ASTM D460-91(2014)

Standard Test Methods for Sampling and Chemical Analysis of Soaps and Soap Products (Withdrawn 2023)

SIGNIFICANCE AND USE
3.1 Soap and soap products are widely used. These test methods are suitable for setting specifications and performing quality control on soap and soap products.
SCOPE
1.1 These test methods cover the sampling and chemical analysis of cake, powdered, flake, liquid, and paste soaps, and soap products.  
1.2 The test methods appear in the following order:    
Sampling    
Section  
General Requirements  
4  
Cake Soaps, Flake and Powdered Soap Products when Packed in Cans or Cartons  
5  
Flake and Powdered Soap Products when in Bulk  
6  
Liquid Soap  
7  
Paste Soap Products  
8  
Preparation of Samples  
9  
Test Methods for Chemical Analysis  
Safety Precautions  
10  
Purity of Reagents  
11  
Duplicate Tests  
12  
Moisture:  
Choice of Method  
13  
Method A—Matter Volatile at 105°C (Oven Method)  
14  
Method B—Distillation Method  
15 – 18  
Total Matter Insoluble in Alcohol  
19 and 20  
Free Alkali or Free Acid  
21  
Matter Insoluble in Water  
22  
Total Alkalinity of Matter Insoluble in Alcohol, Alkaline Salts  
23  
Combined Alkali, Total Anhydrous Soap  
24 and 25  
Combined Sodium and Potassium Oxides  
26 – 29  
Free Alkali and Potassium Carbonate in Potash Paste Soaps  
30 – 32  
Unsaponified plus Unsaponifiable Matter  
33 – 35  
Unsaponifiable Matter  
36 – 38  
Unsaponified Matter  
39  
Rosin (McNicoll Method)  
40 – 43  
Preparation of Total Fatty Matter, Fatty and Rosin Acids, and Unsaponified Matter  
44 and 45  
Titer Test  
46 and 47  
Acid Number of Fatty Acids  
48 and 49  
Iodine Number (Wijs Method)  
50 – 52  
Chlorides  
53 – 55  
Borax  
56 – 58  
Silica Present as Alkaline Silicates  
59 and 60  
Carbon Dioxide (Carbonates):  
Train-Absorption Method  
61 – 64  
Evolution-Volumetric Method  
65 – 68  
Phosphates  
69 – 76  
Tetrasodium Pyrophosphate  
77 – 79  
Sulfates  
80 and 81  
Glycerine, Sugars, and Starch:  
Glycerine in the Absence of Sugars  
82 – 84  
Glycerine in the Presence of Sugars  
85 and 86  
Starch  
87 and 88  
Sugars  
89 and 90  
Volatile Hydrocarbons  
91 – 95  
Copper (Trace Amounts)  
96 – 102  
Precision and Bias  
103
1.3 The values stated in inch-pound units are to be regarded as standard. The values given in parentheses are mathematical conversions to SI units that are provided for information only and are not considered standard.  
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. For specific hazard statements, see Section 10. Material Safety Data Sheets are available for reagents and materials. Review them for hazards prior to usage.
WITHDRAWN RATIONALE
These test methods cover the sampling and chemical analysis of cake, powdered, flake, liquid, and paste soaps, and soap products.
Formerly under the jurisdiction of Committee D12 on Soaps and Other Detergents, this test method was withdrawn in January 2023 in accordance with section 10.6.3 of the Regulations Governing ASTM Technical Committees, which requires that standards shall be updated by the end of the eighth year since the last approval date.

General Information

• Status: Withdrawn
• Publication Date: 31-Dec-2013
• Withdrawal Date: 08-Jan-2023
• 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: D460 − 91 (Reapproved 2014)
Standard Test Methods for
Sampling and Chemical Analysis of Soaps and Soap
Products
This standard is issued under the fixed designation D460; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
These methods are identical in substance with the standard methods of the American Oil Chemists’ Society which were developed by
the Committee on Soap Analysis A-1 of that Society, and with those of the American Chemical Society.
This standard has been approved for use by agencies of the U.S. Department of Defense.
1. Scope
Acid Number of Fatty Acids 48 and 49
Iodine Number (Wijs Method) 50–52
1.1 These test methods cover the sampling and chemical
Chlorides 53–55
analysis of cake, powdered, flake, liquid, and paste soaps, and Borax 56–58
Silica Present as Alkaline Silicates 59 and 60
soap products.
