ASTM D5547-95
(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
SCOPE
1.1 This test method covers atomic absorption tests applicable to powdered laundry detergents containing clay and zeolite.
1.2 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)
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: D 5547 – 95
Standard Test Method for
Clay and Zeolite in Powdered Laundry Detergents by Atomic
Absorption
This standard is issued under the fixed designation D 5547; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope ratio of clay and zeolite contain both clay and zeolite.
5.2 This test method is based on the linear relationship
1.1 This test method covers atomic absorption tests appli-
between the relative composition (or ratio) of clay/zeolite in
cable to powdered laundry detergents containing clay and
detergent powders and the Si/Al ratio of such detergents.
zeolite.
5.3 A calibration equation is derivable, therefore, from just
1.2 The values stated in SI units are to be regarded as the
two experimental points: the Si/Al ratio of the zeolite standard
standard.
(100 zeolite, 0 % clay) and the Si/Al ratio of the clay standard
1.3 This standard does not purport to address all of the
(0 % zeolite, 100 % clay).
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
6. Apparatus
priate safety and health practices and determine the applica-
6.1 Suitable Atomic Absorption Spectrophotometers, fitted
bility of regulatory limitations prior to use.
with a nitrous oxide-acetylene burner and aluminum and
2. Referenced Documents silicon hollow cathode source lamps.
6.2 Nitrous Oxide and Acetylene Tanks, with suitable regu-
2.1 ASTM Standards:
lators.
E 180 Practice for Determining the Precision of ASTM
6.3 Muffle Furnace, capable of reaching 1000°C.
Methods for Analysis and Testing of Industrial Chemicals
6.4 Analytical Balance.
3. Summary of Test Method
6.5 Fisher Burner or Equivalent.
6.6 20-mL or Larger Platinum Crucibles.
3.1 The test sample is fused with lithium metaborate,
6.7 Platinum-tip Tongs.
dissolved in acid, its silicon and aluminum content measured
6.8 25-mL Buret.
by atomic absorption, and the silicon/aluminum (Si/Al) ratio
6.9 100-mL and 200-mL Polypropylene Volumetric Flasks.
calculated. The clay and zeolite content of the test sample is
6.10 10-mL and 25-mL Graduated Cylinders.
calculated from the Si/Al ratio of the test sample and the Si/Al
6.11 150-mL Plastic Beakers.
ratio of the clay and zeolite expected in the test sample.
6.12 Magnetic Stirrer and Magnetic Stirring Bars.
5 6
4. Interferences
6.13 Blender, such as Waring or Osterizer or an industrial
lab model, or a mortar and pestle, if a blender is not available.
4.1 Materials other than clay and zeolite that contain silicon
or aluminum, or both, will interfere.
7. Reagents
5. Principle
7.1 Purity of Reagents—Reagents grade chemicals shall be
used in all tests. Unless otherwise indicated, it is intended that
5.1 Clay and zeolite contain silicon and aluminum at differ-
all reagents conform to the specifications of the Committee on
ent relative levels. The silicon/aluminum ratio is then a
Analytical Reagents of the American Chemical Society, where
measure of the relative level of clay and zeolite in detergent
such specifications are available. Other grades may be used,
powders. That is, detergent powders with a Si/Al ratio match-
provided it is first ascertained that the reagent is of sufficiently
ing clay or zeolite contain only clay or zeolite, respectively.
high purity to permit its use without lessening the accuracy of
Detergent powders with Si/Al ratio falling between the Si/Al
the determination.
This test method is under the jurisdiction of ASTM Committee D-12 on Soaps
and Other Detergents and is the direct responsibility of Subcommittee D12.12 on Waring blenders are available commercially.
Analysis of Soaps and Synthetic Detergents. Osterizer blenders are widely available commercially.
Current edition approved April 15, 1995. Published June 1995. Originally Reagent Chemicals, American Chemical Society Specifications, American
published as D 5547 – 94. Last previous edition D 5547 – 94.
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Silicon and aluminum measurements are by atomic absorption in this test listed by the American Chemical Society, see Analar Standards for Laboratory
method. ICP can be used to make such measurements as well. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Annual Book of ASTM Standards, Vol 15.05. and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
The Si/Al ratio is usually about 1 in zeolites and about 3 in clays. MD.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
D 5547
7.2 Purity of Water—Unless otherwise indicated, reference 9.1.6 Place 90 mL of distilled water into 150-mL plastic
to water shall be understood to mean distilled water or water of beakers. (Use as many beakers as there are standards and
equal purity. samples).
