Designation: E367 09

Standard Test Methods for

Chemical Analysis of Ferroniobium1
This standard is issued under the fixed designation E367; 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 2. Referenced Documents

1.1 These test methods cover the chemical analysis of 2.1 ASTM Standards:2
ferroniobium having chemical compositions within the follow- A550 Specification for Ferrocolumbium
ing limits: E29 Practice for Using Significant Digits in Test Data to
Element Concentration, % Determine Conformance with Specifications
Aluminum 2.00 max E32 Practices for Sampling Ferroalloys and Steel Additives
Carbon 0.30 max
Chromium 2.00 max
for Determination of Chemical Composition
Cobalt 0.25 max E50 Practices for Apparatus, Reagents, and Safety Consid-
Lead 0.01 max erations for Chemical Analysis of Metals, Ores, and
Manganese 3.00 max
Niobium 40.00 to 75.00
Related Materials
Phosphorus 0.05 max E60 Practice for Analysis of Metals, Ores, and Related
Silicon 4.00 max Materials by Spectrophotometry
Sulfur 0.03 max
Tantalum 7.00 max
E135 Terminology Relating to Analytical Chemistry for
Tin 0.15 max Metals, Ores, and Related Materials
Titanium 5.00 max E173 Practice for Conducting Interlaboratory Studies of
Tungsten 0.50 max
Methods for Chemical Analysis of Metals (Withdrawn
1.2 The test methods appear in the following order: 1998)3
Sections E1601 Practice for Conducting an Interlaboratory Study to
Separation of Niobium, Tantalum, and 10-16 Evaluate the Performance of an Analytical Method
Titanium
by the Ion-Exchange Test Method
Titanium by the Photometric Test 17-21 3. Terminology
Method [0.05 % to 5.0 %]
Niobium by the Gravimetric Test 22-23 3.1 For definition of terms used in this test method, refer to
Method [40 % to 75 %] Terminology E135.
Tantalum by the Gravimetric Test 24-25
Method [1 % to 7 %]
Tantalum by the Photometric Test 26-30 4. Significance and Use
Method [0.25 % to 1 %]
4.1 These test methods for the chemical analysis of metals
1.3 The values stated in SI units are to be regarded as and alloys are primarily intended to test such materials for
standard. No other units of measurement are included in this compliance with compositional specifications such as Specifi-
standard. cation A550. It is assumed that all who use these test methods
1.4 This standard does not purport to address all of the will be trained analysts capable of performing common labo-
safety concerns, if any, associated with its use. It is the ratory procedures skillfully and safely. It is expected that work
responsibility of whoever uses this standard to consult and will be performed in a properly equipped laboratory.
establish appropriate safety and health practices and deter-
mine the applicability of regulatory limitations prior to use. 5. Apparatus, Reagents, and Photometric Practice
Specific precautionary statements are given in Section 6, and 5.1 Apparatus, standard solutions, and other reagents re-
specific warning statements in 11.1. quired for each determination are listed in separate sections

1 2
These test methods are under the jurisdiction of ASTM Committee E01 on For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Analytical Chemistry for Metals, Ores, and Related Materials and are the direct contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
responsibility of Subcommittee E01.01 on Iron, Steel, and Ferroalloys. Standards volume information, refer to the standards Document Summary page on
Current edition approved Oct. 1, 2009. Published November 2009. Originally the ASTM website.
3
approved in 1970. Last previous edition approved in 2003 as E367 03. DOI: The last approved version of this historical standard is referenced on
10.1520/E0367-09. www.astm.org.

Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States

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 E367 09
preceding the procedure. Photometers shall conform to the the skin or fingernail must receive immediate first-aid and
requirements prescribed in Practice E60. medical attention should be promptly sought.)
5.2 Photometric practice prescribed in these test methods
12. Interferences
shall conform to Practice E60.
12.1 Any bismuth present will appear in the tantalum
6. Hazards fraction, but this element is seldom present greater than
6.1 For precautions to be observed in the use of certain 0.005 % in this ferroalloy. Trivalent antimony, if present, is
reagents in these test methods, refer to Practices E50. eluted with the titanium and precipitated with cupferron, but it
does not interfere in the photometric test method for titanium.
6.2 Specific warning statements are given in 11.1.
7. Sampling 13. Apparatus
7.1 For procedures for sampling the material, and for 13.1 Ion-Exchange ColumnsThe columns must be con-
particle size of the sample for chemical analysis, refer to structed of polystyrene tubing approximately 300-mm long and
Practices E32. 25 mm in inside diameter. A suitable column can be prepared
as follows: Insert a waxed, No. 5 rubber stopper containing a
8. Rounding Off Calculated Values 5-mm hole into the bottom of the polystyrene tube. Insert into
8.1 Calculated values shall be rounded off to the desired the hole and flush with the upper surface of the stopper a
number of places as directed in Practice E29. 150-mm length of polystyrene tubing, having a 5-mm outside
diameter and a 2-mm bore. Attach another 150-mm length of
9. Interlaboratory Studies this tubing to the smaller tube with an approximately 50-mm
length of polyvinyl tubing,4 and control the flow rate by a
9.1 These test methods have been evaluated in accordance
hosecock on the polyvinyl tubing.
with Practice E173, unless otherwise noted in the precision and
13.1.1 If a number of determinations are to be made, it is
bias section.
convenient to arrange the columns so that they can be operated
NIOBIUM, TANTALUM, AND TITANIUM BY THE with a minimum of attention. Plastic columns equipped with
ION-EXCHANGE TEST METHOD fittings of polystyrene have been developed for such an
assembly.5 Inlet and outlet tubes are polyethylene; flexible
10. Scope connections, where necessary, are of polyvinyl tubing. The
10.1 These test methods cover the determination of flow rate is controlled by hosecocks on these flexible connec-
niobium, tantalum, and titanium in ferroniobium from 40 % to tions. The system must be carefully assembled and checked to
75 %, 0.25 % to 7 %, and 0.05 % to 5.0 %, respectively. avoid possible leakage of the solutions containing HF.
13.2 Plastic WarePolyethylene, polypropylene, or TFE-
11. Summary of Test Method fluorocarbon.
11.1 The sample is dissolved in a HCl-HF acid mixture and 13.2.1 Bottles, 250-mL and 1-L capacity.
transferred to an anion-exchange column. Titanium, iron, and 13.2.2 Graduated Cylinders, 50-mL and 250-mL capacity.
other elements are eluted with anNH4Cl-HCl-HF acid mixture. 13.2.3 Griffn-Form Beakers and Covers, 250-mL, 600-mL,
This eluate is treated with boric acid (H3BO3) and cupferron, and 1-L capacity.
and the precipitate, containing the titanium, is ignited, fused
with potassium hydrogen sulfate, and leached in dilute H2SO4. 14. Reagents
The titanium is oxidized to the yellow pertitanate with hydro- 14.1 Ammonium Chloride Solution (240 g/L)issolve 480
gen peroxide. Photometric measurement is made at approxi- g of ammonium chloride (NH4Cl) in 1600 mL of water by
mately 410 nm. Niobium is removed by eluting with an warming, cool, dilute to 2 L, and mix. Filter, if necessary. Use
ammonium chloride-hydrofluoric acid mixture. Tantalum is this stock solution to prepare the solutions described in
removed by eluting with an ammonium chloride-ammonium 14.2-14.4.
fluoride solution adjusted to a pH of 5 to 6. The eluates are
treated with the H3BO3 to complex the fluorides, and each of 14.2 Ammonium Chloride-Ammonium Fluoride Neutral
the elements, niobium and tantalum, is precipitated with MixtureTransfer 600 mL of the NH4Cl solution and 40 mL of
cupferron, ignited, and weighed as the pentoxide. For tantalum HF to a plastic beaker. Adjust the pH from 5 to 6 with NH4OH
below 1 %, zirconium is added as a gatherer in the cupferron (approximately 80 mL to 85 mL will be required), dilute to 1
separation and the tantalum is converted to the pyrogallol L with water, and mix.
complex. Photometric measurement is made at approximately NOTE 1This solution must be prepared with care. If the pH is too low,
420 nm. (WarningHF produces very serious burns which the volume specified will not completely elute the tantalum; if the pH is
may or may not be painful on first contact. Such burns often too high, tantalum will precipitate in the column, thus leading to error in
the determinations being run as well as the one which follows.
damage bone and other tissue within the body. Standard
procedure is to use gloves and protective clothing when
handling this reagent. After the material is added, the closed 4
Tygon-R tubing has been found satisfactory for this purpose.
container, gloves, and all surfaces that may later be touched are 5
Columns available from Ledoux and Co., Inc., Teaneck, NJ, have been found
rinsed with large quantities of water. Even one drop of HF on satisfactory for this purpose.

