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Designation: E 1081 – 95a
Standard Test Method for
Determination of Total Iron in Iron Ores and Related
Materials by Silver Reduction-Dichromate Titration1
This standard is issued under the fixed designation E 1081; 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
1.1 This test method covers the determination of total iron
in ores, concentrates, and agglomerates in the concentration
range from 35 to 95 % iron, and is free from vanadium
interference.
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 appro-
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
1.3 Use of safety goggles is required for fusion with sodium
peroxide.
2. Referenced Documents
2.1 ASTM Standards:
D 1193 Specification for Reagent Water2
E 50 Practices for Apparatus, Reagents, and Safety Precau-
tions for Chemical Analysis of Metals3
E 877 Practice for Sampling and Sample Preparation of Iron
Ores and Related Materials4
E 882 Guide for Accountability and Quality Control in the
Chemical Analysis Laboratory4
E 1028 Test Method for Total Iron in Iron Ores by the
Dichromate Titrimetric Method4
3. Summary of Test Method
3.1 Acid Decomposition—The test sample is dissolved in
hydrochloric acid. The insoluble residue is removed by filtra-
tion, ignited, treated for the recovery of iron, and added to the
main solution.
3.2 Decomposition by Fusion—The test sample is fused
with sodium peroxide or sintered with sodium peroxide at
400°C, and fused over a burner. The melt is leached with water
and acidified with hydrochloric acid.
3.3 Reduction of Iron—The test sample solution is passed
through a silver-reductor. After addition of phosphoric acid-
1
This test method is under the jurisdiction of ASTM Committee E-1 on
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct
responsibility of Subcommittee E01.02 on Ores, Concentrates, and Related Metal-
lurgical Materials.
Current edition approved Nov. 10, 1995. Published January 1996. Originally
published as E 1081 – 85. Last previous edition E 1085 – 95.
2
Annual Book of ASTM Standards, Vol 11.01.
3 rods, 15 cm in length, crosswise and leave 4 h or overnight. Wash the
Annual Book of ASTM Standards, Vol 03.05.
4
Annual Book of ASTM Standards, Vol 03.06.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
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sulphuric acid mixture and diphenylamine-sulphonate indica-
tor, the total iron, is determined by titration with a standard
solution of potassium dichromate.
4. Significance and Use
4.1 This method for the analysis of iron ores concentrates
and agglomerates is primarily intended as a referee method to
test for compliance with compositional specifications. It is
assumed that all who use this test method will be trained
analysts capable of performing common laboratory procedures
skillfully and safely. It is expected that work will be performed
in a properly equipped laboratory and that proper waste
disposal procedures will be followed. Appropriate quality
control practices must be followed such as those described in
Guide E 882.
4.2 The determination of the total iron content is the
primary means for establishing the commercial value of iron
ores used in international trade and by industry.
5. Interferences
5.1 This test method is written for iron ores containing less
than 0.1 % of copper. Other elements, particularly vanadium,
normally found in iron ores do not interfere with this test
method.
6. Apparatus
6.1 Silver Reductor.
6.1.1 Preparation of Silver Reductor—Use a glass column
(2 cm in diameter and 25 cm in length) fitted with a stopcock
and a reservoir cup (about 100 mL in capacity, 4 cm in
diameter, and 9 cm in length).
6.1.1.1 Place glass wool very lightly above the stopper. Fill
column with HCl (1+11). Place silver powder into a 150-mL
beaker. Add HCl (1+11) and transfer the silver powder into the
column using HCl (1+11), avoiding the entrapment of air. Pass
about 100 mL of HCl (1+11) through the column.
NOTE 1—Care must be taken not to let the column dry. Always maintain
about 1 mL of HCl (1+11) above the silver powder.
