ASTM E539-90(1996)e1
(Test Method)Standard Test Method for X-Ray Emission Spectrometric Analysis of 6AI-4V Titanium Alloy
Standard Test Method for X-Ray Emission Spectrometric Analysis of 6AI-4V Titanium Alloy
SCOPE
1.1 This test method covers the X-ray emission analysis of 6Al-4V titanium alloy for the following elements in the ranges indicated (Note 1): ElementConcentration Range, %Aluminum4.6 to 7.2Vanadium2.6 to 5.4Iron0.1 to 0.3
Note 1—The concentration ranges can be extended by use of suitable reference materials. The ranges for aluminum and vanadium represent the actual concentration ranges of the NIST Standard Reference Materials used when this method was tested. The maximum concentrations of the unknowns used in the cooperative test program were all lower than the reference materials. The iron concentration range was determined by in-house reference materials used by the cooperating laboratories.
1.2 This test method is designed for control analysis in the production of titanium alloys and for inspection testing of the product shipped to the consumer. It is applicable for analyzing cast or wrought samples having a diameter of approximately 32 mm and a thickness of approximately 25 mm.
Note 2—Samples of greater or lesser size than the size designed may be used with specially designed sample holders.
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 8.
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Designation: E 539 – 90 (Reapproved 1996)
Standard Test Method for
X-Ray Emission Spectrometric Analysis of 6AI-4V Titanium
Alloy
This standard is issued under the fixed designation E 539; 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.
e NOTE—Keywords were added editorially in December 1996.
1. Scope E 120 Test Methods for Chemical Analysis of Titanium and
Titanium Alloys
1.1 This test method covers the X-ray emission analysis of
E 135 Terminology Relating to Analytical Chemistry for
6Al-4V titanium alloy for the following elements in the ranges
Metals, Ores, and Related Materials
indicated (Note 1):
Element Concentration Range, %
3. Terminology
Aluminum 4.6 to 7.2
3.1 Definitions:
Vanadium 2.6 to 5.4
3.1.1 Refer to Terminology E 135.
Iron 0.1 to 0.3
NOTE 1—The concentration ranges can be extended by use of suitable 4. Summary of Test Method
standards. The ranges for aluminum and vanadium represent the actual
4.1 The sample is finished to a clean, uniform surface and
concentration ranges of the NIST standard reference materials used when
then irradiated by an X-ray beam of high energy (short
this method was tested. The maximum concentrations of the unknowns
wavelength). The secondary X rays produced are dispersed by
used in the cooperative test program were all lower than the reference
means of crystals and the intensities measured by detectors at
materials. The iron concentration range was determined by in-house
reference materials used by the cooperating laboratories.
selected wavelengths. The outputs of the detectors in voltage
pulses are integrated or counted. Data are collected using time
1.2 This test method is designed for control analysis in the
required to reach a fixed number of counts or using total counts
production of titanium alloys and for inspection testing of the
for a fixed time. Concentrations of the elements are determined
product shipped to the consumer. It is applicable for analyzing
by relating the measured radiation of unknown samples to
cast or wrought samples having a diameter of approximately 32
analytical curves or charts prepared from standard reference
mm and a thickness of approximately 25 mm.
materials of known compositions. A fixed channel or polychro-
NOTE 2—Samples of greater or lesser size than the size designed may
mator system or a sequential system may be used to provide
be used with specially designed sample holders.
simultaneous or sequential determinations of elements.
1.3 This standard does not purport to address all of the
5. Significance and Use
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
5.1 The chemical composition of 6A1-4V titanium alloy
priate safety and health practices and determine the applica-
must be accurately determined to ensure the desired metallur-
bility of regulatory limitations prior to use. Specific precau-
gical properties. This test method is suitable for manufacturing
tionary statements are given in Section 8.
control and inspection testing.
2. Referenced Documents
6. Apparatus
2.1 ASTM Standards:
NOTE 3—It is not within the scope of this test method to prescribe all
details of equipment to be used. Equipment varies between laboratories.
6.1 Sample Preparation Equipment:
6.1.1 Surface Grinder, with 60 to 600-grit silicon carbide
belts or disks capable of providing test specimens with a
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 uniform flat finish. A wet belt or wet disk grinder is preferred
responsibility of Subcommittee E1.06 on Ti, Zr, W, Mo, Ta, Nb, Hf.
to prevent work hardening of the sample.
Current edition approved July 27, 1990. Published September 1990. Originally
6.2 Excitation Source:
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published as E 539 – 75. Last previous edition E 539 – 75 (1989) .
National Institute of Standards and Technology Reference Material Nos. 653,
654, and 655, available from National Institute of Standards and Technology,
Washington, DC 20234. Annual Book of ASTM Standards, Vol 03.05.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
E 539
6.2.1 X-Ray Generator, providing constant potential or Handbook X-Ray Protection, HB76, the booklet Radiation
rectified power of sufficient energy to produce secondary Safety Recommendations for X-Ray Diffraction and Spectro-
radiation of the sample for the elements specified. The genera- graphic Equipment, #MORP 68-14, 1968, by T. M. Moore and
tor may be equipped with a line voltage regulator and current D. J. McDonald, and the U. S. Government Handbook 93,
stabilizer, with voltage and current regulations up to 75 kV and Safety Standard for Non-Medical X-Ray and Sealed Gamma-
40 mA. Ray Sources, Part 1, General, or similar handbooks of latest
6.2.2 X-Ray Tube, with a high-purity tungsten target capable issue.
of continuous operation up to potentials and currents shown in 8.2 X-ray equipment should be used only under the guid-
Table 1. ance and supervision of a responsible, qualified person.
