ASTM E315-88(1999)
(Test Method)Standard Test Methods for Chemical Analysis of Molybdenum
Standard Test Methods for Chemical Analysis of Molybdenum
SCOPE
1.1 These test methods cover the chemical analysis of molybdenum and molybdenum alloys having chemical compositions within the following limits: Element Concentration Range, % Carbon 0.010 to 0.040 Iron 0.020 max Molybdenum 99.25 to 99.99 Nickel 0.010 max Nitrogen 0.0010 max Oxygen 0.0030 max Silicon 0.010 max Titanium 0.005 to 0.55 Zirconium 0.06 to 0.12
1.2 The test methods in this standard are contained in the sections indicated below: Sections Nickel by the Persulfate-Dimethylglyoxime Photometric Method 9 to 18 Iron by the 1,10-Phenanthroline Photometric Method 19 to 29 Silicon by the Molybdenum Blue-Extraction Photometric Method 30 to 40
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 information is given in Section 5.
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Standards Content (Sample)
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Designation:E315–88(Reapproved 1999)
Standard Test Methods for
Chemical Analysis of Molybdenum
This standard is issued under the fixed designation E 315; 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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope Determine Conformance With Specifications
E50 Practices for Apparatus, Reagents, and Safety Precau-
1.1 These test methods cover the chemical analysis of
tions for Chemical Analysis of Metals
molybdenum and molybdenum alloys having chemical com-
E60 Practice for Photometric and Spectrophotometric
positions within the following limits:
Methods for Chemical Analysis of Metals
Element Concentration Range, %
E 173 Practice for Conducting Interlaboratory Studies of
Carbon 0.010 to 0.040
Iron 0.020 max
Methods for Chemical Analysis of Metals
Molybdenum 99.25 to 99.99
Nickel 0.010 max
3. Significance and Use
Nitrogen 0.0010 max
Oxygen 0.0030 max
3.1 These test methods for the chemical analysis of metals
Silicon 0.010 max
and alloys are primarily intended to test such materials for
Titanium 0.005 to 0.55
compliance with compositional specifications. It is assumed
Zirconium 0.06 to 0.12
that all who use these test methods will be trained analysts
1.2 The test methods in this standard are contained in the
capable of performing common laboratory procedures skill-
sections indicated below:
fully and safely. It is expected that work will be performed in
Sections
a properly equipped laboratory.
Nickel by the Persulfate-Dimethylglyoxime Photometric Method 9-18
Iron by the 1,10-Phenanthroline Photometric Method 19-29
4. Apparatus, Reagents, and Photometric Practice
Silicon by the Molybdenum Blue-Extraction Photometric Method 30-40
4.1 Apparatus and reagents required for each determination
1.3 This standard does not purport to address all of the
are listed in separate sections preceding the procedure. The
safety concerns, if any, associated with its use. It is the
apparatus, standard sections, and other reagents used in more
responsibility of the user of this standard to establish appro-
than one procedure are referred to by number and shall
priate safety and health practices and determine the applica-
conform to the requirements prescribed in Practices E 50E50,
bility of regulatory limitations prior to use. Specific precau-
except the photometers shall conform to the requirements
tionary information is given in Section 5.
prescribed in Practice E 60E60.
2. Referenced Documents
4.2 Photometric practice prescribed in these test methods
shall conform to Practice E 60E60.
2.1 ASTM Standards:
B 384 Specification for Molybdenum and MolybdenumAl-
5. Hazards
loy Forgings
5.1 For precautions to be observed in the use of certain
B 385 Specification for Molybdenum and MolybdenumAl-
reagents in these test methods, refer to Practices E 50E50.
loy Billets for Reforging
B 386 Specification for Molybdenum and MolybdenumAl-
6. Sampling
loy Plate, Sheet, Strip, and Foil
6.1 For procedures for sampling the material, refer to
B 387 Specification for Molybdenum and MolybdenumAl-
Specifications B 384, B 385, B 386, and
loy Bar, Rod, and Wire
B 387B 384B 385B 386B 387.
