ASTM D3673-89(1995)e1

Standard Test Methods for Chemical Analysis of Alpha Olefin Sulfonates

SCOPE
1.1 These test methods cover the chemical analysis of alpha olefin sulfonates. The analytical procedures appear in the following order:  Sections Moisture by the Distillation Method 4 to 8 Sodium Sulfate 9 to 14 Neutral Oil 15 to 19 Chlorides Calculated as Sodium Chloride (NaCl) 20 to 24 Alkalinity 25 to 29 pH 30 to 31 Determination of Color 32 to 37 Determination of Active Content by Methylene Blue Titration 38 to 47
1.2 This standard does not purport to address all of the safety concerns, 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. For specific precaution statement see 36.1. Material safety data sheets are available for reagents and materials. Review them for hazards prior to usage.

General Information

• Status: Historical
• Publication Date: 31-Dec-1994
• Technical Committee: D12 - Soaps and Other Detergents
• Drafting Committee: D12.12 - Analysis and Specifications of Soaps, Synthetics, Detergents and their Components

Relations

• Replaced By: ASTM D3673-89(2003) - Standard Test Methods for Chemical Analysis of Alpha Olefin Sulfonates
• Effective Date: 26-May-1989

Standards Content (Sample)

NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
e1
Designation: D 3673 – 89 (Reapproved 1995)
Standard Test Methods for
Chemical Analysis of Alpha Olefin Sulfonates
This standard is issued under the fixed designation D 3673; the number immediately following the designation 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. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
e NOTE—Keywords were added editorially in February 1995.
1. Scope specifications are available. Other grades may be used, pro-
vided it is first ascertained that the reagent is of sufficiently
1.1 These test methods cover the chemical analysis of alpha
high purity to permit its use without lessening the accuracy of
olefin sulfonates. The analytical procedures appear in the
the determination.
following order:
3.2 Unless otherwise indicated, references to water shall be
Sections
understood to mean Type III reagent water conforming to
Moisture by the Distillation Method 4-8
Sodium Sulfate 9-14
Specification D 1193.
Neutral Oil 15-19
Chlorides Calculated as Sodium Chloride (NaCl) 20-24
MOISTURE BY THE DISTILLATION
Alkalinity 25-29
METHOD
pH 30 and 31
Determination of Color 32-37
Determination of Active Content by Methylene Blue Titration 38-47 4. Apparatus
1.2 This standard does not purport to address all of the 4.1 The apparatus required shall consist of a glass flask
heated by suitable means and provided with a reflux condenser
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- discharging into a trap and connected to the flask. The
connections between the trap and the condenser and flask shall
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. For specific be interchangeable ground joints. The trap serves to collect and
measure the condensed water and to return the solvent to the
precaution statement see 36.1. Material safety data sheets are
available for reagents and materials. Review them for hazards flask. A suitable assembly of the apparatus is illustrated in Fig.
1.
prior to usage.
4.1.1 Flask, 1-L capacity, either the short-neck, round-
2. Referenced Documents
bottom type, or the Erlenmeyer type.
2.1 ASTM Standards: 4.1.2 Heat Source—Either an oil bath (for example, stearic
D 1172 Test Method for pH of Aqueous Solutions of Soaps acid or paraffin wax) or an electric heater provided with a
and Detergents
sliding rheostat or other means of heat control.
D 1193 Specification for Reagent Water 4.1.3 Condenser—A water-cooled glass reflux condenser
D 1209 Test Method for Color of Clear Liquids (Platinum-
