ASTM E227-90(1996)

Standard Test Method for Optical Emission Spectrometric Analysis of Aluminum and Aluminum Alloys by the Point-to-Plane Technique (Withdrawn 2002)

SCOPE
1.1 This test method covers the spectrometric analysis of aluminum and aluminum alloys for the following elements in the concentration ranges indicated:  Concentration Element Range, % Copper 0.001 to 30.0 Silicon 0.001 to 14.0 Magnesium 0.001 to 11.0 Zinc 0.001 to 10.0 Nickel 0.001 to 10.0 Manganese 0.001 to 8.0 Tin 0.001 to 7.5 Silver 0.001 to 5.0 Iron 0.001 to 4.0 Chromium 0.001 to 4.0 Cadmium 0.001 to 2.0 Cobalt 0.001 to 2.0 Beryllium 0.001 to 1.2 Zirconium 0.001 to 1.0 Lead 0.002 to 0.7 Bismuth 0.001 to 0.7 Titanium 0.001 to 0.5 Calcium 0.001 to 0.2 Barium 0.001 to 0.05 Boron 0.001 to 0.05 Gallium 0.001 to 0.05 Sodium 0.001 to 0.05 Vanadium 0.001 to 0.05
1.2 The test method is applicable primarily to the control analysis of chill-cast samples. Other forms may be analyzed, provided that ( ) they are sufficiently massive to prevent undue heating, ( ) they permit machining flat surfaces having a minimum dimension of approximately 16 mm (1.6 in.), and ( ) reference materials of similar metallurgical condition and chemical composition are available.
1.3 This standard does not purport to address all of the safety problems, 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.

General Information

• Status: Withdrawn
• Publication Date: 31-Dec-1995
• Withdrawal Date: 09-Oct-2002
• ICS: 77.120.10 - Aluminium and aluminium alloys
• Technical Committee: E01 - Analytical Chemistry for Metals, Ores, and Related Materials
• Drafting Committee: E01.04 - Aluminum and Magnesium

Standards Content (Sample)

Designation: E 227 – 90 (Reapproved 1996)
Standard Test Method for
Optical Emission Spectrometric Analysis of Aluminum and
Aluminum Alloys by the Point-to-Plane Technique
This standard is issued under the fixed designation E 227; 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.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope 2. Referenced Documents
1.1 This test method covers the spectrometric analysis of 2.1 ASTM Standards:
aluminum and aluminum alloys for the following elements in E 130 Practice for Designation of Shapes and Sizes of
the concentration ranges indicated: Graphite Electrodes
E 135 Terminology Relating to Analytical Chemistry for
Concentration
Element Range, %
Metals, Ores, and Related Materials
E 158 Practice for Fundamental Calculations to Convert
Copper 0.001 to 30.0
Intensities into Concentrations in Optical Emission Spec-
Silicon 0.001 to 14.0
Magnesium 0.001 to 11.0
trochemical Analysis
Zinc 0.001 to 10.0
E 172 Practice for Describing and Specifying the Excitation
Nickel 0.001 to 10.0
Manganese 0.001 to 8.0 Source in Emission Spectrochemical Analysis
Tin 0.001 to 7.5
E 305 Practice for Establishing and Controlling Spectro-
Silver 0.001 to 5.0
chemical Analytical Curves
Iron 0.001 to 4.0
E 607 Test Method for Optical Emission Spectrometric
Chromium 0.001 to 4.0
Cadmium 0.001 to 2.0
Analysis of Aluminum and Aluminum Alloys by the
Cobalt 0.001 to 2.0
Point-to-Plane Technique, Nitrogen Atmosphere
Beryllium 0.001 to 1.2
Zirconium 0.001 to 1.0 E 716 Practices for Sampling Aluminum and Aluminum
Lead 0.002 to 0.7
Alloys for Spectrochemical Analysis
Bismuth 0.001 to 0.7
E 876 Practice for Use of Statistics in the Evaluation of
Titanium 0.001 to 0.5
Calcium 0.001 to 0.2 Spectrometric Data
Barium 0.001 to 0.05
Boron 0.001 to 0.05
3. Terminology
Gallium 0.001 to 0.05
Sodium 0.001 to 0.05 3.1 Definitions—Refer to Terminology E 135.
