ASTM D1570-95
(Test Method)Standard Test Methods for Sampling and Chemical Analysis of Fatty Alkyl Sulfates
Standard Test Methods for Sampling and Chemical Analysis of Fatty Alkyl Sulfates
SCOPE
1.1 These test methods cover the sampling and chemical analysis of paste, powder, or liquid detergent fatty alkyl sulfates.
1.2 The procedures for sampling and analysis appear in the following order: Sections Sampling: Powders and Flakes Packed in Cans or Cartons 4 Powders and Flakes in Bulk 5 Liquids 6 Pastes 7 Preparation of Sample 8 Moisture by the Distillation Test Method 11 to 14 pH 15 Alkalinity 16 to 19 Alcohol-Soluble Matter 20 to 22 Alcohol-Insoluble Matter 23 to 24 Unsulfated Material 25 to 28 Combined Alcohols 29 to 32 Ester SO3: Method A. Titration Test Method 36 to 37 Ester SO3: Method B. Gravimetric Test Method 38 to 39 Sodium Sulfate 40 to 43 Chlorides Calculated as Sodium Chloride (NaCl) 44 to 47
1.3 The values stated in either inch-pound or SI units are to be regarded separately as the standard. The values given in parentheses are for information only.
1.4 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. Material Safety Data Sheets are available for reagents and materials. Review them for hazards prior to usage.
General Information
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn. Contact ASTM
International (www.astm.org) for the latest information.
Designation:D1570–95
Standard Test Methods for
Sampling and Chemical Analysis of Fatty Alkyl Sulfates
This standard is issued under the fixed designation D 1570; 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
Sections
Ester SO :
1.1 These test methods cover the sampling and chemical
Method B. Gravimetric Test Method 38 and
analysis of paste, powder, or liquid detergent fatty alkyl
Sodium Sulfate 40-43
sulfates.
Chlorides Calculated as Sodium Chloride (NaCl) 44-47
1.2 The procedures for sampling and analysis appear in the
1.3 The values stated in either inch-pound or SI units are to
following order:
be regarded separately as the standard. The values given in
Sections
Sampling:
parentheses are for information only.
Powders and Flakes Packed in Cans or Cartons 4
1.4 This standard does not purport to address all of the
Powders and Flakes in Bulk 5
safety concerns, if any, associated with its use. It is the
Liquids 6
Pastes 7
responsibility of the user of this standard to establish appro-
Preparation of Sample 8
priate safety and health practices and determine the applica-
Moisture by the Distillation Test Method 11-14
bility of regulatory limitations prior to use. Material Safety
pH 15
Alkalinity 16-19
Data Sheets are available for reagents and materials. Review
Alcohol-Soluble Matter 20-22
them for hazards prior to usage.
Alcohol-Insoluble Matter 23 and
2. Referenced Documents
Unsulfated Material 25-28
Combined Alcohols 29-32
2.1 ASTM Standards:
Ester SO :
D 216 Method for Distillation of Natural Gasoline
Method A. Titration Test Method 36 and
D 1172 Test Method for pH ofAqueous Solutions of Soaps
and Detergents
D 1193 Specification for Reagent Water
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. Discontinued 1988, see 1987 Annual Book of ASTM Standards, Vol 05.01.
Current edition approved April 15, 1995. Published June 1995. Originally Annual Book of ASTM Standards, Vol 15.04.
published as D 1570 – 58 T. Last previous edition D 1570 – 89. Annual Book of ASTM Standards, Vol 11.01.
SAMPLING
3. General Requirement thereof. The gross sample shall in all cases consist of not less
than three cans or cartons taken at random from separate
3.1 The seller shall have the option of being represented at
containers. In the case of very large lots where the sample
the time of sampling and when he so requests, shall be
drawnasabovewillamounttomorethan20lb(9.1kg),reduce
furnished with a duplicate sample.
the percentage of packages sampled so that the amount drawn
4. Powders and Flakes Packed in Cans or Cartons
will not exceed 20 lb (9.1 kg).Tightly wrap the individual cans
or cartons at once in paraffined paper and seal by rubbing the
4.1 Take one can or carton at random from not less than 1%
edges with a heated iron. The inspector shall accurately weigh
of the seller’s shipping containers, provided each package
each wrapped can or carton and record its weight and the date
contains not less than 50 lb (22.7 kg). In the case of smaller
of weighing on the wrapper. Place the wrapped cans or cartons
containers, take a can or carton at random from each lot of
in an airtight container, which should be nearly filled, and
containers totaling not more than 5000 lb (2268 kg) or fraction
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn. Contact ASTM
International (www.astm.org) for the latest information.
