ASTM E34-94(2002)
(Test Method)Standard Test Methods for Chemical Analysis of Aluminum and Aluminum-Base Alloys
Standard Test Methods for Chemical Analysis of Aluminum and Aluminum-Base Alloys
SIGNIFICANCE AND USE
These test methods for the chemical analysis of metals and alloys are primarily intended to test such materials for compliance with compositional specifications. It is assumed that all who use these test methods will be trained analysts capable of performing common laboratory procedures skillfully and safely. It is expected that work will be performed in a properly equipped laboratory.
Note—Shaded areas are suitable for sampling. FIG. 1 Type A and Type B Disks
SCOPE
1.1 These test methods cover the chemical analysis of aluminum and aluminum-base alloys having compositions within the following limits:
Beryllium, ppm0.3 to 100Bismuth, %0.02 to 1.0Boron, %0.005 to 0.060Cadmium, %0.001 to 0.50Chromium, %0.01 to 1.0Copper, %0.01 to 20.0Gallium, %0.001 to 0.05Iron, %0.01 to 3.0Lead, %0.01 to 1.0Lithium, %0.001 to 4.0Magnesium, %0.002 to 12.0Manganese, %0.005 to 2.0Nickel, %0.01 to 4.0Silicon, %0.05 to 20.0Tin, %0.03 to 1.0Titanium, %0.002 to 0.30Vanadium, %0.002 to 0.16Zinc, %0.003 to 12.0Zirconium, %0.01 to 0.30
1.2 The analytical procedures appear in the following order:
SectionsBeryllium by Argon Plasma Optical Emission Spectroscopy283 to 292Beryllium by the Morin (Fluorometric) Test Method8-19Bismuth by the Thiourea (Photometric) Method1aBismuth and Lead by the Atomic Absorption Test Method188 to 198Boron by the Carmine (Photometric) Test Method30 to 38Cadmium by the Atomic Absorption Test Method167 to 177Chromium:Diphenylcarbazide (Photometric) Test Method39 to 47Persulfate Oxidation (Titrimetric) Test Method1bChromium by the Atomic Absorption Test Method199 to 209Copper and Lead by the Electrolytic (Gravimetric) Test Method1cCopper and Zinc by the Atomic Absorption Test Method210 to 220Copper by the Electrolytic (Gravimetric) Test Method303 to 311Copper by the Neocuproine (Photometric) Test Method1aGallium by the Ion Exchange-Atomic Absorption Test Method312 to 323Iron by the 1,10-Phenanthroline (Photometric) Method73 to 81Iron and Manganese by the Atomic Absorption Method221 to 231Lithium by the Atomic Absorption Test Method324 to 334Magnesium:Pyrophosphate (Gravimetric) Method1 bEthylenediamine Tetraacetate (Titrimetric) TestMethod88 to 93Magnesium by the Atomic Absorption Test Method232 to 242Manganese by the Periodate (Photometric) Test Method 293 to 302Nickel:Dimethylglyoxime (Photometric) Test Method1aDimethylglyoxime (Gravimetric) Test Method1bNickel by the Atomic Absorption Test Method243 to 253Silicon:Molybdisilicic Acid (Photometric) Test Method118 to 127Sodium Hydroxide-Perchloric Acid (Gravimetric) Method128 to 133Tin by the Iodate (Titrimetric) Test Method134 to 140Titanium by the Chromotropic Acid (Photometric) Test Method 141 to 150Titanium by the Diantipyrylmethane Photometric Test Method254 to 263Vanadium by an Extraction-Photometric Test Methodusing N-Benzoyl- N-Phenylhydroxylamine264 to 273Zinc:Ammonium Mercuric Thiocyanate or the ZincOxide (Gravimetric) Test Method1 bEthylenediamine Tetraacetate (Titrimetric) Test Method 1dIon Exchange-EDTA Titrimetric Test Method274 to 282Zirconium by the Arsenazo III (Photometric) Method178 to 187
1.3 The values stated in SI units are to be regarded as the standard.
1.4 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. Specific hazard statements are given throughout these test methods.
