ASTM D1570-95(2009)

Standard Test Methods for Sampling and Chemical Analysis of Fatty Alkyl Sulfates

ABSTRACT
These test methods cover the sampling and chemical analysis of paste, powder, or liquid detergent fatty alkyl sulfates. The different procedure for sampling and chemical analysis of past, powder, or liquid detergent are presented and discussed in details. Distillation test, titration test, and gravimetric test shall be performed to meet the requirements prescribed. The calculations methods for chlorides as sodium chloride are presented in details.
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 Method11-14  pH15  Alkalinity16-19  Alcohol-Soluble Matter20-22  Alcohol-Insoluble Matter23 and 24  Unsulfated Material25-28  Combined Alcohols29-32 Ester SO3:  Method A. Titration Test Method36 and 37
Sections Ester SO3:  Method B. Gravimetric Test Method38 and 39  Sodium Sulfate40-43  Chlorides Calculated as Sodium Chloride (NaCl)44-47
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

• Status: Historical
• Publication Date: 30-Sep-2009
• ICS: 71.100.40 - Surface active agents
• Technical Committee: D12 - Soaps and Other Detergents
• Drafting Committee: D12.12 - Analysis and Specifications of Soaps, Synthetics, Detergents and their Components

Relations

• Replaces: ASTM D1570-95(2003) - Standard Test Methods for Sampling and Chemical Analysis of Fatty Alkyl Sulfates
• Effective Date: 01-Oct-2009

