1、Designation: E367 09E367 16Standard Test Methods forChemical Analysis of Ferroniobium1This standard is issued under the fixed designation E367; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number in
2、parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 These test methods cover the chemical analysis of ferroniobium having chemical compositions within the following limits:Element Concentration, %E
3、lement Composition, %Aluminum 2.00 maxCarbon 0.30 maxChromium 2.00 maxCobalt 0.25 maxLead 0.01 maxManganese 3.00 maxNiobium 40.00 to 75.00Phosphorus 0.05 maxSilicon 4.00 maxSulfur 0.03 maxTantalum 7.00 maxTin 0.15 maxTitanium 5.00 maxTungsten 0.50 max1.2 The test methods appear in the following orde
4、r:SectionsSeparation of Niobium, Tantalum, andTitaniumby the Ion-Exchange Test Method10 16Titanium by the Photometric TestMethod 0.05 % to 5.0 %17 21Niobium by the Gravimetric TestMethod 40 % to 75 %22 23Tantalum by the Gravimetric TestMethod 1 % to 7 %24 25Tantalum by the Photometric TestMethod 0.2
5、5 % to 1 %26 30SectionsSeparation of Niobium, Tantalum, and Tita-niumby the Ion-Exchange Test Method15 and 16Titanium by the Spectrophotometric TestMethod 0.05 % to 5.0 %17 21Niobium by the Gravimetric Test Method40 % to 75 %22 23Tantalum by the Gravimetric Test Method1 % to 7 %24 25Tantalum by the
6、Spectrophotometric TestMethod 0.25 % to 1 %26 301.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1 These test methods are under the jurisdiction ofASTM Committee E01 on Analytical Chemistry for Metals, Ores, and Related Mat
7、erials and are the direct responsibilityof Subcommittee E01.01 on Iron, Steel, and Ferroalloys.Current edition approved Oct. 1, 2009May 1, 2016. Published November 2009June 2016. Originally approved in 1970. Last previous edition approved in 20032009 asE367 03.E367 09. DOI: 10.1520/E0367-09.10.1520/
8、E0367-16.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult
9、prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States11.4 This standard does not purport to a
10、ddress all of the safety concerns, if any, associated with its use. It is the responsibilityof whoever uses this standard to consult and establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use. Specific precautionaryhazard statements ar
11、e given in Section 6, and specific warning statementsin 11.1.2. Referenced Documents2.1 ASTM Standards:2A550 Specification for Ferrocolumbium (Ferroniobium)E29 Practice for Using Significant Digits in Test Data to Determine Conformance with SpecificationsE32 Practices for Sampling Ferroalloys and St
12、eel Additives for Determination of Chemical CompositionE50 Practices forApparatus, Reagents, and Safety Considerations for ChemicalAnalysis of Metals, Ores, and Related MaterialsE60 Practice for Analysis of Metals, Ores, and Related Materials by SpectrophotometryE135 Terminology Relating to Analytic
13、al Chemistry for Metals, Ores, and Related MaterialsE173 Practice for Conducting Interlaboratory Studies of Methods for Chemical Analysis of Metals (Withdrawn 1998)3E1601 Practice for Conducting an Interlaboratory Study to Evaluate the Performance of an Analytical Method3. Terminology3.1 For definit
14、ion of terms used in this test method, refer to Terminology E135.4. Significance and Use4.1 These test methods for the chemical analysis of metals and alloys ferroniobium alloy are primarily intended to test suchmaterials for compliance with compositional specifications such as Specification A550. I
15、t is assumed that all who use these testmethods will be trained analysts capable of performing common laboratory procedures skillfully and safely. It is expected thatwork will be performed in a properly equipped laboratory.5. Apparatus, Reagents, and PhotometricSpectrophotometric Practice5.1 Apparat
16、us, standard solutions, and other reagents required for each determination are listed in separate sections precedingthe procedure. PhotometersSpectrophotometers shall conform to the requirements prescribed in Practice E60. (Note 1.)NOTE 1In these methods, cells utilized to contain the reference mate
17、rial and sample solutions in spectrophotometers are referred to as “absorptioncells.” Please note that the radiant energy passed through the cells can be measured as absorbance or transmittance. These methods refer to absorbancemeasurements. Refer to Practice E60 for details.5.2 PhotometricSpectroph
18、otometric practice prescribed in these test methods shall conform to Practice E60.6. Hazards6.1 For precautions to be observed in the use of certain reagents in these test methods, refer to Practices E50.6.2 Specific warning statements are given in 11.1.7. Sampling7.1 For procedures for samplingto s
