ASTM D460-91(1997)
(Test Method)Standard Test Methods for Sampling and Chemical Analysis of Soaps and Soap Products
Standard Test Methods for Sampling and Chemical Analysis of Soaps 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[deg]C (Oven Method) 14 Method B---Distillation Method 15 to 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 to 29 Free Alkali and Potassium Carbonate in Potash Paste Soaps 30 to 32 Unsaponified plus Unsaponifiable Matter 33 to 35 Unsaponifiable Matter 36 to 38 Unsaponified Matter 39 Rosin (McNicoll Method) 40 to 43 Preparation of Total Fatty Matter, Fatty and Rosin Acids, and Unsa-ponified Matter 44 and 45 Titer Test 46 and 47 Acid Number of Fatty Acids 48 and 49 Iodine Number (Wijs Method) 50 to 52 Chlorides 53 to 55 Borax 56 to 58 Silica Present as Alkaline Silicates 59 and 60 Carbon Dioxide (Carbonates): Train-Absorption Method 61 to 64 Evolution-Volumetric Method 65 to 68 Phosphates 69 to 76 Tetrasodium Pyrophosphate 77 to 79 Sulfates 80 and 81 Glycerine, Sugars, and Starch: Glycerine in the Absence of Sugars 82 to 84 Glycerine in the Presence of Sugars 85 and 86 Starch 87 and 88 Sugars 89 and 90 Volatile Hydrocarbons 91 to 95 Copper (Trace Amounts) 96 to 102 Precision and Bias 103
1.3 The values stated in inch-pound units are to be regarded as the standard. The metric equivalents of inch-pound units may be approximate.
1.4 This standard does not purport to address all of the safety problems, 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.
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:D460–91(Reapproved 1997)
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 (e) 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 Department of Defense.
1. Scope
Iodine Number (Wijs Method) 50-52
Chlorides 53-55
1.1 These test methods cover the sampling and chemical
Borax 56-58
analysis of cake, powdered, flake, liquid, and paste soaps, and
Silica Present as Alkaline Silicates 59 and 60
Carbon Dioxide (Carbonates):
soap products.
Train-Absorption Method 61-64
1.2 The test methods appear in the following order:
Evolution-Volumetric Method 65-68
SAMPLING Phosphates 69-76
Tetrasodium Pyrophosphate 77-79
Section
General Requirements 4 Sulfates 80 and 81
Glycerine, Sugars, and Starch:
Cake Soaps, Flake and Powdered Soap Products when
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
Starch 87 and 88
Liquid Soap 7
Paste Soap Products 8 Sugars 89 and 90
Volatile Hydrocarbons 91-95
Preparation of Samples 9
Test Methods for Chemical Analysis Copper (Trace Amounts) 96-102
Precision and Bias 103
Safety Precautions 10
Purity of Reagents 11
1.3 The values stated in inch-pound units are to be regarded
Duplicate Tests 12
Moisture:
as the standard. The metric equivalents of inch-pound units
Choice of Method 13
may be approximate.
Method A—Matter Volatile at 105°C (Oven Method) 14
1.4 This standard does not purport to address all of the
Method B—Distillation Method 15-18
Total Matter Insoluble in Alcohol 19 and 20
safety concerns, if any, associated with its use. It is the
Free Alkali or Free Acid 21
responsibility of the user of this standard to establish appro-
Matter Insoluble in Water 22
priate safety and health practices and determine the applica-
Total Alkalinity of Matter Insoluble in Alcohol, Alkaline Salts 23
Combined Alkali, Total Anhydrous Soap 24 and 25
bility of regulatory limitations prior to use. For specific hazard
Combined Sodium and Potassium Oxides 26-29
statements, see Section 10. Material Safety Data Sheets are
Free Alkali and Potassium Carbonate in Potash Paste
available for reagents and materials. Review them for hazards
Soaps 30-32
Unsaponified plus Unsaponifiable Matter 33-35
prior to usage.
Unsaponifiable Matter 36-38
Unsaponified Matter 39
2. Referenced Documents
Rosin (McNicoll Method) 40-43
Preparation of Total Fatty Matter, Fatty and Rosin Acids,
2.1 ASTM Standards:
and Unsaponified Matter 44 and 45
D216 Method for Distillation of Natural Gasoline
Titer Test 46 and 47
D459 Terminology Relating to Soaps and Other Deter-
Acid Number of Fatty Acids 48 and 49
gents
D1193 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
D12.12 on Analysis of Soaps and Synthetic Detergents. Discontinued, see 1992 Annual Book of ASTM Standards, Vol 05.01.
Current edition approved July 15, 1991. Published September 1991. Originally Annual Book of ASTM Standards, Vol 15.04.
published as D460–37T. Last previous edition D460–90. 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.
