ASTM D279.

5 95 - 0759530 0583223 5T4 m

AMERICAN SOCIETY FOR TESTING AND MATERIALS

Designation: D 2795 - 95 100 Barr Harbor Dr.. West Conshohocken, PA 19428
Reprinted from the Annual Bock of ASTM Standards. Copyright ASTM
If not listed in the current combined index. will appear in the next edition.

Standard Test Methods for

Analysis of Coal and Coke Ash’
This standard is issued under the lixed designation D 2795; 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 (0 indicates an editorial change since the last revision or reapprovaf.

1. Scope 3. Summary of Test Methods

1.1 These test methods cover the analysis of coal and coke 3.1 The coal or coke to be analyzed is ashed under
ash for the commonly determined major elements. standard conditions and ignited to constant weight. Two
1.2 The test methods appear in the following order: solutions are prepared from the ash. Solution A is obtained
Sections by fusing the ash with sodium hydroxide (NaOH) followed
Silicon Dioxide (SiOs) .. . ... .. 10 to 12 by a final dissolution of the melt in dilute hydrochloric acid
Aluminum Oxide (AlsOs) .. .... 13 to 15 (HCl). Solution B is prepared by decomposition of the ash
Ferric Oxide (Fe,03 .,........__.._.....,..,........... 16 to I8 with sulfuric (H2S04), hydrofluoric (HF), and nitric (HNO,)
Titanium Dioxide (TiOs) . 19 to 22
Phosphorus Pentoxide (PsOs) . . . . . 23 lo 25
acids, Solution A is used for the analysis of Si02 and Al,O,,
Calcium Oxide (CaO), and Magnesium Oxide (MgO) .. . . 26 to 29 and Solution B for the remaining elements.
Sodium Oxide (NasO) and Potassium Oxide (K,O) .... 30 to 33 3.2 The two solutions are analyzed by a combination of
NOTE I-Test Methods D 1757 is used for determination of sulfur.
methods: (1) spectrophotometric procedures are used for
Si02, A1203, Fe20s, Ti02, and P,O,; (2) chelatometric
1.3 The values stated in SI units (Practice E 380) shall be titration for CaO and MgO; and (3) flame photometry for
regarded as the standard. The values given in parentheses are Na20 and K,O. See Fig. 1 for a general outline of the
for information only. methods and procedures used for each determination.
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the 4. Significance and Use
responsibilityof the user of this standard to establish appro- 4.1 A compositional analysis of the ash is often useful in
priate safety and healthpractices and determine the applica- the total coal quality description. Knowledge of the ash
bility of regulatorylimitationsprior to use. composition is also useful in predicting the behavior of the
ashes and slags in combustion chambers. Utilization of the
2. Referenced Documents coal combustion ash by-products sometimes depends on the
chemical composition of the ash.
2.1 ASTM Standards: 4.2 It should be noted that chemical composition of
D 346 Practice for Collection and Preparation of Coke laboratory prepared coal ash may not exactly represent the
Samples for Laboratory Analysis’ composition of mineral matter in the coal, or the composi-
D 1193 Specification for Reagent Water3 tion of the fly ash and slags resulting from the commercial
D 1757 Test Methods for Sulfur in Ash from Coal and scale burning of the coal.
Coke2
D 20 13 Test Method for Preparing Coal Samples for
5. Apparatus
Analysis2
D 3 173 Test Method for Moisture in the Analysis Sample 5.1 Balance, sensitive to 0.1 mg.
of Coal and Coke2 5.2 Crucibles-Nickel crucibles of 50-cm3 capacity shall
D 3 174 Test Method for Ash in the Analysis Sample of be used for NaOH fusion of the ash, and platinum crucibles
Coal and Coke from Coal2 of 30-cm3 capacity shall be used for decomposition of the ash
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D 3 180 Practice for Calculating Coal and Coke Analyses with HF.
from As-Determined to Different Bases2 5.3 Emission Flame Photometer.
D 5 142 Test Methods for Proximate Analysis of the 5.4 Muff Furnace-Electrically heated muffle furnace
Analysis Sample of Coal and Coke by Instrumental with good air circulation and capable of maintaining a
Procedures2 temperature of approximately 750°C.
E 380 Practice for Use of the International System of 5.5 Absorption Spectrophotometer,visible region 380 to
Units (SI) (the Modernized Metric System)4 780 nm.
5.6 Sieves, 150 and 250ym (No. 100 and No. 60) U.S.A.
standard.
t These test methods are under the jurisdiction of ASTM Committee DS on
Coal and Coke and are the direct resnonsibiitv of Subcommittee DOS.29 on Major
Elements in Ash and Trace Elements of Coal:
6. Purity of Reagents and Materials
Current edition approved Sept. 10, 1995. Published April 1996. Originally 6.1 Purity of Reagents-Reagent grade chemicals shall be
published as D 2795 -69. Last previous edition D 2795 - 86 (1991)“.
z Annual Book of ASTM Standards, VolO5.05.
used in all tests. Unless otherwise indicated, it is intended
s Annual Book ofASTM Standards, Vol I 1.OI. that all reagents shall conform to the specifications of the
4 Annual Book o/ASTM Standards, Vol 14.02. Committee on Analytical Reagents of the American Chem-

