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ASTM D4608-89(2009)

(Test Method)

Standard Test Method for Citrate in Detergents

Standard Test Method for Citrate in Detergents

SIGNIFICANCE AND USE
This test method is suitable in research, development, and manufacturing control to monitor the level of citrate, a sequestering agent, in powder and liquid detergents.
Accurate determination of sequestering agent is important in evaluating cost and performance of detergent products.
SCOPE
1.1 This test method covers a potentiometric titration procedure for the determination of citrate in liquid and powder detergents.
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 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. Specific safety precautions are given in Section 8.

General Information

Status
Historical
Publication Date
30-Sep-2009
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
Current Stage
Ref Project

Relations

Replaces
ASTM D4608-89(2003) - Standard Test Method for Citrate in Detergents
Effective Date
01-Oct-2009
Replaced By
ASTM D4608-89(2017) - Standard Test Method for Citrate in Detergents
Effective Date
01-Jan-2017

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ASTM D4608-89(2009) - Standard Test Method for Citrate in Detergents
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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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D4608 − 89 (Reapproved 2009)
Standard Test Method for
1
Citrate in Detergents
This standard is issued under the fixed designation D4608; 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 4. Significance and Use
4.1 This test method is suitable in research, development,
1.1 This test method covers a potentiometric titration pro-
and manufacturing control to monitor the level of citrate, a
cedure for the determination of citrate in liquid and powder
sequestering agent, in powder and liquid detergents.
detergents.
4.2 Accurate determination of sequestering agent is impor-
1.2 The values stated in SI units are to be regarded as
tant in evaluating cost and performance of detergent products.
standard. No other units of measurement are included in this
standard.
5. Interferences
1.3 This standard does not purport to address all of the
5.1 Other complexing agents such as nitrilotriacetic acid
safety concerns, if any, associated with its use. It is the
(NTA), ethylenedinitrilotetraacetic acid (EDTA), phosphates,
responsibility of the user of this standard to establish appro-
etc. will titrate as citrate in this method. For accurate citrate
priate safety and health practices and determine the applica-
determinations, such complexing agents must be absent.
bility of regulatory limitations prior to use. Material Safety
Data Sheets are available for reagents and materials. Review
6. Apparatus
them for hazards prior to usage. Specific safety precautions are
4
6.1 pH Meter, with millivolt capability.
given in Section 8.
5
6.2 Copper Ion Selective Electrode.
6
2. Referenced Documents
6.3 Calomel Reference Electrode.
2 7
2.1 ASTM Standards: 6.4 Glass Electrode Triple Purpose.
E70 Test Method for pH of Aqueous Solutions With the
6.5 Buret, semi-micro, 25 mL capacity with 0.1 mL gradu-
Glass Electrode
ations.
E180 Practice for Determining the Precision of ASTM
6.6 Magnetic Stirrer, and TFE-fluorocarbon-coated mag-
Methods for Analysis and Testing of Industrial and Spe-
3
netic stirring bars.
cialty Chemicals (Withdrawn 2009)
7. Reagents
3. Summary of Test Method
7.1 Purity of Reagents—Reagent grade chemicals shall be
3.1 The sample is titrated in an aqueous solution buffered at
used in all tests. Unless otherwise indicated, it is intended that
pH 8.5, with standard copper sulfate solution. The endpoint is
all reagents shall conform to specifications of the Committee
detected potentiometrically using a copper ion selective elec-
on Analytical Reagents of the American Chemical Society,
8
trode. The citrate content is calculated from the amount of
where such specifications are available. Other grades may be
standard copper sulfate solution consumed.
used, provided it is first ascertained that the reagent is of
4
An automatic titrator may be used.
1 5
This test method is under the jurisdiction of ASTM Committee D12 on Soaps Orion Model 94-29A or equivalent has been found suitable for this purpose.
and Other Detergents and is the direct responsibility of Subcommittee D12.12 on Available from Orion Inc.
6
Analysis and Specifications of Soaps, Synthetics, Detergents and their Components. Orion Model 90-22 or equivalent has been found suitable for this purpose.
Current edition approved Oct. 1, 2009. Published March 2010. Originally Available from Orion Inc.
7
approved in 1986. Last previous edition approved in 2003 as D4608 – 89(2003). Corning Model No. 476022 or equivalent has been found suitable for this
DOI: 10.1520/D4608-89R09. purpose. Available from Corning Inc.
2 8
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Reagent Chemicals, American Chemical Society Specifications, American
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Standards volume information, refer to the standard’s Document Summary page on listed by the American Chemical Society, see Analar Standards for Laboratory
the ASTM website. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
3
The last approved version of this historical standard is referenced on and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
www.astm.org. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D4608 − 89 (2009)
sufficiently high purity to permit its use without lessening the
N = normality of Na S O solution, and
2 2 3
accuracy of the determination.
25.0 = a
...

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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.
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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  
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47 – 49  
Total Ammonia  
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Test Method A. In the Absence of Ammonium or Triethanolamine Soaps  
53 – 56  
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57 – 60  
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61 – 63  
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64 – 70  
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These test methods cover procedures for the sampling and chemical analysis of inorganic alkaline detergents. These detergents include caustic soda, soda ash, modified soda (sequicarbonate type), sodium bicarbonate, sodium metasilicate, trisodium phosphate, tetrasodium pyrophosphate, borax, and sodium triphosphate. Different tests shall be conducted in order to determine the following properties of the detergents: total alkalinity, matter insoluble in water content, apparent density, ignition loss, pH level, turbidity, temperature rise, and particle size. Chemical analysis of the samples shall be performed by using either reverse-flow ion-exchange chromatography or paper chromatography.
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1.1 These test methods cover procedures for the sampling and chemical analysis of inorganic alkaline detergents.  
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Sections  
Caustic Soda:  
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Sodium Hydroxide (NaOH)  
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Carbonate as Sodium Carbonate (Na2CO3)  
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Total Alkalinity as Sodium Carbonate (Na2CO3 )  
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Sodium Bicarbonate (NaHCO3)  
23 – 25  
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26 – 28  
Matter Insoluble in Water  
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Apparent Density  
31 and 32  
Modified Soda (Sequicarbonate Type):  
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Total Alkalinity as Sodium Oxide (Na2O)  
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Sodium Bicarbonate (NaHCO3) and Sodium Carbonate (Na2CO3)  
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Matter Insoluble in Water  
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Sodium Bicarbonate:  
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Sodium Bicarbonate, Sodium Carbonate, and Free Moisture  
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Matter Insoluble in Water  
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Loss on Ignition of Sodium Sesquisilicate (3Na2O·2SiO2 ·11H2O)  
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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.
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1.2 The anti-soil deposition performance of detergent products will vary greatly depending on the type of soils and fabrics used in the test. Therefore, selection of the soils, fabrics, reference detergents, and test conditions shall be made by agreement between the interested parties on the basis of experience.  
1.3 There is no single or combination of oily soils or particulate soils, or both, that will precisely predict overall the performance of a product or treatment with respect to anti-redeposition as perceived by a consumer. This guide is intended to assess or compare detergent performance with respect to the anti-redeposition performance for the specific soil chosen.  
1.4 The values stated in either inch-pound or SI units are to be regarded separately as the standard. The values given in parentheses are for information only.  
1.5 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. Material safety data sheets are available for reagents and materials. Review them for hazards prior to usage.  
1.6 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.

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  • Guide
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    English language
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