General Information
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation:E34–94(Reapproved2002)
Standard Test Methods for
Chemical Analysis of Aluminum and Aluminum-Base Alloys
This standard is issued under the fixed designation E34; the number immediately following the designation indicates the year of original
adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.Asuperscript
epsilon (´) 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
1b
Persulfate Oxidation (Titrimetric) Test Method
1.1 These test methods cover the chemical analysis of
Chromium by the Atomic Absorption Test Method 199 to 209
aluminum and aluminum-base alloys having compositions
Copper and Lead by the Electrolytic (Gravimetric) Test
1c
Method
within the following limits:
Copper and Zinc by the Atomic Absorption Test
Beryllium, ppm 0.3 to 100
Method 210 to 220
Bismuth, % 0.02 to 1.0
Copper by the Electrolytic (Gravimetric) Test Method 303 to 311
Boron, % 0.005 to 0.060 1a
Copper by the Neocuproine (Photometric) Test Method
Cadmium, % 0.001 to 0.50
Chromium, % 0.01 to 1.0
Gallium by the Ion Exchange-Atomic Absorption Test
Copper, % 0.01 to 20.0
Method 312 to 323
Gallium, % 0.001 to 0.05
Iron by the 1,10-Phenanthroline (Photometric) Method 73 to 81
Iron, % 0.01 to 3.0
Iron and Manganese by the Atomic Absorption Method 221 to 231
Lead, % 0.01 to 1.0
Lithium by the Atomic Absorption Test Method 324 to 334
Lithium, % 0.001 to 4.0
Magnesium:
Magnesium, % 0.002 to 12.0 1b
Pyrophosphate (Gravimetric) Method
Manganese, % 0.005 to 2.0
Ethylenediamine Tetraacetate (Titrimetric) Test
Nickel, % 0.01 to 4.0
Method 88 to 93
Silicon, % 0.05 to 20.0
Magnesium by the Atomic Absorption Test Method 232 to 242
Tin, % 0.03 to 1.0
Manganese by the Periodate (Photometric) Test
Titanium, % 0.002 to 0.30
Method 293 to 302
Vanadium, % 0.002 to 0.16
Nickel:
Zinc, % 0.003 to 12.0 1a
Dimethylglyoxime (Photometric) Test Method
1b
Zirconium, % 0.01 to 0.30
Dimethylglyoxime (Gravimetric) Test Method
Nickel by the Atomic Absorption Test Method 243 to 253
1.2 The analytical procedures appear in the following order:
Silicon:
Sections Molybdisilicic Acid (Photometric) Test Method 118 to 127
Sodium Hydroxide-Perchloric Acid (Gravimetric)
Beryllium by Argon Plasma Optical Emission
Spectroscopy 283 to 292 Method 128 to 133
Tin by the Iodate (Titrimetric) Test Method 134 to 140
Beryllium by the Morin (Fluorometric) Test Method 8-19
1a
Bismuth by the Thiourea (Photometric) Method Titanium by the Chromotropic Acid (Photometric) Test
Method 141 to 150
Bismuth and Lead by the Atomic Absorption Test
Method 188 to 198 Titanium by the Diantipyrylmethane Photometric Test
Method 254 to 263
Boron by the Carmine (Photometric) Test Method 30 to 38
Cadmium by the Atomic Absorption Test Method 167 to 177 Vanadium by an Extraction-Photometric Test Method
using N-Benzoyl-N-Phenylhydroxylamine 264 to 273
Chromium:
Zinc:
Diphenylcarbazide (Photometric) Test Method 39 to 47
Ammonium Mercuric Thiocyanate or the Zinc
1b
Oxide (Gravimetric) Test Method
Ethylenediamine Tetraacetate (Titrimetric) Test
1d
These test methods are under the jurisdiction of ASTM Committee E01 on
Method
Analytical Chemistry for Metals, Ores, and Related Materials and are the direct
Ion Exchange-EDTATitrimetric Test Method 274 to 282
responsibility of Subcommittee E01.04 on Aluminum and Magnesium.
Zirconium by the Arsenazo III (Photometric) Method 178 to 187
Current edition approved Oct. 10, 2002. Published October 2002. Originally
1.3 The values stated in inch-pound units are to be regarded
approved in 1960. Last previous edition approved in 1998 as E34 – 94 (1998). DOI:
10.1520/E0034-94R02.
as standard. The values given in parentheses are mathematical
1a
Discontinued as of Feb. 25, 1983.
conversions to SI units that are provided for information only
1b
Discontinued as of May 29, 1981.
1c and are not considered standard.
Discontinued as of Oct. 25, 1985.
1d
Discontinued as of March 25, 1983.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
E34–94 (2002)
1.4 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 appro-
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.
2. Referenced Documents
2.1 ASTM Standards:
E29 Practice for Using Significant Digits in Test Data to
Determine Conformance with Specifications
E50 Practices for Apparatus, Reagents, and Safety Consid-
erations for Chemical Analysis of Metals, Ores, and
Related Materials
E55 Practice for Sampling Wrought Nonferrous Metals and
Alloys for Determination of Chemical Composition
E60 Practice for Analysis of Metals, Ores, and Related
Materials by Molecular Absorption Spectrometry
E88 Practice for Sampling Nonferrous Metals andAlloys in
Cast Form for Determination of Chemical Composition
E173 Practice for Conducting Interlaboratory Studies of
Methods for Chemical Analysis of Metals
E716 Practices for Sampling Aluminum and Aluminum
Alloys for Spectrochemical Analysis
E1024 Guide for Chemical Analysis of Metals and Metal
Bearing Ores by Flame Atomic Absorption Spectropho-
tometry
3. Significance and Use
3.1 These test methods for the chemical analysis of metals
and alloys are primarily intended to test such materials for
NOTE 1—Shaded areas are suitable for sampling.
compliance with compositional specifications. It is assumed
FIG. 1 Type A and Type B Disks
that all who use these test methods will be trained analysts
capable of performing common laboratory procedures skill-
fully and safely. It is expected that work will be performed in
6. Sampling
a properly equipped laboratory.