NOTE 2—The height of silver in the column is about 17 cm and is
adequate for about 18 samples prior to regeneration. The flow rate is from
35 to 40 mL/min. Alternatively silver can be prepared by reducing silver
nitrate with zinc as follows: Dissolve 50 g of AgNO3(6.12) in 400 mL of
water in a 600-mL beaker. Add 10 mL of HNO3(6.8). Place two zinc metal
precipitated silver thoroughly by decantation using H2SO4(1+99). A glass
 E 1081
column (2 cm in diameter and 15 cm in length) fitted with a stopcock and
reservoir cup (about 100 mL in capacity, 4 cm in diameter, and 9 cm in
length) is used. Pack glass wool lightly above the stopper. Transfer the
washed, precipitated silver into the column using H2SO4(1+99) and
avoiding any trapped air. Wash the column with HCl (1+99) several times
(150 mL are sufficient) at a flow rate of 30 to 35 mL/min. (Length of the
silver column is about 9 cm.) The silver reductor is now ready. Always
maintain about 1 mL of HCl (1+11) above the column.
6.1.2 Regeneration of Silver Reductor—With the passage of
iron (III) the silver in the reductor darkens at the very top,
forming a greyish ring which extends down. When this ring
extends down to about 10 cm, the column should be regener-
ated as follows: Drain the solution (leaving about 1 cm on the
top and wash with 150 mL of H2SO4(1+99). Finally keep the
level of H2SO4(1+99) in the column about 1 cm above the
silver. Gently rest two zinc rods (6.20) in contact with the silver
in the column. Leave overnight. The dark color changes to
silvery white indicating complete regeneration to metallic
silver.
NOTE 3—Passing 50 mL of H2SO4(1+99) through the column acceler-
ates the regeneration. Then wash the column several times by passing HCl
(1+11). The column is ready for re-use. The regeneration can also be done
by emptying the contents into a beaker, placing zinc-rods and repacking as
in 7.4.1.
NOTE 4—If the flow is slow, remove the silver and the glass wool from
the column and repack as in 6.1.1. Ensure that the new glass wool is
placed very lightly for restoring the flow rate at 30 to 35 mL/min.
6.2 Weighing Spatula of a nonmagnetic material or demag-
netized stainless steel.
6.3 Zirconium (Metal) Crucibles, 50 mL capacity.
7. Reagents and Materials
7.1 Purity of Reagents—Reagent grade chemicals shall be
used in all tests. Unless otherwise indicated, it is intended that
all reagents conform to the specifications of the Committee on
Analytical Reagents of the American Chemical Society where
such specifications are available.5 Other grades may be used,
provided it is first ascertained that the reagent is of sufficient
high purity to permit its use without lessening the accuracy of
the determination.
7.2 Purity of Water—Unless otherwise indicated, references
to water shall be understood to mean reagent water as defined
by Type I of Specification D 1193.
7.3 Ammonium Hydroxide (sp gr 0.90)—Concentrated am-
monium hydroxide (NH4OH).
7.4 Hydrochloric Acid (sp gr 1.19)—Concentrated hydro-
chloric acid (HCl).
7.5 Hydrofluoric Acid (sp gr 1.15)—Concentrated hydrof-
luoric acid (HF).
7.6 Nitric Acid (sp gr 1.42)—Concentrated nitric acid
(HNO3).
7.7 Phosphoric Acid (sp gr 1.57)—Concentrated phosphoric
acid (H3PO4).
5
Reagent Chemicals, American Chemical Society Specifications, 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 States Pharmacopeia
and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
MD.
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7.8 Potassium Dichromate, Standard Solution (0.1 N)—
Pulverize about 6 g of potassium dichromate (K2Cr2O7)
reagent in an agate mortar, dry in an air-bath at 140°C for 3 to
4 h, and cool to room temperature in a desiccator. Dissolve
4.9040 g of the dry reagent in water and dilute the solution with
water to exactly 1 L in a volumetric flask.
7.9 Potassium Pyrosulfate (K2S2O7) Fine Powder.
7.10 Silver Nitrate (AgNO3).
7.11 Silver Powder—Johnson Matthey 40 to 60 mesh is
suitable.
7.12 Sodium Diphenylaminesulfonate Solution (2 g/L)—
Dissolve 0.2 g of the reagent (C6H5NC6H4·SO3Na) in water
and dilute to 100 mL. Store the solution in a brown glass bottle.
7.13 Sodium Peroxide (Na2O2) dry powder.
7.14 Sulfuric Acid (sp gr 1.84)—Concentrated sulfuric acid
(H2SO4).