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 ASTM

Fuse 005 q ash with

NoOH. Dissolve in
water on* HCL.

IOml IOnI lOlS?l 25ml 25 ml 25 ml

I

DllUlO Hydroqen
to 50 ml. pcrozide
USC IO Ill,. in
of dilute 5 QlrClllt
sample.
“2”4
o-phm-
onthrolinc
510 nm 410 nm
: :
I
SiOp “‘203 F’2% COD MO

FIG. 1 Outline of Methodsfor Analysisof Coal Ash

ical Society, where such specifications are available.5 Other

grades may be used, provided it is first ascertained that the 9. Preparation of Analysis Solutions (Sample, Standards,
reagent is of sufficiently high purity to petit its use without and Blank)
lessening the accuracy of the determination. 9.1 Reagents and Materials:
6.2 Purity of Water-Unless otherwise indicated, refer- 9.1.1 HydrochloricAcid (I+ I)-Mix 1 volume of concen-
ences to water shall be understood to mean Type II reagent trated hydrochloric acid (HCl, sp gr 1.19) with 1 volume of
water as defined in specification D 1193. water.
9.1.2 Hydrofluoric Acid (sp gr 1.15)-Concentrated
hydrofluoric acid (HF).
7. Sample 9.1.3 National Institute of Standards and Technology
7.1 Prepare the analysis sample in accordance with Test (NISr) Sample No. 99a Soda Feldspar.6
Method D 2013 or Practice D 346 by pulverizing the mate 9.1.4 Nitric Acid (sp gr 1.42)-Concentrated nitric acid
rial to pass 250 pm (No. 60) sieve. (HNW.
7.2 Analyze separate test portions for moisture and ash 9.1.5 Sodium Hydroxide (NaOH) pellets.
9.1.6 Surfuric Acid (l+l)-Mix carefully while stirring 1
contents in accordance with Test Methods D 3 173, D 3 174,
volume of concentrated sulfuric acid (H$O.,, sp gr 1.84) into
or D 5 142 so that calculations to other bases can be made.
1 volume of water.
9.2 Procedure:
8. Preparation of Coal Ash and Coke Ash 9.2.1 The methods described are for typical ash samples;
however, different dilutions or aliquots than those specified
8.1 Procedure-Prepare 3 to 5 g of ash from the analysis may be preferable to attain suitable concentrations for
sample. Spread the coal or coke in a layer not over 6 mm (*/4 proper intensities for various constituents. Colors developed
in.) in depth in a fireclay or porcelain roasting dish. Place in as specified are stable unless otherwise stated. Although the
a cold muffle furnace and heat gradually so that the methods are described for a single sample, a group of ten or
temperature reaches 5WC in 1 h and 750°C in 2 h. Ignite to more can be processed at the same time. Each numbered
constant weight (+O.OOl g, Note 2), at 750°C. Allow the ash step should be completed for the group of samples being
to cool, transfer to an agate mortar, and grind to pass a analyzed before proceeding to the next step.
150~pm (No. 100) U.S.A. standard sieve. Reignite the ash at 9.2.2 Solution A for Si02 and AlJO Determination-
750°C for 1 h, cool rapidly, and immediately weigh portions Weigh 0.0500 g of sample and transfer to a 50-mL nickel
for analysis. If samples are stored, reignite the ash before crucible. Add 1.5 g of NaOH, cover the crucible, and heat in
weighing or determine loss on ignition at 75o’C on a separate a gas flame to melt the NaOH. Swirl gently to ensure that no
sample weighed out at the same time as the analysis sample. particles of sample float on the surface of the melt. Continue
Thoroughly mix each sample before weighing. fusion for about 5 min at dull red heat; then remove the
crucible from the flame and swirl the melt, while cooling, to
NOTE 2-Coke may be ignited to constant weight at a temperature coat the crucible wall. Add about 25 mL of water to the melt
not exceeding 950°C if diffbzulty in ashing is encountered. and let stand for at least 1 h or overnight if convenient. Pour
the contents of the crucible into a 600-mL beaker containing
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400 mL of water and 20 mL of HCl (l+ 1). (Do not allow the
s Reagenl Chemicals, American Chemical Society Spec$caGons, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United Slates Pharmacopeia 6National Institute of Standards and Technology Sample No. 99a, soda
and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC). feldspar contains 65.2 96 Si02 and 20.5 76 Al,O,. This reagent is used for
Rockville, MD. standardization purposes only.

