ASTM D820-93(2009)
(Test Method)Standard Test Methods for Chemical Analysis of Soaps Containing Synthetic Detergents
Standard Test Methods for Chemical Analysis of Soaps Containing Synthetic Detergents
ABSTRACT
These test methods detail the standard procedures for the chemical analysis of soaps containing synthetic detergents. The analytical procedures include the determination of the following chemical properties and substances: moisture and other matter volatile at a specified temperature; free alkali or free acid; anhydrous, salt-free soda soap; alcohol-soluble matter; matter insoluble in water; total alkalinity of matter insoluble in alcohol (alkaline salts); sodium silicate; phosphates; phosphates by colorimetric method using molybdenum blue); unsaponified and unsaponifiable matter; free fatty matter; chlorides in alcohol-soluble matter; rosin by McNicoll method; synthetic detergent by difference; and neutral inorganic salts.
SCOPE
1.1 These test methods cover procedures for the chemical analysis of soaps containing synthetic detergents.
1.2 The analytical procedures appear in the following order:
Sections Moisture and Other Matter Volatile at 105°C (Oven Method) 5 and 6 Free Alkali or Free Acid 7 and 8 Anhydrous, Salt-Free, Soda Soap 9-12 Alcohol-Soluble Matter13 and 14 Matter Insoluble in Water15 Total Alkalinity of Matter Insoluble in Alcohol (Alkaline Salts)16 and 17 Sodium Silicate18-20 Phosphates21-28 Phosphate (Colorimetric Method Using Molybdenum Blue)29-34 Unsaponified and Unsaponifiable Matter35-39 Free Fatty Matter40 Chlorides in Alcohol-Soluble Matter41-43 Rosin (McNicoll Method)44-47 Synthetic Detergent (by Difference)48 Neutral, Inorganic Salts49
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
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.
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D820 − 93(Reapproved 2009)
Standard Test Methods for
Chemical Analysis of Soaps Containing Synthetic
Detergents
This standard is issued under the fixed designation D820; 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.
1. Scope D216Method of Test for Distillation of Natural Gasoline
(Withdrawn 1988)
1.1 These test methods cover procedures for the chemical
D459Terminology Relating to Soaps and Other Detergents
analysis of soaps containing synthetic detergents.
D875Method for Calculating of Olefins and Aromatics in
1.2 Theanalyticalproceduresappearinthefollowingorder:
Petroleum Distillates from Bromine Number and Acid
Absorption (Withdrawn 1984)
Sections
D1193Specification for Reagent Water
Moisture and Other Matter Volatile at 105°C (Oven Method) 5 and 6
D1768Test Method for Sodium Alkylbenzene Sulfonate in
Free Alkali or Free Acid 7 and 8
Anhydrous, Salt-Free, Soda Soap 9–12 Synthetic Detergents by Ultraviolet Absorption
Alcohol-Soluble Matter 13 and 14
D2357for Qualitative Classification of Surfactants by Infra-
Matter Insoluble in Water 15 and 15
red Absorption
Total Alkalinity of Matter Insoluble in Alcohol (Alkaline Salts) 16 and 17
D2358TestMethodforSeparationofActiveIngredientfrom
Sodium Silicate 18–20
Phosphates 21–28
Surfactant and Syndet Compositions
Phosphate (Colorimetric Method Using Molybdenum Blue) 29–34
D3049Test Method for Synthetic Anionic Ingredient by
Unsaponified and Unsaponifiable Matter 35–39
Free Fatty Matter 40 Cationic Titration
Chlorides in Alcohol-Soluble Matter 41–43
Rosin (McNicoll Method) 44–47
3. Terminology
Synthetic Detergent (by Difference) 48
Neutral, Inorganic Salts 49
3.1 Definitions:
1.3 The values stated in SI units are to be regarded as
3.2 The term synthetic detergent in these test methods is
standard. No other units of measurement are included in this
defined in accordance with Terminology D459, as follows:
standard.
3.3 synthetic detergent—a detergent produced by chemical
1.4 This standard does not purport to address all of the
synthesis and comprising an organic composition other than
safety problems, if any, associated with its use. It is the
soap.
responsibility of the user of this standard to establish appro-
3.4 Fordefinitionsofothertermsusedinthesetestmethods,
priate safety and health practices and determine the applica-
refer to Terminology D459.
bility of regulatory limitations prior to use.
