ASTM E117-64 (1989)

Method for Spectrographic Analysis of Pig-Lead by the Point-To-Plane Technique (Withdrawn 1995)

General Information

• Status: Withdrawn
• Withdrawal Date: 14-Aug-1995
• Technical Committee: E01 - Analytical Chemistry for Metals, Ores, and Related Materials
• Drafting Committee: E01.05 - Cu, Pb, Zn, Cd, Sn, Be, Precious Metals, their Alloys, and Related Metals

Standards Content (Sample)

Designation: E 117 - 64 (Reapproved 1969)
@
Standard Method for
Spectrographic Analysis of Pig Lead by the Point-to-Plane
Technique’
This standard is issued under the fixed designation E 117; 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 (c) indicates an editorial change since the last revision or reapproval.
1. Scope E 135 Terminology Relating to Analytical Atomic Spec-
troscopy3
1.1 This method covers the spectrographic analysis of pig
lead for the following elements in the ranges indicated:
3. Terminology
Concentration Range, %
Element
3.1 For definitions of terms used in this method, refer to
0.0005 to 0.3
Bismuth
Terminology E 135.
Tellurium 0.01 too.1
0.0005 to 0.08
Copper
4. Summary of Method
Arsenic 0.001 to 0.03
Antimony 0.001 to 0.03
4.1 The sample is excited by a controlled spark or
ZincA 0.001 to 0.02
triggered capacitor discharge using the point-to-plane tech-
Silver o.ooo5 to 0.02
Nickel 0.001 to 0.01 nique. The spectra are photographed on a calibrated emul-
0.001 to 0.01
Tin
sion and the intensity ratios of selected pairs of analytical
Cadmium 0.0003 to 0.01
lines and internal standard lead lines are determined photo-
IronA approximately 0.0005
metrically. Concentration of the elements is read from
n Determined only.semiquantitatively because of segregation.
analytical curves relating log intensity ratio to concentration.
1.2 This method is designed for testing specimens in the
5. Significance and Use
form of chill-cast disks or miscellaneous lead samples on
5.1 This method is designed for impurity testing of lead
which a flat surface area of 25 mm (1 in.) in diameter can be
from primary sources (that is, ore-based material). Usually,
prepared. Other forms may be analyzed, provided they are
recycled lead from secondary sources is outside the range of
sufficiently massive (about 50 g) to prevent overheating
elements described in the scope of this method. Also, the
during excitation. For irregularly shaped samples or chipped
samples must be of significant size (at least 50 g) to be
samples, specimens are slowly heated to the melting point
adequately analyzed by this procedure. Users of this method
under palm oil and cast in disk form.
should be cautioned that specimens that are remelted and
1.3 This standard may involve hazardous materials, oper-
recast for analysis may not be representative of the original
ations, and equipment. This standard does not purport to
sample.
address all of the safety problems associated with its use. It is
the responsibility of the user of this standard to establish
6. Apparatus
appropriate safety and health practices and determine the
6.1 Sample Preparation Equipment:
applicability of regulatory limitations prtor to use.
6.1.1 Sample Mold, suitable for forming disks 70 mm (2x/4
in.) in diameter by 13 mm (r/2 in.) thick.
2. Referenced Documents
6.1.2 Lathe.
6.2 Electrode Cutter, for shaping electrodes to the config-
2.1. ASTA4 Standards:
uration described in 7.2.
E 37 Methods for Chemical Analysis of Pig Lead2
6.3 Efcitation Source-A high-voltage controlled spark or
E 50 Practices for Apparatus, Reagents, and Safety Pre-
condensed arc discharge source that will provide the param-
cautions for Chemical Analysis of Metals’
eters listed in 11.1, or equivalent.
E 115 Practice for Photographic Processing in Optical
6.4 Spectrograph-A grating spectrograph having a recip-
Emission Spectrographic Analysis3
rocal linear dispersion of approximately 7 A/mm, or a prism
E 116 Practice for Photographic Photometry in Spectro-
instrument with sufficient dispersion and resolving power to
chemical Analysis3
separate the analytical lines in the spectral region 2150 to
E 130 Practice for Designation of Shapes and Sixes of
4350 A. The spectrograph shall be ilhuninated by an image
Graphite Electrodes3
of the source focused on the grating or collimator. Suitable
filters shall be placed in the light path to control the intensity.
6.5 Photographic Processing Equipment, providing devel-
t This method is under the jurisdiction of ASTM Committee E-l on Analytical
oping, futing, washing, and drying operations and con-
Chemistry of Metals, Ores and Related Materials and is the direct responsibility of
Subcommittee E01.05 on Zn, Sn, Pb, Cd, Be, and Other Metals.
forming to the requirements of Practice E 115.
Current edition approved Aug. 31, 1964. Originally published as E 117 - 56 T.
6.6 Microphotometer, having a precision of at least
Last previous edition E 117 - 59 T.
f 1 .O % for transmittances between 5 and 90 %.
2 Annrral Book of ASTM Standards. VolO3.05.
3 Annual Book ofASTM Standards, VolO3.06. 6.7 Calculating Equipment-A calculating board with
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