E29 Practice for Using Significant Digits in Test Data to
7. Rounding Calculated Values
7.1 Calculated values shall be rounded to the desired num-
These test methods are under the jurisdiction of ASTM Committee E-1 on
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct
ber of places as directed in 3.4 to 3.6 of Practice E 29E29.
responsibility of Subcommittee E01.06 on Titanium, Zirconium, Wolfram, Molyb-
denum, Tantalum, Niobium, Hafnium.
Current edition approved Dec. 31, 1988. Published May 1989. Originally
published as E 315 – 71 T. Last previous edition E 315 – 83. Annual Book of ASTM Standards, Vol 14.02.
2 4
Annual Book of ASTM Standards, Vol 02.04. Annual Book of ASTM Standards, Vol 03.05.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Please contact ASTM International (www.astm.org) for the latest information.
E315–88 (1999)
8. Interlaboratory Studies 15.1.1 Transfer 1.00, 3.00, 4.00, 7.00, and 10.00 mL of
nickel solution A (1 mL = 10 µg Ni) to five 50-mL volumetric
8.1 These test methods have been evaluated in accordance
flasks, dilute to 20 mL, and proceed as directed in 15.3.
with Practice E 173E 173, unless otherwise noted in the
15.1.2 Transfer 1.00, 5.00, 10.00, 15.00, and 20.00 mL of
precision and bias section.
nickel solution B (1 mL = 1 µg Ni) to five 50-mL volumetric
flasks, dilute to 20 mL, and proceed as directed in 15.3.
NICKEL BY THE PERSULFATE-
15.2 Reference Solution—Transfer 20 mL of water to a
DIMETHYLGLYOXIME PHOTOMETRIC TEST
50-mL volumetric flask and proceed as directed in 15.3.
METHOD
15.3 Color Development—Add 4 mL of (NH ) S O solu-
4 2 2 8
9. Scope tion, 5 mL of citric acid solution, and 10 mL of NH OH, and
cool to room temperature. Add 1 mL of sodium dimethylgly-
9.1 This test method covers the determination of nickel in
oximate solution, dilute to volume, and mix.
concentrations from 1 to 400 ppm. The range may be extended
15.4 Photometry—Transfer a suitable portion of the refer-
by suitably varying the sample weight, aliquot size, amount of
encesolutiontoanabsorptioncellwitha2ora5-cmlightpath,
reagents, and cell depth.
as appropriate (see 11.1), and adjust the photometer to the
initial setting, using a light band centered at approximately 445
10. Summary of Test Method
nm. While maintaining this adjustment, take the photometric
10.1 A red soluble salt of trivalent nickel and dimethylgly-
readings of the calibration solutions.
oxime is formed. Photometric measurement is made at ap-
15.5 Calibration Curves—Plot the photometric readings of
proximately 445 nm.
the calibration solutions against micrograms of nickel per 50
mL of solution.
11. Concentration Range
11.1 Therecommendedconcentrationrangesarefrom1.0to
16. Procedure
2.0 µg and from 10 to 100 µg of nickel for each 50 mL of
16.1 Test Solution:
solution, using cell depths of 5 and 2 cm respectively.
16.1.1 Select a sample weight in accordance with the
NOTE 1—This test method has been written for cells having 5 and 2-cm
following table:
light paths. Cells having other dimensions may be used, provided suitable
Nickel, ppm Sample Weight, g
adjustments can be made in the amounts of sample and reagents used.
1to50 1.00
45 to 120 0.50
12. Stability of Color
115 to 400 0.25
12.1 The color develops in 5 min and is stable for 30 min.
16.1.2 Weigh duplicate samples of the size selected to the
nearest 1 mg (Note 2), and transfer to 100-mLbeakers.Add 10
13. Interferences
mL of HCl and heat. Add HNO dropwise until all the metal
13.1 Provision has been made for the correction of any
has decomposed (Note 3). Remove from the hot plate and cool.
interfering elements present.
NOTE 2—Duplicate samples are taken in order to have one available to
determine the sample blank. For the higher concentrations of nickel, a
14. Reagents
larger sample may be dissolved and diluted to volume; duplicate aliquots
14.1 Ammonium Persulfate Solution (150 g/L)—Dissolve
may then be taken from a single sample.