8.3 Suitable monitoring devices, either film badges or do-
simeters, shall be worn by all personnel using the equipment.
TABLE 1 Typical Operating Voltages and Currents
To meet local, state, and national radiation standards, periodic
Element Voltage, kV with Current, mA
radiation surveys of the equipment for leaks and excessive
Iron 60-32, 51-48, 48-48, 48-22
scattered radiation shall be made by a qualified person using an
Aluminum 60-32, 51-48, 41-26, 48-22
ionization-chamber detector. The personal film badge survey
Vanadium 48-24, 40-24, 51-48, 48-46, 48-22
Chromium 48-24, 40-24, 51-48, 48-48, 48-22
record, the radiation survey record, and a maintenance record
shall be available upon request.
8.4 Special precautions for the operator shall be posted.
8.5 X-ray caution signs shall be posted near the X-ray
6.3 Spectrometer, designed for X-ray emission analysis
equipment and at all entrances to the radiation area.
using air and vacuum or helium, and equipped with specimen
holders and specimen chamber. The chamber should contain a 8.6 Fail-safe “X-ray On” warning lights shall be used at the
X-ray tube.
sample specimen spinner.
6.3.1 Analyzing Crystals, flat or curved lithium fluoride
9. Standards
(LiF), pentaerythritol (PET), or ethylenediamine d-tartrate
9.1 Primary Standards shall be NIST 6Al-4V titanium
(EDdT).
reference materials identified as Nos. 653, 654, 655, and 654a,
6.3.2 Collimator, for limiting the characteristic X rays to a
or their replacements. These shall be used for calibration of
parallel bundle when flat crystals are used in the instrument.
the instrument for the determination of aluminum and vana-
For curved crystal optics, no collimation is necessary.
dium. Reference material NIST No. 173 could be melted in a
6.3.3 Detectors—Sealed or gas-flow proportional counters,
button furnace to obtain a disk.
or equivalent.
9.2 Secondary Standards are not available from commer-
6.3.4 Vacuum System, providing for the determination of
,
11 12
cial sources. Produce a series of standards in the laboratory
elements whose radiation is absorbed by air. The system should
to cover the analytical concentration ranges. Select a mini-
consist of a vacuum pump, gage, and electrical controls to
mium of three samples that contain vanadium, aluminum and
provide automatic pump-down of the optical path and to start
iron at the top and bottom of the concentration range and one
the analysis at a pressure of 100 μm or less, controllable to 6
intermediate. Analyze portions of these samples in accordance
20 μm. A helium system can also be used.
with Test Methods E 120, preferably by more than one analyst
6.4 Measuring System—An electronic circuit capable of
and assign the average analysis.
amplifying, counting, and integrating pulses received from the
detector tube. The system should be equipped with visual and
10. Preparation of Standards and Samples
automatic recording devices and have a pulse height analyzer,
10.1 Grind the specimens to provide a flat, clean area over
which is used for pulse energy discrimination.
the entire surface to be exposed to the X-ray beam. Adhere
rigorously to the preparation technique established.
7. Reagents
7.1 Detector Gas (P-10), consisting of a mixture of 90 % 11. Preparation of Apparatus
argon and 10 % methane.
11.1 Start Up—Energize the power supply and electronic
circuits for at least ⁄2 h prior to taking measurements.
8. Safety Precautions
8.1 Occupational Health and Safety Standards on ioniz-
Available from Superintendent of Documents, U. S. Government Printing
ing radiation shall be observed at all X-ray emission spectrom-
Office, Washington, DC 20025.
eter installations. It is also recommended that personnel follow
Available from U. S. Department of Health, Education and Welfare, Rockville,
MD 20850.
the guidelines of safe operating procedures given in the NIST
Radiation Film Badge Service, available from Nuclear-Chicago, 200 Nuclear
Drive, Des Plaines, IL 60018, has been found satisfactory.
A survey meter called a Cutie-Pie, which will meet the requirements, can be
A two-stage mechanical pump meeting the requirements can be purchased from purchased from Nuclear-Chicago.
Precision Scientific Co., Chicago, IL 60647, or Sargent-Welch Scientific Co., Available from National Institute of Standards and Technology, U. S. Depart-
Skokie, IL 60076. ment of Commerce, Washington, DC 20234.
5 11
Federal Register, Vol 36, No. 105, May 29, 1971, Sec. 1910.96 or of latest issue Report on Available Standard Samples. Reference Samples, and High-Purity
of Subpart G; Superintendent of Documents, U. S. Government Printing Office, Materials for Spectrochemical Analysis, ASTM DS2, Am. Soc. Testing Mats., 1964.
Washington DC 20025; National
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