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 E367 09
14.3 Ammonium Chloride-Hydrochloric-Hydrofluoric Acid 14.16 Titanium, Standard Solution (1 mL = 0.100 mg Ti)
MixtureTransfer 240 mL of the NH4Cl solution, 200 mL of Transfer 0.0834 g of titanium dioxide (TiO2) to a platinum
HF and 150 mL of HCl to a plastic bottle. Dilute to 1 L with crucible. Add 1 g of KHSO4, and heat to fuse the oxide. Cool,
water, and mix. and dissolve the melt in 50 mL of warm H2SO4 (1 + 9). Cool,
14.4 Ammonium Chloride-Hydrofluoric Acid Mixture transfer to a 500-mL volumetric flask, dilute to volume with
Transfer 600 mL of the NH4Cl solution and 40 mL of HF to a H2SO4 (1 + 9), and mix.
plastic bottle. Dilute to 1 L with water, and mix. 14.17 Zirconium Solution (1 mL = 1 mg Zr)Dissolve 0.5
14.5 Ammonium Nitrate Wash Solution (20 g/L)Dissolve g of zirconium metal in 10 mL of HF in a plastic bottle, and
20 g of ammonium nitrate (NH4NO3) in water, and dilute to 1 dilute to 500 mL. An equivalent amount of zirconyl chloride
L. may be substituted for the zirconium metal.
14.6 Boric Acid (H3BO3).
15. Preparation of Ion-Exchange Column
14.7 Cupferron Solution (60 g/L)Dissolve 6 g of cupfer-
ron in 80 mL of cold water, dilute to 100 mL, and filter. This 15.1 Place a 6-mm to 10-mm layer of acid-resistant poly-
solution should be prepared fresh as needed and cooled to 5 C (vinyl chloride) plastic fiber in the bottom of the column. Add
before use. the resin suspension in small portions to obtain a settled bed of
the resin 150-mm to 180-mm high. Wash the column with
14.8 Cupferron Wash SolutionAdd 25 mL of cupferron approximately 100 mL of HNO3 (1 + 9), and then perform
solution (14.7) to 975 mL of cold HCl (1 + 9), and mix. Prepare three elution cycles with alternate additions of 100 mL of HCl
as needed. (1 + 9) and 100 mL of HCl (3 + 1) to remove the remainder of
14.9 Hydrochloric-Hydrofluoric Acid MixtureAdd 250 the fines. Finally, wash the column with 200 mL of HCl (1 + 3)
mL of HCl to 300 mL of water, add 200 mL of HF, dilute to 1 to a level about 20 mm above the resin.
L with water, and mix.
NOTE 3Resin columns prepared in this way have been used for
14.10 Hydrogen Peroxide (H2O2), 30 %. several years; the only maintenance may be to empty and refill the column
with the resin charge if the flow rate becomes excessively slow due to
14.11 Ion-Exchange ResinStrongly basic anion-exchange packing.
resin, 200 mesh to 400 mesh, 8 % to 10 % divinyl-benzene
cross linkage.6 Since the mesh size of the resin may vary 16. Preparation of Test Solutions
considerably from lot to lot, air-dry the resin and pass it
through a No. 270 (53-m) sieve (Note 2). Most of the fines are 16.1 Transfer a 0.5-g sample, weighed to the nearest 0.1 mg,
removed from the fraction passing the No. 270 sieve as to a 250-mL plastic beaker. Add 40 mL of the HCl-HF acid
