ASTM E364-94(2000)
(Test Method)Standard Test Methods for Chemical Analysis of Ferrochrome-Silicon (Withdrawn 2006)
Standard Test Methods for Chemical Analysis of Ferrochrome-Silicon (Withdrawn 2006)
SCOPE
1.1 These test methods cover the chemical analysis of ferrochrome-silicon having chemical compositions within the following limits:ElementConcentration,%Aluminum0.50 maxAntimony0.005 maxArsenic 0.005 maxBismuth 0.005 maxBoron 0.005 maxCarbon 0.15 maxChromium34.0 to 47.0Cobalt 0.10 maxColumbium0.050 maxCopper 0.050 maxLead 0.005 maxManganese0.75 maxMolybdenum0.050 maxNickel 0.50 maxNitrogen0.050 maxPhosphorus0.030 maxSilicon 30.0 to 45.0Silver 0.005 maxSulfur 0.030 maxTantalum0.050 maxTin 0.005 maxTitanium0.50 maxVanadium0.50 maxZinc 0.005 maxZirconium0.050 max
1.2 The test methods appear in the following order:SectionsArsenic by the Molybdenum Blue Photometric Method 8-18Chromium by the Acid Dissolution Titrimetric Method 19-25Silicon by the Sodium Peroxide Fusion-Perchloric Acid Dehydration Method26-33
1.3This 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. For precautions to be observed in these test methods, refer to Practices E50, and to precautions included in the individual methods.
WITHDRAWN RATIONALE
These test methods cover the chemical analysis of ferrochrome-silicon having chemical compositions within specified limits.
Formerly under the jurisdiction of Committee E01 on Analytical Chemistry for Metals, Ores, and Related Materials, these test methods were withdrawn in September 2006.
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:E364–94 (Reapproved 2000)
Standard Test Methods for
Chemical Analysis of Ferrochrome-Silicon
This standard is issued under the fixed designation E 364; 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 bility of regulatory limitations prior to use. For precautions to
be observed in these test methods, refer to Practices E 50, and
1.1 These test methods cover the chemical analysis of
to precautions included in the individual methods.
ferrochrome-silicon having chemical compositions within the
following limits:
2. Referenced Documents
Concen-
2.1 ASTM Standards:
tration,
Element %
A 482 Specification for Ferrochrome-Silicon
Aluminum 0.50 max
E 29 Practice for Using Significant Digits in Test Data to
Antimony 0.005 max
Determine Conformance with Specifications
Arsenic 0.005 max
Bismuth 0.005 max
E 32 PracticesforSamplingFerroalloysandSteelAdditives
Boron 0.005 max
for Determination of Chemical Composition
Carbon 0.15 max
E 50 Practices for Apparatus, Reagents, and Safety Precau-
Chromium 34.0 to 47.0
Cobalt 0.10 max
tions for Chemical Analysis of Metals
Columbium 0.050 max
E 60 Practice for Photometric and Spectrophotometric
Copper 0.050 max
Methods for Chemical Analysis of Metals
Lead 0.005 max
Manganese 0.75 max
E 173 Practice for Conducting Interlaboratory Studies of
Molybdenum 0.050 max
Methods for Chemical Analysis of Metals
Nickel 0.50 max
Nitrogen 0.050 max E 360 Test Methods for Chemical Analysis of Silicon and
Phosphorus 0.030 max
Ferrosilicon
Silicon 30.0 to 45.0
Silver 0.005 max
3. Significance and Use
Sulfur 0.030 max
Tantalum 0.050 max
3.1 These test methods for the chemical analysis of metals
Tin 0.005 max
and alloys are primarily intended to test such materials for
Titanium 0.50 max
compliance with compositional specifications. It is assumed
Vanadium 0.50 max
Zinc 0.005 max
that all who use these test methods will be trained analysts
Zirconium 0.050 max
capable of performing common laboratory procedures skill-
1.2 The test methods appear in the following order: fully and safely. It is expected that work will be performed in
Sections a properly equipped laboratory.