Vanadium 0.001 to 0.05
4. Summary of Test Method
1.2 The test method is applicable primarily to the control
4.1 A self-initiating oscillatory capacitor discharge or trig-
analysis of chill-cast samples. Other forms may be analyzed,
gered capacitor discharge is produced between a prepared flat
provided that (1) they are sufficiently massive to prevent undue
surface of the sample and the tip of a shaped graphite electrode.
heating, (2) they permit machining flat surfaces having a
The radiant energies of selected analytical lines and an internal
minimum dimension of approximately 16 mm (1.6 in.), and (3)
standard line are measured by photomultipliers. The output
reference materials of similar metallurgical condition and
current of each tube during the exposure period is accumulated
chemical composition are available.
and stored as a charge on an associated capacitor. At the end of
1.3 This standard does not purport to address all of the
the exposure period, the capacitor potentials corresponding to
safety concerns, if any, associated with its use. It is the
the analytical lines relative to the potential for the internal
responsibility of the user of this standard to establish appro-
standard line are automatically measured and recorded. The
priate safety and health practices and determine the applica-
recording system may be calibrated in terms of relative radiant
bility of regulatory limitations prior to use.
energies or in percent concentration. Refer to Method E 607 for
the analysis of aluminum and its alloys using a nitrogen
atmosphere.
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 for Subcommittee E01.04 on Aluminum and Magnesium.
Current edition approved Jan. 26, 1990. Published March 1990. Originally Annual Book of ASTM Standards, Vol 03.05.
e1 3
published as E 227 – 67 T. Last previous edition E 227 – 67 (1982) . Annual Book of ASTM Standards, Vol 03.06.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
E 227
TABLE 1 Spectrometer Characteristics
A A A
Type A Type B Type C
Focal length, m 1.5 1.5 2.0
Concave grating, grooves/mm, nominal (Note 2) 1000 1000 1000
Reciprocal linear dispersion, A/mm 6.95 6.95 5.2
Primary slit width, μm 50 50 50
Secondary slit width, μm 150 150 150
Focal length, condensing lens, mm, approx 200 130 230
˚
Wavelength coverage, A 2000 to 8000 2100 to 6800 1966 to 8750
Maximum number of multiplier phototube 35 40 68
A
A 1.5-m Production Control Quantometer (Type A), a 1.5-m Industrial Research Quantometer (Type B), or a 2-m Production Control Quantometer (Type C),
manufactured by Applied Research Labs., Glendale Calif., has been found suitable for this purpose.
5. Significance and Use 6.6.2 More than one readout channel may be needed for
each photomultiplier if the readout is controlled with gain and
5.1 This test method is suitable for manufacturing control,
zero controls. This permits defining more than one concentra-
material or product acceptance, and research and development.
tion range for an element. The channel layout shall be designed
Its use over several years has shown that both its precision and
to suit the individual application. A typical design for an
accuracy are well within expected levels.
aluminum foundry is shown in Table 2.
5.2 It is assumed that all who use this method will be trained
analysts capable of performing laboratory procedures skillfully
NOTE 1—Although line spacings may be nominally identical, they may
and safely and that work will be performed in a properly
differ slightly, depending on the manufacturer.
equipped laboratory.
TABLE 2 Typical Channel Layout for Aluminum Foundry
6. Apparatus
Self-Initating Triggered
Oscillatory Capacitor Capacitor
6.1 Sample Preparation Equipment:
Discharge Discharge
˚
Element Wavelength, A
6.1.1 Sample Molds—Refer to Practices E 716.
Concentration Concentration
6.1.2 Lathe—Refer to Practices E 716.
Range, % Range, %
6.2 Electrode Cutter, to shape the end of a 6.15-mm
Silicon Si 2881.58 0.03 to 1.5 .
