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ASTM D6174-01(2006)

(Test Method)

Standard Test Method for Inorganic Sulfate in Surfactants by Potentiometric Lead Titration (Withdrawn 2015)

Standard Test Method for Inorganic Sulfate in Surfactants by Potentiometric Lead Titration (Withdrawn 2015)

SIGNIFICANCE AND USE
Anionic surfactants, such as those listed in 1.1, commonly are used in detergent formulations. Their acceptability for use depends on their purity. Sulfate content, as measured by this test method, can be used to estimate the purity of an anionic surfactant under test.
SCOPE
1.1 This test method describes a potentiometric titration procedure for determining the inorganic sulfate content of surfactants. It is intended for the analysis of -olefin sulfonates, alkane sulfonates, alcohol sulfates, alcohol ether sulfates, alkylbenzenesulfonates, and the like.
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.
WITHDRAWN RATIONALE
This test method describes a potentiometric titration procedure for determining the inorganic sulfate content of surfactants.
Formerly under the jurisdiction of Committee D12 on Soaps and Other Detergents, this test method was withdrawn in January 2015 in accordance with section 10.6.3 of the Regulations Governing ASTM Technical Committees, which requires that standards shall be updated by the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Withdrawn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-Jan-2006
Withdrawal Date
12-Jan-2015
ICS
71.040.40 - Chemical analysis
Technical Committee
D12 - Soaps and Other Detergents
Drafting Committee
D12.12 - Analysis and Specifications of Soaps, Synthetics, Detergents and their Components
Current Stage
Ref Project

Relations

Replaces
ASTM D6174-01 - Standard Test Method for Inorganic Sulfate in Surfactants by Potentiometric Lead Titration
Effective Date
01-Feb-2006

