ASTM D1568-97
(Test Method)Standard Test Methods for Sampling and Chemical Analysis of Alkylbenzene Sulfonates
Standard Test Methods for Sampling and Chemical Analysis of Alkylbenzene Sulfonates
SCOPE
1.1 These test methods cover the sampling and chemical analysis of paste, powder, or liquid detergent alkylbenzene sulfonates.
1.2 The procedures for sampling and analysis appear in the following order: Sections Sampling: Powders and Flakes Packed in Cans or Cartons 3 Powders and Flakes in Bulk 4 Liquids 6 Pastes 7 Preparation of Sample 8 Moisture: Distillation Method 10 to 13 Karl Fischer Method 14 to 19 Total Matter Insoluble in Alcohol 20 to 22 Neutral Oil 23 to 26 Chlorides Calculated as Sodium Chloride (NaCl) 27 to 30 pH 31
1.3 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.
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Designation:D1568–97
Standard Test Methods for
Sampling and Chemical Analysis of Alkylbenzene
Sulfonates
This standard is issued under the fixed designation D 1568; 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.
1. Scope 4. Powders and Flakes Packed in Cans or Cartons
1.1 These test methods cover the sampling and chemical 4.1 One can or carton shall be taken at random from not less
analysis of paste, powder, or liquid detergent alkylbenzene than 1 % of the seller’s shipping containers, provided each
sulfonates. package contains not less than 50 lb (22.7 kg). In the case of
1.2 The procedures for sampling and analysis appear in the smaller containers, a can or carton shall be taken at random
following order: from each lot of containers totaling not more than 5000 lb
(2268 kg) or fraction thereof. The gross sample shall in all
Sections
cases consist of not less than three cans or cartons taken at
Sampling:
random from separate containers. In the case of very large lots
Powders and Flakes Packed in Cans or Cartons 3
Powders and Flakes in Bulk 4 where the sample drawn as above will amount to more than 20
Liquids 6
lb (9.1 kg), the percentage of packages sampled shall be
Pastes 7
reduced so that the amount drawn will not exceed 20 lb (9.1
Preparation of Sample 8
kg). The individual cans or cartons shall be tightly wrapped at
Moisture:
Distillation Method 10-13
once in paraffined paper and sealed by rubbing the edges with
Karl Fischer Method 14-19
a heated iron. The inspector shall accurately weigh each
Total Matter Insoluble in Alcohol 20-22
Neutral Oil 23-26 wrapped can or carton and record its weight and the date of
Chlorides Calculated as Sodium Chloride (NaCl) 27-30
weighing on the wrapper.The wrapped cans or cartons shall be
pH 31
placed in an airtight container which should be nearly filled,
1.3 This standard does not purport to address all of the
and which shall then be sealed, marked, and sent to the
safety concerns, if any, associated with its use. It is the
laboratory for test. Samples shall be kept cool until tested.
responsibility of the user of this standard to establish appro-
5. Powders and Flakes in Bulk
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. 5.1 A grab sample of not less than 0.5 lb (227 g) shall be
taken at random from not less than 1 % of the seller’s shipping
2. Referenced Documents
containers,providedeachpackagecontainsnotlessthan100lb
2.1 ASTM Standards:
(45.4 kg). In the case of smaller containers, a grab sample of
D 1172 Test Method for pH ofAqueous Solutions of Soaps
not less than 0.5 lb (227 g) shall be taken at random from each
and Detergents
lot of containers totaling not more than 10,000 lb (4536 kg) or
D 1193 Specification for Reagent Water
fraction thereof. The gross sample shall in all cases consist of
not less than three grab samples of 0.5 lb (227 g) each taken at
SAMPLING
random from separate containers. In the case of very large lots
the sample drawn as above will amount to more than 20 lb (9.1
3. General Requirements
kg), the percentage of packages sampled shall be reduced so
3.1 The seller shall have the option of being represented at
that the amount drawn shall not exceed 20 lb (9.1 kg). The
the time of sampling and when he so requests shall be
inspector shall rapidly mix the gross sample and place it in an
furnished with a duplicate sample.
airtight container which shall be filled, sealed, marked, accu-
rately weighed, with its weight and the date of weighing
1 recorded on the package, and be sent to the laboratory for test.
These test methods are under the jurisdiction of ASTM Committee D-12 on
Soaps and Other Detergents and is the direct responsibility of D12.12 on Analysis Samples shall be kept cool until tested.
of Soaps and Synthetic Detergents.
Current edition approved March 10, 1997. Published July 1997. Originally
e1
published as D 1568 – 58. Last previous edition D 1568 – 63 (1991) .
Annual Book of ASTM Standards, Vol 15.04.
Annual Book of ASTM Standards, Vol 11.01.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D1568–97
6. Liquids Weigh at once all portions for analysis, preserving the remain-
der in an airtight container in a cool place.