4. Purity of Reagents and Materials
2. Referenced Documents
4.1 Purity of Reagents—Reagent grade chemicals shall be
2.1 ASTM Standards:
used in all tests. Unless otherwise indicated, it is intended that
all reagents shall conform to the specifications of the Commit-
tee onAnalytical Reagents of theAmerican Chemical Society,
where such specifications are available. Other grades may be
used, provided it is first ascertained that the reagent is of
These test methods are under the jurisdiction of ASTM Committee D12 on
Soaps and Other Detergentsand are the direct responsibility of Subcommittee
D12.12 on Analysis and Specifications of Soaps, Synthetics, Detergents and their
Components. The last approved version of this historical standard is referenced on
Current edition approved Oct. 1, 2009. Published December 2009. Originally www.astm.org.
approved in 1945. Last previous edition approved in 2003 as D820–93(2003). Reagent Chemicals, American Chemical Society Specifications, American
DOI: 10.1520/D0820-93R09. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
For referenced ASTM standards, visit the ASTM website, www.astm.org, or listed by the American Chemical Society, see Analar Standards for Laboratory
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Standards volume information, refer to the standard’s Document Summary page on and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
the ASTM website. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D820 − 93 (2009)
sufficiently high purity to permit its use without lessening the 9.2 Stokes Flask, 100-mL, round-bottom (with the bottom
accuracy of the determination. blownout),sealedontoa150-mLErlenmeyerflask.Adiagram
of the Stokes flask is shown in Fig. 1.
4.2 Unless otherwise indicated, references to water shall be
understood to mean reagent water conforming to Specification 9.3 Siphon, consisting of a two-hole rubber stopper fitted
D1193. with small-diameter glass tubing as shown in Fig. 2.
MOISTURE AND OTHER MATTER VOLATILE AT
10. Reagents
105°C (OVEN METHOD)
10.1 Ethyl Alcohol, Neutral (95%) —Freshly boiled, re-
agent grade, ethyl alcohol, 95 % or higher, neutral to
5. Apparatus
phenolphthalein, and containing only volatile denaturants, 95
5.1 Dish—A porcelain or glass dish about 6 to 8 cm in
mL, plus 5 mL of water.
diameter and about 2 to 4 cm in depth will be required.
10.2 Methyl Orange Indicator Solution(1g/litre)—Dissolve
0.1 g of methyl orange in water and dilute to 100 mL.
6. Procedure
10.3 Petroleum Ether—The solvent used shall be of the
6.1 Weigh 5 6 0.01 g of the sample in the dish, and dry to
pentane type, containing a minimum amount of isopentane,
constant weight in an air oven at a temperature of 105 6 2°C.
isohexane, and hexane, and boiling in the range 35 to 60°C.
Constant weight is attained when heating for successive 1-h
A
Distillation test:
periods shows a loss (or gain) of not more than 0.1%.
Initial boiling point 35 to 38°C
Dry flask end point 52 to 60°C
NOTE 1—Because of its established use in the trade, the term weight is
Distilling under 54°C, min 95 %
employed in these methods in place of the technically correct term mass.
Distilling under 40°C, max 60 %
Specific gravity at 15.5/15.5°C (60/60°F) 0.630 to 0.660
FREE ALKALI OR FREE ACID
Color water-white
Doctor test sweet
7. Reagents Evaporation residue, 100 mL, max 0.0011 g
B
Copper-strip corrosion test noncorrosive
C
7.1 Ethyl Alcohol, Neutral (95%) —Freshly boiled, reagent
Unsaturated compounds trace only permitted
Residue in distilling flask neutral to methyl orange
grade, ethyl alcohol, 95 % or higher, neutral to
D
Blotter-strip odor test odorless within 12 min
phenolphthalein, and containing only volatile denaturants, 95
E
Aromatic compounds no nitrobenzene odor
mL, plus 5 mL of water.
Saponification value less than 1.0 mg KOH/100 mL
7.2 Phenolphthalein Indicator Solution (10 g/litre)—
A
The distillation test shall be made in accordance with Method D216. As a check
Dissolve1gof phenolphthalein in 50 mL of neutral ethyl
on the evaporation residue, 250 mL of the petroleum ether and 0.25 g of stearin or
alcohol (95%) and mix with 50 mL of water (see 7.1). other hard fat (previously brought to constant weight by heating) when dried as in
the actual determination (10.4) shall not show an increase in weight exceeding
0.003 g.