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 ASTM D2795 95 - 0759530 0583225 377 -

nickel crucible to come in contact with the acid.) With a mixing during the additions. Dilute contents of this flask
rubber policeman, remove any residue from the crucible and immediately to the lOO-mL mark and mix before proceeding
wash it into a beaker. Clean a lOOO-mLvolumetric flask with to the next flask. Let each solution stand 1 h; then determine
HCl ( 1+ 1), rinse with water, and then transfer the solution in its absorbance at 650 nm, using the blank solution as a
the beaker to it. Dilute with water to the lOOO-mL mark and reference, assumed to have zero absorbance.
mix.
9.2.2.1 Standard Solutionfor SiOz and AlJO Determina-
tion-prepare duplicate standard solutions in the same 12. Calculation
manner (see 9.2.2) using 0.0500-g portions of NIST Sample 12.1 Compute factorsfi and fi for each standard solution
No. 99a, soda feldspar.6 Also prepare a blank solution as in as follows:
9.2.2, but omit the soda feldspar. Store the standard and fi = C,JA, and& = WA2 (1)
blank solutions in plastic bottles.
where:
9.2.3 Solution B for Fe,O,, Ti02, P,O,, CaO, MgO,
CS = concentration of Si02 in the standard
Na,O, and K,O Determinations-Treat 0.400 * 0.0005 g of
sample, %, and
sample in a 30-mL platinum crucible with 3 cm3 of HzS04
A,andA2 = absorbances for replicate standard solution
( 1+ 1) and 10 mL of HF. Evaporate on an air bath until most
each containing 50 mg of standard sample.
of the HF is removed then add 1 mL of HN03, and continue
12.2 Calculate the percent of silica in the ash as follows:
heating until strong fumes of sulfur trioxide (SO,) evolve.
Cool the crucible and contents, add water to dissolve the Si02, % = FA (2)
residue, and digest on an air bath for l/2 h. Transfer the where:
contents of the crucible to a 250-mL volumetric flask. Cool F = Cfi +.iW, and
to room temperature then dilute to the 250-mL mark and A = absorbance of the sample solution containing 50 mg of
mix (Note 3). Also prepare a blank Solution B (8.2.3), ash.
omitting the sample. Because of the possibility of alkali
contamination from the glass from which the flask is made,
determine sodium and potassium the same day that Solution ALUMINUM OXIDE (Al,O,)
B is prepared, or withdraw 25 mL with a pipet and store in a
plastic bottle. 13. Reagents
NOTE 3-Although some calcium sulfate (CasO,) from samples high 13.1 Acetic Acid, Glacial (CH,COOH).
in calcium may not dissolve during digestion in the crucible, it normally 13.2 Alizarin Red-S Solution (0.1 % in water).
will dissolve on further dilution. A small quantity of insoluble barium
sulfate (BaSO,) may still remain with some samples. This will settle to
13.3 Calcium Chloride Solution (CaC12) (7 g/500 mL)-