15gofammoniumpersulfate[(NH ) S O ]inwateranddilute
4 2 2 8 NOTE 3—If any molybdic oxide precipitates, add more HCl dropwise
to 100 mL. Prepare fresh as needed. and boil gently until the molybdenum is completely in solution.
14.2 Citric Acid Solution (100 g/L)—Dissolve 10 g of citric
16.1.3 Transferthesolutionsto50-mLvolumetricflasksand
acid in water and dilute to 100 mL.
dilute to about 20 mL.
14.3 Nickel, Standard Solution A (1 mL = 10 µg Ni)—
16.2 Reference Solution—Distilled water.
Dissolve 0.1000 g of nickel (purity 99.9 % min) in 10 mL of
16.3 Reagent Blank Solution—Carry a reagent blank
water and 5 mL of HNO in a 150-mL beaker. When dissolu-
through the entire procedure using the same amount of all
tion is complete boil to remove oxides of nitrogen. Cool to
reagents.
room temperature, transfer to a 1-L volumetric flask, dilute to
16.4 Sample Blank Solution—Treattheduplicateasdirected
volume, and mix. Transfer a 50-mL aliquot of this solution to
in15.3butomittheadditionofthesodiumdimethylglyoximate
a 500-mL volumetric flask, dilute to volume, and mix.
solution.
14.4 Nickel, Standard Solution B (1 mL = 1 µg Ni)—
16.5 Color Development—Proceed as directed in 15.3.
Transfer a 10-mL aliquot of nickel solution A (1 mL = 10 µg
16.6 Photometry—Take the photometric readings of the
Ni) to a 100-mL volumetric flask, dilute to volume, and mix.
reagent blank solution, the sample blank solution, and the test
14.5 Sodium Dimethylglyoximate Solution (30 g/L)—
solution as directed in 15.4.
Dissolve 30 g of sodium dimethylglyoximate in water and
dilute to 1 L.
17. Calculation
15. Preparation of Calibration Curves
17.1 Convert the photometric readings of the test solution to
15.1 Calibration Solutions: micrograms of nickel, and of the reagent blank and sample
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Please contact ASTM International (www.astm.org) for the latest information.
E315–88 (1999)
blanksolutionstotheequivalentmicrogramsofnickelfromthe 23. Interferences
appropriate calibration curve. Calculate the parts per million of
23.1 Nickel, copper, and cobalt interfere if present in the
nickel as follows:
final test solution in amounts greater than 800 µg, 1600 µg, and
Nickel, ppm 5 [A 2 ~B 1 C!#/D (1) 800 µg, respectively. Reduced molybdenum produces a posi-
tive error and provision has been made in the method to
where:
eliminate this interference.
A = micrograms of nickel found in 50 mL of the final
solution,
24. Apparatus
B = reagent blank correction, in equivalent micrograms of
24.1 Plastic (TFE-Fluorocarbon) Beakers and Covers,
nickel,
50-mL capacity.
C = sample blank correction, in equivalent micrograms of
NOTE 5—Platinum beakers and covers may be used.
nickel, and
D = grams of sample represented in 50 mL of the final
25. Reagents
solution.
25.1 Ammonium Citrate-Sodium Borate Solution—Dissolve
200 g of ammonium citrate in 800 mL of water, and dilute to
18. Precision and Bias
1L.Dissolve85gofsodiumtetraborate,(Na B O ·10H O)in
2 4 7 2
18.1 Precision—Data on this test method were obtained by
900 mL of hot water, cool, and dilute to 1 L. Transfer the two
nine cooperators. Repeatability, standard deviation, and coef-
solutions to a 2-L bottle, and mix.
ficient of reproducibility were graphically calculated as di-
25.2 Hydroxylamine Hydrochloride (10 g/L)—Dissolve 1 g
rected in Practices E 173E 173, and were found to be as listed
of hydroxylamine hydrochloride (NH OH·HCl) in water and
in Table 1.