8. Procedure B
The copper-strip corrosion test shall be made by inserting a small polished
copper strip into the petroleum ether in the distilling flask. There should be no
8.1 Weigh 5 to 10 6 0.01 g of the sample into a 300-mL
appreciable darkening of the copper.
C
Erlenmeyer flask.Add 200 mLof neutral ethyl alcohol (95%).
Unsaturated compounds shall be determined by the method for determining
olefins described in Method D875.
Equip the flask with an air-cooled reflux condenser, and digest
thesampleonasteambathuntilthesoapisdissolved(seeNote
2). Remove the condenser, add 0.5 mL of the phenolphthalein
indicator solution, and titrate immediately with standard acid
or alkali. Calculate as NaOH, if alkaline, or as oleic acid, if J. T. Baker Analyzed Reagent 9268, or its equivalent, is suitable for this
purpose.
acid.
NOTE 2—In the analysis of soaps known to contain little or no alkaline
salts, it is unnecessary to filter the hot alcoholic soap solution. However,
the filtration should be carried out in all cases where alkaline salts such as
silicates, phosphates, borates, and similar salts are present, since these are
knowntoaffectthefreealkalidetermination.Freealkalifiguresinsoapor
surfactant mixtures containing borax are unreliable, due to solubility of
borax in hot alcohol.
ANHYDROUS, SALT-FREE, SODA SOAP
9. Apparatus
9.1 Extraction Cylinder, 250-mL, graduated, glass-
stoppered, about 39 mm (1 ⁄2 in.) in diameter and about 35.5
cm (14 in.) in length.
Fischer Scientific A962, or its equivalent, is suitable for this purpose. FIG. 1 Stokes Flask
D820 − 93 (2009)
Stokes flask. Cool the cylinder or flask under tap water to a
temperaturenottoexceed25°C.Add50mLofpetroleumether
and allow to stand for ⁄2 h without shaking. Remove the
greater part of the fatty acids by drawing off the petroleum
ether layer as closely as possible, by means of a glass siphon,
into a 500-mL separatory funnel. Repeat the extractions five
more times with petroleum ether, using 50-mL portions, and
shaking the cylinder thoroughly each time.
NOTE 3—If an emulsion appears at this point, it may be broken by the
addition of 10 g of anhydrous Na SO .
2 4
11.3 Combine the petroleum ether extracts and wash with
smallportionsofdistilledwateruntilthewaterwashingsareno
longer acid to methyl orange indicator solution. Dry the
combined, washed, petroleum ether extracts with anhydrous
FIG. 2 Siphon Na SO ,andfilterthroughpaperintotheoriginaltared250-mL
2 4
beaker. Wash the separatory funnel with two small portions of
petroleum ether, filtering and adding the washings to the
D
Odor test: Immerse 1 in. of a strip of white unglazed blotting paper, approxi-
beaker.
mately 1 by 4 by 0.166 in. in size, in the petroleum ether for 30 s, remove the strip,
and allow to dry at room temperature in still air for 12 min.
11.4 Evaporate the petroleum ether extract on the steam
E
Aromatic compounds: Add 5 drops of petroleum ether to 40 drops of sulfuric acid
bath until about 1 mL remains. Then swirl manually until the
(H SO , sp gr 1.84) and 10 drops of nitric acid (HNO , sp gr 1.42) in a test tube,
2 4 3
warm for 10 min, allow to cool for 30 min, transfer to a shallow dish, and dilute with
lasttraceofsolventevaporatesandtheodorofpetroleumether
water.
isnolongerperceptible.Coolinadesiccatorandweighastotal
10.4 Phenolphthalein Indicator Solution (10 g/litre)—
fatty matter, which is defined as fatty and rosin acids plus
Dissolve1gof phenolphthalein in 50 mL of neutral ethyl
unsaponified and unsaponifiable fatty matter.
alcohol (95%) and then mix with 50 mL of water (see 10.1).
11.5 Dissolvethetotalfattymatterin50mLofneutralethyl
10.5 Sodium Hydroxide, Standard Solution (0.1 N)
alcohol(95%v)withwarming.Addphenolphthaleinindicator
—Prepare and standardize a 0.1 N sodium hydroxide (NaOH)
and titrate with 0.1 NaOH solution to a pink end point.
solution.