D460–91 (1997)
E1 Specification for ASTM Thermometers from separate containers. In the case of very large lots where
thesampledrawnasabovewillamounttomorethan20lb(9.1
3. Significance and Use
kg), the percentage of packages sampled shall be reduced so
3.1 Soap and soap products are widely used. These test that the amount drawn shall not exceed 20 lb. The inspector
shall rapidly mix the gross sample and place it in an airtight
methods are suitable for setting specifications and performing
quality control on soap and soap products. container, which shall be filled, sealed, marked, accurately
weighed, its weight and the date of weighing recorded on the
SAMPLING
package, and sent to the laboratory for test. Samples shall be
kept cool until tested.
4. General Requirements
7. Liquid Soap
4.1 The seller shall have the option of being represented at
the time of sampling, and when he so requests shall be
7.1 A sample of not less than 0.5 pt (236.6 mL) shall be
furnished with a duplicate sample.
taken at random from not less than 1% of the seller’s shipping
containers,providedeachpackagecontainsnotlessthan10gal
5. Cake Soaps, Flake and Powdered Soap Products
(37.9 L). In the case of smaller containers, a sample of not less
When Packed in Cans or Cartons
than0.5ptshallbetakenatrandomfromeachlotofcontainers
5.1 One cake (can or carton) shall be taken at random from
totaling not more than 1000 gal (3785.4 L) or fraction thereof.
not less than 1% of the seller’s shipping containers, provided
Thegrosssampleshallinallcasesconsistofnotlessthanthree
eachpackagecontainsnotlessthan50lb(22.7kg).Inthecase
samples of 0.5 pt each taken at random from separate contain-
of smaller containers, a cake (can or carton) shall be taken at
ers.Beforedrawingthesamplefromthecontainerselected,the
randomfromeachlotofcontainerstotalingnotmorethan5000
contents of the container shall be thoroughly agitated. The
lb (2268 kg), or fraction thereof. The gross sample shall in all
inspector shall thoroughly mix the gross sample, place it in
casesconsistofnotlessthanthreecakes(cansorcartons)taken
clean, dry cans or bottles, which shall be completely filled and
at random from separate containers. To illustrate, if a total
securely stoppered with clean corks or caps, then sealed,
shipment consists of 70 000 lb, all in 1400 containers weigh-
marked, and sent to the laboratory for test.
ing 50 lb each, then 14 containers are chosen at random and
8. Paste Soap Products
one cake taken from each for a total sample of 14 cakes. If a
total shipment of 70 000 lb includes containers weighing less
8.1 When Packed in Cans or Cartons of 5 lb (2.27 kg) or
than 50 lb, then the shipment must be divided into 14 lots of
Less—Onecanorcartonshallbetakenatrandomfromnotless
containersweighingapproximately5000lbeach,andonecake
than 1% of the seller’s shipping containers, provided each
taken from each lot, again for a total sample size of 14 cakes.
package contains not less than 50 lb (22.7 kg). In the case of
Thegrosssampleshallinallcasesconsistofnotlessthanthree smaller containers, a can or carton shall be taken at random
cakes (cans or cartons) taken at random from separate contain-
from each lot of containers totaling not more than 5000 lb
ers. In the case of very large lots where the sample drawn as (2268 kg) or fraction thereof. The gross sample shall in all
above will amount to more than 20 lb (9.1 kg), the percentage
cases consist of not less than three cans or cartons taken at
ofpackagessampledshallbereducedsothattheamountdrawn random from separate containers. In the case of very large lots
shall not exceed 20 lb. The individual cakes (cans or cartons)
where the sample drawn as above will amount to more than 20
shall be sealed at once in moisture-proof containers such as
lb (9.1 kg), the percentage of packages sampled shall be
polyethylene bags, or tightly wrapped in paraffined paper and
reduced so that the amount drawn shall not exceed 20 lb. The
sealed by rubbing the edges with a heated iron. The inspector
samples shall be wrapped, sealed, marked, and sent to the
shall accurately weigh each wrapped cake (can or carton), and
laboratory for test.
record its weight and the date of weighing on the wrapper.The
8.2 When Packed in Bulk—A trier sample of not less than
wrapped cakes (cans or cartons) shall be placed in an airtight
0.5 lb (227 g) shall be taken at random from not less than 1%
container, which should be nearly filled, and which shall then
of the seller’s shipping containers, provided each package
be sealed, marked, and sent to the laboratory for test. Samples
contains not less than 50 lb. In the case of smaller containers,
shall be kept cool until tested.
a trier sample of not less than 0.5 lb shall be taken at random
from each lot of containers totaling not more than 5000 lb or
6. Flake and Powdered Soap Products When in Bulk
fraction thereof. The gross sample shall in all cases consist of
6.1 A grab sample of not less than 0.5 lb (227 g) shall be
not less than three 0.5-lb samples, each taken at random from
taken at random from not less than 1% of the seller’s shipping separate containers. With very large lots where the sample
containers,providedeachpackagecontainsnotlessthan100lb drawn as above will amount to more than 10 lb (4.5 kg), the
(45.4 kg). In the case of smaller containers, a grab sample of percentage of packages sampled shall be reduced so that the
not less than 0.5 lb shall be taken at random from each lot of amount drawn shall not exceed 10 lb. The inspector shall
containers totaling not more than 10 000 lb (4536 kg) or
fraction thereof. The gross sample shall in all cases consist of
A trier sample is obtained by inserting a trier into the material. A trier is a
notlessthanthreegrabsamplesof0.5lbeachtakenatrandom
1 3
half-round steel cylinder ⁄2 to ⁄4 in. (12.7 to 19.1 mm) in diameter, 6 to 36 in. (152
to914mm)inlength,pointedononeendandhavingagriphandleontheotherend.