(0.242-in.) diameter graphite rod to the configuration of the
Si 3905.53 0.50 to 4.0 .
Type C-5a electrode as described in Practice E 130.
Si 3905.53 3.0 to 12.0 .
6.3 Excitation Source, providing a self-initiating oscillatory
Iron Fe 2395.62 0.03 to 2.0 .
capacitor discharge and a spark-initiated triggered capacitor
discharge with the parameters described in 10.2, or equivalent.
Copper Cu 3273.96 0.001 to 0.40 .
Cu 5105.54 0.05 to 5.0 .
6.4 Excitation Stand, Petrey stand or other suitable stand
Cu 5105.54 4.0 to 15.0 .
for mounting in optical alignment a flat surface of the specimen
in opposition to a graphite counter electrode. A water-cooled
Manganese Mn 2593.73 0.01 to 0.50 0.001 to 0.05
Mn 3460.33 0.20 to 2.0 .
aluminum upper support shall be equipped with a clamp to
hold the sample in a slightly inclined position, so arranged that
Magnesium Mg 2852.13 0.001 to 0.50 .
an extension of the plane of the machined sample surface
Mg 5183.62 0.30 to 5.0 .
Mg 5183.62 4.0 to 11.0 .
passes through the top of the condensing lens, and the center of
the spark column is on the optical axis. A gage shall be
Chromium Cr 4254.35 0.01 to 1.0 .
provided to position the lower electrode so as to produce a
Nickel Ni 3414.76 0.01 to 1.0 0.001 to 0.05
3.0-mm (0.12-in.) gap.
Ni 2316.04 0.50 to 5.0 .
6.5 Spectrometer, having characteristics equivalent to those
listed in Table 1. Zinc Zn 3345.02 0.01 to 0.50 0.001 to 0.05
Zn 4810.53 0.20 to 4.0 .
6.6 Measuring System, consisting of photomultipliers hav-
Zn 4810.53 3.0 to 8.5 .
ing individual dynode voltage adjustment, capacitors on which
the output of each photomultiplier is stored, an amplifier and Titanium Ti 3372.80 0.01 to 0.4 0.001 to 0.05
Vanadium V 4379.24 0.01 to 0.20 0.001 to 0.05
recording system suitable for registering a function of the
Lead Pb 4057.82 0.01 to 1.0 0.001 to 0.05
voltage on the capacitors, and the necessary switching arrange-
Tin Sn 3175.02 0.01 to 1.0 0.001 to 0.05
ments to provide the desired sequence of operation. There may
A
Sn 3175.02 1.0 to 8.0 0.001 to 0.05
be provison for switching pairs of zero and gain controls into
the amplifier circuit.
Boron B 2497.73 0.01 to 0.10 0.001 to 0.05
6.6.1 The dynode adjustment for each photomultiplier shall Beryllium Be 3130.42 0.001 to 0.05 .
Sodium Na 5889.95 0.001 to 0.05 .
control its output. The rheostat used for this purpose may be
Calcium Ca 3933.67 0.001 to 0.05 .
referred to as the attenuator.
Bismuth Bi 3067.72 0.01 to 1.0 0.001 to 0.05
Gallium Ga 2943.64 0.01 to 0.10 0.001 to 0.05
Zirconium Zr 3391.98 0.01 to 1.0 0.001 to 0.05
4 Cadmium Cd 5035.82 0.01 to 1.5 0.005 to 0.05
Churchill, J. R., “Techniques of Quantitative Spectrochemical Analysis,”
A
Aluminum Al 2567.99 internal standard internal standard
Industrial and Engineering Chemistry, Analytical Edition, Vol 16, 1944, pp.
A
653–670. Second order.