6.1 Wrought products shall be sampled in accordance with
Practice E55. Cast products shall be sampled in accordance
4. Apparatus, Reagents, and Photometric Practice
with Practice E88.
4.1 Apparatus and reagents required for each determination
6.2 Chill cast disks produced for analysis by spectrochemi-
are listed in separate sections preceding the procedure. The
cal methods (see Practices E716) shall be considered cast
apparatus, standard solutions, and certain other reagents used
products. The principles of Practice E88 shall apply.
in more than one procedure are referred to by number and shall
6.2.1 Prepare such disks for chemical analysis by drilling or
conform to the requirements prescribed in Practices E50,
milling through the entire thickness of an unmachined disk
except that photometers shall conform to the requirements
(Note 1). Use a minimum of two positions approximately
prescribed in Practice E60.
opposite each other and combine the drillings or millings.
4.2 Photometric practice prescribed in these test methods
NOTE 1—The use of a machined disk may result in the exclusion of an
shall conform to Practice E60.
element-rich portion of the sample. This practice should be avoided
wherever possible, especially for analyses affecting product acceptance.
5. Precautions
6.2.2 The outer edges of the holes shall be approximately
5.1 For precautions to be observed in the use of certain
0.48 cm ( ⁄16 in.) from the edge of the disk. Drills shall be not
reagents in these test methods, reference shall be made to
less than 0.95 cm ( ⁄8 in.) in diameter and not larger than 1.27
Practices E50.
cm ( ⁄2 in.) in diameter.
6.2.3 Milldisksatsimilarpointstoadistanceof40 %ofthe
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
sample diameter. Use a 0.95-cm ( ⁄8 in.) milling cutter.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
3 4
Withdrawn. The last approved version of this historical standard is referenced Olson, H. A., and Macy, D. W., “Metallurgical Approach to Evaluating
on www.astm.org. Chemical Sample Disks,” Light Metals, Vol 2, 1978, pp. 301–311.
E34–94 (2002)
6.2.4 Sample book mold disks (Type A, Practices E716)at 14.3 Ammonium Nitrate Wash Solution (10 g/L)—Dissolve
approximately the 9 o’clock and the 3 o’clock positions when 5 g of ammonium nitrate (NH NO ) in water and dilute to 500
4 3
the sprue is at the 12 o’clock position. Center pour (Type B,
mL.
Practices E716) and vacuum cast disks may be sampled around
14.4 Beryllium, Standard Solution A (1 mL = 100 µg Be)—
the entire circumference. Fig. 1 illustrates the areas suitable for
Dissolve 1.964 g of beryllium sulfate (BeSO ·4H O) in water,
4 2
sampling Type A and Type B disks. Vacuum cast disks are
add 10 mL of HClO , transfer to a 1-L volumetric flask, dilute
sampled in the same manner as Type B disks.
to volume, and mix. Standardize as follows: transfer a 100-mL
6.2.5 Drilling or milling techniques ideally should produce
aliquot of this solution to a 250-mLbeaker, add NH OH (1+1)
uniformly small chips. Break large continuous pieces into
until a permanent turbidity forms, and then add 10 mL in
1 3
smallerpieces0.64cm( ⁄4in.)to0.95cm( ⁄8in.)long.Drilling
excess. Allow to stand for 2 to3hor overnight. Filter using a
or milling techniques should minimize production of fine,
low-ash, medium paper and wash well with NH NO wash
4 3
dust-like material.
solution. Transfer the precipitate and paper to a weighed,
covered platinum crucible and char. Finally ignite to constant
7. Rounding Calculated Values
weight at 1000°C and weigh as beryllium oxide (BeO).
7.1 Calculated values shall be rounded to the desired num-
14.5 Beryllium, Standard Solution B (1 mL = 0.10 µg Be)—
ber of places in accordance with the rounding method given in
Transfer a 10-mLaliquot of Beryllium SolutionAto a 100-mL
3.4 and 3.5 of Practice E29.
volumetric flask. Add 1 mL of HClO , dilute to volume, and
mix. Transfer a 10-mL aliquot of this solution to a 1-L
BERYLLIUM BY THE MORIN (FLUOROMETRIC)
volumetric flask. Add 10 mL of HClO , dilute to volume, and
TEST METHOD
mix.