Afterinsertion,thetrieristurnedtwoorthreetimes,anduponremovalacoreofthe
Annual Book of ASTM Standards, Vol 14.03. material being sampled is obtained.
D460–91 (1997)
promptly place the gross sample in a clean, dry, airtight and 9.2 Powdered and Chip Soaps—Rapidly disintegrate and
watertight container, which shall be filled, sealed, marked, and mix the sample of powdered, flake, or chip soap. If desired,
sent to the laboratory for test.
quarter down to about 1 lb (454 g). Weigh at once all portions
for analysis, preserving the remainder in an airtight container
9. Preparation of Samples
in a cool place.
9.1 Cake Soap—Grind all bars through a suitable food
9.3 Liquid Soap—No preparation of the sample of liquid
chopper. In the case of large samples, it is permissible to
soap, other than a thorough mixing, is necessary unless it is
quarterthebarsandgrindonequarterfromeachbar.However,
received during very cold weather, when it should be allowed
each ground sample should consist of at least 3 lb (1.36 kg).
to stand at least 1 h after it has warmed to room temperature
Mix all ground samples thoroughly on a clean, dry, nonabsor-
(20 to 30°C) before it is tested, particularly for its lathering
bent, impervious surface with a spatula. Divide into four
qualities.
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
(0.91 kg). Place this portion in a clean, dry sample container. lb (454 g). Weigh at once all portions for analysis, preserving
Closetightlyandlabelcompletelyforidentification.Thisisthe the remainder in an airtight container in a cool place.
sample for analysis and must be preserved in a cool dry place.
METHODS FOR CHEMICALANALYSIS
10. Hazards must be made if accurate results are desired. These exceptions
include the following:
10.1 Precaution—All reagents and chemicals should be
13.1.1 For soaps containing appreciable amounts of sodium
handled with care. Before using any chemical, read and follow
silicate, the distillation method (Sections 15-18) is preferred.
all safety precautions and instructions on the manufacturer’s
13.1.2 Soaps of linseed and other oxidizing oils absorb
label. Clean up any spill immediately. Consult the Material
oxygen, and if the oven method is used may gain weight near
Safety Data Sheet for specific handling and disposal informa-
the end of the test. Therefore, either an inert atmosphere or
tion.
vacuum oven should be used. The distillation method is also
10.2 Use of glass wool in place of asbestos cloth is
applicable to these types of soap.
recommended where applicable.
13.1.3 Soaps containing appreciable amounts of glycerin,
11. Purity of Reagents
such as cold-made and semiboiled (including paste soaps),
11.1 Purity of Reagents—Reagent grade chemicals shall be usually give high results by the oven method. The distillation
method is preferred for most accurate results on these types of
used in all tests. Unless otherwise indicated, it is intended that
all reagents shall conform to the specifications of the Commit- soaps.
tee onAnalytical Reagents of theAmerican Chemical Society,
7 Method A—Matter Volatile at 105°C (Oven Method)
where such specifications are available. Other grades may be
used, provided it is first ascertained that the reagent is of
14. Procedure
sufficiently high purity to permit its use without lessening the
14.1 Weigh 5 6 0.01 g of the sample in a porcelain or glass
accuracy of the determination.
dish about 6 to 8 cm in diameter and about 2 to 4 cm in depth,
11.2 Unlessotherwiseindicated,referencestowatershallbe
and dry to constant weight in an air oven at a temperature of
understood to mean Type III reagent water conforming to
105 6 2°C. Constant weight is attained when successive
Specification D1193.
heating for 1-h periods shows a loss (or gain) of not more than
12. Duplicate Tests
0.1%.
12.1 When a determination shows nonconformity with the
Method B—Distillation Method
specifications a duplicate test shall be made.
15. Apparatus
MOISTURE
15.1 The apparatus required consists of a glass flask heated
13. Choice of Test Method
by suitable means and provided with a reflux condenser
13.1 The oven method described in Section 14 is generally
discharging into a trap and connected to the flask. The
applicable to all soaps, but certain exceptions to this method
connections between the trap and the condenser and flask shall
beinterchangeablegroundjoints.Thetrapservestocollectand
measure the condensed water and to return the solvent to the
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
flask.Asuitable assem
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