E 227
6.6.3 For an instrument using a fixed integration time, as is standard, the reading displayed for each channel will be, in
typical in a computer readout, the ratio of the radiant energy of effect, a relative ratio of radiant energy. In a special application
the analytical line to that of the internal standard will be
with a strip-chart recorder, the chart paper may be graduated in
calculated from the voltages developed on the integrators. For
units of concentration.
an instrument in which integration is controlled by the internal
TABLE 3 Analytical Lines Background Equivalents and Detection Limits Using a Self-Initiating Oscillatory Capacitor Discharge
Background
Wavelengths A
Equivalent %
Concentration Shape of Analytical
A
Element of Suitable Detection Limit %
Range, % Curves
1.5-m 2.0-m
˚
Lines, A
Spectrometer Spectrometer
Silicon Si 2516.12 0.001 to 14.0 . . 0.0005 nonlinear
Si 2881.58 0.001 to 14.0 0.05 0.03 0.0005 nonlinear
Si 3905.53 0.50 to 14.0 1.2 . . linear
Iron Fe 2382.04 0.001 to 4.0 0.02 . 0.0004 nonlinear
Fe 2395.62 0.001 to 4.0 . . nonlinear
Fe 3020.64 0.01 to 1.0 . 0.02 . nonlinear
Copper Cu 2247.00 0.01 to 5.0 . . . nonlinear
Cu 3273.96 0.001 to 1.5 0.01 0.01 0.0003 nonlinear
Cu 5105.54 0.05 to 30.0 0.75 0.54 . linear to 14 %
Manganese Mn 2593.73 0.001 to 8.0 0.01 . 0.0002 nonlinear
Mn 3460.33 0.05 to 8.0 . 0.10 . linear
Magnesium Mg 2795.53 0.001 to 1.5 . . . nonlinear
Mg 2852.13 0.001 to 1.5 0.003 . 0.00006 nonlinear
Mg 5167.34 0.05 to 11.0 . . . linear to 8 %
Mg 5172.70 0.05 to 11.0 . . . linear to 8 %
Mg 5183.62 0.05 to 11.0 0.08 0.04 . linear to 8 %
Chromium Cr 2766.54 0.10 to 4.0 . . . nonlinear
Cr 4254.35 0.001 to 4.0 0.05 0.02 0.0005 nonlinear
Nickel Ni 2316.04 0.10 to 10.0 0.05 . . nonlinear
Ni 3414.76 0.001 to 3.0 0.05 . 0.0003 nonlinear
Ni 3515.05 0.001 to 3.0 0.12 . 0.001 nonlinear
Zinc Zn 2138.56 0.001 to 0.5 . . . nonlinear
Zn 3345.02 0.001 to 10.0 0.10 . 0.001 linear
Zn 4810.53 0.01 to 8.0 0.13 0.06 . linear
Titanium Ti 3372.80 0.001 to 0.5 0.02 . 0.0003 linear
Ti 3685.20 0.01 to 1.0 . . 0.0003 linear
Vanadium V 3183.41 0.001 to 0.05 . . . linear
V 4379.24 0.001 to 0.05 0.08 . 0.001 linear
Lead Pb 4057.82 0.002 to 0.7 0.08 . 0.001 linear
Tin Sn 3175.02 0.001 to 7.5 0.15 . 0.001 linear
Boron B 2497.73 0.001 to 0.05 0.01 . 0.0002 linear
Beryllium Be 2348.61 0.001 to 0.05 . . . linear
Be 3130.42 0.001 to 1.2 . . 0.0001 linear
Sodium Na 5889.95 0.001 to 0.05 0.002 . 0.00004 nonlinear
Calcium Ca 3933.67 0.001 to 0.2 0.002 . 0.00004 nonlinear
Bismuth Bi 3067.72 0.001 to 0.7 0.07 . 0.001 linear
Gallium Ga 2874.24 0.001 to 0.05 . . 0.001 linear
Ga 2943.64 0.001 to 0.05 . . 0.001 linear
Zirconium Zr 3391.98 0.001 to 1.0 0.020 . 0.0006 linear