(Fig. 1), having a jacket approximately 15 ⁄4 in. (400 mm) in
3 1
Cobalt Scale) length, with an inner tube ⁄8 to ⁄2 in. (9.5 to 12.7 mm) in
D 3049 Test Method for Synthetic Anionic Ingredient by outside diameter, and not less than ⁄4 in. (6.35 mm) in inside
Cationic Titration diameter. The end of the condenser to be inserted in the trap
may be ground off at an angle of 30° from the vertical axis of
3. Purity of Reagents
the condenser. When inserted into the trap, the tip of the
3.1 Reagent-grade chemicals shall be used in all tests. condenser shall be about ⁄4 in. (7 mm) above the surface of the
Unless otherwise indicated, it is intended that all reagents shall
liquid in the trap after the distillation conditions have been
conform to the specifications of the Committee on Analytical established. Fig. 1 shows a conventional sealed-in type of
Reagents of the American Chemical Society, where such
condenser, but any other condenser fulfilling the detailed
requirements of this paragraph may be used.
4.1.4 Trap—For greatest accuracy several trap sizes are
These test methods are under the jurisdiction of ASTM Committee D-12 on
Soaps and Other Detergents, and are the direct responsibility of Subcommittee
D12.12on Analysis of Soaps and Synthetic Detergents.
Reagent Chemicals, American Chemical Society Specifications, American
Current edition approved May 26, 1989. Published July 1989. Originally Chemical Society, Washington, DC. For suggestions on the testing of reagents not
published as D 3673 – 78. Last previous edition D 3673 – 87. listed by the American Chemical Society, see Analar Standards for Laboratory
Annual Book of ASTM Standards, Vol 15.04. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Annual Book of ASTM Standards, Vol 11.01. and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
Annual Book of ASTM Standards, Vol 06.04. MD.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
D 3673
0.1-mL divisions and from 1 to 25 mL in 0.2-mL divisions.
NOTE 1—The condenser and trap should be thoroughly cleaned before
use.
5. Solvent
5.1 Xylene—Saturate xylene with water by shaking with a
small quantity of water and distill. Use the distillate for the
determination.
6. Procedure
6.1 Transfer to the 1000-mL flask (equipped with the size of
the trap specified in 4.1.4) an amount of sample according to
the percentage of moisture expected, as follows:
Weight of Sample
A
Moisture Expected, % to Be Used, g
0 to 5, incl 50 6 5
Over 5 to 17, incl 50 6 5
Over 17 to 30, incl 40 6 4
Over 30 to 50, incl 30 6 3
Over 50 to 70, incl 30 6 3
Over 70 to 85, incl 25 6 2
A
Weighed to the nearest 0.25 g.
Immediately add about 250 mL of xylene. Place a small, thin
sheet of long-fiber, chemical-resistant glass wool on the
surface of the xylene. The glass wool should be thoroughly
dried in the oven and held in the desiccator before use.
6.2 Connect the flask and receiver to the condenser and pour
sufficient xylene down the condenser tube to cause a slight
overflow through the side tube. Wrap the flask and tube leading
to the receiver with glass wool, so that refluxing will be under
better control.
6.3 Heat the oil bath with a gas burner or other source of
heat, or apply heat directly to the flask with an electric heater
and distill slowly. The rate at the start should be approximately
100 drops per minute. When the greater part of the water has
distilled over, increase the distillation rate to 200 drops per
minute until no more water is collected. Rinse during the
distillation with 5-mL portions of xylene to wash down any
moisture adhering to the walls of the condenser. The water in
FIG. 1 Assembly of Distillation Apparatus
the receiver may be made to separate from the xylene by using
a spiral copper or Nichrome wire. Move the wire up and down
allowable, depending upon the percentage of moisture ex-
