ASTM E34-94(1998)

NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
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Designation: E 34 – 94 (Reapproved 1998)
Standard Test Methods for
Chemical Analysis of Aluminum and Aluminum-Base Alloys
This standard is issued under the fixed designation E 34; 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
Sections
1a
Copper by the Neocuproine (Photometric) Test Method
1.1 These test methods cover the chemical analysis of
aluminum and aluminum-base alloys having compositions Gallium by the Ion Exchange-Atomic Absorption Test
Method 312 to 323
within the following limits:
Iron by the 1,10-Phenanthroline (Photometric) Method 73 to 81
Beryllium, ppm 0.3 to 100
Iron and Manganese by the Atomic Absorption Method 221 to 231
Bismuth, % 0.02 to 1.0
Lithium by the Atomic Absorption Test Method 324 to 334
Boron, % 0.005 to 0.060
Magnesium:
Cadmium, % 0.001 to 0.50 1b
Pyrophosphate (Gravimetric) Method
Chromium, % 0.01 to 1.0
Ethylenediamine Tetraacetate (Titrimetric) Test
Copper, % 0.01 to 20.0
Method 88 to 93
Gallium, % 0.001 to 0.05
Magnesium by the Atomic Absorption Test Method 232 to 242
Iron, % 0.01 to 3.0
Manganese by the Periodate (Photometric) Test
Lead, % 0.01 to 1.0
Method 293 to 302
Lithium, % 0.001 to 4.0
Nickel:
Magnesium, % 0.002 to 12.0 1a
Dimethylglyoxime (Photometric) Test Method
1b
Manganese, % 0.005 to 2.0
Dimethylglyoxime (Gravimetric) Test Method
Nickel, % 0.01 to 4.0
Nickel by the Atomic Absorption Test Method 243 to 253
Silicon, % 0.05 to 20.0
Silicon:
Tin, % 0.03 to 1.0
Molybdisilicic Acid (Photometric) Test Method 118 to 127
Titanium, % 0.002 to 0.30
Sodium Hydroxide-Perchloric Acid (Gravimetric)
Vanadium, % 0.002 to 0.16
Method 128 to 133
Zinc, % 0.003 to 12.0
Tin by the Iodate (Titrimetric) Test Method 134 to 140
Zirconium, % 0.01 to 0.30
Titanium by the Chromotropic Acid (Photometric) Test
Method 141 to 150
1.2 The analytical procedures appear in the following order:
Titanium by the Diantipyrylmethane Photometric Test
Method 254 to 263
Sections
Beryllium by Argon Plasma Optical Emission Vanadium by an Extraction-Photometric Test Method
using N-Benzoyl-N-Phenylhydroxylamine 264 to 273
Spectroscopy 283 to 292
Beryllium by the Morin (Fluorometric) Test Method 8-19 Zinc:
1a
Ammonium Mercuric Thiocyanate or the Zinc
Bismuth by the Thiourea (Photometric) Method
1b
Oxide (Gravimetric) Test Method
Bismuth and Lead by the Atomic Absorption Test
Method 188 to 198 Ethylenediamine Tetraacetate (Titrimetric) Test
1d
Method
Boron by the Carmine (Photometric) Test Method 30 to 38
Cadmium by the Atomic Absorption Test Method 167 to 177 Ion Exchange-EDTA Titrimetric Test Method 274 to 282
Zirconium by the Arsenazo III (Photometric) Method 178 to 187
Chromium:
Diphenylcarbazide (Photometric) Test Method 39 to 47
1b
1.3 The values stated in SI units are to be regarded as the
Persulfate Oxidation (Titrimetric) Test Method
Chromium by the Atomic Absorption Test Method 199 to 209
standard.
Copper and Lead by the Electrolytic (Gravimetric) Test
1.4 This standard does not purport to address all of the
1c
Method
safety problems, if any, associated with its use. It is the
Copper and Zinc by the Atomic Absorption Test
Method 210 to 220
responsibility of the user of this standard to establish appro-
Copper by the Electrolytic (Gravimetric) Test Method 303 to 311
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. Specific hazard
statements are given throughout these test methods.
These test methods are under the jurisdiction of ASTM Committee E-1 on
2. Referenced Documents
Analytical Chemistry for Metals, Ores, and Related Materials and are the direct
responsibility of Subcommittee E01.04 on Aluminum and Magnesium.
2.1 ASTM Standards:
Current edition approved Jan. 15, 1994. Published March 1994. Originally
E 29 Practice for Using Significant Digits in Test Data to
published as E 34 – 60 T. Last previous edition E 34 – 88.
1a
Discontinued as of Feb. 25, 1983.
1b
Discontinued as of May 29, 1981.
1c
Discontinued as of Oct. 25, 1985.
1d
Discontinued as of March 25, 1983.
