ASTM E360-96(2001)
(Test Method)Standard Test Methods for Chemical Analysis of Silicon and Ferrosilicon (Withdrawn 2006)
Standard Test Methods for Chemical Analysis of Silicon and Ferrosilicon (Withdrawn 2006)
SCOPE
DESIG: E360 96 (Reapproved 2001) ^TITLE: Standard Test Methods for Chemical Analysis of Silicon and Ferrosilicon ^SCOPE:
1.1 These test methods cover the chemical analysis of silicon and ferrosilicon having chemical compositions within the following limits:ElementConcentration, %Aluminum2.0 maxArsenic0.10 maxCalcium1.00 maxCarbon0.50 maxChromium0.50 maxCopper0.30 maxManganese1.00 maxNickel0.30 maxPhosphorus0.10 maxSilicon20.00 to 99.5Sulfur0.025 maxTitanium0.20 max
1.2 The test methods appear in the following order: SectionsArsenic by the Molybdenum Blue Photometric MethodAluminum by the Quinolinate Photometric and GravimetricMethodsSilicon by the Sodium Peroxide Fusion-Perchloric Acid Dehydration Method
1.3 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. Specific precautionary statements are given in Section 5 and 26.8.1, 27.4.1.1, and 36.3.1.
WITHDRAWN RATIONALE
These test methods cover the chemical analysis of silicon and ferrosilicon having chemical compositions within established 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jurisdiction of Committee E01 on Analytical Chemistry for Metals, Ores, and Related Materials, these test methods were withdrawn in September 2006.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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:E360–96(Reapproved2001)
Standard Test Methods for
Chemical Analysis of Silicon and Ferrosilicon
This standard is issued under the fixed designation E 360; 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 Determine Conformance with Specifications
E32 Practices for Sampling Ferroalloys and SteelAdditives
1.1 These test methods cover the chemical analysis of
for Determination of Chemical Composition
silicon and ferrosilicon having chemical compositions within
E50 Practices forApparatus, Reagents, and Safety Consid-
the following limits:
erations for Chemical Analysis of Metals, Ores, and
Element Concentration, %
Related Materials
Aluminum 2.0 max
E60 Practice for Analysis of Metals, Ores, and Related
Arsenic 0.10 max
Materials by Molecular Absorption Spectrometry
Calcium 1.00 max
E 173 Practice for Conducting Interlaboratory Studies of
Carbon 0.50 max
Chromium 0.50 max
Methods for Chemical Analysis of Metals
Copper 0.30 max
E 362 Test Methods for ChemicalAnalysis of Silicomanga-
Manganese 1.00 max
nese and Ferrosilicon Manganese
Nickel 0.30 max
Phosphorus 0.10 max
E 363 Methods for Chemical Analysis of Chromium and
Silicon 20.00 to 99.5
Ferrochromium
Sulfur 0.025 max
Titanium 0.20 max E 364 Test Methods for ChemicalAnalysis of Ferrochrome-
Silicon
1.2 The test methods appear in the following order:
Sections
3. Significance and Use
3.1 These test methods for the chemical analysis of metals
Arsenic by the Molybdenum Blue Photometric Method 9-19
Aluminum by the Quinolinate Photometric and Gravimetric
and alloys are primarily intended to test such materials for
Methods 20-30
compliance with compositional specifications. It is assumed
Silicon by the Sodium Peroxide Fusion-Perchloric Acid
that all who use these test methods will be trained analysts
Dehydration Method 31-38
capable of performing common laboratory procedures skill-
1.3 This standard does not purport to address all of the
fully and safely. It is expected that work will be performed in
safety concerns, if any, associated with its use. It is the
a properly equipped laboratory.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
4. Apparatus, Reagents, and Photometric Practice
bility of regulatory limitations prior to use. Specific precau-
4.1 Apparatus and reagents required for each determination
tionary statements are given in Section 5 and 26.8.1, 27.4.1.1,
are listed in separate sections preceding the procedure. The
and 36.3.1.
apparatus, standard solutions, and certain other reagents used
in more than one procedure are referred to by number and shall
2. Referenced Documents
conform to the requirements prescribed in Practices E50,
2.1 ASTM Standards:
except the photometers shall conform to the requirements
A 100 Specification for Ferrosilicon
prescribed in PracticeE60.