19、ample the material, and for particle size requirements of the sample for chemical analysis,sample, refer to Practices E32.8. Rounding Off Calculated Values8.1 Calculated values shall be rounded off to the desired number of places as directed in Practice E29.9. Interlaboratory Studies9.1 These test m
20、ethods have been evaluated in accordance with Practice E173, unless otherwise noted in the precision and biassection. Practice E173 has been replaced by Practice E1601. The Reproducibility R2 corresponds to the Reproducibility Index Rof Practice E1601. The Repeatability R1 of Practice E173 correspon
21、ds to the Repeatability Index r of Practice E1601.NIOBIUM, TANTALUM, AND TITANIUM BY THEION-EXCHANGE TEST METHOD10. Scope10.1 These test methods cover the determination of niobium, tantalum, and titanium in ferroniobium from 40 % to 75 %, 0.25 %to 7 %, and 0.05 % to 5.0 %, respectively.2 For referen
22、cedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. ForAnnual Book ofASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.3 The last approved version of this historical standard is referenced on www
23、astm.org.E367 16211. Summary of Test Method11.1 The sample is dissolved in a HCl-HF acid mixture and transferred to an anion-exchange column. Titanium, iron, and otherelements are eluted with anNHa NH4Cl-HCl-HF acid mixture. solution. This eluate is treated with boric acid (H3BO3) andcupferron, and
24、 the precipitate, containing the titanium, is ignited, fused with potassium hydrogen sulfate, and leached in diluteH2SO4. The titanium is oxidized to the yellow pertitanate with hydrogen peroxide. Photometric Spectrophotometric absorbancemeasurement is made at approximately 410 nm. Niobium is remove
25、d by eluting with an ammoniuma NH4 chloride-hydrofluoricacid mixture. Cl-HF solution. Tantalum is removed by eluting with an ammoniuma NH4Cl-NH4 chloride-ammonium fluoride Fsolution adjusted to a pH of 5 to 6. The eluates are treated with the H3BO3 to complex the fluorides, and each of the elements,
26、niobium and tantalum, is precipitated with cupferron, ignited, and weighed as the pentoxide. For tantalum below 1 %, zirconiumis added as a gatherer in the cupferron separation and the tantalum is converted to the pyrogallol complex. PhotometricSpectrophotometric absorbance measurement is made at ap
27、proximately 420 nm. (WarningHF produces very serious burnswhich may or may not be painful on first contact. Such burns often damage bone and other tissue within the body. Standardprocedure is to use gloves and protective clothing when handling this reagent. After the material is added, the closed co
28、ntainer,gloves, and all surfaces that may later be touched are rinsed with large quantities of water. Even one drop of HF on the skin orfingernail must receive immediate first-aid and medical attention should be promptly sought.)12. Interferences12.1 Any bismuth present will appear in the tantalum f
29、raction, but this element is seldom present greater than 0.005 % in thisferroalloy. Trivalent antimony, if present, is eluted with the titanium and precipitated with cupferron, but it does not interfere inthe photometricspectrophotometric test method for titanium.13. Apparatus13.1 Ion-Exchange Colum
30、nsThe columns must be constructed of polystyrene tubing approximately 300-mm long in lengthand 25 mm in inside diameter. A suitable column can be prepared as follows: Insert a waxed, No. 5 rubber stopper containing a5-mm hole into the bottom of the polystyrene tube. Insert into the hole and flush wi
31、th the upper surface of the stopper a 150-mmlength of polystyrene tubing, having a 5-mm outside diameter and a 2-mm bore. Attach another 150-mm length of this tubing tothe smaller tube with an approximately 50-mm length of polyvinyl tubing,4 and control the flow rate by a hosecock on thepolyvinyl tu
32、bing.13.1.1 If a number of determinations are to be made, it is convenient to arrange the columns so that they can be operated witha minimum of attention. Plastic columns equipped with fittings of polystyrene have been developed for such an assembly. Inletand outlet tubes are polyethylene; flexible
33、connections, where necessary, are of polyvinyl tubing. The flow rate is controlled byhosecocks on these flexible connections. The system must be carefully assembled and checked to avoid possible leakage of thesolutions containing HF.13.2 Plastic WarePolyethylene, polypropylene, or TFE-fluorocarbon.1
34、3.2.1 Bottles, 250-mL and 1-L capacity.13.2.2 Graduated Cylinders, 50-mL and 250-mL capacity.13.2.3 Griffn-Form Beakers and Covers, 250-mL, 600-mL, and 1-L capacity.14. Reagents14.1 Ammonium Chloride Solution (240 g/L)issolveg/L)Dissolve 480 g of ammonium chloride (NH4Cl) in 1600 mL ofwater by warmi
