ASTM D500-95(2009)
(Test Method)Standard Test Methods of Chemical Analysis of Sulfonated and Sulfated Oils
Standard Test Methods of Chemical Analysis of Sulfonated and Sulfated Oils
ABSTRACT
These test methods cover the chemical analysis of sulfonated and sulfated oils. Water by distillation with volatile solvent and moisture and volatile matter by hot-plate shall be tested to meet the requirements prescribed. Titration test, extraction-titration test, and ash-gravimetric test shall be performed to meet the requirements specified. Total desulfated fatty matter, total active ingredients, unsaponifiable non-volatile matter, inorganic salts, total alkalinity, and total ammonia shall be tested to meet the requirements prescribed. In the absence of ammonium or triethanolamine soaps test method, brine test method, and in the presence of ammonium or triethanolamine soaps test method shall be performed to meet the requirements prescribed. Water-immiscible organic solvents volatile with steam shall be tested to meet the requirements prescribed.
SCOPE
1.1 These test methods cover the chemical analysis of sulfonated and sulfated oils. The analytical procedures appear in the following order:
Section Moisture: Test Method A. Water by Distillation with Volatile Solvent4-9 Test Method B. Moisture and Volatile Matter by Hot-Plate Method10-14 Organically Combined Sulfuric Anhydride: Test Method A. Titration Test15-19 Test Method B. Extraction-Titration Test20-24 Test Method C. Ash-Gravimetric Test (in the Presence of True
Sulfonates)25-28 Total Desulfated Fatty Matter29-32 Total Active Ingredients33-36 Unsaponifiable Nonvolatile Matter37-41 Inorganic Salts42-46 Total Alkalinity47-49 Total Ammonia50-52 Acidity as Free Fatty Acids or Acid Number: Test Method A. In the Absence of Ammonium or Triethanolamine Soaps53-56 Test Method B. In the Presence of Dark Colored Oils but in the
Absence of Ammonium or Triethanolamine Soaps (Brine Test)57-60 Test Method C. In the Presence of Ammonium or Triethanolamine Soaps61-63 Water-Immiscible Organic Solvents Volatile with Steam64-70
1.2 The values stated in inch-pound units are to be regarded as the standard. The metric equivalents of inch-pound units may be approximate.
1.3 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.
4.1 This test method covers the determination of water existing in a sample of sulfonated or sulfated oil, or both, by distilling the sample with a volatile solvent. The method is applicable only to sulfonated and sulfated oils that do not contain the following: mineral acids, free sulfonic acids, or free sulfuric acid esters; or alkali hydroxides, carbonates or acetates; or alcohol, glycerin, diethylene glycol, acetone, or other water-miscible volatile compounds.
10.1 This test method covers the determination of the percentage of water and other compounds volatile at about 100°C existing in a sample of sulfonated or sulfated oil, or both, by rapid evaporation. The test method is applicable only to sulfonated and sulfated oils that do not contain the following: mineral acids, free sulfonic acids or free sulfuric acid esters, ammonia, acetic acid or similar volatile acids, alkali hydroxides, carbonates, acetates or similar salts that may react with oleic acid at elevated temperatures liberating volatile acids, or glycerin, diethylene glycol, xylene, or other compounds of similar volatility.
15.1 This test method covers the determination of the organically combined sulfuric anhydride existing in a sample of sulfated oil by boiling the sample with sulfuric acid and determining the acidity of the reaction mixture. This method is applicable only to oils that split off their combined SO3 upon boiling with mineral acids and that do not contain compounds that cannot be accurately titrated in wat...
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Designation: D500 − 95(Reapproved 2009)
Standard Test Methods of
1
Chemical Analysis of Sulfonated and Sulfated Oils
This standard is issued under the fixed designation D500; 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 2. Referenced Documents
2
1.1 These test methods cover the chemical analysis of 2.1 ASTM Standards:
sulfonated and sulfated oils. The analytical procedures appear D1193Specification for Reagent Water
in the following order:
3. Purity of Reagents
Section
3.1 Purity of Reagents—Reagent grade chemicals shall be
Moisture:
used in all tests. Unless otherwise indicated, it is intended that
Test Method A. Water by Distillation with Volatile Solvent 4–9
all reagents shall conform to the specifications of the Commit-
Test Method B. Moisture and Volatile Matter by Hot-Plate Method 10–14
Organically Combined Sulfuric Anhydride:
tee onAnalytical Reagents of theAmerican Chemical Society,
Test Method A. Titration Test 15–19
3
where such specifications are available. Other grades may be
Test Method B. Extraction-Titration Test 20–24
Test Method C. Ash-Gravimetric Test (in the Presence of True 25–28 used, provided it is first ascertained that the reagent is of
Sulfonates)
sufficiently high purity to permit its use without lessening the
Total Desulfated Fatty Matter 29–32
accuracy of the determination.
Total Active Ingredients 33–36
Unsaponifiable Nonvolatile Matter 37–41
3.2 Purity of Water—Unless otherwise indicated, references
Inorganic Salts 42–46
towatershallbeunderstoodtomeanreagentwaterconforming
Total Alkalinity 47–49
Total Ammonia 50–52
to Specification D1193.