E29 Practice for Using Significant Digits in Test Data to
4.2 Photometric practice prescribed in these test methods
shall conform to PracticeE60.
These methods are under the jurisdiction of ASTM Committee E01 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 April 10, 1996. Published June 1996. Originally
Annual Book of ASTM Standards, Vol 14.02.
e1
published as E 360 – 70 T. Last previous edition E 360 – 85 (1991) .
Annual Book of ASTM Standards, Vol 03.05.
Annual Book of ASTM Standards, Vol 01.02.
Discontinued; see 1997 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.
E360–96 (2001)
5. Safety Hazards 11. Concentration Range
5.1 For precautions to be observed in the use of certain 11.1 The recommended concentration range is 0.01 to 0.15
reagents in these test methods, refer to PracticesE50. mg of arsenic per 50 mL of solution using a 1-cm cell.
NOTE 1—This method has been written for cells having a 1-cm light
6. Sampling
path. Cells having other dimensions may be used, provided suitable
adjustments can be made in the amount of sample and reagents used.
6.1 For procedures for sampling the material, and for
particle size of the sample for chemical analysis, refer to
12. Stability of Color
PracticesE32.
12.1 The color is stable for at least 2 h.
7. Rounding Off Calculated Values
13. Interferences
7.1 Calculated values shall be rounded off to the desired
13.1 The elements ordinarily present do not interfere if their
number of places as directed in 3.4 to 3.6 of PracticeE29.
concentrations are under the maximum limits shown in 1.1.
8. Interlaboratory Studies
14. Apparatus
8.1 These test methods have been evaluated in accordance
14.1 Distillation Apparatus, Fig. 1.
with Practice E 173, unless otherwise noted in the Precision
14.2 Zirconium Crucibles, 30-mL capacity.
and Bias section.
15. Reagents
ARSENIC BY THE MOLYBDENUM BLUE
15.1 Ammonium Bromide (NH Br).
PHOTOMETRIC METHOD
15.2 Ammonium Molybdate Solution (10 g/L)—Dissolve
2.5 g of ammonium heptamolybdate tetrahydrate ((NH )
4 6-
9. Scope
Mo O ·4H O) in 40 mL of warm water. Add 128 mL of
7 24 2
9.1 This method covers the determination of arsenic in
H SO (1+3), dilute to 250 mL, and mix.
siliconandferrosiliconinconcentrationsfrom0.001to0.10 %.
15.3 Ammonium Molybdate-Hydrazine Sulfate Solution—
Dilute 100 mL of ammonium molybdate solution to 900 mL,
10. Summary of Method
add 10 mLof hydrazine sulfate solution, dilute to 1 L, and mix.
10.1 Arsenic is first separated by distillation as the trivalent Do not use a solution that has stood more than 1 h.
chloride. Ammonium molybdate is added to form arsenomo- 15.4 Arsenic, Standard Solution A (1 mL=0.10 mg As)—
lybdate which is then reduced by hydrazine sulfate to form the Transfer 0.1320 g of arsenic trioxide (As O)toa1-L
2 3
molybdenum blue complex. Photometric measurement is made volumetric flask, dissolve in 100 mL of HCl, cool, dilute to
at approximately 850 nm. volume, and mix.
FIG. 1 Arsenic Distillation Apparatus
E360–96 (2001)
15.5 Arsenic, Standard Solution B (1 mL=0.01 mg As)— gradually to avoid spattering. When the contents are molten,
Using a pipet, transfer 100 mL of arsenic Solution A (1 give the crucible a rotary motion to stir up any unattacked
mL = 0.10 mg As) to a 1-L volumetric flask, dilute to volume, particles of the alloy adhering to the bottom or sides. Finally,
and mix. increase the temperature until the crucible is bright red for 1
15.6 Hydrazine Sulfate ((NH ) ·H SO ). min. Cool the crucible to room temperature. Transfer the
2 2 2 4
15.7 Hydrazine Sulfate Solution (1.5 g/L)—Dissolve 1.5 g crucible to an 800-mL beaker containing 60 mL of H SO
2 4
of hydrazine sulfate ((NH ) ·H SO ) in water, dilute to 1 L, (1+1) and 200 mL of water. Dissolve the melt; remove and
2 2 2 4
and mix. Do not use a solution that has stood more than 1 day. rinse the crucible.