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ASTM D6174-01(2006) - Standard Test Method for Inorganic Sulfate in Surfactants by Potentiometric Lead Titration (Withdrawn 2015)ASTM D6174-01(2006) - Standard Test Method for Inorganic Sulfate in Surfactants by Potentiometric Lead Titration (Withdrawn 2015)
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ASTM D6174-01(2006) - Standard Test Method for Inorganic Sulfate in Surfactants by Potentiometric Lead Titration (Withdrawn 2015)
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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: D6174 − 01(Reapproved 2006)
Standard Test Method for
Inorganic Sulfate in Surfactants by Potentiometric Lead
Titration
This standard is issued under the fixed designation D6174; 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 forusedependsontheirpurity.Sulfatecontent,asmeasuredby
this test method, can be used to estimate the purity of an
1.1 This test method describes a potentiometric titration
anionic surfactant under test.
procedure for determining the inorganic sulfate content of
surfactants.Itisintendedfortheanalysisofα-olefinsulfonates,
6. Apparatus
alkane sulfonates, alcohol sulfates, alcohol ether sulfates,
6.1 Potentiometric Titration Assembly, consisting of an
alkylbenzenesulfonates, and the like.
automatic titrator fitted with a lead ion-selective electrode, a
1.2 This standard does not purport to address all of the
double-junction reference electrode, and a 10-mL buret. The
safety concerns, if any, associated with its use. It is the
reference electrode should be filled with the standard inner and
responsibility of the user of this standard to establish appro-
outer filling solutions supplied with it. A TFE-fluorocarbon-
priate safety and health practices and determine the applica-
coated magnetic stirring bar should be used for mixing during
bility of regulatory limitations prior to use. Material Safety
titration, with a separate magnetic stirring motor if the autoti-
Data Sheets are available for reagents and materials. Review
trator is not so equipped.
them for hazards prior to usage.
NOTE 1—Proper care of the lead-selective electrode is essential for
2. Referenced Documents obtaining high-quality titration curves. Follow manufacturer’s instruc-
tions.
2.1 ASTM Standards:
D1193 Specification for Reagent Water
7. Reagents
7.1 Glacial Acetic Acid.
3. Terminology
7.2 Lead Nitrate, reagent grade.
3.1 Definitions of Terms Specific to This Standard:
3.1.1 inorganic sulfate, n—sulfate species present as sulfu-
7.3 Sodium Sulfate, anhydrous, reagent grade.
ric acid, ionic salts of this acid, or mixtures of these.
7.4 Sodium Perchlorate, reagent grade.
4. Summary of Test Method
7.5 Ethanol, denatured, formula 3A.
4.1 A surfactant sample containing inorganic sulfate is
7.6 Water, Type III reagent water conforming to Specifica-
titrated in ethanolic medium with a standard lead solution.
tion D1193.
Lead sulfate precipitate is formed during the titration. Ethanol
8. Preparation of Standard Solutions
and sodium perchlorate are present to decrease the solubility of
lead sulfate, thus sharpening the endpoint.Acetic acid is added
8.1 10 % Acetic Acid—Dilute glacial acetic acid 1/10 with
to remove possible interference from carbonate. The endpoint
water.
is signaled by an increase in lead ion activity, as measured by
8.2 Lead Titrant, 0.05 M—Dissolve 16.6 g lead nitrate in
a lead-selective electrode.
300 mL water. Pour into a 1-L bottle and fill with 3A ethanol.
Mix well. Standardize according to 9.1.
5. Significance and Use
8.3 Sulfate Standard, 0.05 M—Dry 5 g anhydrous sodium
5.1 Anionic surfactants, such as those listed in 1.1, com-
sulfate at 110°C for 1 h. Accurately weigh about 3.5 g into a
monly are used in detergent formulations. Their acceptability
1 2
This test method is under the jurisdiction of ASTM Committee D12 on Soaps Reagent Chemicals, American Chemical Society Specifications, American
and Other Detergents and is the direct responsibility of Subcommittee D12.12 on Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Analysis of Soaps and Synthetic Detergents. listed by the American Chemical Society, see Analar Standards for Laboratory
Current edition approved Feb. 1, 2006. Published March 2006. Originally Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
approved in 1997. Last previous edition approved in 2001 as D6174-01. DOI: and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
10.1520/D6174-01R06. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D6174 − 01 (2006)
500-mLvolumetric flask, dilute to volume with water, and mix 10.2 Transfer a portion of test surfactant, equivalent to
to dissolve. Calculate the exact concentration as follows: 30–50 mg sodium sulfate, to a 50-mL beaker. For example, if
a surfactant is expected to contain 1 % sodium sulfate, weigh
G
5 Molarity (1)
3–5 g to analytical precision into
...

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1.2 The procedures in this guide are focused on “matrix spike” preparation, analysis, results, and interpretation. The applicability of these procedures to the preparation of calibration standards, calibration check standards, laboratory control standards, reference materials, and other quality control materials by spiking is incidental. A sample (the matrix) is fortified (spiked) with the analyte of interest for a variety of analytical and quality control purposes. While the spiking of multiple sample test portions is discussed, the method of standard additions is not covered.  
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5.1 Chloride present in aviation turbine fuel can originate from refinery salt drier carryover or possibly from seawater contamination (for example, product transferred by barge). Elevated chloride levels have caused corrosive and abrasive wear of aircraft fuel control systems leading to engine failure.4
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1.1 This test method covers a rapid means of determining chloride content of aviation turbine fuel. This methodology is applicable for chloride concentrations between 0 mg/L to 0.5 mg/L. This methodology will not detect chlorine originating from chlorinated organic compounds (that is, covalent bond).  
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Standard Test Method for Water Using Volumetric Karl Fischer Titration