12. Calculations
10.6 Sodium Sulfate (Na SO ), anhydrous.
2 4
12.1 Calculate the percentage of anhydrous, salt-free, soda
10.7 SulfuricAcid, Standard(0.5N)—Prepareandstandard-
soap as follows:
ize a 0.5 N sulfuric acid (H SO ) solution.
2 4
A 5 G 2 F (1)
10.8 Sulfuric Acid (sp gr 1.84)—Concentrated sulfuric acid
(H SO ).
2 4
G 5 VN 30.022 1E /W 3100
@~~ ! ! #
10.9 Sulfur Acid (1+1)—Gradually pour 10 g of concen-
where:
trated sulfuric acid (H SO ) (sp gr 1.84) onto 10 g of cracked
2 4
A = weight percent of anhydrous, salt-free, soda soap,
ice made from distilled water, gently swirling the mixing
G = weight percent of soda soap plus unsaponified and
vessel;orgraduallypourtheaciddownthesidesofthemixing
unsaponifiable fatty matter,
vessel into an equal weight of water, swirling gently, while
F = weight percent of unsaponified and unsaponifiable
submersing the vessel in an ice bath.
fatty matter (Section 39),
V = millilitres of NaOH solution used in titration (11.5),
11. Procedure
N = normality of NaOH solution,
11.1 Weigh 2 6 0.001 g of the sample into a tared 250-mL
E = grams of extract (11.4), and
beaker.Add25mLofwaterand25mLofneutralethylalcohol
W = grams of sample (11.1), and
(95%),andwarmonthesteambathuntilsolutioniscomplete.
0.022 = net gain in milliequivalent weight from the conver-
Cool, add 5 drops of methyl orange indicator solution, and
sion of the fatty acid to the sodium salt by replace-
titrate with 0.5 N H SO to a pink color. Add 5 mL of H SO
ment of a proton with a sodium ion.
2 4 2 4
(1+1) in excess.
ALCOHOL-SOLUBLE MATTER
11.2 Transfer the contents of the beaker to a 250-mL
extraction cylinder or a Stokes flask, equipped with a siphon.
13. Reagents
Wash the beaker alternately with equal parts of hot water and
13.1 Ethyl Alcohol, Neutral (95%) —Freshly boiled, re-
hotethylalcohol(95%),addingthewashingstotheextraction
agent grade, ethyl alcohol, 95 % or higher, neutral to
cylinder or Stokes flask. Keep the total volume for extraction
phenolphthalein, and containing only volatile denaturants, 95
under 160 mL in the extraction cylinder, or within the
mL plus 5 mL of water.
constricted portion of the Stokes flask. Wash the beaker with a
small amount of petroleum ether to remove any traces of fatty 13.2 Ethyl Alcohol, Neutral (absolute) —Freshly boiled
acids and fatty matter and add to the extraction cylinder or absolute ethyl alcohol, neutral to phenolphthalein.
D820 − 93 (2009)
14. Procedure Na CO , % weight 5 106VN/20W (2)
2 3
14.1 Weigh 2 6 0.001 g of the sample into a 250-mL
where:
beaker.Add 100 mLof neutral ethyl alcohol (95%), cover the
V = millilitres of standard acid used,
beaker, and heat on the steam bath with frequent stirring and
N = normality of standard acid, and
maceration of the sample until completely disintegrated. Let
W = weight of sample (14.1), g
settle and filter the supernatant liquid through a tared Gooch
SODIUM SILICATE
crucible with a glass wool pad, with suction into a tared
300-mL Erlenmeyer flask, retaining as much of the residue as
18. Reagents
possible in the beaker. Repeat this extraction three times with
25-mL portions of hot neutral ethyl alcohol (95%), each time 18.1 Hydrochloric Acid (sp gr 1.19)—Concentrated hydro-
retaining as much of the residue as possible in the beaker. chloric acid (HCl).
Finally, evaporate any remaining alcohol and dissolve the
18.2 Hydrofluoric Acid (sp gr 1.15)—Prepare a solution of
residue in the smallest possible quantity of hot water (5 mL if
hydrofluoric acid (HF) having a specific gravity of 1.15.
sufficient). Reprecipitate the alcohol-insoluble matter by
18.3 Sulfuric A
...
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