Zr 3438.23 0.001 to 1.0 0.041 . 0.001 linear
Cadmium Cd 2288.02 0.01 to 2.0 0.03 . 0.01 nonlinear
Cd 5085.82 0.01 to 2.0 0.10 . . linear
Cobalt Co 3453.50 0.001 to 2.0 0.01 . 0.001 nonlinear
Co 3465.80 0.001 to 2.0 0.17 . 0.001 nonlinear
Barium Ba 4554.04 0.001 to 0.05 0.007 . 0.001 linear
E 227
TABLE 3 Continued
Background
A
Wavelengths
Equivalent %
Concentration Shape of Analytical
A
Element of Suitable Detection Limit %
Range, % Curves
˚ 1.5-m 2.0-m
Lines, A
Spectrometer Spectrometer
Ba 4934.09 0.001 to 0.05 0.016 . 0.001 linear
Silver Ag 3280.68 0.001 to 5.0 0.005 . 0.0005 nonlinear
B
Aluminum Al 2567.99 internal standard . . . .
A
See 11.6.
B
Preferably second order.
TABLE 4 Analytical Lines Background Equivalents and Detection
7. Materials
Limits Using a Condensed Arc
7.1 Counter Electrodes, high-purity graphite rod, 6.15 mm
Background
Wavelengths,
(0.242 in.) in diameter. A
Concentration Equivalents Detection
Element of Suitable
A
Range, % %, 1.5-m Limit, %
˚
Lines, A
8. Reference Materials
Spectrometer
8.1 Calibrants—Analyzed aluminum materials that are ho- Silicon Si 2881.58 0.001 to 0.05 0.004 0.00008
Iron Fe 2395.62 0.001 to 0.5 0.02 0.0003
mogeneous and free of voids or porosity. If not of similar
Copper Cu 3273.96 0.001 to 0.05 0.002 0.00005
metallurgical condition to the samples being analyzed, they
Manganese Mn 2593.73 0.001 to 0.05 0.002 0.00005
Magnesium Mg 2852.13 0.001 to 0.05 0.002 0.00005
may be used if it has been established that their responses are
Chromium Cr 4254.35 0.001 to 0.05 0.009 0.0002
consistent with the specimens being analyzed. Calibrants are
available in a variety of compositions. Some have nominal
Nickel Ni 3414.76 0.001 to 0.05 0.006 0.0001
(typical) compositions while others have compositions that are Ni 3515.05 0.001 to 0.05 0.047 0.001
variations of particular alloys. Calibrants may also be used as
Zinc Zn 3345.02 0.001 to 0.05 0.03 0.0005
verifiers (8.4). A wide variety of potential calibrants are
Titanium Ti 3372.80 0.001 to 0.05 0.02 0.0005
Vanadium V 4379.24 0.001 to 0.05 0.03 0.001
available commercially.
Lead Pb 4057.82 0.002 to 0.05 0.05 0.002
8.2 High-Purity Aluminum—An aluminum specimen with
Tin Sn 3175.02 0.001 to 0.05 0.02 0.0002
purity in excess of 99.99 % aluminum. It shall be of high
Boron B 2497.73 0.001 to 0.05 0.003 0.0003
Beryllium Be 3130.42 0.001 to 0.05 . 0.0001
uniformity, but its composition need not be known precisely.
Sodium Na 5889.95 0.001 to 0.02 0.0008 0.00003
8.3 Standardants—Aluminum materials of high uniformity
Calcium Ca 3933.67 0.001 to 0.02 0.002 0.00004
that contain appropriate amounts of various elements. Their
Bismuth Bi 3067.72 0.001 to 0.05 0.02 0.0002
Gallium Ga 2943.64 0.001 to 0.05 0.008 0.0002
exact chemical composi
...