Designation: E 887 – 88 (Reapproved 2004)

Standard Test Method for

Silica in Refuse-Derived Fuel (RDF) and RDF Ash1
This standard is issued under the fixed designation E 887; 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 4.2 Muffle Furnace—The furnace shall have an operating

1.1 This test method covers the determination of silica in temperature of up to 1200°C.
RDF, RDF ash, fly ash, bottom ash, or slag. 4.3 Hot Plate or Steam Bath.
1.2 The test method is an acid dehydration gravimetric 4.4 Platinum Crucibles, 35 to 85-mL capacity.
procedure and is independent of interferences. 4.5 Graphite Crucibles, 35 to 85-mL capacity.
1.3 The values stated in SI units are to be regarded as the 4.6 Fused Quartz Dishes, 35 to 85-mL capacity.
standard. The values given in parentheses are for information 5. Reagents and Materials
only.
1.4 This standard does not purport to address all of the 5.1 Purity of Reagents—Reagent grade chemicals shall be
safety concerns, if any, associated with its use. It is the used in this test. Unless otherwise indicated, it is intended that
responsibility of the user of this standard to establish appro- all reagents shall conform to the specifications of the Commit-
priate safety and health practices and determine the applica- tee on Analytical Reagents of the American Chemical Society
bility of regulatory limitations prior to use. For hazard state- where such specifications are available.3 Other grades may be
ment, see Section 6. used, provided it is first ascertained that the reagent is of
sufficiently high purity to permit its use without lessening the
2. Referenced Documents accuracy of the determination.
2.1 ASTM Standards: 2 5.2 Purity of Water—Unless otherwise indicated, reference
D 1193 Specification for Reagent Water to water shall be understood to mean at least Type III reagent
E 791 Test Method for Calculating Refuse-Derived Fuel water conforming to Specification D 1193.
Analysis Data from As-Determined to Different Bases 5.3 Sodium Carbonate (Na2CO3), anhydrous powder.
E 829 Practice for Preparing Refuse-Derived-Fuel (RDF) 5.4 Hydrochloric Acid (HCl), concentrated, sp gr 1.19.
Laboratory Samples for Analysis 5.5 Hydrochloric Acid (1 + 3), Mix 1 volume of concen-
E 830 Test Method for Ash in the Analysis Sample of trated HCl with 3 volumes of water.
Refuse-Derived Fuel 5.6 Hydrochloric Acid (1 + 1)—Mix 1 volume of concen-
E 856 Definitions of Terms and Abbreviations Relating to trated HCl with 1 volume of water.
Physical and Chemical Characteristics of Refuse-Derived 5.7 Hydrochloric Acid (1 + 99)—Mix 1 volume of concen-
Fuel trated HCl with 99 volumes of water.
5.8 Sulfuric Acid (1 + 1)—Mix 1 volume of concentrated
3. Summary of Test Method sulfuric acid (H2SO4, sp gr 1.84) with 1 volume of water.
3.1 Silicon compounds in RDF ash, fly ash, bottom ash, or 5.9 Hydrofluric Acid (HF), concentrated 48 to 51 %.
slag are dissolved by alkali fusion and dehydrated with
6. Hazards
hydrochloric acid (HCl). Dehydration is completed by ignition,
and the silica is volatilized as silicon tetrafluoride. 6.1 Due to the origins of RDF in municipal waste, common
sense dictates that precautions should be observed when
4. Apparatus conducting tests on the samples. Recommended hygienic
4.1 Analytical Balance, capable of weighing to 0.0001 g. practices include use of gloves when handling RDF; wearing
dust masks (NIOSH-approved type), especially while milling
RDF samples; conducting tests under negative pressure hoods
1
when possible; and washing hands before eating or smoking.
This test method is under the jurisdiction of ASTM Committee D34 on Waste
Management and is the direct responsibility of Subcommittee D34.03 on Treatment.
Current edition approved March 25, 1988. Published May 1988. Originally
published as E 887 – 82. Last previous edition E 887 – 82.
2 3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or “Reagent Chemicals, American Chemical Society Specifications,” Am. Chemi-
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM cal Soc., Washington, DC. For suggestions on the testing of reagents not listed by
Standards volume information, refer to the standard’s Document Summary page on the American Chemical Society, see “Analar Standards for Laboratory U.K.
the ASTM website. Chemicals,” BDH Ltd., Poole, Dorset, and the “United States Pharmacopeia.”

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.