the bottom of the flask and not interfere in determining the main Transfer 7 g of calcium carbonate (CaCO,) to a 250-mL
constituents. If appreciable insoluble residue is present, the solution can beaker. Add about 50 mL of water and HCl (l+ 1) in drops
be filtered into another 250-mL flask before finally diluting to the mark. until the CaCO, is dissolved. Boil the solution for 1 to 2 min,
cool, and dilute with water to 500 mL.
SILICON DIOXIDE (SiO,) 13.4 Bufir Solution-Dissolve 70 g of sodium acetate
(CH,COONa. 3H,O) in water, add 30 mL of CH,COOH,
10. Reagents
and dilute to 500 mL.
10.1 Ammonium Molybdate Solution (7.5 g/l00 mL)- 13.5 Hydroxylamine Hydrochloride Solution (10 % in
Dissolve 7.5 g of ammonium molybdate ((NH,),Mo,02, - water)-Prepare fresh.
4H20) in 75 mL of water. Add 10 mL H2S04 (l+l) and 13.6 Thioglycollic Acid (5 %)-Dilute 5 mL of
dilute to 100 mL. Store in a plastic bottle. thioglycollic acid to 100 mL with water. Prepare fresh.
10.2 Reducing Solution-Dissolve 0.7 g of sodium sulfite
(Na$O, . 7Hz0) in 10 cm3 of water. Add 0.15 g of l-
amino-2-naphthol+sulfonic acid and stir until dissolved. 14. Procedure
Dissolve 9.0 g of sodium metabisulfite (Na,S,O,) in 90 mL 14.1 Pipet a IO-mL aliquot of Sample Solution A, 20 mL
of water, and add this solution to the solution above and of each Standard Solution A, and 20 mL of blank solution
mix. Store in a plastic bottle. Unless this solution is freshly into separate lOO-mL volumetric flasks. Then pipet 10 mL of
prepared, check the reducing properties of the solution blank solution to the flask containing 10 mL of sample
against a known standard. solution to maintain correct pH. For ash samples that
10.3 Tartaric Acid Solution (10 % in water)-Store in a contain less than 20 % A120a take a 20-mL aliquot directly
plastic bottle. from Sample Solution A. Add from pipets, in the following
order, mixing thoroughly after addition of each reagent, 1
11. Procedure cm3 of CaCl, solution, 1 mL of hydroxylamine hydrochlo-
11.1 Pipet a lo-mL aliquot of blank solution and 10 mL ride solution, and 1 mL of thioglycollic acid solution. From a
of each standard solution and Sample Solution A into graduated cylinder add 10 mL of buffer solution to each flask
separate lOO-mL volumetric flasks. Dilute each solution to and allow to stand 10 min. Add 5 mL of alizarin red-S
50 or 60 mL with water and mix. Add 1.5 mL of ammonium solution with a pipet, dilute to 100 mL, and mix. Allow each
molybdate solution with a measuring pipet, mix, and let solution to stand for 1 h, and measure absorbance at 475 nm
stand 10 min. Pipet 4 mL of tartaric acid solution followed using the blank solution as a reference, assumed to have zero
immediately by 1 mL of reducing solution into the first flask, absorbance.