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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(Reapproved 2009)
Standard Test Methods for
Sampling and Chemical Analysis of Fatty Alkyl Sulfates
This standard is issued under the fixed designation D1570; 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 (´) 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 39
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
parentheses are for information only.
Sampling:
1.4 This standard does not purport to address all of the
Powders and Flakes Packed in Cans or Cartons 4
Powders and Flakes in Bulk 5
safety concerns, if any, associated with its use. It is the
Liquids 6
responsibility of the user of this standard to establish appro-
Pastes 7
priate safety and health practices and determine the applica-
Preparation of Sample 8
Moisture by the Distillation Test Method 11–14
bility of regulatory limitations prior to use. Material Safety
pH 15
Data Sheets are available for reagents and materials. Review
Alkalinity 16–19
Alcohol-Soluble Matter 20–22 them for hazards prior to usage.
Alcohol-Insoluble Matter 23 and
2. Referenced Documents
Unsulfated Material 25–28
2.1 ASTM Standards:
Combined Alcohols 29–32
Ester SO :
D216 Method for Distillation of Natural Gasoline
Method A. Titration Test Method 36 and
D1172 Guide for pH of Aqueous Solutions of Soaps and
Detergents
D1193 Specification for Reagent Water
These test methods are under the jurisdiction of ASTM Committee D12 on
Soaps and Other Detergents and are the direct responsibility of Subcommittee
D12.12 on Analysis and Specifications of Soaps, Synthetics, Detergents and their
Components. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Oct. 1, 2009. Published December 2009. Originally contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
approved in 1958 as D1570 – 58 T. Last previous edition approved in 2003 as Standards volume information, refer to the standard’s Document Summary page on
D1570 – 95(2003). DOI: 10.1520/D1570-95R09. the ASTM website.
SAMPLING
3. General Requirement
3.1 The seller shall have the option of being represented at thereof. The gross sample shall in all cases consist of not less
the time of sampling and when he so requests, shall be
than three cans or cartons taken at random from separate
furnished with a duplicate sample.
containers. In the case of very large lots where the sample
drawnasabovewillamounttomorethan20lb(9.1kg),reduce
4. Powders and Flakes Packed in Cans or Cartons
the percentage of packages sampled so that the amount drawn
will not exceed 20 lb (9.1 kg).Tightly wrap the individual cans
4.1 Take one can or carton at random from not less than 1%
or cartons at once in paraffined paper and seal by rubbing the
of the seller’s shipping containers, provided each package
edges with a heated iron. The inspector shall accurately weigh
contains not less than 50 lb (22.7 kg). In the case of smaller
each wrapped can or carton and record its weight and the date
containers, take a can or carton at random from each lot of
containers totaling not more than 5000 lb (2268 kg) or fraction of weighing on the wrapper. Place the wrapped cans or cartons
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D1570 − 95 (2009)
in an airtight container, which should be nearly filled, and containers. In the case of very large lots where the sample
which shall then be sealed, marked, and sent to the laboratory drawnasabovewillamounttomorethan20lb(9.1kg),reduce
for test. Samples shall be kept cool until tested. the percentage of packages sampled so that the amount drawn
shall not exceed 20 lb (9.1 kg). The samples shall be wrapped,
5. Powders and Flakes in Bulk
sealed, marked, and sent to the laboratory for test.
5.1 Take a grab sample of not less than 0.5 lb (227 g) at
7.2 Pastes Packed in Bulk—Take a “trier” sample (Note 1)
random from not less than 1 % of the seller’s shipping
of not less than 0.5 lb (227 g) at random from not less than 1 %
containers,providedeachpackagecontainsnotlessthan100lb
of the seller’s shipping containers, provided each package
(45.4 kg). In the case of smaller containers, take a grab sample
contains not less than 50 lb (22.7 kg). In the case of smaller
of not less than 0.5 lb (227 g) at random from each lot of
containers, take a “trier” sample of not less than 0.5 lb (227 g)
containers totaling not more than 10 000 lb (4536 kg) or
at random from each lot of containers totaling not more than
fraction thereof. The gross sample shall in all cases consist of
5000lb(2268kg)orfractionthereof.Thegrosssampleshallin
not less than three grab samples of 0.5 lb (227 g) each taken at
all cases consist of not less than three 0.5-lb (227-g) samples,
random from separate containers. In the case of very large lots
each taken at random from separate containers.With very large
where the sample drawn as above will amount to more than 20
lotswherethesampledrawnasabovewillamounttomorethan
lb (9.1 kg), reduce the percentage of packages sampled so that
10 lb (4.5 kg), reduce the percentage of packages sampled so
the amount drawn shall not exceed 20 lb (9.1 kg). The
that the amount drawn shall not exceed 10 lb (4.5 kg). The
inspector shall rapidly mix the gross sample and place it in an
inspector shall promptly place the gross sample in a clean, dry,
airtight container, which shall be filled, sealed, marked, accu-
airtight and watertight container, which shall be filled, sealed,
rately weighed, with its weight and the date of weighing
marked, and sent to the laboratory for test.
recorded on the package, and be sent to the laboratory for test.
NOTE 1—A trier sample is obtained by inserting a “trier” into the
Samples shall be kept cool until tested.
1 3
material.Atrier is a half-round steel cylinder ⁄2 to ⁄4 in. (12.7 to 19 mm)
in diameter, 6 to 36 in. (152 to 914 mm) in length, pointed on one end and
6. Liquids
having a grip handle on the other end. After insertion, the trier is turned
6.1 Take a sample of not less than 0.5 pt (236.6 mL) at
two or three times, and upon removal a core of the material being sampled
is obtained.
random from not less than 1 % of the seller’s shipping
containers,providedeachpackagecontainsnotlessthan10gal
8. Preparation of Sample
(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
8.1 Powders and Flakes—Minimizing exposure to air, rap-
containers totaling not more than 1000 gal (3785.4 L) or
idly disintegrate and mix the sample of powdered, flake, or
fraction thereof. The gross sample shall in all cases consist of