7.3 Aluminum Standard, 1000 μg Al/mL or equivalent. 9.1.7 Add a magnetic stirring bar to each beaker, and place
7.4 Silicon Standard, 1000 μg Si/mL.
on a magnetic stirrer. Mix rapidly to make the water swirl in
7.5 Potassium Chloride, Baker-analyzed reagent or equiva- the beaker, but do not allow anything to splash out. This
lent.
apparatus should be near the furnace containing the ashed
7.6 Potassium Chloride Solution (1 %)—Dissolve1gof standards and sample(s).
potassium chloride in 100 mL of distilled water. Mix well and
9.1.8 Using platinum-tip tongs, remove one crucible at a
store in plastic container. time from the furnace, and immediately place over a Fisher
7.7 Concentrated Hydrochloric Acid, Baker-analyzed re-
burner flame without allowing the melted sample to solidify.
agent or equivalent. 9.1.9 Add about 2 mg (a pinch on the end of a spatula) of
7.8 Hydrochloric Acid Solution (1 + 1)—Mix equal parts of
potassium iodide (KI) to the melted sample. A molten ball will
concentrated HCl and distilled water by volume. Mix well and form. Roll the ball around the inside of the dish to pick up any
store in plastic container.
droplets or particles. The KI releasing agent is volatile, and it
7.9 Potassium Iodide, Baker-analyzed reagent or equiva- is necessary to carry out this step rather quickly (about 2 min).
lent.
If the ball collapses and flows into the dish, start again by
7.10 Lithium Metaborate SPEX Grade, Special for Fu- adding fresh KI.
sions .
9.1.10 Drop each molten ball quickly into the swirling water
7.11 Zeolite Standard—The same material expected in the
of each plastic beaker.
test sample, to be used as standard.
NOTE 2—Precaution: Use face shield and protective clothing.
7.12 Clay Standard—The same material expected in the test
9.1.11 Add 20 mL of 1 + 1 HCl and 20 mL of 1 %
sample, to be used as standard.
potassium chloride solution and mix until completely dis-
8. Instrumental Conditions
solved. Quantitatively transfer to a 200-mL plastic volumetric
8.1 Following the instrument manufacturer’s instructions,
flask with distilled water. Dilute to volume and mix well.
set up the atomic absorption instrument as follows:
9.1.12 Using a buret, add 5, 7.5, and 10 mL of 1000-ppm
To measure Aluminum To measure Silicon
aluminum standard into 3 separate 100-mL plastic volumetric
flasks. These standards contain 50, 75, and 100 μg Al/mL
Wavelength, nm 309.3 251.6
respectively. (Make these standards fresh each day).
Range UV UV
Slit, nm 0.2 0.2
9.1.13 Add 10 mL 1 + 1 HCl, 10 mL 1 % KCl, and1gof
Flame Nitrous oxide-acetylene. Nitrous oxide-acetylene.
lithium metaborate to each flask. Dilute to volume with
Rich, red. Strongly reducing red cone 2–3
distilled water and mix until completely dissolved.
cm high with yellow outer
edge.
9.1.14 Prepare a reagents blank.
9.1.15 Set up the atomic absorption instrument as described
9. Procedure
in 8.1.
9.1 Determination of Aluminum:
9.1.16 Zero the instrument with the reagents blank. Measure
9.1.1 Accurately weigh 0.1 g (to the nearest 0.1 mg) of
the absorbance of the aluminum standards, the zeolite standard,
zeolite standard (the same material expected in the test sample)
the clay standard and the test sample at 309.3 nm. Repeat the
into a clean, dry, platinum crucible. Also accurately weigh 0.2
measurement three more times for each flask and calculate the
g of clay standard (the same material expected in the test
average absorbance. Save the solutions, except the aluminum
sample) into another clean, dry, platinum crucible.
standards, for silicon determination in 9.2.
9.1.2 Grind a representative powdered detergent test sample
9.1.17 Prepare a standard curve by plotting the average
in a blender to a fine, homogenous powder. (If a blender is not
absorbance versus concentration in μg/mL of each aluminum
available, use a mortar and pestle).
standard.
9.1.3 Accurately weigh 0.3 g (to the nearest 0.1 mg) of the
9.1.18 Determine the concentration of aluminum in the test
ground test sample(s) into still another clean, dry, platinum
sample(s) by comparing the average absorbance to the standard
crucible.
curve and reading aluminum concentration in μg/mL directly.
9.1.4 Add2g(60.1 g) of lithium metaborate to each
platinum crucible, and mix t
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.