6.1 A sample of not less than 0.5 pt (236.6 mL) shall be
8.2 Liquids—No preparation of the sample of liquid, other
taken at random from not less than 1 % of the seller’s shipping
than a thorough mixing, is necessary unless it is received
containers, provided each package contains not less than 10 gal
during very cold weather, when it should be allowed to stand
(37.9 L). In the case of smaller containers, a sample of not less
at least 1 h after it has warmed to room temperature (20 to
than 0.5 pt (236.6 mL) shall be taken at random from each lot
30°C) before it is tested, particularly for its lathering qualities.
of containers totaling not more than 1000 gal (3785.4 L) or
fraction thereof. The gross sample shall in all cases consist of
NOTE 2—If pastes or liquids are known to be acidic, and decomposition
not less than three samples of 0.5 pt (236.6 mL) each taken at of sample can result from heating, the samples shall be adequately labeled
for precautionary treatment and warmed to room temperature or other
random from separate containers. Before drawing the sample
maximum temperature as agreed upon for mixing and sampling.
from the container selected, the contents of the container shall
be thoroughly agitated. The inspector shall thoroughly mix the
8.3 Pastes—Store preferably in glass. If crystals separate,
gross sample, place it in clean, dry cans or bottles, which shall melt on water bath (Note 1).
be completely filled and securely stoppered with clean corks or
METHODS OF CHEMICAL ANALYSIS
caps, then sealed, marked, and sent to the laboratory for test.
9. Purity of Reagents
7. Pastes
9.1 Reagent grade chemicals shall be used in all tests.
7.1 Pastes Packed in Cans or Cartons of 5 lb (2.27 kg) or
Unless otherwise indicated, it is intended that all reagents shall
Less—Onecanorcartonshallbetakenatrandomfromnotless
conform to the specifications of the Committee on Analytical
than 1 % of the seller’s shipping containers, provided each
Reagents of the American Chemical Society, where such
package contains not less than 50 lb (22.7 kg). In the case of
specifications are available. Other grades may be used, pro-
smaller containers, a can or carton shall be taken at random
vided it is first ascertained that the reagent is of sufficiently
from each lot of containers totaling not more than 5000 lb
high purity to permit its use without lessening the accuracy of
(2268 kg) or fraction thereof. The gross sample shall in all
the determination.
cases consist of not less than three cans or cartons taken at
9.2 Unless otherwise indicated, references to water shall be
random from separate containers. In the case of very large lots
understood to mean reagent water conforming to Specification
where the sample drawn as above will amount to more than 20
D 1193.
lb (9.1 kg), the percentage of packages sampled shall be
reduced so that the amount drawn shall not exceed 20 lb (9.1
MOISTURE BY THE DISTILLATION METHOD
kg).The samples shall be wrapped, sealed, marked, and sent to
(Preferred Method)
the laboratory for test.
10. Apparatus
7.2 PastesPackedinBulk—A“trier”sample(Note1)ofnot
less than 0.5 lb (227 g) shall be taken at random from not less
10.1 The apparatus required shall consist of a glass flask
than 1 % of the seller’s shipping containers, provided each
heated by suitable means and provided with a reflux condenser
package contains not less than 50 lb (22.7 kg). In the case of
discharging into a trap and connected to the flask. The
smaller containers, a “trier” sample of not less than 0.5 lb (227
connections between the trap and the condenser and flask shall
g) shall be taken at random from each lot of containers totaling
be interchangeable ground joints.The trap serves to collect and
not more than 5000 lb (2268 kg) or fraction thereof. The gross
measure the condensed water and to return the solvent to the
sample shall in all cases consist of not less than three 0.5-lb
flask.Asuitable assembly of the apparatus is illustrated in Fig.
(227-g) samples, each taken at random from separate contain-
1.
ers. With very large lots where the sample drawn as above will
10.1.1 Flask—A 1000-mL flask of either the short-neck,
amount to more than 10 lb (4.5 kg), the percentage of packages
round-bottom type or the Erlenmeyer type.
sampled shall be reduced so that the amount drawn shall not
10.1.2 Heat Source—Either an oil bath (stearic acid, paraf-
exceed 10 lb (4.5 kg). The inspector shall promptly place the
fin wax, etc.), or an electric heater provided with a sliding
gross sample in a clean, dry, airtight and watertight container,
rheostat or other means of heat control.
which shall be filled, sealed, marked, and sent to the laboratory
10.1.3 Condenser—A water-cooled glass reflux condenser
for test. 3
(Fig. 1), having a jacket approximately 15 ⁄4 in. (400 mm) in
3 1
length, with an inner tube ⁄8 to ⁄2 in. (9.5 to 12.7 mm) in
NOTE 1—A trier sample is obtained by inserting a “trier” into the
outside diameter, and not less than ⁄4 in. (6.35 mm) in inside
1 3
material. A trier is a halfround steel cylinder ⁄2 to ⁄4 in. (12.7 to 19 mm)
diameter, shall be used.The end of the condenser to be inserted
in diameter, 6 to 36 in. (152 to 914 mm) in length, pointed on one end and
having a grip handle on the other end. After insertion, the trier is turned in the trap may be ground off at an angle of 30° from the
two or three times, and upon removal a core of the material being sampled
is obtained.