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 E 887 – 88 (2004)
7. Sampling 8.2.4 Place the dish in the muffle at a low temperature (not
7.1 Refuse-Derived Fuel (RDF): greater than 100°C), and gradually heat to redness at such a
rate as to avoid mechanical loss from too rapid expulsion of
NOTE 1—ASTM Subcommittee E38.01 is currently in the process of volatile matter.
developing procedures for sampling RDF. 8.2.5 Complete the conversion to ash at a temperature of
7.1.1 RDF products are frequently nonhomogeneous. For 800 to 900°C (1470 to 1659°F).
this reason, significant care should be exercised to obtain a 8.2.6 Cool in a desiccator and stir the ash to ensure
representative laboratory sample from the RDF lot to be homogeneity of particle sizes. Be careful not to lose any ash
characterized. from the dish during this stirring.
7.1.2 The sampling method for these procedures should be 8.2.7 Spread the ash in a thin layer in the dish and ignite in
based on agreement between involved parties. a stream of oxygen for 11⁄2 h at 800 to 850°C (1470 to 1560°F)
7.1.3 The laboratory sample must be air-dried and particle to ensure complete and uniform oxidation of the ash.
size reduced to pass a 0.5-mm screen for analysis. This 8.2.8 Cool the ash to room temperature in a desiccator.
procedure must be performed carefully to preserve the sam- 8.2.9 Weigh the dish and the ash.
ple’s representative characteristics (other than particle size) 8.2.10 Calculate the percent residue after ignition as fol-
while preparing the analysis sample to be used in this proce- lows:
dure (see Practice E 829). % Residue after ignition 5 ~F 2 D!/~E 2 D! 3 100 (2)
7.2 Refuse-Derived Fuel Ash, Fly Ash, Bottom Ash, or
Slag—The method of sampling for this procedure should be where:
based on agreement between involved parties. D = weight of fused quartz dish, g,
E = weight of fused quartz dish and sample, of RDF ash,
8. Sample Preparation fly ash, bottom ash or slag, g, and
F = weight of fused quartz dish and residue after ignition of
8.1 Refuse-Derived Fuel: RDF ash, fly ash, bottom ash, or slag, g.
8.1.1 Weigh accurately 30 to 50 g of RDF analysis sample
as prepared in 7.16.1 into a conditioned and preweighed fused 9. Procedure
quartz dish.
9.1 Sample Fusion:
8.1.2 Spread out the analysis sample of RDF in a layer not
9.1.1 Weigh accurately 0.010 to 0.100 g of the prepared
over 38.1 mm (11⁄2 in.) in depth.
RDF ash as prepared in 8.1 or the residue of RDF ash, fly ash,
8.1.3 Place the dish in the muffle at a low temperature (not
bottom ash, or slag as prepared in 8.2 into a platinum or
greater than 100°C) and gradually heat to redness at such a rate
graphite crucible.
as to avoid mechanical loss from too rapid expulsion of volatile
9.1.2 Add 1.0 g of Na2CO3. Mix the ash and Na2CO3 well,
matter.
then add an additional 0.5 g of Na2CO3 to cover the mixture.
8.1.4 Complete the conversion to ash at a temperature of
9.1.3 Place the crucible into a clean silica or refractory tray,
800 to 900°C (1470 to 1650°F).
and place in a muffle furnace preheated to 1000°C and maintain
8.1.5 Cool in a desiccator and stir the ash to ensure until the mass is quiescent (about 45 min).
homogeneity of particle sizes. Be careful not to lose any ash 9.1.4 Set the crucible aside to cool.
from the dish during this stirring. 9.1.5 Rinse off the outside of the crucible, and place it on its
8.1.6 Spread the ash in a thin layer in the dish, and ignite in side in a 300-mL casserole or beaker about one-third full of
a stream of oxygen for 11⁄2 h at 800 to 850°C (1470 to 1560°F) water. Warm and stir until the cake disintegrates and can be
to ensure complete and uniform oxidation of the ash. easily removed.
8.1.7 Cool the ash to room temperature in a desiccator. 9.1.6 By means of platinum tipped tongs, lift the crucible
8.1.8 Weigh the dish and the ash. out of the liquid, rinsing it thoroughly with water followed by
8.1.9 Calculate the percent ash as follows: rinsing with dilute hydrochloric acid (HCl, 1 + 3); adding the
% Ash 5 ~C 2 A!/~B 2 A! 3 100 (1) rinse to the casserole or beaker.
9.2 Acid Dehydration:
where: 9.2.1 Very slowly and cautiously add 20 mL of concentrated
A = weight of fused quartz, g, hydrochloric acid (HCl, sp gr 1.19) to the covered casserole or
B = weight of fused quartz dish and sample, g, and
beaker (see Note 2). Remove the cover and rinse. If any gritty
C = weight of fused quartz dish and ash, g.
particles are present, the fusion is incomplete and must be
8.2 Refuse-Derived Fuel Ash, Fly Ash, Bottom Ash, or Slag:
repeated, using a new sample and a larger amount of Na2CO3.
8.2.1 Prepare the RDF ash, fly ash, bottom ash, or slag by
grinding the sample in an agate mortar to a particle size to pass NOTE 2—This solution will tend to “creep” over the rim of the casserole
a No. 200 (75-µm) sieve. unless the rim is kept hot and dry. This can be accomplished by applying
heat from above by means of infrared lamps.
8.2.2 Weigh accurately 6 to 10 g of RDF ash, fly ash, bottom
ash, or slag as prepared in 8.2.1 into a conditioned preweighed 9.2.2 Evaporate the solution to dryness on a steam bath.
fused quartz dish. 9.2.3 Without heating the residue any further, treat it with 5
8.2.3 Spread out the analysis sample of the ash to be to 10 mL of HCl (concentrated), wait at least 2 min, then add
analyzed in a layer not over 6.4 mm (1⁄4 in.) in depth. an equal amount of water.

