ASTM D5547-95(2017)
(Test Method)Standard Test Method for Clay and Zeolite in Powdered Laundry Detergents by Atomic Absorption
Standard Test Method for Clay and Zeolite in Powdered Laundry Detergents by Atomic Absorption
ABSTRACT
This test method covers atomic absorption tests applicable to powdered laundry detergents containing clay and zeolite. The test sample is fused with lithium metaborate, dissolved in acid, its silicon and aluminum content measured by atomic absorption, and the silicon/aluminum (Si/Al) ratio calculated. The clay and zeolite content of the test sample is calculated from the Si/Al ratio of the test sample and the Si/Al ratio of the clay and zeolite expected in the test sample. This test method is based on the linear relationship between the relative composition (or ratio) of clay/zeolite in detergent powders and the Si/Al ratio of such detergents.
SCOPE
1.1 This test method covers atomic absorption tests applicable to powdered laundry detergents containing clay and zeolite.2
1.2 The values stated in SI units are to be regarded as the 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.
General Information
Relations
Standards Content (Sample)
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.
Designation: D5547 − 95 (Reapproved 2017)
Standard Test Method for
Clay and Zeolite in Powdered Laundry Detergents by Atomic
Absorption
This standard is issued under the fixed designation D5547; 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. Principle
1.1 This test method covers atomic absorption tests appli- 5.1 Clay and zeolite contain silicon and aluminum at differ-
cable to powdered laundry detergents containing clay and ent relative levels. The silicon/aluminum ratio is then a
zeolite. measure of the relative level of clay and zeolite in detergent
powders. That is, detergent powders with a Si/Al ratio match-
1.2 The values stated in SI units are to be regarded as the
ing clay or zeolite contain only clay or zeolite, respectively.
standard.
Detergent powders with Si/Al ratio falling between the Si/Al
1.3 This standard does not purport to address all of the
ratio of clay and zeolite contain both clay and zeolite.
safety concerns, if any, associated with its use. It is the
5.2 This test method is based on the linear relationship
responsibility of the user of this standard to establish appro-
between the relative composition (or ratio) of clay/zeolite in
priate safety and health practices and determine the applica-
detergent powders and the Si/Al ratio of such detergents.
bility of regulatory limitations prior to use.
5.3 A calibration equation is derivable, therefore, from just
2. Referenced Documents
two experimental points: the Si/Al ratio of the zeolite standard
2.1 ASTM Standards: (100 zeolite, 0 % clay) and the Si/Al ratio of the clay standard
E180 Practice for Determining the Precision of ASTM (0 % zeolite, 100 % clay).
Methods for Analysis and Testing of Industrial and Spe-
4 6. Apparatus
cialty Chemicals (Withdrawn 2009)
6.1 Suitable Atomic Absorption Spectrophotometers, fitted
3. Summary of Test Method
with a nitrous oxide-acetylene burner and aluminum and
silicon hollow cathode source lamps.
3.1 The test sample is fused with lithium metaborate,
dissolved in acid, its silicon and aluminum content measured
6.2 Nitrous Oxide and Acetylene Tanks, with suitable regu-
by atomic absorption, and the silicon/aluminum (Si/Al) ratio
lators.
calculated. The clay and zeolite content of the test sample is
6.3 Muffle Furnace, capable of reaching 1000°C.
calculated from the Si/Al ratio of the test sample and the Si/Al
6.4 Analytical Balance.
ratio of the clay and zeolite expected in the test sample.
6.5 Fisher Burner or Equivalent.
4. Interferences
6.6 20-mL or Larger Platinum Crucibles.
4.1 Materials other than clay and zeolite that contain silicon
6.7 Platinum-tip Tongs.
or aluminum, or both, will interfere.
6.8 25-mL Buret.
This test method is under the jurisdiction of ASTM Committee D12 on Soaps
6.9 100-mL and 200-mL Polypropylene Volumetric Flasks.
and Other Detergents and is the direct responsibility of Subcommittee D12.12 on
6.10 10-mL and 25-mL Graduated Cylinders.
Analysis and Specifications of Soaps, Synthetics, Detergents and their Components.
Current edition approved Jan. 1, 2017. Published February 2017. Originally
6.11 150-mL Plastic Beakers.
approved in 1994. Last previous edition approved in 2009 as D5547 – 95(2009).
DOI: 10.1520/D5547-95R17.
6.12 Magnetic Stirrer and Magnetic Stirring Bars.
Silicon and aluminum measurements are by atomic absorption in this test
6 7
method. ICP can be used to make such measurements as well. 6.13 Blender, such as Waring or Osterizer or an industrial
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
lab model, or a mortar and pestle, if a blender is not available.
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
the ASTM website. The Si/Al ratio is usually about 1 in zeolites and about 3 in clays.