Carbon Dioxide (Carbonates):
Train-Absorption Method 61–64
1.2 The test methods appear in the following order:
Evolution-Volumetric Method 65–68
SAMPLING
Phosphates 69–76
Section
Tetrasodium Pyrophosphate 77–79
General Requirements 4
Sulfates 80 and 81
Cake Soaps, Flake and Powdered Soap Products when
Glycerine, Sugars, and Starch:
Packed in Cans or Cartons 5
Glycerine in the Absence of Sugars 82–84
Flake and Powdered Soap Products when in Bulk 6
Glycerine in the Presence of Sugars 85 and 86
Liquid Soap 7
Starch 87 and 88
Paste Soap Products 8
Sugars 89 and 90
Preparation of Samples 9
Volatile Hydrocarbons 91–95
Test Methods for Chemical Analysis
Copper (Trace Amounts) 96 – 102
Safety Precautions 10
Precision and Bias 103
Purity of Reagents 11
1.3 Thevaluesstatedininch-poundunitsaretoberegarded
Duplicate Tests 12
Moisture:
as standard. The values given in parentheses are mathematical
Choice of Method 13
conversions to SI units that are provided for information only
Method A—Matter Volatile at 105°C (Oven Method) 14
and are not considered standard.
Method B—Distillation Method 15–18
Total Matter Insoluble in Alcohol 19 and 20
1.4 This standard does not purport to address all of the
Free Alkali or Free Acid 21
safety concerns, if any, associated with its use. It is the
Matter Insoluble in Water 22
Total Alkalinity of Matter Insoluble in Alcohol, Alkaline Salts 23
responsibility of the user of this standard to establish appro-
Combined Alkali, Total Anhydrous Soap 24 and 25
priate safety and health practices and determine the applica-
Combined Sodium and Potassium Oxides 26–29
bility of regulatory limitations prior to use. For specific hazard
Free Alkali and Potassium Carbonate in Potash Paste
Soaps 30–32
statements, see Section 10. Material Safety Data Sheets are
Unsaponified plus Unsaponifiable Matter 33–35
available for reagents and materials. Review them for hazards
Unsaponifiable Matter 36–38
Unsaponified Matter 39 prior to usage.
Rosin (McNicoll Method) 40–43
Preparation of Total Fatty Matter, Fatty and Rosin Acids,
2. Referenced Documents
and Unsaponified Matter 44 and 45
Titer Test 46 and 47
2.1 ASTM Standards:
D216Method for Distillation of Natural Gasoline
D459Terminology Relating to Soaps and Other Detergents
These test methods are under the jurisdiction of ASTM Committee D12 on D1193Specification for Reagent Water
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 Jan. 1, 2014. Published February 2014. Originally contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
approved in 1937. Last previous edition approved in 1997 as D460–91(2005). Standards volume information, refer to the standard’s Document Summary page on
DOI: 10.1520/D0460-91R14. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D460 − 91 (2014)
E1Specification for ASTM Liquid-in-Glass Thermometers kg), the percentage of packages sampled shall be reduced so
that the amount drawn shall not exceed 20 lb. The inspector
3. Significance and Use shall rapidly mix the gross sample and place it in an airtight
container, which shall be filled, sealed, marked, accurately
3.1 Soap and soap products are widely used. These test
weighed, its weight and the date of weighing recorded on the
methods are suitable for setting specifications and performing
package, and sent to the laboratory for test. Samples shall be
quality control on soap and soap products.
kept cool until tested.
SAMPLING
7. Liquid Soap
4. General Requirements
7.1 A sample of not less than 0.5 pt (236.6 mL) shall be
4.1 The seller shall have the option of being represented at takenatrandomfromnotlessthan1%oftheseller’sshipping
containers,providedeachpackagecontainsnotlessthan10gal
the time of sampling, and when he so requests shall be
furnished with a duplicate sample. (37.9 L). In the case of smaller containers, a sample of not less
than0.5ptshallbetakenatrandomfromeachlotofcontainers
5. Cake Soaps, Flake and Powdered Soap Products
totaling not more than 1000 gal (3785.4 L) or fraction thereof.