in the condenser occasionally, thus causing the water to settle
pected:
at the bottom of the receiver. Reflux for at least 2 h, and shut
Moisture Expected, % Size of Trap, mL
off the heat at the end of this period.
0 to 5, incl 5
NOTE 2—In especially difficult cases of boil-over, add 10 to 15 mL of
Over 5 to 17, incl 10
oleic acid before beginning the distillation. Wash down the condenser with
Over 17 to 30, incl 25
10 mL of xylene. Adjust the temperature of the distillate to 20°C and read
Over 30 to 50, incl 25
the volume of water.
Over 50 to 70, incl 25
Over 70 to 85, incl 25
7. Calculation
Traps made of well-annealed glass, constructed essentially
7.1 Calculate the percentage of moisture as follows:
as shown in Fig. 1, and graduated to contain one of the
Moisture, % 5 @~V 3 0.998!/W# 3 100 (1)
following specified volumes at 20°C shall be used:
4.1.4.1 Trap, 5-mL capacity, subdivided into 0.1-mL divi-
where:
sions with each 1-mL line numbered (5 mL at top). The error
in any indicated capacity may not be greater than 0.05 mL.
4.1.4.2 Trap, 10-mL capacity, subdivided from 0 to 1 mL in
0.1-mL divisions and from 1 to 10 mL in 0.2-mL divisions.
Borosilicate glass has been found satisfactory for this purpose.
4.1.4.3 Trap, 25-mL capacity, subdivided from 0 to 1 mL in “Nichrome” is a trademark of the Driver-Harris Co.
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
D 3673
where W 5 grams of Na SO .
V 5 volume of water, mL at 20°C, and
2 4
10.8 Sulfonazo III Indicator Solution —Dissolve 0.1 g of
W 5 weight of sample, g.
Sulfonazo III in 100 mL of water. Pass the solution through a
8. Precision and Bias
cation exchange column if it looks blue rather than lavender
when edge-lighted by a tungsten lamp.
8.1 Repeatability (Single Analyst)—The standard deviation
10.9 Filter Paper, smooth, hardened, ashless.
of results (each the average of duplicates) obtained by the same
analyst on different days, has been estimated to be 0.16 %
11. Standardization
absolute at 9 degrees of freedom. Two such averages should be
11.1 Pipet 5.0-mL aliquots of standard Na SO solution into
2 4
considered suspect (95 % confidence level) if they differ by
each of two 50-mL beakers. Place stirring bars in each beaker.
more than 0.5 % absolute.
Add 20 mL of acetone, 2 drops of 1 N HCl, and 4 to 5 drops
8.2 Reproducibility (Multilaboratory)—The standard devia-
of Sulfonazo III indicator solution to each beaker.
tion of results (each the average of duplicates) obtained by
11.2 Titrate each Na SO solution with Ba(ClO ) solution
2 4 4 2
analysts in different laboratories, has been estimated to be
using a 10-mL buret. Stir the solution magnetically. Illuminate
0.47 % absolute at 8 degrees of freedom. Two such averages
the solution horizontally with a small tungsten lamp at the side
should be considered suspect (95 % confidence level) if they
of the beaker. Titrate slowly to a color change from lavender-
differ by more than 1.5 % absolute.
pink to blue (about 0.3 mL of Ba(ClO ) solution is required to
4 2
8.3 Checking Limits for Duplicates—Report the moisture
produce a good initial lavender color).
content of the sample to the nearest 0.01 %. Duplicate runs that
11.3 From each titration, calculate the normality of the
agree within 1.3 % are acceptable for averaging (95 % confi-
Ba(ClO ) solution as follows. Average the values obtained.
4 2
dence level).
5 3 N
Normality, N 5 (3)
V
SODIUM SULFATE
where:
9. Apparatus
N 5 normality of the Na SO solution, and
1 2 4
9.1 Beakers, 50 and 100-mL capacity.
V 5 millilitres of Ba(ClO ) solution required for 5-mL
4 2
9.2 Buret, 10-mL capacity, with 0.05-mL divisions.
aliquot of Na SO solution.
2 4
9.3 Volumetric Flasks, 50, 250, and 1000-mL capacity.
9.4 Magnetic Stirrer, with TFE-fluorocarbon-coated stirring 12. Procedure