2
 E 887 – 88 (2004)
9.2.4 Cover the casserole or beaker, and digest for 10 min 10. Calculation
on the steam bath or hot plate.
10.1 Calculate the concentration of SiO2 as follows:
9.2.5 Dilute the solution with an equal volume of hot water,
immediately filter through medium-textured ashless paper, and 10.1.1 Percent SiO2 on prepared sample as used in 9.1.1.
wash the residue thoroughly with hot HCl (1 + 99), then with % SiO2 5 ~W1 2 W2! 2 ~W3 2 W4!/W5 3 100 (3)
hot water.
9.2.6 Reserve the residue. where:
9.2.7 Again, evaporate the filtrate to dryness and bake the W1 = weight of residue after first ignition as in 9.2.11, g,
W2 = weight of blank after first ignition, g,
residue in an oven for 1 h at 105 to 110°C.
W3 = weight of residue after treatment with HF and second
9.2.8 Cool, add 10 to 15 mL HCl (1 + 1) and digest on the
ignition as in 9.3.4, g,
steam bath or hot plate for 10 min. W4 = weight of blank after treatment with HF and second
9.2.9 Dilute with an equal volume of water, filter immedi- ignition, g, and
ately on a fresh filter paper, and wash the small amount of W5 = weight of sample of prepared RDF, RDF ash, fly ash,
residue thoroughly with hot HCl (1 + 99), then with hot water. bottom ash, or slag as used in 9.1.1, g.
9.2.10 Transfer the papers containing the residues (from
10.1.2 Percent SiO2 in RDF (6.1).
9.2.6 and 9.2.9) to a weighed conditioned platinum crucible.
9.2.11 Dry and ignite the papers, first at a low heat until the % SiO2 in RDF 5 ~G 3 H!/~100! (4)
carbon of the filter paper is completely consumed without
where:
flaming, and finally ignite at 1100 to 1200°C until the weight
G = ash as found in 8.1.9, %, and
becomes constant. Record weight of residue after ignition. H = SiO2 as found in 10.1.1, %.
9.3 Volatilization of Silicon Tetrafluoride:
9.3.1 Treat the silica (SiO2) thus obtained, which will con- 10.1.3 Percent SiO2 in RDF ash, fly ash, bottom ash, or slag
tain impurities, in the crucible with 0.5 to 1 mL of water, 2 (8.2).
drops of H2SO4 (1 + 1) and 10 mL of HF. % SiO2 in RDF Ash, fly ash, bottom ash, or slag 5 ~I 3 H!/~100!
9.3.2 Cautiously evaporate to dryness on a hot plate or hot (5)
sand bath.
where:
9.3.3 Finally, ignite the small residue at 1050 to 1100°C I = residue after ignition as found in 8.2.10, %, and
(1922 to 2012°F) for 5 min. H = SiO2 as found in 10.1.1, %.
9.3.4 Cool in a desiccator and weigh. See Method E 791 for procedures to convert values to other
9.3.5 The difference between this weight and the weight
bases.
previously obtained in 9.2.11 represents the amount of SiO2.
9.4 Blank—Make a blank determination, following the
11. Precision and Bias
same procedures as used in 9.1.2 through 9.3.5 using the same
amounts of reagents and correct the obtained in the analysis 11.1 Precision and bias statements cannot be made at this
accordingly. time for the measurement of SiO2 by this test method.

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