Arsenic by the Molybdenum Blue Photometric Method 8-18
Chromium by the Acid Dissolution Titrimetric Method 19-25
4. Apparatus, Reagents, and Photometric Practice
Silicon by the Sodium Peroxide Fusion-Perchloric Acid Dehydration
Method 26-33 4.1 Apparatus and reagents required for each determination
are listed in separate sections preceding the procedure. The
1.3 This standard does not purport to address all of the
apparatus, standard solutions, and certain other reagents used
safety concerns, if any, associated with its use. It is the
in more than one procedure are referred to by number and shall
responsibility of the user of this standard to establish appro-
conform to the requirements prescribed in Practices E 50,
priate safety and health practices and determine the applica-
except that photometers shall conform to the requirements
prescribed in Practice E 60.
These test methods are under the jurisdiction of ASTM Committee E-1 on
Analytical Chemistry for Metals, Ores, and Related Materials and are the direct
responsibility of Subcommittee E01.01 on Iron, Steel and Ferroalloys.
Current edition approved July 15, 1994. Published September 1994. Originally Annual Book of ASTM Standards, Vol 01.02.
published as E 364 – 70 T. Last previous edition E 364 – 87. Annual Book of ASTM Standards, Vol 14.02.
2 5
These test methods are intended for use in determining the composition of Annual Book of ASTM Standards, Vol 03.05.
ferrochrome-silicon as specified in Specification A 482. Annual Book of ASTM Standards, Vol 03.06.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
E364–94 (2000)
4.2 Photometric practice prescribed in these test methods 14. Reagents
shall conform to Practice E 60.
14.1 Ammonium Bromide (NH Br).
14.2 Ammonium Molybdate Solution (10 g/L)—Dissolve
5. Sampling
2.5 g of ammonium heptamolybdate tetrahydrate
5.1 For procedures for sampling the material, and for
((NH ) Mo O ·4H O) in 40 mL of warm water.Add 128 mL
6 7 24 2
particle size of the sample for chemical analysis, refer to
of H SO (1 + 3), dilute to 250 mL, and mix.
2 4
Practices E 32.
14.3 Ammonium Molybdate-Hydrazine Sulfate Solution—
Dilute 100 mL of ammonium molybdate solution to 900 mL,
6. Rounding Off Calculated Values
add 10 mLof hydrazine sulfate solution, dilute to 1 L, and mix.
6.1 Calculated values shall be rounded off to the desired
Do not use a solution that has stood more than 1 h.
number of places as directed in the Rounding Off and Special
14.4 Arsenic, Standard Solution A (1 mL = 0.10 mg As)—
Case Rounding Off procedures in the Rounding-Off Method
Transfer 0.1320 g of arsenic trioxide (As O)toa1-L
2 3
Section of Practice E 29.
volumetric flask, dissolve in 100 mL of HCl, cool, dilute to
volume, and mix.
7. Interlaboratory Studies
14.5 Arsenic, Standard Solution B (1 mL = 0.01 mg As)—
7.1 These methods have been evaluated in accordance with
Using a pipet, transfer 100 mL of arsenic standard solution A
PracticeE 173,unlessotherwisenotedintheprecisionandbias
(1 mL = 0.10 mg As) to a 1-L volumetric flask, dilute to
section.
volume, and mix.
ARSENIC BY THE MOLYBDENUM BLUE 14.6 Hydrazine Sulfate —((NH ) ·H SO ).
2 2 2 4
PHOTOMETRIC METHOD 14.7 Hydrazine Sulfate Solution (1.5 g/L)—Dissolve 1.5 g
of hydrazine sulfate ((NH )·H SO ) in water, dilute to 1 L,
2 2 2 4
8. Scope
and mix. Do not use a solution that has stood more than 1 day.
8.1 This method covers the determination of arsenic in
14.8 Sodium Carbonate (Na CO ).
2 3
ferrochrome-silicon in concentrations from 0.001 to 0.005 %.
14.9 Sodium Peroxide (Na O ).
2 2
8.2 The limits of the scope have been set at 0.001 to
0.005 % because test materials containing other arsenic con-
15. Preparation of Calibration Curve
centrations were unavailable for testing. However, recognizing
15.1 Calibration Solutions:
that the procedure should give satisfactory results at lower and
15.1.1 Using pipets, transfer 1, 2, 5, 10, and 15 mL of
higher concentrations, the calibration and procedure section
arsenic standard solution B (1 mL = 0.01 mg As) to 125-mL
cover the range from 0.001 to 0.1 %.
Erlenmeyer flasks.