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 ASTM DE’795 95 m 07595lro 0583226 203 m

15. Calculation 3.2 mg of sample (B). For samples containing more than 15 % of Fe,O,,
take a S-mL aliquot of the diluted sample solution which contains 1.6
15.1 Compute factors fi and fi for each standard test as mg of sample.
follows:
TITANIUM DIOXIDE (Pi03
h = GI-4 and.4 = CAlA2 (3)
where: 19. Reagents
CA = concentration of AlzO, in standard feldspar 19.1 Hydrogen Peroxide (3 %)--Prepare a 3 % solution of
sample, %, and hydrogen peroxide (H202) in water.
A, and A2 = absorbances for replicate standard solutions.
19.2 Titanium, Standard Solution (1 mL = 0.20 mg
15.2 Calculate the percent Al,Os as follows:
TiOJ-Transfer 0.2008 f 0.0005 g of NIST Sample No.
For lo-mL aliquot of Sample Solution A:
154a (99.6 % TiOl) or the appropriate amount of reagent
A&O,, % in ash = 2 FA (4) TiOz of known composition to a platinum crucible. Fuse
For 20-mL aliquot of Sample Solution A: with potassium pyrosulfate (in the ratio of about 4+1).
Dissolve the melt in 50 mL of H2S04 (I+ 1) cool, and dilute
AlaOs, % m ash = FA (5)
to 1000 mL in a volumetric flask.
where:
F = C.h +.I%& and 20. Calibration
A = absorbance of sample solution. 20.1 Transfer 5.0 mL of standard titanium solution to a
50-mL volumetric Flask No. 1, and add about 25 mL of
FERRIC OXIDE (Fe,O,)
water. Add 25 mL of water to Flask No. 2. To each flask, add
5 mL of H,SO, (1+ 1) and cool to room temperature. Add 5
16. Reagents
mL of H202 to Flask No. 1, fill both flasks to the 50-mL
16.1 Hydroxylamine Hydrochloride Solution (10 %)- mark with water, and mix. Measure the absorbance of the
Prepare a 10 % solution of hydroxylamine hydrochloride solution from Flask No. 1 at 410 nm and use the reagent
(NH,OH . HCl) in water. blank in Flask No. 2 as the reference, assumed to have zero
16.2 Orthophenanthroline(0.1 %)-Prepare a 0.1 % solu- absorbance.
tion in water.
16.3 Sodium Citrate (10 %)-Prepare a 10 % solution of 21. Procedure
sodium citrate (Na,CsHs0,*2H20) in water. 21.1 Pipet a 25-mL portion of Sample Solution B (see
16.4 Iron, Standard Solution (1 mL = 0.1 mg FeZOs)- 9.2.3) into a 50-mL volumetric flask (No. 1) and for the
Dissolve 0.2455 st 0.0005 g of ferrous ammonium sulfate reference solution pipet a second 25-mL portion of Solution
Fe(NH&(SO& v6HzO in water, add 3 mL of H2S04 (l+l), B to another 50-mL flask (No. 2). Add 5 cm of HzSO., (I+ 1)
and dilute to 500 mL. to each flask, mix, and cool to room temperature. Then add
5 mL of Hz02 to Flask No. 1. Fill both flasks to the 50-mL
17. Procedure mark with water and mix. Measure absorbance at 4 10 nm of
17.1 Dilute 10 mL of Sample Solution B to 50 mL in a solution from Flask No. 1 using the solution from Flask No.
volumetric flask. Pipet 10 cm3 of diluted sample solution 2 as the reference, assumed to have zero absorbance.
into a IOO-mL volumetric flask, pipet 5 cm3 of standard iron
solution into another lOO-mL flask, and add nothing to a 22. Calculation
third flask for reagent blank. Add 5 mL of hydroxylamine 22.1 Calculate the percent TiOz as follows:
hydrochloride solution with a graduated cylinder to each
TiO,, % - (AC,/A,B) x 100 (7)
flask, and allow to stand for 10 min. Then add 10 mL of
orthophenanthroline solution with a graduated cylinder to where:
each flask and mix. Finally, add 10 mL of sodium citrate A = absorbance of sample solution,
solution with a graduated cylinder to each flask, dilute to 100 Al = absorbance of standard titanium solution,
mL with water, and mix. After 1 h measure absorbance at B = sample contained in final dilution of Solution B, mg,
5 10 nm, using the reagent blank as reference, assumed to and
have zero absorbance. CT = TiOz in aliquot taken for standard titanium solution,
mg.
18. Calculation NOTES-For the dilutions given, CT = 1 mg TiO, and B = 40 mg of
18.1 Calculate the percent FeZOs as follows: sample. Using these figures the above equation reduces to:
Fe,O,, % = (AC,/A,B) X 100 Ti02, % = 2.5 A/A,
(6)
where: PHOSPHORUS PENTOXIDE (PzOs)
A = absorbance of sample solution.
Al = absorbance of standard iron solution, 23. Reagents
B = sample contained in the final dilution of Solution B 23.1 Molybdivunudate Solution-Dissolve 0.625 g of
(9.23 and Section 17), mg, and ammonium metavanadate (NH,VO,) in 200 mL HN03
C, = Fe,03 in aliquot taken for standard iron solution, mg. (l+l) (1 volume of HN03, sp gr 1.42, and 1 volume of
NOTE4-For the dilutions given, 5 mL of standard iron solution water). Dissolve 25 g of ammonium molybdate
contains 0.5 mg of Fe,O, (C,) and the diluted sample solution contains ((NH4)6M07024.4H20) in 200 mL of water. Pour the
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 ASTM DE!795 95 m 0759530 0583227 LYT m