bars.
12.1 Weigh a 2-g sample into a 100-mL beaker or a 50-mL
9.5 Transfer Pipet, 5-mL capacity.
flask. Record the weight to 61 mg.
9.6 Viewing Lamp—Small tungsten lamp or flashlight.
12.2 Place a stirring bar in the container. Add 25 mL of
water and stir until the sample is dissolved.
10. Reagents and Materials
12.3 Add a few drops of phenolphthalein indicator solution.
10.1 Acetone.
Add 0.1 N HCl until the solution is just acid. Do not
10.2 Barium Perchlorate Solution (0.02N)—Dissolve 3.4 g
over-acidify.
of anhydrous Ba(ClO ) in water and dilute the solution to 1 L.
4 2 12.4 Place the container in a cold-water bath (below 20°C)
10.3 2-Benzyl-2-thiopseudourea Hydrochloride Solution
on the magnetic stirrer. Add 10 mL of 2-benzyl-2-
—(7 %) —Dissolve7gin100 mL of water. Prepare the
thiopseudourea hydrochloride at a fast drip through a buret
solution fresh daily.
with vigorous stirring. Do not whip the liquid into a foam.
10.4 Hydrochloric Acid (1 N)—Dilute 83 mL of hydrochlo-
12.5 Stir the solution for 15 min more in the cold bath.
ric acid (HCl, sp gr 1.19) to 1 L with water.
Remove the solution from the bath and let it settle for a few
10.5 Hydrochloric Acid (0.1 N)—Dilute 8.3 mL of HCl (sp
minutes at room temperature.
gr 1.19) to 1 L with water.
12.6 Filter the solution through filter paper into a 50-mL
10.6 Phenolphthalein Indicator Solution (10 g/L)—
volumetric flask. Wash the filter cake with water. Use the
Dissolve1gof phenolphthalein in 100 mL of 95 % ethanol.
washes to dilute the solution to volume.
10.7 Sodium Sulfate Solution (0.02 N)—Dry the anhydrous,
12.7 Pipet a 5-mL aliquot into a 50-mL beaker. Add 20 mL
reagent-grade salt (Na SO )for4hat 105°C. Weigh about
of acetone, 2 drops of 1 N HCl, and 4 to 5 drops of Sulfonazo
2 4
0.355 g of the dried salt into a 100-mL beaker. Record the
III indicator solution.
weight within 60.1 mg. Dissolve the salt water. Quantitatively
12.8 Titrate the solution slowly with 0.02 N Ba(ClO )
4 2
transfer the solution to a 250-mL volumetric flask and dilute it
solution. Use magnetic stirring. Illuminate the solution hori-
to volume with water. Calculate the normality of the solution as
zontally with a small tungsten lamp at the side of the beaker.
follows:
Titrate to a color change from lavender-pink to a blue color that
persists for 1 min.
Normality, N 5 0.05632 3 W (2)
NOTE 3—The titration should be between 1 and 5 mL. If the titration is
greater than 5 mL, use a smaller aliquot of the sample and add water to
Supporting data are available from ASTM Headquarters, 100 Barr Harbor
Drive, West Conshohoken, PA 19428. Request RR:D12-1002 and RR: D12-1007.
9 10
Eastman Organic Chemical No. 2124 has been found satisfactory for this Sulfonazo III [3,6-bis-(o-sulfophenylazo)-4,5-dihydroxy-2,7-naphthalenedi-
purpose. sulfonic acid] is available from the Aldrich Chemical Co.
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
D 3673
bring the aqueous volume to 5 mL total. If the titration is less than 1 mL,
0.01 g. Add an equivalent volume of 1 + 1 ethanol-water. If, on
pipet a 10-mL aliquot into a 100-mL beaker and add 40 mL of acetone, 4
the addition of 2 drops of phenolphthalein indicator solution,
drops of 1 N HCl, and 8 to 10 drops of Sulfonazo III indicator solution.
the sample solution remains colorless, neutralize the sample
with 0.1 N NaOH solution to the appearance of the pink color.
13. Calculation
17.2 Quantitatively transfer the neutralized solution to a
13.1 Calculate the concentration of Na SO as follows:
2 4
250-mL separatory funnel, rinsing the flask, first with 10 mL of
355 N 3 V
2 water, followed by 10 mL of ethanol and then by 100 mL of
Na SO ,wt% 5 (4)
2 4
A 3 W
1 + 1 ethanol-water. Add each rinsing to the separatory funnel.
Finally, rinse the flas
...