8. Scope
14.6 Chloroform (CHCl ).
8.1 This test method covers the determination of beryllium
14.7 Diethylenetriaminepentaacetic Acid (DTPA), Recrys-
in concentrations from 1 to 100 ppm.
tallized (Note 2)—Add 100 g of DTPA to 800 mL of boiling
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
9.1 In an alkaline solution, beryllium and morin form a
through a hardened retentive paper.Transfer the clear filtrate to
compound which produces a yellow-green fluorescence at
a 1-L beaker and stir vigorously to induce crystallization
approximately 520 nm when excited by light at approximately
throughout the solution. Cool thoroughly in a water bath. Filter
430 nm.
withsuctionusingahardenedpaperandremoveasmuchwater
as possible. Dry the salts at 110°C.
10. Concentration Range
10.1 The recommended concentration range is from 0.05 to NOTE 2—It is essential that the DTPA salts be recrystallized since
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
11. Stability of Fluorescence
fluorescence.
11.1 The fluorescence is stable for at least 1 h if the test
solutions are kept at constant temperature.
14.8 Disodium Ethylenediaminetetraacetate (EDTA) Solu-
tion (100 g/L)—Dissolve 100 g of EDTAin water and dilute to
12. Interferences
1L.
12.1 Silicon must be removed by dehydration or volatiliza-
14.9 EDTA Wash Solution—Add5mLofH SO and10mL
2 4
tion. Beryllium is separated from interfering ions by an
of the EDTA solution to 300 mL of water. Add 2 drops of
acetylacetone extraction. Fluoride and pyrophosphate interfere
phenol red indicator solution and NH OH until the solution
in the extraction.
turns red. Cool and dilute to 500 mL.
14.10 Morin Solution (0.075 g/L)—Dissolve 0.0075 g of
13. Apparatus
anhydrous morin (3,5,7,28,48-penta-hydroxyflavone), reagent
13.1 Bottles, plastic, 500-mL capacity.
grade, in 40 mL of ethanol. Transfer to a 100-mL volumetric
13.2 Constant-Temperature Bath, 20 or 25°C.
flask with water, dilute to volume, and mix.
13.3 Fluorescence-Measuring Instrument—Asuitable filter
14.11 Phenol Red Indicator Solution (1 g/L)—Dissolve 0.1
fluorometer or spectrofluorometer with primary excitation at
g of phenol red in 50 mL of methanol and dilute to 100 mL
approximately 430 nm and a means of isolating and measuring
with water.
the secondary fluorescent emission at approximately 520 nm.
14.12 Piperidine Buffer Solution—Dissolve 15 g of the
14. Reagents recrystallized DTPA in 200 mL of water. Add 75 mL of
redistilled piperidine and cool.Add 20 g of anhydrous sodium
14.1 Acetylacetone (2,4-pentanedione), practical.
sulfite(Na SO )anddiluteto500mL.Storeinaplasticbottle.
14.2 Aluminum Sulfate Solution (49 g/L)—Dissolve 4.9 g of 2 3
This solution slowly decomposes and should be discarded after
aluminum sulfate (Al (SO ) ·18H O) in 70 mL of water, add
2 4 3 2
6 months.
1 mL of HClO , transfer to a 100-mL volumetric flask, dilute
to volume, and mix. 14.13 Potassium Iodide-Starch Paper.
E34–94 (2002)
14.14 Quinine Sulfate Solution (0.1 g/L)—Dissolve 0.1 g of 16.5 Calibration Curve—Plot the fluorometric readings of
quinine sulfate in 300 mL of water. Add 10 mL of HClO and the calibration solutions against micrograms of beryllium per
dilute to 1 L. 25 mL of solution.
14.15 Sodium Hydroxide-Sodium Perchlorate-DTPA-
Triethanolamine (TEA) Solution—Dissolve 60 g of sodium 17. Procedure
hydroxide (NaOH) and 320 g of anhydrous sodium perchlorate
17.1 Test Solution:
(NaClO ) in 250 mL of water. Filter through a double 7-cm
17.1.1 Transfer 1.00 g of the sample, weighed to the nearest
glass-fiber filter.Add 10 mLofTEAsolution (20 volume %) to
1 mg, to a 250-mL beaker. Add 25 mL of water and 10 mL of
13.0 g of the recrystallized DTPA and dissolve in 50 mL of
HCl. Warm the solution, if necessary, to hasten dissolution.
water and about 20 mL of the NaOH-NaClO solution. When
When dissolution is complete, boil for a few minutes.
dissolution is complete, add the remainder of the NaOH-
17.1.2 Add 5 mL of HNO and 20 mL of HClO and
3 4
NaClO solutionanddiluteto500mL.Storeinaplasticbottle.
evaporate to the appearance of HClO fumes. Reduce the heat
Acidify a small portion of the solution and test for oxidizing
to avoid bumping
...
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