15.8 Sodium Carbonate (Na CO ).
17.1.3 If manganese dioxide is present, add H SO drop-
2 3
2 3
15.9 Sodium Peroxide (Na O ). wise until the solution clears.
2 2
17.1.4 Heat to boiling, and cool. While stirring vigorously,
16. Preparation of Calibration Curve
add NH OH until the solution is alkaline to litmus, and then
add 3 to 5 mLin excess. Heat to boiling, remove from the heat,
16.1 Calibration Solutions:
and allow the precipitate to settle. Filter on a coarse filter paper
16.1.1 Using pipets, transfer 1, 2, 5, 10, and 15 mL of
and wash five times with hot water. Discard the filtrate.
arsenicSolutionB(1mL = 0.01mgAs)to125-mLErlenmeyer
Remove the filter paper, carefully open it, and place it on the
flasks.
inside wall of the original 800-mLbeaker.Wash the precipitate
16.1.2 Add 10 mL of HNO and evaporate the solution to
from the paper using a fine stream of water. Pass 25 mL of
dryness on a hot plate. Bake for 30 min at 150 to 180°C.
HNO (1+1) over the paper, and wash well with water but do
Remove from the hot plate. Add 45 mL of ammonium
not exceed a total volume of 40 mL. Discard the paper. Warm
molybdate-hydrazine sulfate solution to each flask, warm
gently until the precipitate dissolves.
gently to dissolve the residue, and transfer the solution to a
17.1.5 Transfer the solution to the distillation flask, add 1 g
50-mL volumetric flask. Proceed as directed in 16.3.
ofNH Brand0.75gofhydrazinesulfate.Add20mLofHNO
16.2 Reference Solution—Transfer 10 mL of HNO to a
3 4 3
(1+1) to the receiving flask, and place the flask in an 800-mL
125-mL Erlenmeyer flask and proceed as directed in 16.1.2.
beaker containing cold water.Assemble the apparatus (Fig. 1),
16.3 Color Development—Heat the flask in a boiling water
bath for 15 min. Remove the flask, cool to room temperature, heat the distillation flask, and distill into the receiving flask.
dilute to volume with ammonium molybdate-hydrazine sulfate 17.1.6 Distill until the volume is reduced to 10 mL or until
solution and mix. oxides of nitrogen are noted in the distillation flask. Remove
16.4 Photometry: the distillation flask from the heat source. Place the receiving
16.4.1 Multiple-Cell Photometer—Measure the cell correc- flask on a hot plate and evaporate the solution to dryness. Bake
tion using absorption cells with a 1-cm light path and a light for 30 min at 150 to 180°C. Add 45 mL of ammonium
band centered at approximately 850 nm. Using the test cell, molybdate-hydrazine sulfate solution to the flask, warm gently
take the photometric readings of the calibration solutions. to dissolve the residue, and transfer the solution to a 50-mL
16.4.2 Single-Cell Photometer—Transfer a suitable portion volumetric flask. Proceed as directed in 17.3.
of the reference solution to an absorption cell with a 1-cm light 17.2 ReferenceSolution—Carry a reagent blank through the
path and adjust the photometer to the initial setting, using a entire procedure using the same amounts of all reagents with
light band centered at approximately 850 nm. While maintain- the sample omitted, for use as a reference solution.
ing this adjustment, take the photometric readings of the
17.3 Color Development—Proceed as directed in 16.3.
calibration solutions.
17.4 Photometry—Take the photometric reading of the test
16.5 Calibration Curve—Plot the net photometric readings
solution as directed in 16.4.
of the calibration solutions against milligrams of arsenic per 50
mL of solution.
18. Calculation
18.1 Convertthenetphotometricreadingofthetestsolution
17. Procedure
to milligrams of arsenic by means of the calibration curve.