8.2.1 Users of this method are cautioned that its use on
15.1.2 Add 10 mL of HNO and evaporate the solution to
samples outside of the 0.001 to 0.005 % range is not supported
dryness on a hot plate. Bake for 30 min at 150 to 180°C.
by interlaboratory testing.
Remove from the hot plate. Add 45 mL of ammonium
9. Summary of Method molybdate-hydrazine sulfate solution to each flask, warm
gently to dissolve the residue, and transfer the solution to a
9.1 Arsenic is first separated by distillation as the trivalent
50-mL volumetric flask. Proceed as directed in 15.3.
chloride. Ammonium molybdate is added to form arsenomo-
15.2 Reference Solution—Transfer 10 mL of HNO to a
lybdate ion which is then reduced by hydrazine sulfate to form 3
125-mLErlenmeyerflaskandevaporatethesolutiontodryness
the molybdenum blue complex. Photometric measurement is
on a hot plate. Bake for 30 min at 150 to 180°C. Remove from
made at approximately 850 nm.
the hot plate. Add 45 mL of ammonium molybdate-hydrazine
10. Concentration Range
sulfate solution to the flask, warm gently to dissolve the
residue, transfer to a 50-mL volumetric flask and proceed as
10.1 The recommended concentration range is 0.01 to 0.15
directed in 15.3.
mg of arsenic per 50 mL of solution using a 1-cm cell.
15.3 Color Development—Heat the flask in a boiling water
NOTE 1—This method has been written for cells having a 1-cm light
bath for 15 min. Remove the flask, cool to room temperature,
path. Cells having other dimensions may be used, provided suitable
dilute to volume with ammonium molybdate-hydrazine sulfate
adjustments can be made in the amount of sample and reagents used.
solution, and mix.
11. Stability of Color
15.4 Photometry:
15.4.1 Multiple-Cell Photometer—Measure the cell correc-
11.1 The color is stable for at least 2 h.
tion with water using absorption cells with a 1-cm light path
12. Interferences
and a light band centered at approximately 850 nm. Using the
test cell, take the photometric readings of the calibration
12.1 The elements ordinarily present do not interfere if their
solutions using the solution prepared in 15.2 as a reference.
concentrations are under the maximum limits shown in 1.1.
15.4.2 Single-Cell Photometer—Transfer a suitable portion
13. Apparatus
of the reference solution (15.2) to an absorption cell with a
13.1 Distillation Apparatus, Fig. 1, Methods E 360. 1-cm light path and adjust the photometer to the initial setting,
13.2 Zirconium Crucibles, 30-mL capacity. using a light band centered at approximately 850 nm. While
E364–94 (2000)
maintaining this adjustment, take the photometric readings of 16.2 Reference Solution—Carry a reagent blank through the
the calibration solutions. entire procedure using the same amounts of all reagents with
15.5 Calibration Curve—Plot the net photometric readings the sample omitted, for use as a reference solution.
of the calibration solutions against milligrams of arsenic per 50 16.3 Color Development—Proceed as directed in 15.3.
mL of solution. 16.4 Photometry—Take the photometric reading of the test
solution as directed in 15.4.
16. Procedure
17. Calculation
16.1 Test Solution:
17.1 Convertthenetphotometricreadingofthetestsolution
16.1.1 Select and weigh a sample to the nearest 0.1 mg in
to milligrams of arsenic by means of the calibration curve.
accordance with the following:
Calculate the percentage of arsenic as follows:
Arsenic, % Sample Weight, g
0.001 to 0.015 0.500
Arsenic, % 5 A/~B 3 10! (1)
0.01 to 0.04 0.250
0.035 to 0.10 0.125
where:
A = arsenic found in 50 mL of final test solution, mg, and
Transfer the sample to a 30-mL zirconium crucible contain-
B = sample represented in 50 mL of final test solution, g.
ing10gofNa O and2gofNa CO or8gofNa O plus 2
2 2 2 3 2 2
gofNa CO .
