-73

Method for Analysis of Calcium and Barium Petroleum Sulfonates by Liquid Chromatography (Withdrawn 1978)

General Information

• Status: Withdrawn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

Standards Content (Sample)

~~r~ oesign••ion: o 2s94 - 13
Standard Method for
ANALYSIS OF CALCIUM AND BARIUM PETROLEUM
1
SULFONAJES BY LIQUID CHROMATOGRAPHY
This Standard is issued under the rixed dcsign:.ition D 2894; the number immediately following the designation indicates the
year of original adoption or, in the cast: of n:vision. the ye n:approval.
I. Scope
3.3 Vacuum Desiccator, shielded.
3.4 Vacuum O.ven, capable of being main­
I. I This method covers the determination or
tained at 212 F (100 C) and connected to 22 to
mineral oil, calciu1n or barium sulfonate, aver­
25 in. (259 to 635 mm) Hg vacuum.
age molecular weight, water, and specific grav­
3.5 Muffle Furnace, capable of operating at
ity of crude and refined natural and synthetic
1500 to 1800 F (800 to 1000 C).
calcium and barium sulfonates.
3.6 Water Bath, capable of being maintained
NOTE I-A method for analysis of the same type
at 77 ± 0.3 F (25 ± 0.2 C).
of materials is described in ASTM Method D 1216,
Analysis of Calcium and Barium Petroleum
3.7 Distillation Apparatus, as described in
Sulfonates. ~
Method D 95.
NOTE 2-The values slated in U.S. customary
3.8 Dish, platinum, 100-ml capacity.
units are to be regarded as the standard.
3.9 Pycnometer, as shown in Fig. 2 of
2. Summary of Methods
Method D 1216. To calibrate, weigh to the
2.1 The sample is dissolved in ethyl ether nearest 1 mg, with cap in place, then fill with
and converted to sulfonic acid, using dilute distilled water at 60 to 68 F (15 to 20 C) and
hydrochloric acid. The sulfonic acid and min­
place in a water bath at 77 ± 0.3 F (25 ±
0.2 C). After 30 min, adjust the water meniscus
eral oil, after extraction, are converted to
sodium sulfonate and the isolated sodium sulfo­ at the top of the neck so that it is exactly level.
nate and mineral oil dissolved in chloroform. To obtain a nat meniscus, add a minute amount
of wetting agent to the water surface. Remove
An aliquot of the chloroform solution is ad­
sorbed on silica gel. The oil is eluted with the pycnometer from the bath and dry the
chloroform and the sulfonate with ethyl alco­ outside. Replace the cap and weigh to the
hol, and both are determined gravimetrically. nearest I mg. Record the weight of water
Average molecular weight is calculated from contained as W c·
the average equivalent weight of the isolated
sodium sulfonate, which is determined by ash­
4. Reagents and Materials
ing a portion of the isolated sodium sulfonate.
4.1 Purity of Reagents-Reagent grade
Water is determined by ASTM Method D 95,
chemicals shall be used in all tests. Unless
Test for Water in Petroleum Products and
otherwise indicated, .it is intended that all
2
Bituminous Materials By Distillation. Specific
reagents shall conform to the specifications of
gravity is determined by pycnometer.
the Committee on Analytical Reagents of the
American Chemical Society, where such speci­
3. Apparatus
3
fications are available. Other grades may be
3.1 Chromatographic Column, made of
glass and consisting of a reservoir and a
1
This method is under the jurisdiction of ASTM Commit­
separator section, and fitted with TFE-fluoro­
tee D-2 on Petroleum Products and Lubric.ints.
Current edition approved Aug. 27, 1973. Published No­
carbon stopcock with a 2-mm bore, as shown in
vember 1973. Origin.illy published .is D 2894 - 70 T. Last
Fig. I of ASTM Method D 2548, Analysis of
previous edition D 2894 - 70T.
'Annual Book of ASTM Standards, Part 18.
Oil-Soluble Sodium Petroleum Sulfonates by
'"Reagent Chemicals, American Chemical Society
2
Liquid Chromatography. A column with a
Specifications," Am. Chemical Soc., Washington, D.C. For
suggestions on the testing or reagents nOt lisied by the
detachable reservoir connected by a standard­
American Chemical Society, see "Reagent Chemicals and
taper joint may be used.
St:ind.irds," by Joseph Rosin, D. Van Nostrand Co., Inc.,
3.2 Steam Bath. New York, N. Y., and the "United States Pharmacopeia."
829

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D 2894
used, provided it is first ascertained that the
10 ml of solution ren1ain.
reagent is of sufficiently high purity to permit 5.2 Conversion of Sulfonic Acid to Sodi1u11
its use without lessening the accuracy of the Sulfonate-Add 75 ml of ethyl alcohol (95
percent) . to the ethyl ether concentrate and
determination.
neutralize with 1 N NaOH solution to a
4.2 Acetone.
4.3 Chloroform. phenolphthalein end point. Evaporate the
4.4 Ethyl Alcohol (95 percent)-Either pure ethanolic solution of sodium sulfonate on the
grain or denatured ethyl alcohol conforming to steam bath, adding sn1a\1 portions of acetone or
Formula 3A of the U.S. Bureau of internal isopropyl alcohol (99 percent) to aid in remov­
Revenue.
ing water. Using a volumetric flask dissolve the
4.5 Ethyl Ether. sodium sulfonate and oil residue in enough
4.6 Hydrochloric Acid (/+/)
...