Reagent Chemicals, American Chemical Society Specifications, American
8. Preparation of Sample
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory
8.1 Powders and Flakes—Minimizing exposure to air, rap-
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
idly disintegrate and mix the sample of powdered, flake, or
and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
chip product. If desired, quarter down to about 1 lb (453.6 g). MD.
D1568–97
A
Moisture Expected, % Weight of Sample to be Used, g
0 to 5, incl 50 6 5
Over 5 to 17, incl 50 6 5
Over 17 to 30, incl 406 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.
Add immediately about 100 mL of xylene or toluene. Place
a small, thin sheet of long-fiber, chemical-resistant glass wool
on the surface of the toluene. The glass wool should be
thoroughly dried in the oven and held in the desiccator before
use.
12.2 Connect the flask and receiver to the condenser and
pour sufficient xylene or toluene down the condenser tube to
cause a slight overflow through the side tube. Wrap the flask
andtubeleadingtothereceiverwithaninsulatingcloth,sothat
refluxing will be under better control.
12.3 Heat the oil bath with a gas burner or other source of
heat, or apply heat directly to the flask with an electric heater
FIG. 1 Assembly of Distillation Apparatus
and distill slowly. The rate at the start should be approximately
100 drops/min. When the greater part of the water has distilled
vertical axis of the condenser. When inserted into the trap, the
over, increase the distillation rate to 200 drops/min until no
tip of the condenser shall be about ⁄4 in. (7 mm) above the
more water is collected. Purge the reflux condenser during the
surface of the liquid in the trap after the distillation conditions
distillation with 5-mL portions of xylene (or toluene) to wash
have been established. Fig. 1 shows a conventional sealed-in
down any moisture adhering to the walls of the condenser. The
type of condenser, but any other condenser fulfilling the
water in the receiver may be made to separate from the xylene
detailed requirements of this paragraph may be used.
(or toluene) by using a spiral copper or nichrome wire. Move
10.1.4 Trap—For greatest accuracy several trap sizes are
the wire up and down in the condenser occasionally, thus
allowable, depending upon the percentage of moisture ex-
causing the water to settle at the bottom of the receiver. Reflux
pected:
for at least 2 h, and shut off the heat at the end of this period.
Moisture Expected, percent Size of Trap, mL
12.4 Wash down condenser with 1 mL of absolute ethanol
0to5,incl 5
(CH CH OH). Adjust the temperature of the distillate to 20°C
3 2
Over 5 to 17, incl 10
and read the volume of water.
Over 17 to 30, incl 10
Over 30 to 50, incl 25
Over 50 to 70, incl 25
13. Calculations
Over 70 to 85, incl 25
13.1 Calculate the percentage of moisture as follows:
Traps made of well-annealed glass, constructed essentially
Moisture, % 5 @~V3 0.998!/W# 3 100 (1)
as shown in Fig. 1, and graduated to contain one of the
following specified volumes at 20°C shall be used:
10.1.4.1 5-mL Trap—Subdivided into 0.1-mL divisions
where:
with each 1 mL line numbered (5 mL at top). The error in any V = volume of water, mL at 20°C, and
W = weight of the sample, g.
indicated capacity may not be greater than 0.05 mL.
10.1.4.2 10-mL Trap—Subdivided from 0 to 1 mL in
WATER BYTHE KARLFISCHER TITRATION
0.1-mL divisions and from 1 to 10 mL in 0.2-mL divisions.
METHOD
10.1.4.3 25-mL Trap—Subdivided from 0 to 1 mL in
(Alternative Method)
0.1-mL divisions and from 1 to 25 mL in 0.2-mL divisions.
NOTE 3—The condenser and trap should be thoroughly cleaned before
14. Application
use.
14.1 This method is intended to be used where the amount
of moisture is low.
11. Solvent
11.1 Xylene (orToluene)—Saturate xylene (or toluene) with
15. Apparatus
water by shaking with a small quantity of water and distill. Use
15.1 Automatic Buret (Machlett Type), 50-mL capacity,
the distillate for the determination.
1000-mLreservoir of amber glass with a straight tip.The buret
12. Procedure
should also be equipped with a drying tube containing a
12.1 Transfer to the 1000-mL flask, equipped with the size
of the trap specified in 10.1.4, an amount of sample according
to the percentage of moisture expected, as follows: Borosilicate glass has been found satisfactory for this purpose.
D1568–97
suitable drying agent such as an
...
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