ASTM D1570-95(2016)

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 Method  
11 – 14  
pH  
15  
Alkalinity  
16 – 19  
Alcohol-Soluble Matter  
20 – 22  
Alcohol-Insoluble Matter  
23 and 24  
Unsulfated Material  
25 – 28  
Combined Alcohols  
29 – 32  
Ester SO3:  
Method A. Titration Test Method  
36 and 37    
Sections  
Ester SO3:  
Method B. Gravimetric Test Method  
38 and 39  
Sodium Sulfate  
40 – 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-Jun-2016
• 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

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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 2016)
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
them for hazards prior to usage.
Alcohol-Soluble Matter 20 – 22
Alcohol-Insoluble Matter 23 and
2. Referenced Documents
Unsulfated Material 25 – 28
Combined Alcohols 29 – 32 2.1 ASTM Standards:
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 July 1, 2016. Published August 2016. 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 2009 as Standards volume information, refer to the standard’s Document Summary page on
D1570 – 95(2009). DOI: 10.1520/D1570-95R16. 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
drawn as above will amount to more than 20 lb (9.1 kg), 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
containers, take a can or carton at random from each lot of each wrapped can or carton and record its weight and the date
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 (2016)
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 drawn as above will amount to more than 20 lb (9.1 kg), 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, provided each package contains not less than 100 lb
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
5000 lb (2268 kg) or fraction thereof. The gross sample shall in
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
lots where the sample drawn as above will amount to more than
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. A trier 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, provided each package contains not less than 10 gal
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 (2016)
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
0 to 5, incl 5
flask. A suitable 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-mL divisions 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, shall be used. The end of the condenser to be inserted
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 (2016)
A
17. Reagents
Moisture Expected, % Weight of Sample to be Used, g
17.1 Hydrochloric or Sulfuric Acid, Standard—Prepare and
0 to 5, 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
and standardize a 1.0 N NaOH solution. A0.5 N NaOH solution
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
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D1570 − 95 (Reapproved 2009) D1570 − 95 (Reapproved 2016)
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
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 – 14
pH 15
Alkalinity 16 – 19
Alcohol-Soluble Matter 20 – 22
Alcohol-Insoluble Matter 23 and
Unsulfated Material 25 – 28
Combined Alcohols 29 – 32
Ester SO :
Method A. Titration Test Method 36 and
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.
Current edition approved Oct. 1, 2009July 1, 2016. Published December 2009August 2016. Originally approved in 1958 as D1570 – 58 T. Last previous edition approved
in 20032009 as D1570 – 95(2003).(2009). DOI: 10.1520/D1570-95R09.10.1520/D1570-95R16.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D1570 − 95 (2016)
Sections
Ester SO :
Method B. Gravimetric Test Method 38 and
Sodium Sulfate 40 – 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.
2. Referenced Documents
2.1 ASTM Standards:
D216 Method for Distillation of Natural Gasoline
D1172 Guide for pH of Aqueous Solutions of Soaps and Detergents
D1193 Specification for Reagent Water
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
SAMPLING
3. General Requirement
3.1 The seller shall have the option of being represented at the time of sampling and when he so requests, shall be furnished
with a duplicate sample.
4. Powders and Flakes Packed in Cans or Cartons
4.1 Take one can or carton at random from not less than 1% of the seller’s shipping containers, provided each package contains
not less than 50 lb (22.7 kg). In the case of smaller containers, take a can or carton at random from each lot of containers totaling
not more than 5000 lb (2268 kg) or fraction thereof. The gross sample shall in all cases consist of not less than three cans or cartons
taken at random from separate containers. In the case of very large lots where the sample drawn as above will amount to more
than 20 lb (9.1 kg), reduce the percentage of packages sampled so that the amount drawn 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 edges with a heated iron. The inspector shall
accurately weigh each wrapped can or carton and record its weight and the date of weighing on the wrapper. Place the wrapped
cans or cartons in an airtight container, which should be nearly filled, and which shall then be sealed, marked, and sent to the
laboratory for test. Samples shall be kept cool until tested.
5. Powders and Flakes in Bulk
5.1 Take a grab sample of not less than 0.5 lb (227 g) at random from not less than 1 % of the seller’s shipping containers,
provided each package contains not less than 100 lb (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 each lot of containers totaling not more than 10 000 lb (4536 kg) or 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 random from separate containers.
In the case of very large lots where the sample drawn as above will amount to more than 20 lb (9.1 kg), reduce the percentage
of packages sampled so that the amount drawn shall not exceed 20 lb (9.1 kg). The inspector shall rapidly mix the gross sample
and place it in an airtight container, which shall be filled, sealed, marked, accurately weighed, with its weight and the date of
weighing recorded on the package, and be sent to the laboratory for test. Samples shall be kept cool until tested.
6. Liquids
6.1 Take a sample of not less than 0.5 pt (236.6 mL) at random from not less than 1 % of the seller’s shipping containers,
provided each package contains not less than 10 gal (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 containers totaling not more than 1000 gal (3785.4 L) or fraction thereof. The gross
sample shall in all cases consist of not less than three samples of 0.5 pt (236.6 mL) each taken at random from separate containers.
Before drawing the sample from the container selected, thoroughly agitate the contents of the container. The inspector shall
thoroughly mix the gross sample, place it in clean, dry cans or bottles, which shall be completely filled and securely stoppered with
clean corks or caps, then sealed, marked, and sent to the laboratory for test.