7.15 Sulfuric Acid Phosphoric Acid Mixture—Pour 150 mL
of phosphoric acid (H3PO4) into about 400 mL of water. While
stirring, add 150 mL of sulfuric acid (H2SO4). Cool in a water
bath and dilute with water to 1 L.
7.16 Zinc Metal Rods, about 8 mm in diameter and about
150 mm in length.
8. Sampling and Sample Preparation
8.1 Collect and prepare gross samples in accordance with
Practice E 877.
8.2 The laboratory sample shall be pulverized to pass a No.
100 (150-µm) sieve.
NOTE 5—To facilitate decomposition, some ores, such as specular
hematite, require grinding to pass a No. 200 (75-µm) sieve.
9. Procedure
NOTE 6—If the procedure is based on acid decomposition, use steps in
9.1. If the procedure is based on fusion, use steps in 9.2.
9.1 Acid Decomposition:
9.1.1 Weigh approximately 0.3 g of prepared sample into a
small weighing bottle previously dried at about 105°C. Dry the
bottle and contents for 1 h at 105 to 110°C. Cap the bottle and
cool to room temperature in a desiccator. Momentarily release
the cap to equalize the pressure and weigh the capped bottle
and sample to the nearest 0.1 mg. Repeat the drying and
weighing until there is no further weight loss. Transfer the test
sample to a 250-mL beaker and reweigh the capped bottle to
the nearest 0.1 mg. The difference between the two weights is
the weight of the test sample taken for analysis.
9.1.2 Add 20 mL of HCl, cover the beaker with a watch
glass, and heat the solution gently without boiling, to decom-
pose the ore. Wash the watch glass with a jet of water and
dilute to 50 mL with warm water. Filter the insoluble residue
on a close texture paper. Wash the residue with warm HCl
(1+50), until the yellow color of iron (III) chloride is no longer
observed. Then wash with warm water six to eight times.
Collect the filtrate and washings in a 400-mL beaker.
9.1.3 Place the filter paper and residue in a platinum
crucible, dry, and ignite at 750 to 800°C. Allow the crucible to
cool, moisten the residue with H2SO4(1+1), add about 5 mL of
HF (7.5), and heat gently to remove silica and sulfuric acid.
Add to the cold crucible 2 g of K2S2O7, heat gently at first then
strongly until a clear melt is obtained. Cool, place the crucible
 E 1081
TABLE 1 Statistical Information 9.3 Place a 600-mL beaker under the silver reductor. Pass
Repeatability, r Reproducibility, R the solution through the silver reductor at a rate of 35 mL/min,
Mean Iron, (2.8 s r) (2.8 s L) retaining about 1 cm over the silver top. Rinse the reservoir and
Sample
% Acid Acid
Fusion
Decomposition
Fusion
Decomposition column 2 to 3 times with HCl (1+11) and drain the rinsings.
76-17 67.18 0.22 0.18 1.54 0.21 Finally pass 150 mL of hydrochloric acid (1+11) at a rate of 35
81-2 59.57 0.21 0.21 1.47 0.23 mL/min to elute the reduced iron completely from the silver
76-12 60.67 0.21 0.20 1.47 0.23
reductor, leaving 1 cm of the acid over the silver top (Note 1).
9.4 To the reduced iron and washings in the 600-mL beaker,
TABLE 2 Bias Fusion Decomposition add 30 mL of sulfuric acid phosphoric acid mixture and add 5
Standard Fe Average Fe Content
to 6 drops of sodium diphenylamine-sulphonate indicator
Sample Designation solution (2 g/L).
Content, % Reported
JSS-852 Savage River Pellets 67.23 67.084 9.5 Titrate immediately with standard K2Cr2O7 solution to a
JSS-850-1 Marcona Pellets 66.78 66.781 permanent purple endpoint. The endpoint is discernible within
NBS-692 Labrador 59.58 59.613 0.02 mL (Note 9).
SCH-1 Canadian Standard 60.73 60.648

10. Calculation
TABLE 3 Bias Acid Decomposition 10.1 Calculate the iron content as follows:
Standard or T 3 0.0055847 3 100 T 3 0.55847
Sample Designation Assumed Fe
Average Fe Content Iron, % ~m/m! 5 m 5 m (1)
Reported
Content, %
JSS-850-3 Marcona Pellets 66.78 66.814 where:
SCH-1 Canadian Standard 60.73 60.669 T 5 the volume in millilitres of potassium dichromate
NBS-692 Labrador 59.58 59.636 standard solution used for the titration (Note 9), and
LM-07 Brazilian Ore 45.96 45.928
m 5 the mass, in grams of the test portion.