ammonium molybdate solution into the metavanadate solu- triethanolamine with water to 1000 mL and mix.
tion while stirring and dilute to 500 mL with water.
23.2 Phosphorw Pentoxide, Standard ConcentratedStock 27. Procedure for CaO
SoluCion-Dissolve 0.3835 f 0.0005 g of potassium 27.1 Pipet 25 mL of Sample Solution B and 25 mL of the
dihydrogen phosphate (KH,PO,), which has been dried at blank solution into separate 500-mL Erlenmeyer flasks.
1lo”C, in water, and dilute to 1000 mL with water. Dilute with water to approximately 100 mL. Add 20 drops of
23.3 Phosphorus Pentoxide, Standard Working Solu- concentrated HCl, 5 mL of the triethanolamine solution, 5
tion-Dilute 50 mL of concentrated stock solution to 500 mL of NH,OH, and 10 mL of KOH solution in that order,
mL with water. Each 25 mL of this solution contains 0.50 mixing afier addition of each reagent. Dilute with water to
mg of PZOs. about 200 mL. Add approximately 40 mg of calcein indi-
cator and titrate with standard EDTA solution until the color
24. Procedure changes from a green fluorescence to purple. Observe the
24.1 Pipet a 25-mL aliquot from Sample Solution B, 25 color change in diffused light looking down through the flask
mL of standard working solution, and 25 mL of the blank to a black surface.
solution into separate 50-mL volumetric flasks. With a pipet
add 10 mL of molybdivanadate solution to each flask, dilute 28. Procedure for MgO
with water to the mark, and allow to stand for 5 min. 28.1 Pipet 25 mL of Sample Solution B and 25 mL of
Measure the absorbance at 430 nm, using the reagent blank blank solution into separate 500-mL Erlenmeyer flasks.
as the reference, assumed to have zero absorbance. Dilute with water to about 100 mL. Add 20 drops of
concentrated HCl, 20 mL of triethanolamine solution, and
25. Calculation 25 mL of NH,OH, mixing after addition of each reagent.
25.1 Calculate the percent P,O, as follows: Dilute with water to approximately 200 mL. Add a volume
P,O,, % = (AC,/A,B) x 100 0-U of standard EDTA solution slightly less than the calcium
titer; then add about 40 mg of phthalein purple indicator.
where: Continue the titration until the color changes from pale
A = absorbance of the sample solution, purple to colorless or pale grey. A slight excess of EDTA
A, = absorbance of the standard phosphorus solution, solution produces a green coloration. Observe the color
B = sample contained in final dilution of Solution B, mg, change in diffused light looking down through the flask to a
and white surface.
cp = PZOs in the aliquot taken for the standard phos-
phorus solution, mg. 29. Calculations
NOTE6-For the dilutions given, C, = 0.50 mg and B = 40 mg of 29.1 Calculate the percent CaO as follows:
sample. Using these figures the above equation reduces to:
cao ~ _ v, x w50/4
P,O,, % = 1.25 A/A, , a- x 100
W (9)
CALCIUM OXIDE (CaO) AND MAGNESIUM OXIDE (MgO) where:
V, = volume of EDTA solution required for the calcium
26. Reagents
titration, minus the volume of EDTA solution re-
26.1 Ammonium Hydroxide (sp gr 0.90)-Concentrated quired for the blank titration, mL,
ammonium hydroxide (NH,OH). F = grams of CaO = 1 mL EDTA,
26.2 Calcein Indicator-Mix 0.2 g of calcein, 0.12 g of W = grams of sample, and
thymolphthalein, and 20 g of finely ground potassium A = volume of aliquot, mL.
chloride (KCl).
NOTE7-If W = 0.4 g, F = 0.0056 g, and A = 25 mL, then percent of
26.3 EDTA Solution-Dissolve 3.720 g of the disodium CaO = 1.4 V,.
salt of ethylenediaminetetraacetic acid (EDTA) in water and
dilute to 1000 mL. Standardize against the standard calcium 29.2 Calculate the percent MgO as follows:
solution using calcein or phthalein purple indicator. - V,NO.7 19F)G5O/A) x 1oo
MgO, % = (”
26.4 Hydrochloric Acid (sp gr 1.19)-Concentrated hy- W (10)
drochloric acid (HCI). where:
26.5 Hydrochforic Acid (l+l)-Mix 1 volume of con- = volumes of EDTA required for calcium plus
v2
centrated HCl (sp gr 1.19) with 1 volume of water. magnesium titration minus volume of EDTA
26.6 Phthalein Purple Indicator-Mix 0.1 g of phthalein
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solution required for blank titration, mL, and