chip product. If desired, quarter down to about 1 lb (453.6 g).
not less than three samples of 0.5 pt (236.6 mL) each taken at
Weigh at once all portions for analysis, preserving the remain-
random from separate containers. Before drawing the sample
der in an airtight container in a cool place.
from the container selected, thoroughly agitate the contents of
8.2 Liquids—No preparation of the sample of liquid, other
the container. The inspector shall thoroughly mix the gross
than a thorough mixing, is necessary unless it is received
sample, place it in clean, dry cans or bottles, which shall be
during very cold weather, when it should be allowed to stand
completely filled and securely stoppered with clean corks or
at least 1 h after it has warmed to room temperature (20 to
caps, then sealed, marked, and sent to the laboratory for test.
30°C) before it is tested, particularly for its lathering qualities
7. Pastes
(Note 2).
7.1 Pastes Packed in Cans or Cartons of 5 lb (2.27 kg) or
8.3 Pastes—Store preferably in glass. If crystals separate,
Less—Take one can or carton at random from not less than 1 %
melt on water bath.
of the seller’s shipping containers, provided each package
NOTE 2—If pastes or liquids are known to be acidic, and decomposition
contains not less than 50 lb (22.7 kg). In the case of smaller
of sample can result from heating, the samples shall be adequately labeled
containers, take a can or carton at random from each lot of
for precautionary treatment and warmed to room temperature or other
containers totaling not more than 5000 lb (2268 kg) or fraction
maximum temperature as agreed upon for mixing and sampling.
thereof. The gross sample shall in all cases consist of not less
than three cans or cartons taken at random from separate
D1570 − 95 (2009)
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
D1193.
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
11. Apparatus
11.1 The apparatus shall consist of a glass flask heated by
FIG. 1 Assembly of Distillation Apparatus
suitable means and provided with a reflux condenser discharg-
ing into a trap and connected to the flask. The connections
between the trap and the condenser and flask shall be inter-
changeable ground joints. The trap serves to collect and
Moisture Expected, % Size of Trap, mL
measure the condensed water and to return the solvent to the
0to5,incl 5
flask.Asuitable assembly of the apparatus is illustrated in Fig.
Over 5 to 17, incl 10
1.
Over 17 to 30, incl 10
11.1.1 Flask—A 1000-mL flask of either the short-neck,
Over 30 to 50, incl 25
Over 50 to 70, incl 25
round-bottom type or the Erlenmeyer type.
Over 70 to 85, incl 25
11.1.2 Heat Source, either an oil bath (stearic acid, paraffin
Traps made of well-annealed glass, constructed essentially
wax, etc.), or an electric heater provided with a sliding rheostat
as shown in Fig. 1, and graduated to contain one of the
or other means of heat control.
following specified volumes at 20°C shall be used:
11.1.3 Condenser—A water-cooled glass reflux condenser
(Fig. 1), having a jacket approximately 15 ⁄4 in. (400 mm) in
11.1.4.1 5-mL Trap—Subdivided into 0.1-mLdivisions with
3 1
length, with an inner tube ⁄8 to ⁄2 in. (9.5 to 12.7 mm) in
each 1-mL line numbered (5 mL at top). The error in any
outside diameter, and not less than ⁄4-in. (6-mm) inside
indicated capacity may not be greater than 0.05 mL.
diameter,shallbeused.Theendofthecondensertobeinserted
11.1.4.2 10-mL Trap—Subdivided from 0 to 1 mL in 0.1-
in the trap may be ground off at an angle of 30° from the
mL divisions from 1 to 10 mL in 0.2-mL divisions.
vertical axis of the condenser. When inserted into the trap, the
11.1.4.3 25-mL Trap—Subdivided from 0 to 1 mL in 0.1-
tip of the condenser shall be about ⁄4 in. (6 mm) above the
mL divisions and from 1 to 25 mL in 0.2-mL divisions.
surface of the liquid in the trap after the distillation conditions
have been established. Fig. 1 shows a conventional sealed-in
NOTE 3—The condenser and trap should be thoroughly cleaned before
type of condenser, but any other condenser fulfilling the
use.
detailed requirements of this paragraph may be used.
11.1.4 Trap—For greatest accuracy several trap sizes are 12. Solvent
allowable, depending upon the percentage of moisture ex-
12.1 Xylene (or Toluene)—Saturate xylene (or toluene) with
pected:
water by shaking with a small quantity of water and distill. Use
the distillate for the determination.
Reagent Chemicals, American Chemical Society Specifications, American
13. Procedure
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory
13.1 Transfer to the 1000-mL flask, equipped with the size
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
of trap specified in 11.1.4, an amount of sample according to
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
MD. the percentage of moisture expected, as follows:
D1570 − 95 (2009)
A
17. Reagents
Moisture Expected, % Weight of Sample to be Used, g
17.1 Hydrochloric or Sulfuric Acid, Standard—Prepare and
0to5,incl 50±5
Over 5 to 17, incl 50 ± 5
standardize 1 N hydrochloric acid or sulfuric acid. Hydrochlo-
Over 17 to 30, incl 40 ± 4
ric acid is preferable. Standard acid weaker than 1 N may be
Over 30 to 50, incl 30 ± 3
used and titrations calculated to the equivalent in terms of 1 N
Over 50 to 70, incl 30 ± 3
Over 70 to 85, incl 25 ± 2
solution.
17.2 Indicator Solutions—Phenolphthalein and methyl or-
A
Weighed to the nearest 0.25 g.
ange indicator solutions.
Add immediately about 100 mL of xylene or toluene. Place
17.3 Sodium Hydroxide, Standard Solution 1.0 N—Prepare
a small, thin sheet of long-fiber, chemical-resistant glass 328
andstandardizea1.0 NNaOHsolution.A0.5 NNaOHsolution
on the surface of the toluene. The glass wool should be
may be used with proper corrections in calculation.
thoroughly dried in the oven and held in the desiccator before
use.
18. Procedure
13.2 Connect the flask and receiver to the condenser and
18.1 Weigh 5 6 0.001 g of the sample into a 400-mL
pour sufficient xylene or toluene down the condenser tube to
beaker. Dissolve in 100 to 150 mL of warm water (about
cause a slight overflow through the side tube. Wrap the flask
35°C). Add 2 drops of methyl orange indicator and 2 drops of
and tube leading to the receiver with asbestos cloth, so that
phenolphthalein indicator and titrate in accordance with 18.2,
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
heat, or apply heat directly to t
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