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NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
E34
NOTE 1—The use of a machined disk may result in the exclusion of an
Determine Conformance with Specifications
element-rich portion of the sample. This practice should be avoided
E 50 Practices for Apparatus, Reagents, and Safety Precau-
3 wherever possible, especially for analyses affecting product acceptance.
tions for Chemical Analysis of Metals
E 55 Practice for Sampling Wrought Nonferrous Metals and 6.2.2 The outer edges of the holes shall be approximately
0.48 cm ( ⁄16 in.) from the edge of the disk. Drills shall be not
Alloys for Determination of Chemical Composition
E 60 Practice for Photometric and Spectrophotometric less than 0.95 cm ( ⁄8 in.) in diameter and not larger than 1.27
3 4
cm ( ⁄2 in.) in diameter.
Methods for Chemical Analysis of Metals
E 88 Practice for Sampling Nonferrous Metals and Alloys 6.2.3 Mill disks at similar points to a distance of 40 % of the
3 4
sample diameter. Use a 0.95-cm ( ⁄8 in.) milling cutter.
in Cast Form for Determination of Chemical Composition
E 173 Practice for Conducting Interlaboratory Studies of 6.2.4 Sample book mold disks (Type A, Practices E 716) at
approximately the 9 o’clock and the 3 o’clock positions when
Methods for Chemical Analysis of Metals
E 716 Practices for Sampling Aluminum and Aluminum the sprue is at the 12 o’clock position. Center pour (Type B,
Practices E 716) and vacuum cast disks may be sampled
Alloys for Spectrochemical Analysis
E 1024 Guide for Chemical Analysis of Metals and Metal around the entire circumference. Fig. 1 illustrates the areas
suitable for sampling Type A and Type B disks. Vacuum cast
Bearing Ores by Flame Atomic Absorption Spectropho-
4 4
tometry disks are sampled in the same manner as Type B disks.
6.2.5 Drilling or milling techniques ideally should produce
3. Significance and Use
uniformly small chips. Break large continuous pieces into
1 3
3.1 These test methods for the chemical analysis of metals smaller pieces 0.64 cm ( ⁄4 in.) to 0.95 cm ( ⁄8 in.) long. Drilling
or milling techniques should minimize production of fine,
and alloys are primarily intended to test such materials for
compliance with compositional specifications. It is assumed dust-like material.
that all who use these test methods will be trained analysts
7. Rounding Calculated Values
capable of performing common laboratory procedures skill-
7.1 Calculated values shall be rounded to the desired num-
fully and safely. It is expected that work will be performed in
ber of places in accordance with the rounding method given in
a properly equipped laboratory.
3.4 and 3.5 of Practice E 29.
4. Apparatus, Reagents, and Photometric Practice
4.1 Apparatus and reagents required for each determination
are listed in separate sections preceding the procedure. The
apparatus, standard solutions, and certain other reagents used
in more than one procedure are referred to by number and shall
conform to the requirements prescribed in Practices E 50,
except that photometers shall conform to the requirements
prescribed in Practice E 60.
4.2 Photometric practice prescribed in these test methods
shall conform to Practice E 60.
5. Precautions
5.1 For precautions to be observed in the use of certain
reagents in these test methods, reference shall be made to
Practices E 50.
6. Sampling
6.1 Wrought products shall be sampled in accordance with
Practice E 55. Cast products shall be sampled in accordance
with Practice E 88.
6.2 Chill cast disks produced for analysis by spectrochemi-
cal methods (see Practices E 716) shall be considered cast
products. The principles of Practice E 88 shall apply.
6.2.1 Prepare such disks for chemical analysis by drilling or
milling through the entire thickness of an unmachined disk
(Note 1). Use a minimum of two positions approximately
opposite each other and combine the drillings or millings.
Annual Book of ASTM Standards, Vol 14.02.
Annual Book of ASTM Standards, Vol 03.05.
Annual Book of ASTM Standards, Vol 03.06.
NOTE 1—Shaded areas are suitable for sampling.
Olson, H. A., and Macy, D. W., “Metallurgical Approach to Evaluating
Chemical Sample Disks,” Light Metals, Vol 2, 1978, pp. 301–311. FIG. 1 Type A and Type B Disks
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
E34
BERYLLIUM BY THE MORIN (FLUOROMETRIC) mix. Transfer a 10-mL aliquot of this solution to a 1-L
TEST METHOD volumetric flask. Add 10 mL of HClO , dilute to volume, and
mix.
8. Scope
14.6 Chloroform (CHCl ).
8.1 This test method covers the determination of beryllium 14.7 Diethylenetriaminepentaacetic Acid (DTPA), Recrys-
tallized (Note 2)—Add 100 g of DTPA to 800 mL of boiling
in concentrations from 1 to 100 ppm.
water and heat to boiling. Add 8 to 10 g of high-quality
9. Summary of Test Method
decolorizing carbon and mix thoroughly. Filter with suction
through a hardened retentive paper. Transfer the clear filtrate to
9.1 In an alkaline solution, beryllium and morin form a
a 1-L beaker and stir vigorously to induce crystallization
compound which produces a yellow-green fluorescence at
throughout the solution. Cool thoroughly in a water bath. Filter
approximately 520 nm when excited by light at approximately
with suction using a hardened paper and remove as much water
430 nm.
as possible. Dry the salts at 110°C.