D1570
which shall then be sealed, marked, and sent to the laboratory than three cans or cartons taken at random from separate
for test. Samples shall be kept cool until tested. containers. In the case of very large lots where the sample
drawnasabovewillamounttomorethan20lb(9.1kg),reduce
5. Powders and Flakes in Bulk
the percentage of packages sampled so that the amount drawn
5.1 Take a grab sample of not less than 0.5 lb (227 g) at shall not exceed 20 lb (9.1 kg). The samples shall be wrapped,
random from not less than 1 % of the seller’s shipping
sealed, marked, and sent to the laboratory for test.
containers,providedeachpackagecontainsnotlessthan100lb 7.2 Pastes Packed in Bulk—Take a “trier” sample (Note 1)
(45.4 kg). In the case of smaller containers, take a grab sample
of not less than 0.5 lb (227 g) at random from not less than 1 %
of not less than 0.5 lb (227 g) at random from each lot of of the seller’s shipping containers, provided each package
containers totaling not more than 10 000 lb (4536 kg) or
contains not less than 50 lb (22.7 kg). In the case of smaller
fraction thereof. The gross sample shall in all cases consist of containers, take a “trier” sample of not less than 0.5 lb (227 g)
not less than three grab samples of 0.5 lb (227 g) each taken at
at random from each lot of containers totaling not more than
random from separate containers. In the case of very large lots 5000 lb (2268 kg) or fraction thereof.The gross sample shall in
where the sample drawn as above will amount to more than 20
all cases consist of not less than three 0.5-lb (227-g) samples,
lb (9.1 kg), reduce the percentage of packages sampled so that
each taken at random from separate containers.With very large
the amount drawn shall not exceed 20 lb (9.1 kg). The lotswherethesampledrawnasabovewillamounttomorethan
inspector shall rapidly mix the gross sample and place it in an
10 lb (4.5 kg), reduce the percentage of packages sampled so
airtight container, which shall be filled, sealed, marked, accu- that the amount drawn shall not exceed 10 lb (4.5 kg). The
rately weighed, with its weight and the date of weighing
inspector shall promptly place the gross sample in a clean, dry,
recorded on the package, and be sent to the laboratory for test. airtight and watertight container, which shall be filled, sealed,
Samples shall be kept cool until tested.
marked, and sent to the laboratory for test.
NOTE 1—A trier sample is obtained by inserting a “trier” into the
6. Liquids
1 3
material.Atrier is a half-round steel cylinder ⁄2 to ⁄4 in. (12.7 to 19 mm)
6.1 Take a sample of not less than 0.5 pt (236.6 mL) at
in diameter, 6 to 36 in. (152 to 914 mm) in length, pointed on one end and
random from not less than 1 % of the seller’s shipping
having a grip handle on the other end. After insertion, the trier is turned
containers, provided each package contains not less than 10 gal two or three times, and upon removal a core of the material being sampled
is obtained.
(37.9 L). In the case of smaller containers, take a sample of not
less than 0.5 pt (236.6 mL) at random from each lot of
8. Preparation of Sample
containers totaling not more than 1000 gal (3785.4 L) or
8.1 Powders and Flakes—Minimizing exposure to air, rap-
fraction thereof. The gross sample shall in all cases consist of
idly disintegrate and mix the sample of powdered, flake, or
not less than three samples of 0.5 pt (236.6 mL) each taken at
chip product. If desired, quarter down to about 1 lb (453.6 g).
random from separate containers. Before drawing the sample
Weigh at once all portions for analysis, preserving the remain-
from the container selected, thoroughly agitate the contents of
der in an airtight container in a cool place.
the container. The inspector shall thoroughly mix the gross
8.2 Liquids—No preparation of the sample of liquid, other
sample, place it in clean, dry cans or bottles, which shall be
than a thorough mixing, is necessary unless it is received
completely filled and securely stoppered with clean corks or
during very cold weather, when it should be allowed to stand
caps, then sealed, marked, and sent to the laboratory for test.
at least 1 h after it has warmed to room temperature (20 to
7. Pastes
30°C) before it is tested, particularly for its lathering qualities
7.1 Pastes Packed in Cans or Cartons of 5 lb (2.27 kg) or (Note 2).
8.3 Pastes—Store preferably in glass. If crystals separate,
Less—Takeonecanorcartonatrandomfromnotlessthan1 %
of the seller’s shipping containers, provided each package melt on water bath.
contains not less than 50 lb (22.7 kg). In the case of smaller
NOTE 2—If pastes or liquids are known to be acidic, and decomposition
containers, take a can or carton at random from each lot of
of sample can result from heating, the samples shall be adequately labeled
containers totaling not more than 5000 lb (2268 kg) or fraction
for precautionary treatment and warmed to room temperature or other
thereof. The gross sample shall in all cases consist of not less maximum temperature as agreed upon for mixing and sampling.
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn. Contact ASTM
International (www.astm.org) for the latest information.
D1570
TEST METHODS OF CHEMICAL ANALYSIS
9. Purity of Reagents
9.1 Reagent grade chemicals shall be used in all tests.
Unless otherwise indicated, it is intended that all reagents shall
conform to the specifications of the Committee on Analytical
Reagents of the American Chemical Society, where such
specifications are available. Other grades may be used, pro-
vided it is first ascertained that the reagent is of sufficiently
high purity to permit its use without lessening the accuracy of
the determination.