17.1 Test Solution:
Calculate the percentage of arsenic as follows:
17.1.1 Select and weigh a sample to the nearest 0.2 mg in
Arsenic, % 5A/~B 3 10! (1)
accordance with the following:
Arsenic, % Sample Weight, g
where:
A = milligrams of arsenic found in 50 mL of final test
0.001 to 0.015 0.500
solution, and
0.01 to 0.04 0.250
B = grams of sample represented in 50 mL of final test
0.035 to 0.10 0.125
solution.
Transfer the sample to a 30-mL zirconium crucible contain-
ing10gofNa O and1gofNa CO if ferrosilicon, or8gof
2 2 2 3
19. Precision and Bias
Na O plus2gofNa CO if silicon metal.
2 2 2 3
17.1.2 Mix thoroughly with a metal spatula. Fuse carefully 19.1 Although samples covered by this method were not
over a free flame by holding the crucible with a pair of tongs available for testing, the precision data obtained for other types
and slowly revolving it around the outer edge of the flame until of alloys, using the methods indicated inTable 1, should apply.
the contents have melted down quietly; raise the temperature The user is cautioned to verify by the use of reference
E360–96 (2001)
TABLE 1 Statistical Information—Arsenic
in water, add 15 mL of HCL (1+1), dilute to volume, and mix.
Repeatability Reproducibility Using a pipet, transfer 50 mL to a 1-L volumetric flask, dilute
Ferroalloy Type Arsenic Found, %
(R , E 173) (R , E 173)
1 2
to volume, and mix. Store the solution in a polyethylene bottle.
1. No. 1, E 363 0.0015 0.0001 0.0005
26.2 Ammonium Acetate Buffer Solution (180 g/L)—
2. No. 1, E 364 0.0018 0.0003 0.0003
Dissolve 90 g of ammonium acetate in water and dilute to 500
3. No. 1, E 362 0.025 0.001 0.002
mL.
4. No. 2, E 362 0.039 0.001 0.002
26.3 BromineWater(Saturated)—Add 20 mLof bromine to
400 mL of water, and shake. Store in a glass stoppered bottle.
26.4 Bromocresol Purple Indicator Solution (0.4 g/L)—
materials, if available, that the precision and bias of this
method is adequate for the contemplated use. Reagent No. 120.
26.5 Chloroform (CHCl ).
ALUMINUM BY THE QUINOLINATE
26.6 Cupferron Solution (60 g/L)—Reagent No. 115.
PHOTOMETRIC AND GRAVIMETRIC
26.7 8-Quinolinol Solution (50 g/L)—Dissolve 25 g of
METHODS
8-quinolinol in 60 mL of acetic acid, dilute to 300 mL with
warm water, mix, filter through a medium filter paper, and
20. Scope
dilute to 500 mL. Store in an amber bottle away from direct
20.1 This method covers the determination of aluminum in
sunlight. Do not use a solution that has stood for more than one
concentrations from 0.01 to 2.0 %.
month.
26.8 Sodium Cyanide Solution (100 g/L)—Dissolve 100 g
21. Summary of Method
of sodium cyanide (NaCN) in 800 mL of water and dilute to 1
21.1 Thesampleisdissolvedinnitricandhydrofluoricacids
L. Store in a polyethylene bottle.
and fumed with perchloric acid. After the removal of interfer-
26.8.1 Warning: The preparation, storage, and use of
ing elements, aluminum is separated as the quinolinate. The
NaCN solution require care and attention. Avoid inhalation of
determination is completed gravimetrically when aluminum is
fumes and exposure of the skin to the chemical and its
present in concentrations greater than 0.2 % or photometrically
solutions.Work in a well-ventilated hood. Refer to Section 6 of
when aluminum is present in concentrations less than 0.2 %.
PracticesE50. Because of the strongly alkaline properties of
Photometric measurement is made at approximately 395 nm.
NaCN solution, contact with glass may result in appreciable
contamination of the reagent with aluminum.
22. Concentration Range (Photometric Method)
26.9 Sodium Hydroxide Solution (200 g/L)—Dissolve 40 g
22.1 The recommended concentration range is 0.005 to 0.10
of sodium hydroxide (NaOH) in 150 mL of water in a plastic
mg of aluminum per 25 mL of solution, using a 1-cm cell.
beaker and dilute to 200 mL.
26.10 Tartaric Acid Solution (100 g/L)—Dissol
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