purpIe, 0.005 g of methyl red, and 0.05 g of naphthol green B 0.719F = grams MgO = 1 mL EDTA.
with 10 g of finely ground KCl. Remaining symbols are the same as for computing percent
26.7 Potassium Hydroxide Solution (224.4 g/L)-Dis- CaO.
solve 224.4 g of potassium hydroxide (KOH 85 X) in water
and dilute to 1000 mL. Store in a plastic bottle, SODIUM OXIDE (Na,O) AND POTASSIUM OXIDE (K20)
26.8 Calcium Standard Solution (1.000 g/L) (1 mL =
0.00056 g CaO)-Dissolve 1.000 g of calcium carbonate 30. Reagents
(CaC03) in water with 4 mL of HCl (l+l). Heat to boiling 30.1 Potassium, Concentrated Stock Solution ( 100
to expel carbon dioxide (CO,), cool, and dilute to 1000 mL. ppm)-Dissolve 0.2228 + 0.0005 g of potassium sulfate
26.9 Triethanolamine Solution-Dilute 500 mL of (K2S04) in water and dilute to 1000 mL.

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30.2 Potassium, Standard Solution (50 ppm)-Pipet 50 for the standard potassium solutions at a wavelength of 768
mL of potassium stock solution into a IOO-mL volumetric nm, and plot the data obtained.
flask. Add 10 mL of synthetic ash solution and 10 mL of
sodium stock solution, dilute with water to the mark, and 32. Procedure
mix. The solution contains 50 ppm of potassium. As the 32.1 Operate the flame spectrophotometer in the manner
standard lO-ppm sodium solution contains 10 ppm of used for calibration. Rinse a sample cup with the solution it
potassium, use it also for the standard IO-ppm potassium is to contain, and fill separate cups with standard 50 and 10
solution. Store in plastic bottles. ppm of sodium solution, Sample Solution B, Blank Solution
30.3 Sodium, Concentrated Stock Solution (100 ppm)- B, and water, Adjust the instrument for the 10 to 50-ppm
Dissolve 0.3088 f 0.0005 g of dried sodium sulfate (Na,SO,) range at the sodium wavelength (589 nm), using the standard
in water and dilute to 1000 mL. 50-ppm sodium solution, and determine readings for the
30.4 Sodium, Standard Solutions(10 and 50 ppm)-Pipet sample solution and the blank. When the sample solution
10 and 50 mL of sodium stock solution into separate contains less than 10 ppm of sodium, make readings in the 1
lOO-mL volumetric flasks. Add 10 mL of synthetic ash to IO-ppm range after adjusting the instrument with the
solution and 10 mL of potassium stock solution to each lo-ppm sodium solution. For samples rich in sodium, dilute
flask, dilute with water to the lOO-mL mark, and mix. The an aliquot of Solution B for the test. Make similar readings at
solutions contain 10 and 50 ppm of sodium. 768 nm for potassium, using the standard 50 and IO-ppm
30.5 Ash (Synthetic) Solution: potassium solutions to adjust the spectrophotometer. Sub
30.5.1 Dissolve 2.0 g of iron in 10 mL of sulfuric acid tract the blank reading from the sample reading, and
(H2S04) (l+l) and 100 mL of water. determine the concentration of sodium and potassium (C,
30.5.2 Dissolve 1.O g of aluminum in 10 mL of H,SO., and C,) in the test solution from the appropriate working
(l+l) and 100 mL of water. curve.
30.5.3 Dissolve 1.25 g of CaC03 in 3 mL of H$O, (1+ 1) 32.2 When using a flame filter photometer for determina-
and about 600 mL of water. tion of sodium, these spectral interferences should be noted.
30.5.4 Dissolve 1.0 g of magnesium sulfate (MgSO, A 5:1 concentration of potassium-to-sodium and a 1O:l
. 7Hz0) in water. concentration of calcium-to-sodium produce spectral inter-
30.5.5 Combine the solutions in 30.5.1 through 30.5.4, ferences that can result in an apparent increase in sodium
filter, and dilute with water to 1000 mL. content at the 589-nm sodium line.