Acidity as Free Fatty Acids or Acid Number:
Test Method A. In the Absence of Ammonium or Triethanolamine 53–56
MOISTURE
Soaps
Test Method B. In the Presence of Dark Colored Oils but in the 57–60
Method A. Water by Distillation with Volatile Solvent
Absence of Ammonium or Triethanolamine Soaps (Brine Test)
Test Method C. In the Presence of Ammonium or Triethanolamine 61–63
Soaps 4. Scope
Water-Immiscible Organic Solvents Volatile with Steam 64–70
4.1 This test method covers the determination of water
1.2 The values stated in inch-pound units are to be regarded
existing in a sample of sulfonated or sulfated oil, or both, by
as the standard. The metric equivalents of inch-pound units
distilling the sample with a volatile solvent. The method is
may be approximate.
applicable only to sulfonated and sulfated oils that do not
1.3 This standard does not purport to address all of the
containthefollowing:mineralacids,freesulfonicacids,orfree
safety concerns, if any, associated with its use. It is the
sulfuric acid esters; or alkali hydroxides, carbonates or ac-
responsibility of the user of this standard to establish appro-
etates;oralcohol,glycerin,diethyleneglycol,acetone,orother
priate safety and health practices and determine the applica-
water-miscible volatile compounds.
bility of regulatory limitations prior to use. Material Safety
Data Sheets are available for reagents and materials. Review
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
them for hazards prior to usage.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
1
These test methods are under the jurisdiction of ASTM Committee D12 on the ASTM website.
3
SoapsandOtherDetergentsandisthedirectresponsibilityofSubcommitteeD12.12 Reagent Chemicals, American Chemical Society Specifications, American
on Analysis and Specifications of Soaps, Synthetics, Detergents and their Compo- Chemical Society, Washington, DC. For suggestions on the testing of reagents not
nents. listed by the American Chemical Society, see Analar Standards for Laboratory
Current edition approved Oct. 1, 2009. Published December 2009. Originally Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
approved in 1937. Last previous edition approved in 2003 as D500–95(2003). and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
DOI: 10.1520/D0500-95R09. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
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D500 − 95 (2009)
5. Apparatus each 1-mL line numbered (5 mL at top). The error in any
indicated capacity may not be greater than 0.05 mL.
5.1 The apparatus required consists of a glass flask heated
by suitable means and provided with a reflux condenser
6. Reagents
discharging into a trap and connected to the flask. The
6.1
...
This document is not anASTM standard and is intended only to provide the user of anASTM 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: D500 – 95 (Reapproved 2003)
Standard Test Methods of
1
Chemical Analysis of Sulfonated and Sulfated Oils
This standard is issued under the fixed designation D500; 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
1.1 These test methods cover the chemical analysis of sulfonated and sulfated oils. The analytical procedures appear in the
following order:
Section
Moisture:
Test Method A. Water by Distillation with Volatile Solvent 4-9
Test Method B. Moisture and Volatile Matter by Hot-Plate Method 10-14
Organically Combined Sulfuric Anhydride:
Test Method A. Titration Test 15-19
Test Method B. Extraction-Titration Test 20-24
Test Method C. Ash-Gravimetric Test (in the Presence of True 25-28
Sulfonates)
Total Desulfated Fatty Matter 29-32
Total Active Ingredients 33-36
Unsaponifiable Nonvolatile Matter 37-41
Inorganic Salts 42-46
Total Alkalinity 47-49
Total Ammonia 50-52
Acidity as Free Fatty Acids or Acid Number:
Test Method A. In the Absence of Ammonium or Triethanolamine 53-56
Soaps
Test Method B. In the Presence of Dark Colored Oils but in the 57-60
Absence of Ammonium or Triethanolamine Soaps (Brine Test)
Test Method C. In the Presence of Ammonium or Triethanolamine 61-63
Soaps
Water-Immiscible Organic Solvents Volatile with Steam 64-70
1.2 The values stated in inch-pound units are to be regarded as the standard. The metric equivalents of inch-pound units may
be approximate.
1.3 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
2.1 ASTM Standards:
D1193 Specification for Reagent Water
3. Purity of Reagents
3.1 Purity of Reagents—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
3
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.
1
These test methods are under the jurisdiction of ASTM Committee D12 on Soaps and Other Detergents and is the direct responsibility of Subcommittee D12.12 on
Analysis of Soaps and Synthetic Detergents.
Current edition approved April 15, 1995. Published June 1995. Originally published as D500–37. Last previous edition D500–89. DOI: 10.1520/D0500-95R039.
2
Annual Book of ASTM Standards, Vol 11.01.
3
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. Pharmaceutical Convention, Inc. (USPC), Rockville, MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1
---------------------- Page: 1 ----------------------
D500 – 95 (2003)
3.2 Purity of Water—Unless otherwise indicated, references to water shall be understood to mean reagent water conforming to
Specification D1193.
MOISTURE
Method A. Water by Distillation with Volatile Solvent
4. Scope
4.1 This test method covers the determination of water existing in a sample of sulfonated or sulfated oil, or both, by distilling
the sample with a volatile solvent.The method is applicable only to sulfonated and sulfated oils that do not contain the following:
mineral acids, free sulfonic acids, or free sulfuric acid esters; or alkali hydroxides, carbonates or acetates; or alcohol, glycerin,
diethylene glycol, acetone, or other water-miscible volatile compounds.
5. Apparatus
5.1 The apparatus required consists 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 interchangea
...
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