dilute to 100 mL. Do not use a solution that has stood longer
18.2 Bias—Data on bias is not available because of the lack
than 8 h.
of standard samples. However, one cooperator prepared syn-
25.3 Iron, Standard Solution (1 mL = 100 µg Fe)—Dissolve
thetic samples containing the equivalent of 53.9 ppm of nickel
0.1000gofiron(purity:99.8 %min) in60mLofHCl(1 + 1).
and recoveries within 0.8 ppm were obtained. Another coop-
Cool, transfer to a 1-L volumetric flask, dilute to volume, and
erator added 25 µg of nickel, equivalent to 25 ppm, to four 1-g
mix.
samples of Material A. Nickel recoveries (25 ppm plus 4 ppm
25.4 1,10-Phenanthroline Solution (2 g/L)—Dissolve 0.4 g
present) ranged between 28 and 30 ppm.
of 1,10-phenanthroline monohydrate in 150 mLof warm water
and dilute to 200 mL.
IRON BY THE 1, 10-PHENANTHROLINE
25.5 Reagent Mixture— Transfer 10 mLof HF and 8 mLof
PHOTOMETRIC TEST METHOD
HNO to a 50-mL plastic beaker (Note 5) and evaporate to
about 10 mL. Add about 30 mL of water and transfer to a
19. Scope
500-mL volumetric flask containing 360 mL of ammonium
19.1 This test method covers the determination of iron in
citrate-sodium borate solution. Cool, dilute to volume, and
concentrations from 50 to 750 ppm.
mix.
20. Summary of Test Method
26. Preparation of Calibration Curve
20.1 The iron is reduced with hydroxylamine hydrochloride
26.1 Calibration Solution—Using pipets, transfer 0.5, 1, 2,
and converted to the 1,10-phenanthroline complex. Photomet-
and 3 mL of iron solution (1 mL = 100 µg Fe) to 100-mL
ric measurement is made at approximately 510 nm.
volumetric flasks containing 50 mL of reagent mixture, and
dilute to about 75 mL. Proceed as directed in 26.3.
21. Concentration Range
26.2 Reference Solution—Transfer 50 mL of reagent mix-
21.1 The recommended concentration range is from 50 to
ture to a 100-mL volumetric flask and dilute to about 75 mL.
300 µg of iron for each 100 mL of solution, using a 2-cm cell.
26.3 Color Development—Using pipets, transfer 5 mL of
NH OH·HCl solution and 10 mL of 1,10-phenanthroline solu-
NOTE 4—This test method has been written for cells having a 2-cm 2
light path. Cells having other dimensions may be used, provided suitable tion. Dilute to about 90 mL and heat in a water bath at 60 to
adjustments can be made in the amounts of sample and reagents used.
70°C for 30 min. Cool, dilute to volume, and mix.
26.4 Photometry:
22. Stability of Color
26.4.1 Multiple-Cell Photometer—Measure the cell correc-
22.1 The color develops fully after heating at 60 to 70°C for
tion using absorption cells with a 2-cm light path (see Note 4)
30 min and is stable for 15 to 20 h.
and a light band centered at approximately 510 nm. Using the
test cell, take the photometric readings of the calibration
solutions.
TABLE 1 Statistical Information
26.4.2 Single-Cell Photometer—Transfer a suitable portion
Standard
Test Mean, Repeatability, Coefficient of of the reference solution to an absorption cell with a 2-cm light
Deviation,
Material ppm Ni ppm Ni Reproducibility, %
ppm Ni
A 3.9 0.737 0.226 18.9
B 114 11.04 3.45 9.7 National Institute of Standards and Technology Sample 55 has been found
satisfactory for this purpose.
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Please contact ASTM International (www.astm.org) for the latest information.
E315–88 (1999)
TABLE 2 Statistical Information
path (see Note 4) and adjust the photometer to the initial
setting, using a light band centered at approximately 510 nm. Test Iron Found, Repeatability Reproducibility
Material ppm (R , E173) (R , E173)
1 2
While maintaining this adjustment, take the photometric read-
...
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