31. Calibration 33. Calculation

31.1 Prepare additional standard sodium solutions con- 33.1 Calculate the percent Nat0 as follows:
taining 1, 4, 20, 30, and 40 ppm of sodium and standard Na,O, % = C, x 1.348/16 (11)
potassium solutions containing 1, 4, 20, 30 and 40 ppm of where:
potassium. These are prepared by taking appropriate aliquots c, = ppm sodium when 0.4 g of sample in 250 mL of
from the concentrated stock solutions (30.1 and 30.3) and Solution B is used.
proceeding as described in 30.2 and 30.4. Also prepare blank
solutions, the sodium blank containing 10 mL of synthetic 33.2 Calculate the percent KzO as follows:
ash solution and 10 mL of stock potassium solution per 100 K,O, % = C, x 1.2046/16 (12)
mL, and the potassium blank containing 10 mL of synthetic where:
ash solution and 10 mL of sodium stock solution per 100 C,= ppm potassium when 0.4 g of sample in 250 mL of
mL. Rinse each sample cup two times with the solution it is Solution B is used.
to contain before filling with the test solution. Afier adjusting
NOTI?8-If C,, = 10 ppm, then the sodium contained in 250 mL =
the flame spcctrophotometer according to the manufactur-
0.0025 g which originally came from 0.4 g ash; that is,
er’s directions, set the wavelength to 589 nm and aspirate the
50-ppm sodium solution. Move the wavelength control [(ppmNa X Na,0/2Na)/ppm of sample] x 100 = Na,O, %
slightly back and forth at the sodium wavelength to find the or
setting for maximum response. Finally, while aspirating the Na,O, % = [(0.0025)(1.348)/0.4] x 100 = 0.84.
50-ppm sodium solution, adjust the slit width and sensitivity The factor 16used in the above equationswasderived from this kind of
to achieve a transmittance reading of 80 %. Rinse the calculation and permits use of “parts per million” directly without
aspirator with water, and determine the transmittance conversion to “grams” of sodium or potassium.
reading for the 40-ppm sodium solution. Repeat this opera-
tion, checking that the transmittance reads 80 % for the 34. Report
50-ppm sodium solution, and take readings for the 30, 20, 34.1 Report the percentages for the elemental oxides in
and IO-ppm sodium solutions. Test the blank solution, and the ash as specified in sections 12, 15, 18,22,25, 29, and 33.
subtract the blank reading from each determination. Prepare 34.2 Report the method used for concurrent moisture and
a working curve for the range from 10 to 50-ppm sodium. ash determinations, if applicable.
Make another working curve for the range from 1 to IO-ppm 34.3 Use Practice D 3 180 for procedures to convert values
sodium. To do this, aspirate the IO-ppm sodium solution to other bases.
and increase the slit width sufficiently to obtain a transmit-
tance reading of 80, and then determine readings for the 4 35. Precision and Bias
and l-ppm sodium solutions. Make similar measurements 35.1 Precision:

6
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 ASTM D2795 95 - 0759530 0583229 T12 W

TABLE 1 Repeatability and Reproducibility Limits or both, of the test results. The repeatability limits deter-
Percentof Ash mined by these test methods are listed in Table 1.
ElementalOxide
Repeatabilii Reproducibility 35.1.2 Reproducibility-The difference in absolute value
of replicate determinations carried out in different laborato-
SOP 1.o 2.0
ries, on representative samples prepared from the same bulk
4203
Fe203 0.7
0.3 ;:; ash sample, should not exceed the reproducibility limit for
no2 0.10 0.25 more than 5 % of such paired values (95 % confidence level).
P206 0.05 0.15
CaO 0.2 0.4 When such a difference is found to exceed the reproduc-
MO 0.3 0.5 ibility limit, there is reason to question one, or both, of the
NM’ 0.1 0.3 test results. The reproducibility limits determined by these
K,O 0.1 0.3
test methods are listed in Table 1.
35.2 Bias-Bias has not been determined.
35.1.1 Repeutabz’lify-The difference in absolute value
between the results of two consecutive tests, carried out on 36. Keywords
the same ash sample, in the same laboratory, by the same 36.1 aluminum oxide (A&OS); calcium oxide (CaO); ele-
operator, using the same apparatus, should not exceed the mental ash composition; ferric oxide (Fe,O,); flame photom-
repeatability limits for more than 5 % of such paired values etry; magnesium oxide (MgO); phosphorus pentoxide
(95 % confidence level). When such a difference is found to (P,O,); potassium oxide (K,O); silicon dioxide (SiO,); so-
exceed the repeatability limit, there is reason to question one, dium oxide (Na,O); titanium dioxide (TiOJ

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