9.2 Unless otherwise indicated, references to water shall be
understood to mean reagent water conforming to Specification
D 1193.
10. Duplicate Tests
10.1 When a determination shows nonconformity with the
specifications, a duplicate test shall be made.
MOISTURE BY THE DISTILLATION TEST
METHOD
FIG. 1 Assembly of Distillation Apparatus
11. Apparatus
11.1 The apparatus shall consist of a glass flask heated by
Moisture Expected, % Size of Trap, mL
suitable means and provided with a reflux condenser discharg-
ing into a trap and connected to the flask. The connections
0to5,incl 5
Over 5 to 17, incl 10
between the trap and the condenser and flask shall be inter-
Over 17 to 30, incl 10
changeable ground joints. The trap serves to collect and
Over 30 to 50, incl 25
measure the condensed water and to return the solvent to the Over 50 to 70, incl 25
Over 70 to 85, incl 25
flask.Asuitable assembly of the apparatus is illustrated in Fig.
1.
Traps made of well-annealed glass, constructed essentially
11.1.1 Flask—A 1000-mL flask of either the short-neck,
as shown in Fig. 1, and graduated to contain one of the
round-bottom type or the Erlenmeyer type.
following specified volumes at 20°C shall be used:
11.1.2 Heat Source, either an oil bath (stearic acid, paraffin
11.1.4.1 5-mLTrap—Subdividedinto0.1-mLdivisionswith
wax, etc.), or an electric heater provided with a sliding rheostat
each 1-mL line numbered (5 mL at top). The error in any
or other means of heat control.
indicated capacity may not be greater than 0.05 mL.
11.1.3 Condenser—A water-cooled glass reflux condenser
11.1.4.2 10-mL Trap—Subdivided from 0 to 1 mL in 0.1-
(Fig. 1), having a jacket approximately 15 ⁄4 in. (400 mm) in
mL divisions from 1 to 10 mL in 0.2-mL divisions.
3 1
length, with an inner tube ⁄8 to ⁄2 in. (9.5 to 12.7 mm) in
11.1.4.3 25-mL Trap—Subdivided from 0 to 1 mL in 0.1-
outside diameter, and not less than ⁄4-in. (6-mm) inside
mL divisions and from 1 to 25 mL in 0.2-mL divisions.
diameter, shall be used.The end of the condenser to be inserted
NOTE 3—The condenser and trap should be thoroughly cleaned before
in the trap may be ground off at an angle of 30° from the
use.
vertical axis of the condenser. When inserted into the trap, the
tip of the condenser shall be about ⁄4 in. (6 mm) above the
12. Solvent
surface of the liquid in the trap after the distillation conditions
12.1 Xylene (or Toluene)—Saturate xylene (or toluene) with
have been established. Fig. 1 shows a conventional sealed-in
water by shaking with a small quantity of water and distill. Use
type of condenser, but any other condenser fulfilling the
the distillate for the determination.
detailed requirements of this paragraph may be used.
11.1.4 Trap—For greatest accuracy several trap sizes are
13. Procedure
allowable, depending upon the percentage of moisture ex-
13.1 Transfer to the 1000-mL flask, equipped with the size
pected:
of trap specified in 11.1.4, an amount of sample according to
the percentage of moisture expected, as follows:
A
Moisture Expected, % Weight of Sample to be Used, g
Reagent Chemicals, American Chemical Society Specifications, American
0 to 5, incl 50 6 5
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Over 5 to 17, incl 50 6 5
listed by the American Chemical Society, see Analar Standards for Laboratory
Over 17 to 30, incl 40 6 4
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Over 30 to 50, incl 30 6 3
and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
Over 50 to 70, incl 30 6 3
MD.
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn. Contact ASTM
International (www.astm.org) for the latest information.
D1570
17.2 Indicator Solutions—Phenolphthalein and methyl or-
Over 70 to 85, incl 25 6 2
ange indicator solutions.
A
Weighed to the nearest 0.25 g.
17.3 Sodium Hydroxide, Standard Solution 1.0 N—Prepare
Add immediately about 100 mL of xylene or toluene. Place
and standardize a 1.0 N NaOH solution.A0.5 N NaOH solution
a small, thin sheet of long-fiber, chemical-resistant glass 328
may be used with proper corrections in calculation.
on the surface of the toluene. The glass wool should be
thoroughly dried in the oven and held in the desiccator before
18. Procedure
use.
18.1 Weigh 5 6 0.001 g of the sample into a 400-mL
13.2 Connect the flask and receiver to the condenser and
beaker. Dissolve in 100 to 150 mL of warm water (about
pour sufficient xylene or toluene down the condenser tube to
35°C). Add 2 drops of methyl orange indicator and 2 drops of
cause a slight overflow through the side tube. Wrap the flask
phenolphthalein indicator and titrate in accordance with 18.2,
and tube leading to the receiver with asbestos cloth, so that
refluxing will be under better control. 18.3, or 18.4.
13.3 Heat the oil bath with a gas burner or other source of
18.2 If the sample solution is acid to methyl orange, titrate
hea
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