The last approved version of this historical standard is referenced on Waring blenders are available commercially.
www.astm.org. Osterizer blenders are widely available commercially.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D5547 − 95 (2017)
7. Reagents 9.1.1 Accurately weigh 0.1 g (to the nearest 0.1 mg) of
zeolitestandard(thesamematerialexpectedinthetestsample)
7.1 Purity of Reagents—Reagents grade chemicals shall be
into a clean, dry, platinum crucible.Also accurately weigh 0.2
used in all tests. Unless otherwise indicated, it is intended that
g of clay standard (the same material expected in the test
all reagents conform to the specifications of the Committee on
sample) into another clean, dry, platinum crucible.
Analytical Reagents of theAmerican Chemical Society, where
9.1.2 Grind a representative powdered detergent test sample
such specifications are available. Other grades may be used,
in a blender to a fine, homogenous powder. (If a blender is not
provided it is first ascertained that the reagent is of sufficiently
available, use a mortar and pestle).
high purity to permit its use without lessening the accuracy of
9.1.3 Accurately weigh 0.3 g (to the nearest 0.1 mg) of the
the determination.
ground test sample(s) into still another clean, dry, platinum
7.2 Purity of Water—Unless otherwise indicated, reference
crucible.
towatershallbeunderstoodtomeandistilledwaterorwaterof
9.1.4 Add2g(60.1 g) of lithium metaborate to each
equal purity.
platinum crucible, and mix the contents with a plastic rod.
7.3 Aluminum Standard, 1000 µg Al/mL or equivalent.
9.1.5 Place the crucibles containing the mixtures in a cool
muffle furnace and turn on the heat. When the temperature
7.4 Silicon Standard, 1000 µg Si/mL.
reaches 1000°C, maintain heat for at least 5 additional min.
7.5 Potassium Chloride, Baker-analyzed reagent or equiva-
NOTE 1—The sample will ignite and splatter if placed in a hot furnace.
lent.
Ifitisnotpossibletostartwithacoolfurnace,gentlycharthesamplewith
7.6 Potassium Chloride Solution (1 %)—Dissolve1gof
a Fisher burner first, avoiding ignition, then place in the furnace.
potassium chloride in 100 mL of distilled water. Mix well and
9.1.6 Place 90 mL of distilled water into 150-mL plastic
store in plastic container.
beakers. (Use as many beakers as there are standards and
7.7 Concentrated Hydrochloric Acid, Baker-analyzed re-
samples).
agent or equivalent.
9.1.7 Add a magnetic stirring bar to each beaker, and place
on a magnetic stirrer. Mix rapidly to make the water swirl in
7.8 Hydrochloric Acid Solution (1 + 1)—Mix equal parts of
the beaker, but do not allow anything to splash out. This
concentrated HCl and distilled water by volume. Mix well and
apparatus should be near the furnace containing the ashed
store in plastic container.
standards and sample(s).
7.9 Potassium Iodide, Baker-analyzed reagent or equiva-
9.1.8 Using platinum-tip tongs, remove one crucible at a
lent.
time from the furnace, and immediately place over a Fisher
7.10 Lithium Metaborate SPEX Grade, Special for Fu-
burner flame without allowing the melted sample to solidify.
sions.
9.1.9 Add about 2 mg (a pinch on the end of a spatula) of
potassium iodide (KI) to the melted sample.Amolten ball will
7.11 Zeolite Standard—The same material expected in the
form. Roll the ball around the inside of the dish to pick up any
test sample, to be used as standard.
droplets or particles. The KI releasing agent is volatile, and it
7.12 Clay Standard—The same material expected in the test
is necessary to carry out this step rather quickly (about 2 min).
sample, to be used as standard.
If the ball collapses and flows into the dish, start again by
adding fresh KI.
8. Instrumental Conditions
9.1.10 Dropeachmoltenballquicklyintotheswirlingwater
8.1 Following the instrument manufacturer’s instructions,
of each plastic beaker.
set up the atomic absorption instrument as follows:
NOTE 2—Precaution: Use face shield and protective clothing.
To measure Aluminum To measure Silicon
9.1.11 Add 20 mL of 1 + 1 HCl and 20 mL of 1 %
Wavelength, nm 309.3 251.6
potassium chloride solution and mix until completely dis-
Range UV UV
Slit, nm 0.2 0.2 solved. Quantitatively transfer to a 200-mL plastic volumetric
Flame Nitrous oxide-acetylene. Nitrous oxide-acetylene.
flask with distilled water. Dilute to volume and mix well.
Rich, red. Strongly reducing red cone 2–3
9.1.12 Using a buret, add 5, 7.5, and 10 mL of 1000-ppm
cm high with yellow outer
edge.
aluminum standard into 3 separate 100-mL plastic volumetric
flasks. These standards contain 50, 75, and 100 µg Al/mL
9. Procedure
respectively. (Make these standards fresh each day).
9.1 Determination of Aluminum:
9.1.13 Add 10 mL 1 + 1 HCl, 10 mL 1 % KCl, and1gof
lithium metaborate to each flask. Dilute to volume with
distilled water and mix until completely dissolved.
Reagent Chemicals, American Chemical Society Specifications, American
9.1.14 Prepare a reagents blank.
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
9.1.15 Set up the atomic absorption instrument as described
listed by the American Chemical Society, see Analar Standards for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
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