35、ng, cool, dilute to 2 L, and mix. Filter, if necessary. Use this stock solution to prepare the solutions described in14.2 14.4.14.2 Ammonium Chloride-Ammonium Fluoride Neutral MixtureSolutionTransfer 600 mLof the NH4Cl solution and 40 mLof HF to a plastic beaker. Adjust the pH from 5 to 6 with NH4OH
36、 (approximately 80 mL to 85 mL will be required), dilute to 1L with water, and mix.NOTE 1This solution must be prepared with care. If the pH is too low, the volume specified will not completely elute the tantalum; if the pH is toohigh, tantalum will precipitate in the column, thus leading to error i
37、n the determinations being run as well as the one which follows.14.2.1 This solution must be prepared with care. If the pH is too low, the volume specified will not completely elute thetantalum; if the pH is too high, tantalum will precipitate in the column, thus leading to error in the determinatio
38、ns being run aswell as the one which follows.14.3 Ammonium Chloride-Hydrochloric-Hydrofluoric Acid MixtureSolutionTransfer 240 mL of the NH4Cl solution, 200mL of HF and 150 mL of HCl to a plastic bottle. Dilute to 1 L with water, and mix.14.4 Ammonium Chloride-Hydrofluoric Acid MixtureSolutionTransf
39、er 600 mL of the NH4Cl solution and 40 mL of HF toa plastic bottle. Dilute to 1 L with water, and mix.4 Tygon-R tubing has been found satisfactory for this purpose.E367 16314.5 Ammonium Nitrate Wash Solution (20 g/L)Dissolve 20 g of ammonium nitrate (NH4NO3) in water, and dilute to 1 L.14.6 Boric Ac
40、id (H3BO3).14.7 Cupferron Solution (60 g/L)Dissolve 6 g of cupferron in 80 mL of cold water, dilute to 100 mL, and filter. This solutionshould be prepared fresh as needed and cooled to 5 C before use.14.8 Cupferron Wash SolutionAdd 25 mL of cupferron solution (14.7) to 975 mL of cold HCl (1 + 9), an
41、d mix. Prepare asneeded.14.9 Hydrochloric-Hydrofluoric Acid MixtureSolutionAdd 250 mL of HCl to 300 mL of water, add 200 mL of HF, diluteto 1 L with water, and mix.14.10 Hydrogen Peroxide (H2O2), 30 %.14.11 Ion-Exchange ResinStrongly basic anion-exchange resin, 200 mesh to 400 mesh, 8 % to 10 % divi
42、nyl-benzene crosslinkage.5 Since the mesh size of the resin may vary 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 removed from the fraction passing the No. 270 sieve as follows: Prepare a suspensionof the resin in HCl (1 +
43、9). Allow the coarser fraction to settle 10 min to 15 min and remove the fines by decantation. Repeat theprocess several times until most of the very fine material has been removed from the suspension.NOTE 2Material retained on the No. 270 sieve may be used for other purposes.14.12 Oxalate-Citrate-S
44、ulfuric Acid SolutionDissolve 35 g of ammonium oxalate (NH4)2C2O4H2O) and 35 g ofdiammonium hydrogen citrate (NH4)2HC8H5O7) in 1 L of H2SO4 (1 + 39).14.13 Pyrogallol (C6H3-1,2,3-(OH)3).14.14 Sodium Hydroxide Solution (100 g/L)Dissolve 20 g of sodium hydroxide (NaOH) NaOH in 150 mL of water, cool,dil
45、ute to 200 mL, and mix. Store in a plastic bottle.14.15 Tantalum, Standard Solution (1 mL = 0.500 mg Ta)Transfer 0.1221 g of tantalum pentoxide (Ta2O5) to a platinumcrucible. Add 2.5 g of potassium hydrogen sulfate (KHSO4) and heat to fuse the oxide. Dissolve the cooled melt in warmoxalate-citrate-s
46、ulfuric acid solution. Transfer to a 200-mL volumetric flask, cool, dilute to volume with oxalate-citrate-sulfuricacid solution and mix.14.16 Titanium, Standard Solution (1 mL = 0.100 mg Ti)Transfer 0.0834 g of titanium dioxide (TiO2) to a platinum crucible.Add 1 g of KHSO4, and heat to fuse the oxi
47、de. Cool, and dissolve the melt in 50 mL of warm H2SO4 (1 + 9). Cool, transfer toa 500-mL volumetric flask, dilute to volume with H2SO4 (1 + 9), and mix.14.17 Zirconium Solution (1 mL = 1 mg Zr)Dissolve 0.5 g of zirconium metal in 10 mL of HF in a plastic bottle, and diluteto 500 mL. An equivalent a
48、mount of zirconyl chloride may be substituted for the zirconium metal.SEPARATION OF NIOBIUM, TANTALUM, AND TITANIUM BY THE ION-EXCHANGE TEST METHOD15. Preparation of Ion-Exchange Column15.1 Place a 6-mm to 10-mm layer of acid-resistant poly(vinyl chloride) plastic fiber in the bottom of the column.A
49、dd the resinsuspension in small portions to obtain a settled bed of the resin 150-mm to 180-mm high. in height. Wash the column withapproximately 100 mL of HNO3 (1 + 9), and then perform three elution cycles with alternate additions of 100 mL of HCl (1 + 9)and 100 mL of HCl (3 + 1) to remove the remainder of the fines. Finally, wash the column with 200 mL of HCl (1 + 3) to a levelabout 20 mm above the resin.NOTE 3Resin columns prepared in this way have been used for several years; the only maintenance may be t
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