When Packed in Cans or Cartons Thegrosssampleshallinallcasesconsistofnotlessthanthree
samples of 0.5 pt each taken at random from separate contain-
5.1 One cake (can or carton) shall be taken at random from
ers.Beforedrawingthesamplefromthecontainerselected,the
not less than 1% of the seller’s shipping containers, provided
contents of the container shall be thoroughly agitated. The
eachpackagecontainsnotlessthan50lb(22.7kg).Inthecase
inspector shall thoroughly mix the gross sample, place it in
of smaller containers, a cake (can or carton) shall be taken at
clean, dry cans or bottles, which shall be completely filled and
randomfromeachlotofcontainerstotalingnotmorethan5000
securely stoppered with clean corks or caps, then sealed,
lb (2268 kg), or fraction thereof. The gross sample shall in all
marked, and sent to the laboratory for test.
casesconsistofnotlessthanthreecakes(cansorcartons)taken
at random from separate containers. To illustrate, if a total
8. Paste Soap Products
shipment consists of 70 000 lb, all in 1400 containers weigh-
8.1 When Packed in Cans or Cartons of 5 lb (2.27 kg) or
ing 50 lb each, then 14 containers are chosen at random and
Less—Onecanorcartonshallbetakenatrandomfromnotless
one cake taken from each for a total sample of 14 cakes. If a
than 1% of the seller’s shipping containers, provided each
total shipment of 70 000 lb includes containers weighing less
package contains not less than 50 lb (22.7 kg). In the case of
than 50 lb, then the shipment must be divided into 14 lots of
smaller containers, a can or carton shall be taken at random
containersweighingapproximately5000lbeach,andonecake
from each lot of containers totaling not more than 5000 lb
taken from each lot, again for a total sample size of 14 cakes.
(2268 kg) or fraction thereof. The gross sample shall in all
Thegrosssampleshallinallcasesconsistofnotlessthanthree
cases consist of not less than three cans or cartons taken at
cakes (cans or cartons) taken at random from separate contain-
random from separate containers. In the case of very large lots
ers. In the case of very large lots where the sample drawn as
where the sample drawn as above will amount to more than 20
above will amount to more than 20 lb (9.1 kg), the percentage
lb (9.1 kg), the percentage of packages sampled shall be
ofpackagessampledshallbereducedsothattheamountdrawn
reduced so that the amount drawn shall not exceed 20 lb. The
shall not exceed 20 lb. The individual cakes (cans or cartons)
samples shall be wrapped, sealed, marked, and sent to the
shall be sealed at once in moisture-proof containers such as
laboratory for test.
polyethylene bags, or tightly wrapped in paraffined paper and
sealed by rubbing the edges with a heated iron. The inspector
8.2 When Packed in Bulk—A trier sample of not less than
shall accurately weigh each wrapped cake (can or carton), and
0.5 lb (227 g) shall be taken at random from not less than 1%
record its weight and the date of weighing on the wrapper.The
of the seller’s shipping containers, provided each package
wrapped cakes (cans or cartons) shall be placed in an airtight
contains not less than 50 lb. In the case of smaller containers,
container, which should be nearly filled, and which shall then
a trier sample of not less than 0.5 lb shall be taken at random
be sealed, marked, and sent to the laboratory for test. Samples
from each lot of containers totaling not more than 5000 lb or
shall be kept cool until tested.
fraction thereof. The gross sample shall in all cases consist of
not less than three 0.5-lb samples, each taken at random from
6. Flake and Powdered Soap Products When in Bulk
separate containers. With very large lots where the sample
drawn as above will amount to more than 10 lb (4.5 kg), the
6.1 A grab sample of not less than 0.5 lb (227 g) shall be
takenatrandomfromnotlessthan1%oftheseller’sshipping percentage of packages sampled shall be reduced so that the
amount drawn shall not exceed 10 lb. The inspector shall
containers,providedeachpackagecontainsnotlessthan100lb
(45.4 kg). In the case of smaller containers, a grab sample of promptly place the gross sample in a clean, dry, airtight and
not less than 0.5 lb shall be taken at random from each lot of
containers totaling not more than 10 000 lb (4536 kg) or
A trier sample is obtained by inserting a trier into the material. A trier is a
fraction thereof. The gross sample shall in all cases consist of
1 3
half-roundsteelcylinder ⁄2 to ⁄4 in.(12.7to19.1mm)indiameter,6to36in.(152
notlessthanthreegrabsamplesof0.5lbeachtakenatrandom
to914mm)inlength,pointedononeendandhavingagriphandleontheotherend.
from separate containers. In the case of very large lots where
Afterinsertion,thetrieristurnedtwoorthreetimes,anduponremovalacoreofthe
thesampledrawnasabovewillamounttomorethan20lb(9.1 material being sampled is obtained.