10. Concentration Range
NOTE 2—It is essential that the DTPA salts be recrystallized since
10.1 The recommended concentration range is from 0.05 to
commercial DTPA contains impurities that absorb ultraviolet and visible
0.5 μg of beryllium in 25 mL of solution. light. These impurities produce bright blue fluorescence under ultraviolet
light, and react under certain conditions to produce a bright yellow
fluorescence.
11. Stability of Fluorescence
11.1 The fluorescence is stable for at least1hifthe test 14.8 Disodium Ethylenediaminetetraacetate (EDTA) Solu-
tion (100 g/L)—Dissolve 100 g of EDTA in water and dilute to
solutions are kept at constant temperature.
1L.
12. Interferences
14.9 EDTA Wash Solution—Add5mLofH SO and 10 mL
2 4
of the EDTA solution to 300 mL of water. Add 2 drops of
12.1 Silicon must be removed by dehydration or volatiliza-
phenol red indicator solution and NH OH until the solution
tion. Beryllium is separated from interfering ions by an
turns red. Cool and dilute to 500 mL.
acetylacetone extraction. Fluoride and pyrophosphate interfere
14.10 Morin Solution (0.075 g/L)—Dissolve 0.0075 g of
in the extraction.
anhydrous morin (3,5,7,28,48-penta-hydroxyflavone), reagent
13. Apparatus
grade, in 40 mL of ethanol. Transfer to a 100-mL volumetric
flask with water, dilute to volume, and mix.
13.1 Bottles, plastic, 500-mL capacity.
14.11 Phenol Red Indicator Solution (1 g/L)—Dissolve 0.1
13.2 Constant-Temperature Bath, 20 or 25°C.
g of phenol red in 50 mL of methanol and dilute to 100 mL
13.3 Fluorescence-Measuring Instrument— A suitable filter
with water.
fluorometer or spectrofluorometer with primary excitation at
approximately 430 nm and a means of isolating and measuring 14.12 Piperidine Buffer Solution—Dissolve 15 g of the
recrystallized DTPA in 200 mL of water. Add 75 mL of
the secondary fluorescent emission at approximately 520 nm.
redistilled piperidine and cool. Add 20 g of anhydrous sodium
14. Reagents
sulfite (Na SO ) and dilute to 500 mL. Store in a plastic bottle.
2 3
This solution slowly decomposes and should be discarded after
14.1 Acetylacetone (2,4-pentanedione), practical.
6 months.
14.2 Aluminum Sulfate Solution (49 g/L)—Dissolve 4.9 g of
14.13 Potassium Iodide-Starch Paper.
aluminum sulfate (Al (SO ) ·18H O) in 70 mL of water, add
2 4 3 2
14.14 Quinine Sulfate Solution (0.1 g/L)—Dissolve 0.1 g of
1 mL of HClO , transfer to a 100-mL volumetric flask, dilute
quinine sulfate in 300 mL of water. Add 10 mL of HClO and
to volume, and mix.
dilute to 1 L.
14.3 Ammonium Nitrate Wash Solution (10 g/L)—Dissolve
14.15 Sodium Hydroxide-Sodium Perchlorate-DTPA-
5 g of ammonium nitrate (NH NO ) in water and dilute to 500
4 3
Triethanolamine (TEA) Solution—Dissolve 60 g of sodium
mL.
hydroxide (NaOH) and 320 g of anhydrous sodium perchlorate
14.4 Beryllium, Standard Solution A (1 mL = 100 μg Be)—
(NaClO ) in 250 mL of water. Filter through a double 7-cm
Dissolve 1.964 g of beryllium sulfate (BeSO ·4H O) in water,
4 2 4
glass-fiber filter. Add 10 mL of TEA solution (20 volume %) to
add 10 mL of HClO , transfer to a 1-L volumetric flask, dilute
13.0 g of the recrystallized DTPA and dissolve in 50 mL of
to volume, and mix. Standardize as follows: transfer a 100-mL
aliquot of this solution to a 250-mL beaker, add NH OH (1+1) water and about 20 mL of the NaOH-NaClO solution. When
dissolution is complete, add the remainder of the NaOH-
until a permanent turbidity forms, and then add 10 mL in
excess. Allow to stand for 2 to3hor overnight. Filter using a NaClO solution and dilute to 500 mL. Store in a plastic bottle.
Acidify a small portion of the solution and test for oxidizing
low-ash, medium paper and wash well with NH NO wash
4 3
solution. Transfer the precipitate and paper to a weighed, agents with the potassium iodide-starch paper. If the presence
of an oxidizing agent is indicated, add sodium sulfite (Na SO )
covered platinum crucible and char. Finally ignite to constant
2 3
weight at 1000°C and weigh as beryllium oxide (BeO). in small portions until the oxidizing agent is destroyed.
14.5 Beryllium, Standard Solution B (1 mL = 0.10 μg Be)— 14.16 Sodium Hydroxide Solution (40 g/L)—Dissolve 20 g
Transfer a 10-mL aliquot of Beryllium Solution A to a 100-mL of NaOH in water and dilute to 500 mL. Store in a plastic
volumetric flask. Add 1 mL of HClO , dilute to volume, and bottle.
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
E34
15. Hazards approximately 40 mL. Add 2 drops of phenol red indicator
solution and NH
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