D1570 − 95 (2016)
7. Pastes
7.1 Pastes Packed in Cans or Cartons of 5 lb (2.27 kg) or Less—Take one can or carton at random from not less than 1 % of
the seller’s shipping containers, provided each package contains not less than 50 lb (22.7 kg). In the case of smaller containers,
take a can or carton at random from each lot of containers totaling not more than 5000 lb (2268 kg) or fraction thereof. The gross
sample shall in all cases consist of not less than three cans or cartons taken at random from separate containers. In the case of very
large lots where the sample drawn as above will amount to more than 20 lb (9.1 kg), reduce the percentage of packages sampled
so that the amount drawn shall not exceed 20 lb (9.1 kg). The samples shall be wrapped, sealed, marked, and sent to the laboratory
for test.
7.2 Pastes Packed in Bulk—Take a “trier” sample (Note 1) of not less than 0.5 lb (227 g) at random from not less than 1 % of
the seller’s shipping containers, provided each package contains not less than 50 lb (22.7 kg). In the case of smaller containers,
take a “trier” sample of not less than 0.5 lb (227 g) at random from each lot of containers totaling not more than 5000 lb (2268
kg) or fraction thereof. The gross sample shall in all cases consist of not less than three 0.5-lb (227-g) samples, each taken at
random from separate containers. With very large lots where the sample drawn as above will amount to more than 10 lb (4.5 kg),
reduce the percentage of packages sampled so that the amount drawn shall not exceed 10 lb (4.5 kg). The inspector shall promptly
place the gross sample in a clean, dry, airtight and watertight container, which shall be filled, sealed, marked, and sent to the
laboratory for test.
1 3
NOTE 1—A trier sample is obtained by inserting a “trier” into the material. A trier 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 having a grip handle on the other end. After insertion, the trier is turned two or three times,
and upon removal a core of the material being sampled is obtained.
8. Preparation of Sample
8.1 Powders and Flakes—Minimizing exposure to air, rapidly disintegrate and mix the sample of powdered, flake, or chip
product. If desired, quarter down to about 1 lb (453.6 g). Weigh at once all portions for analysis, preserving the remainder in an
airtight container in a cool place.
8.2 Liquids—No preparation of the sample of liquid, other than a thorough mixing, is necessary unless it is received during very
cold weather, when it should be allowed to stand at least 1 h after it has warmed to room temperature (20 to 30°C) before it is
tested, particularly for its lathering qualities (Note 2).
8.3 Pastes—Store preferably in glass. If crystals separate, melt on water bath.
NOTE 2—If pastes or liquids are known to be acidic, and decomposition of sample can result from heating, the samples shall be adequately labeled
for precautionary treatment and warmed to room temperature or other maximum temperature as agreed upon for mixing and sampling.
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, provided 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 suitable means and provided with a reflux condenser discharging into
a trap and connected to the flask. The connections between the trap and the condenser and flask shall be interchangeable ground
joints. The trap serves to collect and measure the condensed water and to return the solvent to the flask. A suitable assembly of
the apparatus is illustrated in Fig. 1.
Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed by
the American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and National
Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.
D1570 − 95 (2016)
FIG. 1 Assembly of Distillation Apparatus
11.1.1 Flask—A 1000-mL flask of either the short-neck, round-bottom type or the Erlenmeyer type.
11.1.2 Heat Source, either an oil bath (stearic acid, paraffin wax, etc.), or an electric heater provided with a sliding rheostat or
other means of heat control.
11.1.3 Condenser—A water-cooled glass reflux condenser (Fig. 1), having a jacket approximately 15 ⁄4 in. (400 mm) in length,
3 1 1
with an inner tube ⁄8 to ⁄2 in. (9.5 to 12.7 mm) in outside diameter, and not less than ⁄4-in. (6-mm) inside diameter, shall be used.
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 the condenser.
When inserted into the trap, the tip of the condenser shall be about ⁄4 in. (6 mm) above the surface of the liquid in the trap after
the distillation conditions have been established. Fig. 1 shows a conventional sealed-in type of condenser, but any other condenser
fulfilling the detailed requirements of this paragraph may be used.
11.1.4 Trap—For greatest accuracy several trap sizes are allowable, depending upon the percentage of moisture expected:
Moisture Expected, % Size of Trap, mL
0 to 5, incl 5
Over 5 to 17, incl 10
Over 17 to 30, incl 10
Over 30 to 50, incl 25
Over 50 to 70, incl 25
Over 70 to 85, incl 25
Traps made of well-annealed glass, constructed essentially as shown in Fig. 1, and graduated to contain one of the following
specified volumes at 20°C shall be used:
11.1.4.1 5-mL Trap—Subdivided into 0.1-mL divisions with each 1-mL line numbered (5 mL at top). The error in any indicated
capacity may not be greater than 0.05 mL.
11.1.4.2 10-mL Trap—Subdivided from 0 to 1 mL in 0.1- mL divisions from 1 to 10 mL in 0.2-mL divisions.
11.1.4.3 25-mL Trap—Subdivided from 0 to 1 mL in 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 use.
12. Solvent
12.1 Xylene (or Toluene)—Saturate xylene (or toluene) with water by shaking with a small quantity of water and distill. Use
the distillate for the determination.
D1570 − 95 (2016)
13. Procedure
13.1 Transfer to the 1000-mL flask, equipped with the size 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
0 to 5, incl 50 ± 5
Over 5 to 17, incl 50 ± 5
Over 17 to 30, incl 40 ± 4
Over 30 to 50, incl 30 ± 3
Over 50 to 70, incl 30 ± 3
Over 70 to 85, incl 25 ± 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 328 on
the surface of the toluene. The glass wool should be thoroughly dried in the oven and held in the desiccator before use.
13.2 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 and tube leading to the receiver with asbestos cloth, so that refluxing will
be under better control.
13.3 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/min. When the greater part of the water has distilled over,
increase the distillation rate to 200 drops/min until no more water is collected. Purge the reflux condenser during the distillation
wit
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