follows: Prepare a suspension of the resin in HCl (1 + 9). mixture. Place a plastic cover on the beaker, and heat gently.
Allow the coarser fraction to settle 10 min to 15 min and After the reaction ceases, add HNO3 dropwise until the
remove the fines by decantation. Repeat the process several solution clears (Note 4). Digest on the steam bath for 20 min to
times until most of the very fine material has been removed 30 min to remove nitrous oxide fumes. Rinse the plastic cover
from the suspension. and wall of the beaker with the HCl-HF acid mixture, and
dilute the solution to 70 mL with the same acid mixture.
NOTE 2Material retained on the No. 270 sieve may be used for other
purposes. NOTE 4The addition of HNO3 should be kept to a minimum because
of its strong replacing power for niobium on the exchange column.
14.12 Oxalate-Citrate-Sulfuric Acid SolutionDissolve 35 Approximately 6 drops to 8 drops will be required.
g of ammonium oxalate ((NH4)2C2O4H2O) and 35 g of
diammonium hydrogen citrate ((NH4)2HC8H5O7) in 1 L of 16.2 Transfer 50 mL of HCl-HF acid mixture to the column
H2SO4 (1 + 39). in 5-mL to 10-mL increments. Drain the acid to a level 100 mm
above the resin bed, collecting the eluate in a 600-mL plastic
14.13 Pyrogallol (C6H3-1,2,3-(OH)3). beaker. Transfer the sample solution in 5-mL to 10-mL
14.14 Sodium Hydroxide Solution (100 g/L)Dissolve 20 g increments to the column. As the sample solution moves down
of sodium hydroxide (NaOH) in 150 mL of water, cool, dilute the column, continue to add the small increments until all of
to 200 mL, and mix. Store in a plastic bottle. the solution has been transferred. Wash the beaker four or five
14.15 Tantalum, Standard Solution (1 mL = 0.500 mg Ta) times with 4-mL portions of the HCl-HF acid mixture, trans-
Transfer 0.1221 g of tantalum pentoxide (Ta2O5) to a platinum ferring the washings to the column. Wash the sides of the
crucible. Add 2.5 g of potassium hydrogen sulfate (KHSO4) column with 10 mL to 15 mL of the HCl-HF acid mixture
and heat to fuse the oxide. Dissolve the cooled melt in warm followed by several washings with the NH4Cl-HCl-HF acid
oxalate-citrate-sulfuric acid solution. Transfer to a 200-mL mixture.
volumetric flask, cool, dilute to volume with oxalate-citrate- 16.3 Pass a total of 300 mL of the NH4Cl-HCl-HF acid
sulfuric acid solution and mix. mixture through the column at a flow rate of approximately 100
mL/h to 125 mL/h. Allow the solution to drain to the top of the
resin. Remove the beaker containing the first fraction and
6
Dowex I anion-exchange resin has been found satisfactory. Comparable results reserve this solution for the determination of titanium. Replace
may not be obtained with other resins. the beaker with another 600-mL plastic beaker.