D460 − 91 (2014)
watertight container, which shall be filled, sealed, marked, and quarter down to about 1 lb (454 g). Weigh at once all portions
sent to the laboratory for test. for analysis, preserving the remainder in an airtight container
in a cool place.
9. Preparation of Samples
9.3 Liquid Soap—No preparation of the sample of liquid
9.1 Cake Soap—Grind all bars through a suitable food
soap, other than a thorough mixing, is necessary unless it is
chopper. In the case of large samples, it is permissible to
received during very cold weather, when it should be allowed
quarterthebarsandgrindonequarterfromeachbar.However,
to stand at least 1 h after it has warmed to room temperature
each ground sample should consist of at least 3 lb (1.36 kg).
Mix all ground samples thoroughly on a clean, dry, (20 to 30°C) before it is tested, particularly for its lathering
nonabsorbent, impervious surface with a spatula. Divide into qualities.
four quarters and discard the two opposite quarters. Combine,
9.4 Paste Soap Products—Mix the sample of paste soap
remix, and requarter the remaining two quarters. Continue in
products thoroughly by kneading and quarter down to about 1
this manner until the sample is reduced to approximately 2 lb
lb (454 g). Weigh at once all portions for analysis, preserving
(0.91 kg). Place this portion in a clean, dry sample container.
the remainder in an airtight container in a cool place.
Closetightlyandlabelcompletelyforidentification.Thisisthe
sample for analysis and must be preserved in a cool dry place.
9.2 Powdered and Chip Soaps—Rapidly disintegrate and
mix the sample of powdered, flake, or chip soap. If desired,
METHODS FOR CHEMICAL ANALYSIS
10. Hazards
10.1 Precaution—All reagents and chemicals should be MOISTURE
handled with care. Before using any chemical, read and follow
13. Choice of Test Method
all safety precautions and instructions on the manufacturer’s
13.1 The oven method described in Section 14 is generally
label. Clean up any spill immediately. Consult the Material
applicable to all soaps, but certain exceptions to this method
Safety Data Sheet for specific handling and disposal informa-
must be made if accurate results are desired. These exceptions
tion.
include the following:
10.2 Use of glass wool in place of asbestos cloth is
13.1.1 For soaps containing appreciable amounts of sodium
recommended where applicable.
silicate, the distillation method (Sections15–18) is preferred.
13.1.2 Soaps of linseed and other oxidizing oils absorb
11. Purity of Reagents
oxygen, and if the oven method is used may gain weight near
11.1 Purity of Reagents—Reagent grade chemicals shall be
the end of the test. Therefore, either an inert atmosphere or
used in all tests. Unless otherwise indicated, it is intended that
vacuum oven should be used. The distillation method is also
all reagents shall conform to the specifications of the Commit-
applicable to these types of soap.
tee onAnalytical Reagents of theAmerican Chemical Society, 13.1.3 Soaps containing appreciable amounts of glycerin,
where such specifications are available. Other grades may be
such as cold-made and semiboiled (including paste soaps),
used, provided it is first ascertained that the reagent is of usually give high results by the oven method. The distillation
sufficiently high purity to permit its use without lessening the
method is preferred for most accurate results on these types of
accuracy of the determination. soaps.
11.2 Unlessotherwiseindicated,referencestowatershallbe
Method A—Matter Volatile at 105°C (Oven Method)
understood to mean Type III reagent water conforming to
14. Procedure
Specification D1193.
14.1 Weigh 5 6 0.01 g of the sample in a porcelain or glass
12. Duplicate Tests
dish about 6 to 8 cm in diameter and about 2 to 4 cm in depth,
and dry to constant weight in an air oven at a temperature of
12.1 When a determination shows nonconformity with the
105 6 2°C. Constant weight is attained when successive
specifications a duplicate test shall be made.
heating for 1-h periods shows a loss (or gain) of not more than
0.1%.
Reagent Chemicals, American Chemical Society Specifications, American
Method B—Distillation Method
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory
15. Apparatus
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
15.1 The apparatus required consist
...