NOTE 9—The procedure blank has been established to be 0.02 mL, the
same volume required to discern the endpoint.
in a 250-mL beaker, add about 25 mL of water and about 5 mL
of HCl, and warm to dissolve the melt. Remove and wash the 11. Precision and Bias 6
crucible. Adjust the solution to a slight alkalinity with ammo-
11.1 Precision—Thirty-three laboratories in 9 countries in-
nia solution (NH4OH). Heat to coagulate the precipitate, filter
cluding laboratories from the USA, participated in the interna-
on a coarse-texture paper, and wash several times with hot
tional testing of the fusion decomposition procedure of this test
water. Discard the filtrate. Place the beaker containing the main
method using four iron ore samples of varying composition.
solution under the funnel and dissolve the precipitate on the
Also 17 laboratories in 5 countries analyzed four iron ore
filter paper by pouring over it 5 mL of hot HCl (1+2) wash the
samples of varying composition by the acid decomposition
filter, first six to eight times with warm HCl (1+50) then twice
procedure of this test method.
with hot water. Dilute to about 180 mL with water and follow
11.1.1 The test results were conducted under the auspices of
the procedure given under 9.3-9.5.
WG17B of ISO Committee TC-102/SC2. The precision of this
9.2 Fusion Decomposition:
test method is expressed by the following regression formulae:
9.2.1 Dry and weigh the test sample in accordance with
Fusion Decomposition Acid Decomposition
9.1.1 and transfer to a dry zirconium crucible containing 2 g of r 5 0.0012 X + 0.1484 r 5 −0.0032 X + 0.3944
sodium peroxide. Mix the contents with a dry spatula. p 5 0.0085 X + 0.8789 p 5 −0.0025 X + 0.4309
9.2.1.1 Fuse over a Meker burner (low heat) swirling the sigma r 5 0.0004 X + 0.0525 sigma r 5 −0.0011 X + 0.1393
sigma L 5 0.0034 X + 0.3208 sigma L 5 −0.0006 X + 0.1170
crucible until the melt is cherry red and clear. Remove the
crucible from the heat and swirl it until the melt solidifies on where:
the crucible wall. X 5 the iron content in percent (m/m), of the test
NOTE 7—In case of high humidity, place the crucible on a hot plate for
sample,
10 to 15 min to dry the contents. r 5 the permissible tolerance within laboratory (re-
NOTE 8—If desired, place the crucible in a muffle furnace at 400°C peatability),
(prior to fusion) for 10 to 15 min. p 5 the permissible tolerance between laboratories,
sigma r 5 the within laboratory standard deviation, and
9.2.2 Allow the crucible to cool in air for 1 to 2 min and sigma L 5 the between laboratory standard deviation.
place it in a dry 250-mL beaker. Add about 10 mL of water into 11.1.2 Precision results are shown in Table 1.
the crucible, while covering the beaker with a watch glass. 11.2 Bias—Evidence for the absence of any measurable bias
After effervescence has ceased, empty the crucible contents is provided by a comparison of the ISO results reported in 11.1
into the beaker and wash the crucible with 15 to 20 mL of by this test method with the results obtained on the same
water. Introduce 10 mL of HCl (7.4), via the crucible, into the samples by two other test methods WG16B and WG23A
beaker and rinse the crucible with water. Boil the solution in
the beaker for 3 to 4 min. Wash the sides of the beaker and
watch glass with water and continue boiling for about 30 s. 6
Supporting data are available from ASTM Headquarters. Request RR: E16-
Cool and dilute the solution to about 60 mL with water. 1010.

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 E 1081
(similar to Test Method E 1028). These test methods have been 12. Keywords
accepted in the meantime as ISO (DIS) Standards, the com- 12.1 agglomerates and related materials; concentrates; iron
parison is tabulated in Table 2 and Table 3. content; iron ores

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