3
 E367 09
16.4 Wash the sides of the column with four or five portions 19.5 Calibration CurvePlot the net photometric readings
(a total of about 25 mL) of the NH4Cl-HF acid mixture, of the calibration solutions against milligrams of titanium per
allowing the solution to drain to the top of the resin each time. 100 mL of solution.
Pass a total of 300 mL of the NH4Cl-HF acid mixture through
20. Procedure
the column at the flow rate specified in 16.3 (Note 5). Remove
the beaker containing the second fraction and reserve this 20.1 Transfer the first fraction containing the titanium and
solution for the determination of niobium. Replace the beaker iron reserved as directed in 16.3 to a 1500-mL beaker contain-
with another 600-mL plastic beaker. ing 50 g of H3BO3 dissolved in 700 mL of warm water. Add
125 mL of HCl and cool to 5 C.
NOTE 5This point in the preparation of the test solutions provides a
convenient and satisfactory place to stop, for example overnight, if the 20.2 Add 50 mL of cupferron solution slowly while stirring
elutions otherwise cannot be carried through as a continuous operation. the solution. Add filter paper pulp, stir well, and allow to stand
16.5 Wash the sides of the column with five or six 5-mL for 10 min to 15 min. Filter, using moderate suction, on a
portions of the NH4Cl-NH4F neutral mixture. Pass a total of Buchner funnel, using double thickness 9-cm, low-ash, fine
350 mL of the NH4Cl-NH4F neutral mixture through the filter paper precoated with a little filter paper pulp. Transfer the
column, at the flow rate specified in 16.3. Remove the beaker precipitate to the funnel, clean the beaker with a piece of
containing the third fraction and reserve this solution for the moistened filter paper and add this to the funnel. Wash the
determination of tantalum as directed in Section 24 or Section paper and precipitate with 400 mL of cold (5 C) cupferron
29. Prepare the column for the next sample by adding 50 mL wash solution.
of HCl (1 + 3) in 10-mL increments and discarding the 20.3 Transfer the paper and precipitate to a porcelain
effluents. crucible, and ignite at 550 C to 600 C until the carbon is
destroyed.
TITANIUM BY THE PHOTOMETRIC TEST METHOD
20.4 If vanadium is present, fuse the ignited oxides with 2 g
17. Concentration Range to 3 g of KHSO4, cool, and dissolve the melt in 30 mL of HCl
(1 + 9) in a 150-mL beaker. Add NaOH solution until alkaline
17.1 The recommended concentration range is 0.100 mg to to litmus and add 5 mL in excess. Boil for 3 min, and then add
2.50 mg of titanium for each 100 mL of solution, using a 2-cm some filter paper pulp. Filter using a medium filter paper and
cell. wash the precipitate with the NH4NO3 wash solution. Transfer
NOTE 6This test method has been written for a cell having a 2-cm the paper and precipitate to a porcelain crucible and ignite at
light path. Cells having other dimensions may be used, provided suitable 550 C to 600 C until the carbon is destroyed.
adjustments can be made in the amounts of sample and reagents used.
20.5 Fuse the ignited oxides obtained in 20.3 and 20.4 with
18. Stability of Color 2 g to 3 g of KHSO4 and leach in 30 mL of H2SO4 (1 + 9).
20.6 Transfer the solution, selecting the size of the volumet-
18.1 The color is stable for at least 2 h.
ric flask in accordance with the following:
Equivalent Sample
19. Preparation of Calibration Curve Initial Dilution, Aliquot Volume, Weight in Aliquot
19.1 Calibration SolutionsUsing pipets, transfer (1, 5, 10, Titanium, % mL mL Volume, g
0.05 to 1.25 50 20 0.2
15, and 25) mL of titanium solution (1 mL = 0.100 mg Ti) to 1.24 to 2.50 50 10 0.1
100-mL volumetric flasks, dilute to approximately 80 mL with 2.49 to 5.00 100 10 0.05
H2SO4 (1 + 9), and mix. Proceed as described in 19.3. (Filter through a fine filter paper into the appropriate size
19.2 Reference SolutionsUsing pipets, transfer (1, 5, 10, volumetric flask if the solution is not clear and wash with
15, and 25) mL of titanium solution (1 mL = 0.100 mg Ti) to H2SO4 (1 + 9).) Dilute to volume with H2SO4 (1 + 9) and
100-mL volumetric flasks, dilute to volume with H2SO4 mix.
(1 + 9), and mix. 20.7 Transfer two aliquots to 100-mL volumetric flasks,
19.3 Color DevelopmentAdd 1.0 mL of H2O2, dilute to selecting the aliquot volume in accordance with 20.6. Dilute to
volume with H2SO4 (1 + 9), and mix. approximately 80 mL with H2SO4 (1 + 9); treat one as directed
in 20.2 and the other as directed in 20.3.
19.4 Photometry:
20.8 Reference SolutionDilute to volume with H2SO4
19.4.1 Multiple-Cell PhotometerMeasure the cell
(1 + 9), and mix. Proceed as directed in 19.4.
correction, using absorption cells with a 2-cm light path and a
light band centered at approximately 410 nm. Using the test 20.9 Color DevelopmentProceed as directed in 19.3.
cell, take the photometric readings of the calibration solutions. 20.10 PhotometryTake the photometric reading of the test
19.4.2 Single-Cell PhotometerTransfer a suitable portion solution as directed in 19.4.
of the reference solution to an absorption cell with a 2-cm light
path and adjust the photometer to the initial setting, using a 21. Calculation
light band centered at approximately 410 nm. While maintain- 21.1 Convert the net photometric reading of the test solution
ing this adjustment, take the photometric readings of the to milligrams of titanium by means of the calibration curve.
calibration solutions. Calculate the percentage of titanium as follows:

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 E367 09
Titanium, % 5 A/ ~ B 3 10! (1) NOTE 8This test method has been written for cells having a 1-cm light
path. Cells having other dimensions may be used, provided suitable
where: adjustments can be made in the amounts of sample and reagents used.
A = milligrams of titanium found in 100 mL of final test
27. Stability of Color
solution, and
B = grams of sample represented in 100 mL of final test 27.1 The color is stable for at least 1 h.
solution.
28. Preparation of Calibration Curve
NIOBIUM BY THE GRAVIMETRIC TEST METHOD 28.1 Calibration SolutionsUsing pipets, transfer (2, 4, 7,
and 10) mL of tantalum solution (1 mL = 0.50 mg Ta) to
22. Procedure 100-mL volumetric flasks and dilute to approximately 80 mL
22.1 To the second fraction containing the niobium (see with the oxalate-citrate-sulfuric acid solution, and mix. Pro-
16.4), add 15 g of H3BO3, 75 mL of HCl, and 95 mL of water. ceed as directed in 28.3.
Heat at 30 C to 35 C until the H3BO3 is dissolved. Cool to 28.2 Reference SolutionTransfer 1 g of KHSO4 to a
5 C and proceed as directed in 20.2 using 65 mL of cupferron 100-mL volumetric flask, add 80 mL of oxalate-citrate-sulfuric
solution. acid solution and proceed as directed in 28.3.
22.2 Transfer the precipitate and paper to a weighed plati- 28.3 Color DevelopmentAdd 12 g of pyrogallol and shake
num crucible, and ignite at a low temperature until the carbon to dissolve (Note 9). Dilute to volume with the oxalate-citrate-
is destroyed. Finally ignite to constant weight at 1200 C and sulfuric acid solution, and mix.
weigh as niobium pentoxide (Nb2O5).
NOTE 9A mechanical shaker is desirable since dissolution time is
NOTE 7Reagent blanks usually amount to less than 0.5 mg and hence about 10 min with continuous shaking.
are considered to be offset by the few tenths of a milligram of earth acid
lost in the precipitation. 28.4 Photometry:
28.4.1 Multiple-Cell PhotometerMeasure the cell correc-
23. Calculation tion using absorption cells with a 1-cm light path and a light
band centered at approximately 420 nm. Using the test cell,
23.1 Calculate the percentage of niobium as follows: take the photometric readings of the calibration solutions.
Niobium, % 5 ~ A 3 0.699/B ! 3 100 (2) 28.4.2 Single-Cell PhotometerTransfer a suitable portion
of the reference solution to an absorption cell with a 1-cm light
where:
path and adjust the photometer to the initial setting, using a
A = grams of Nb2O5, and light band centered at approximately 420 nm. While maintain-
B = grams of sample used. ing this adjustment, take the photometric readings of the
TANTALUM BY THE GRAVIMETRIC TEST METHOD calibration solutions.
(GREATER THAN 1 %) 28.4.3 Calibration CurvePlot the net photometric read-
ings of the calibration solutions against milligrams of tantalum
24. Procedure per 100 mL of solution.
24.1 To the third fraction containing the tantalum (see 16.5), 29. Procedure
add 9 g of H3BO3, 95 mL of HCl, and 85 mL of water. Heat at 29.1 Test SolutionTo the third fraction containing the
30 C to 35 C until the H3BO3 is dissolved. Cool to 5 C and tantalum (see 16.5), add 25 mL of zirconium solution (1
proceed as directed in 20.2 using 65 mL of cupferron solution. mL = 1 mg Zr), 9 g of H3BO3, 95 mL of HCl, and 85 mL of
Proceed as directed in 22.2. Weigh as tantalum pentoxide water. Cool to 5 C and proceed as directed in 20.2. Ignite at a
(Ta2O5). temperature just sufficient to destroy carbonaceous material.
Fuse the oxide with 1 g of KHSO4, cool, and dissolve the melt
25. Calculation in 80 mL of oxalate-citrate-sulfuric acid solution. Transfer the
25.1 Calculate the percentage of tantalum as follows: solution to a 100-mL volumetric flask.
Tantalum, % 5 ~ A 3 0.819/B ! 3 100 (3) 29.2 Reference SolutionProceed as directed in 28.2.
where: 29.3 Color DevelopmentProceed as directed in 28.3.
A = grams of Ta2O5, and NOTE 10If more than 5 mg of tantalum is present, transfer the
B = grams of sample used. dissolve melt to a 100-mL volumetric flask, dilute to volume with
oxalate-citrate-sulfuric acid solution, and take a suitable aliquot.
TANTALUM BY THE PHOTOMETRIC TEST 29.4 PhotometryTake the photometric reading of the test
METHOD solution as directed in 28.4.
(LESS THAN 1 %)
30. Calculation
26. Concentration Range 30.1 Convert the net photometric reading of the test solution
26.1 The recommended concentration range is 1 mg to 5 mg to milligrams of tantalum by means of the calibration curve.
of tantalum for each 100 mL of solution, using a 1-cm cell. Calculate the percentage of tantalum as follows:

