ASTM D4954-89(2009)

Standard Test Method for Determination of Nitrilotriacetates in Detergents

SIGNIFICANCE AND USE
This test method is suitable in research, development, and manufacturing control to monitor the level of NTA, a sequestering agent, in powder and liquid detergents.
Accurate determination of a sequestering agent is important in evaluating cost and performance of detergent products.
SCOPE
1.1 This test method describes the determination of nitrilotriacetates (NTA) in 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. For specific safety precautions, see 6.5.

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

Relations

• Replaces: ASTM D4954-89(2003) - Standard Test Method for Determination of Nitrilotriacetates in Detergents
• Effective Date: 01-Oct-2009
• Replaced By: ASTM D4954-89(2017) - Standard Test Method for Determination of Nitrilotriacetates in Detergents
• Effective Date: 01-Jan-2017

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:D4954 −89(Reapproved 2009)
Standard Test Method for
1
Determination of Nitrilotriacetates in Detergents
This standard is issued under the fixed designation D4954; 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 5. Apparatus
1.1 This test method describes the determination of nitrilo- 5.1 Volumetric Flasks, 200-mL, 500-mL, 1000-mL.
triacetates (NTA) in detergents.
5.2 Beakers, 200-mL (tall form), 250-mL, 1000-mL.
1.2 The values stated in SI units are to be regarded as
5.3 Pipets, 25-mL, 100-mL.
standard. No other units of measurement are included in this
5.4 Graduated Cylinders, 10-mL, 25-mL.
standard.
5.5 Copper Ion Electrode (Orion Model 94-29).
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
5.6 Single Junction Reference Electrode (Orion Model 90-
responsibility of the user of this standard to establish appro-
01), filled with Orion 90-00-01 solution.
priate safety and health practices and determine the applica-
5.7 pH Combination Electrode.
bility of regulatory limitations prior to use. For specific safety
5.8 Burets, 10-mL, 25-mL, 50-mL.
precautions, see 6.5.
5.9 pH Meter, with millivolt capabilities.
2. Summary of Test Method
5.10 Automatic Titrator—may be substituted for 5.8 and
2.1 A known excess amount of copper nitrate solution is
5.9.
added to the detergent sample under controlled pH conditions.
5.11 Magnetic Stirrer/Hot Plate.
The uncomplexed copper is back-titrated potentiometrically
5.12 Balance, with 1-mg sensitivity.
with a standard NTA solution using a copper ion specific
electrode. The millimoles of NTAin the sample are equivalent
6. Reagents
to the millimoles of copper added, less the millimoles of the
NTA titrant.
6.1 Purity of Reagents—Reagent grade chemicals shall be
used in all tests. Unless otherwise indicated, it is intended that
3. Significance and Use
all reagents shall conform to specifications of the Committee
on Analytical Reagents of the American Chemical Society,
3.1 This test method is suitable in research, development,
2
where such specifications are available. Other grades may be
and manufacturing control to monitor the level of NTA, a
substituted, provided it is first ascertained that the reagent is of
sequestering agent, in powder and liquid detergents.
sufficiently high purity to permit its use without lessening the
3.2 Accurate determination of a sequestering agent is im-
accuracy of the determination.
portant in evaluating cost and performance of detergent prod-
3
6.2 DisodiumEthylenediaminetetraacetate(EDTA), 0.1 M.
ucts.
6.3 Nitric Acid, concentrated.
4. Interferences
6.4 Sodium Hydroxide, 50 % reagent solution.
4.1 The presence of substances that will make copper
6.5 SodiumHydroxide, 20 % solution. Mix 40 g of the 50 %
complex like citrate, formate, ethylenediaminetetraacetate, and
solution with 60 g of water. Cool. Wear a face shield during
phosphonate, will interfere positively in the determination of
mixing.
NTA.
6.6 Cupric Nitrate, 0.1 M. Weigh (to the nearest 0.1 g) 6.3
gofcoppermetalandtransferintoa600-mLbeaker.Addabout
100 mL of water. Place a magnetic bar into the beaker and
1
This test method is under the jurisdiction of ASTM Committee D12 on Soaps
and Other Detergents and is the direct responsibility of Subcommittee D12.12 on
Analysis and Specifications of Soaps, Synthetics, Detergents and their Components.
2
Current edition approved Oct. 1, 2009. Published December 2009. Originally American Chemical Society, 1155 16th St., NW, Washington, DC 20036.
3
approved in 1989. Last previous edition approved in 2003 as D4954-89(2003). DOI: EDTA solution is available from J. T. Baker Inc., already standardized against
10.1520/D4954-89R09. NIST Reference Material Calcium Carbonate.
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D4954−89(2009)
A
TABLE 1 Determination of Inflection Point
place on a stirrer/hotplate. Add 30 mL of concentrated nitric
acid while stirring and heat gently. Stir until the copper metal
NOTE 1—Volume of NTArequired to react with 25 mLof cupric nitrate
dissolves. Add more nitric acid if undissolved metal remains. solution (0.0972 M).
After dissolution, cool and transfer quantitatively to a 1-L NTA, mL mV, (+)
volumetric flask. Dilute to the mark and mix the solution well.
0 303
1.00 300
6.6.1 Alternatively, weigh out (to the nearest 1 g) 23 g of
2.00 297
1
reagent grade cupric nitrate, 2 ⁄2 hydrate crystals, and transfer
3.00 294
...