SIGNIFICANCE AND USE
4.1 Titration techniques using KF reagent are one of the most widely used for the determination of water.  
4.2 Although the volumetric KF titration can determine low levels of water, it is generally accepted that coulometric KF titrations (see Test Method E1064) are more accurate for routine determination of very low levels of water. As a general rule, if samples routinely contain water concentrations of 500 mg/kg or less, the coulometric technique should be considered.  
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4.4 Water can be determined directly in the presence of the following types of compounds:    
Organic Compounds  
Acetals  
Ethers  
Acids (Note 1)  
Halides  
Acyl halides  
Hydrocarbons (saturated and unsaturated)  
Alcohols  
Ketones, stable (Note 4)  
Aldehydes, stable (Note 2)  
Nitriles  
Amides  
Orthoesters  
Amines, weak (Note 3)  
Peroxides (hydro, dialkyl)  
Anhydrides  
Sulfides  
Disulfides  
Thiocyanates  
Esters  
Thioesters  
Inorganic Compounds  
Acids (Note 5)  
Cupric oxide  
Acid oxides (Note 6)  
Desiccants  
Aluminum oxides  
Hydrazine sulfate  
Anhydrides  
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Barium dioxide  
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1.4 Review the current Safety Data Sheets (SDS) for detailed information concerning toxicity, first aid procedures, and safety precautions for chemicals used in this test procedure.  
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5.1 High levels of antimony are commonly used in flame retardant formulations for various materials. NAA is a test method that can be useful for verifying these levels and, for other materials, NAA can also be useful in establishing the amount of low level contamination, if any, with high sensitivity and high precision.  
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5.1 This test method is useful for the determination of elemental concentrations in the range of approximately 0.1 µgg-1 to 10 percent (%) (See Table X1.1) in soda-lime glass samples (7 and 8). A standard test method can aid in the interchange of data between laboratories and in the creation and use of glass databases.  
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5.1 Organic as well as inorganic chlorine compounds can prove harmful to equipment and reactions in processes involving hydrocarbons.  
5.2 Maximum chloride levels are often specified for process streams and for hydrocarbon products.  
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1.1 This test method covers the determination of organic chloride in aromatic hydrocarbons, their derivatives, and related chemicals.  
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SIGNIFICANCE AND USE
5.1 This test method is useful in determining the extrapolated onset temperature, the peak heat flow temperature and the heat of reaction of a material. Any onset temperature determined by this test method is not valid for use as the sole information used for determination of storage or processing conditions.  
5.2 This test method is useful in determining the fraction of a reaction that has been completed in a sample prior to testing. This fraction of reaction that has been completed can be a measure of the degree of cure of a thermally reactive polymer or can be a measure of decomposition of a thermally reactive material upon aging.  
5.3 The heat of reaction values may be used in Practice E1231 to determine hazard potential figures-of-merit Explosion Potential and Shock Sensitivity.  
5.4 This test method may be used in research, process control, quality assurance, and specification acceptance.
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1.1 This test method determines the exothermic heat of reaction of thermally reactive chemicals or chemical mixtures, using milligram specimen sizes, by differential scanning calorimetry. Such reactive materials may include thermally unstable or thermoset materials.  
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1.3 This test method may be performed on solids, liquids or slurries.  
1.4 The applicable temperature range of this test method is 25 °C to 600 °C.  
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.6 This standard is related to Test Method E537, but provides additional information.  
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ASTM
ASTM E2403-23(Test Method)
Standard Test Method for Sulfated Ash of Organic Materials by Thermogravimetry

SIGNIFICANCE AND USE
5.1 The sulfated ash value indicates the level of known metal-containing additives or impurities in an organic material. When phosphorus is absent, barium, calcium, magnesium, sodium and potassium are converted to their sulfates. Tin and zinc are converted to their oxides.  
5.2 This test method may be used for research and development, specification acceptance, and quality assurance purposes.
SCOPE
1.1 This test method describes the determination of sulfated ash content (sometimes called residue-on-ignition) of organic materials by thermogravimetry. This test method converts common metals found in organic materials (such as sodium, potassium, lithium, calcium, magnesium, zinc, and tin) into their sulfate salts permitting estimation of their total content as sulfates or oxides. The range of this test method is from 0.1 % to 100 % metal content.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

  • Standard
    4 pages
    English language
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  • Standard
    4 pages
    English language
    sale 15% off