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 E367 09
TABLE 1 Statistical Information
Repeatability Reproducibility
Test Specimen Nb Found, %
(R1, Practice E173)A (R2, Practice E173)A
1. Ferroniobium (NIST 340, 57.51 Nb) 57.51 0.16 0.26
2. 65.40 0.29 0.11

Ta Found, %
1. Ferroniobium (NIST 340, 3.73 Ta) 3.71 0.16 0.26
2. 0.47 0.04 0.06

Ti Found, %
1. Ferroniobium (NIST 340, 0.89 Ti) 0.89 0.10 0.07
2. 0.046 0.005 0.010
A
This test method has been evaluated in accordance with Practice E173 (discontinued 1997). The Reproducibility R2 of Practice E173 corresponds to the Reproducibility
Index R of Practice E1601. The Repeatability R1 of Practice E173 corresponds to the Repeatability Index r of Practice E1601.

Tantalum, % 5 A/ ~ B 3 10! (4) by the use of reference materials, if available, that the precision
and accuracy of this test method is adequate for the contem-
where:
plated use.
A = milligrams of tantalum found in 100 mL of final test
solution, and 31.2 BiasThe accuracy of this test method has been
B = grams of sample represented in 100 mL of final test deemed satisfactory based upon the data for the standard
solution. reference material in Table 1. Users are encouraged to use this
or similar reference materials to verify that the test method is
31. Precision and Bias performing accurately in their laboratories.
31.1 PrecisionNine laboratories cooperated in testing this
test method and obtained the data summarized in Table 1. 32. Keywords
Samples with concentrations covering the limits of the scope 32.1 chemical analysis; ferroniobium; niobium; tantalum;
were not available for testing. The user is cautioned to verify, titanium

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