2 3
18. Precision and Bias
16.1.2 Mix thoroughly with a metal spatula (Note 2). Fuse
18.1 Precision—Nine laboratories cooperated in testing this
carefully over a free flame by holding the crucible with a pair
method and obtained the data summarized in Table 1. Samples
of tongs and slowly revolving it around the outer edge of the
with arsenic concentrations near the upper limit of the scope
flame until the contents have melted down quietly; raise the
were not available for testing.
temperature gradually to avoid spattering. When the contents
18.2 Bias—The accuracy of the method could not be
are molten, give the crucible a rotary motion to stir up any
evaluated because adequate certified standard reference mate-
unattached particles of the alloy adhering to the bottom or
rials were unavailable at the time of testing. The user is
sides. Finally, increase the temperature until the crucible is
cautioned to verify by the use of certified reference materials,
bright red for 1 min. Cool the crucible to room temperature.
ifavailable,thattheaccuracyofthismethodisadequateforthe
Transfer the crucible to an 800-mLbeaker containing 60 mLof
contemplated use.
H SO (1 + 1) and 200 mLof water. Dissolve the melt; remove
2 4
and rinse the crucible.
CHROMIUM BY THE ACID DISSOLUTION
NOTE 2—Precaution: Use proper safety practices and equipment when TITRIMETRIC METHOD
performing sodium peroxide fusions.
19. Scope
16.1.3 If manganese dioxide is present, add H SO drop-
2 3
19.1 This method covers the determination of chromium in
wise until the solution clears.
ferrochrome-silicon in concentrations from 30 to 60 %.
16.1.4 Heat to boiling, and cool. While stirring vigorously,
add NH OH until the solution is alkaline to litmus, and then
20. Summary of Method
add 3 to 5 mLin excess. Heat to boiling, remove from the heat,
20.1 The alloy is dissolved in sulfuric, nitric, and hydrof-
and allow the precipitate to settle. Filter on a coarse filter paper
luoric acids, and the excess of the latter is complexed with
and wash five times with hot water. Discard the filtrate.
boric acid. The chromium and manganese ions are oxidized to
Remove the filter paper, carefully open it, and place it on the
dichromate and permanganate ions, respectively, by ammo-
inside wall of the original 800-mLbeaker.Wash the precipitate
nium peroxydisulfate with silver nitrate as a catalyst. After
from the paper using a fine stream of water. Pass 25 mLof HCl
adding HCl to reduce permanganate ions, the dichromate ions
over the paper, and wash well with water but do not exceed a
are reduced by adding an excess of standard ferrous ammo-
total volume of 40 mL. Discard the paper. Warm gently until
nium sulfate (salt or solution). The excess ferrous ions are
the precipitate dissolves.
titrated with standard potassium permanganate solution.
16.1.5 Transfer the solution to the distillation flask, add 1 g
of NH Br and 0.75 g of hydrazine sulfate. Add 20 mL of
21. Interferences
HNO (1 + 1) to the receiving flask, and place the flask in an
21.1 The elements ordinarily present do not interfere if their
800-mL beaker containing cold water. Assemble the apparatus
concentrations are under the maximum limits shown in 1.1.
(Fig. 1, Methods E 360), heat the distillation flask, and distill
into the receiving flask.
22. Reagents
16.1.6 Distill until the volume is reduced to 10 mL or until
22.1 Ammonium Peroxydisulfate —((NH ) -S O ).
4 2 2 8
oxides of nitrogen are noted in the distillation flask. Remove
22.2 Boric Acid (H BO ).
3 3
the distillation flask from the heat source. Place the receiving
flask on a hot plate and evaporate the solution to dryness. Bake
TABLE 1 Statistical Information—Arsenic
for 30 min at 150 to 180°C. Add 45 mL of ammonium
Ferroalloy Arsenic Found, Repeatability Reproducibility
molybdate-hydrazine sulfate solution to the flask, warm gently
Type % (R , E 173) (R , E 173)
1 2
to dissolve the residue, and transfer the solution to a 50-mL
Cr40-Si42-C0.05 0.0018 0.0003 0.0003
volumetric flask. Proceed as directed in 16.3.
E364–94 (2000)
TABLE 2 Statistical Information—Chromium
22.6 PotassiumPermanganateStandardSolution (0.1N)—
Reproduc- Reagent No. 13.
Chromium Repeatability
Test Specimen ibility
22.7 Potassium Permanganate Solution (20 g/L)—Reagent
Found, % (R , E 173)
(R , E 173)
No. 134.
Ferrochrome-silicon, No. 4 34.79 0.1
...
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