(558) Yakovlev, P. Y., Orzhekhovskaya, A. I., Zavodsk. Lab. 33,425 (1967). (559) Yakovlev, P. Y., Razumova, G. P., Zbid., 31, 1307 (1965). (560) Yakovleva, E. F., Dubrovina, I. M., Zharkova, D. N., Ibid., 33, 792 (1967). (561) Yamaguchi, N., Araki, S., Japan Analyst 16,243.(1967). (562) Yamaguchi, N., Hata, A,, Hasegawa, M., Zbid., 16,253 (1967). (563) Yanagida, M., Kato, K., Sugiyama, T., Denki Seiko 37,272 (1966). (564) Yanagiharo, T., Fukuda, Y., Nipp o n Kinsekhi Gakk 27, 156 (1963). (565) Yanagisawa, M., Takeeichi, T., Kogyo Kagaku Zasshi 70, 254 (1967). (566) Yoshimori, T., Arai, M., Iheda, Y., Nippon Kanwku Gakk 31, 1258 (1967). (567) Young Hwang, J., Taghamonty, J. J., Parsons, F. B., Daehan Hioahak Hwocjee IO, 133 (1966).
(568) Yurchinko, E. I., Sawin, S. B.,
Zubashiva, L. V., Garam, V. F., Mishinskaya, I. S., Zauodsk. Lab. 32, 12 (1966). (569) Zaitseva, E. I., Rodionova, G. P., Romanov, A. A., Serbin, A. P., Shipuh a , T. P., Ibid., 82,1055 (1966). (570) Zakarina, N. A., Lazeeva, G. S., Petrov, A. A., Vest. L a i n g r . Gos. Univ., Ser. Fiz. Khim, 4,38 (1966). (571) Zeller, C., Reithler, J. C., Bolfa, J., Labour, F., Compt. R a d . Ser. C 263, 1050 (1966). (572) Zhalybina, V. D., Kovalinko, 0. A., Borodulina, L. M., Zavodsk. Lab. 32, 807 (1966). (573) Zhalybina, V. D., Sin’ko,, R. D., Prikhod’ko, R. I., Zbid., 32, 808 (1966). (574) Zhdanov, A. K., Yatrudakis, S.M., Zbid., 32,1336 (1966). (575) Zhukov, A. A., Kokora, A. N.,
Nikeforova, E. F., Zhukova, V. L., Komyakov, L. I., Termodin. Fiz. Kinst. Strukturoobrazov. stuli. Chugune, 1967, 291. (576) Zil’bermints,
S. M., Shavnin, A. M., Uch. Zap. Perm. GOS. Univ. 159,
222 (1966). (577) Ziolowski, Z., Jasna, B., Prace Insty Hutniczych 19,329 (1967). (578) Zlotowska, Z., Przegl. Elektrm. 7, 445 (1966). (579) Zolotariva, N. M., Bessonova, T. A., Zavodsk. Lab. 33,175 (1967). (580) Zueva, V. L., Polishehuk, V. A.,
Klecner, L. M., Teor. Prakt. Met., Chelyabimk 8,242 (1966).
WORKsupported by Jones & Laughlin Steel Cow.
Nonferrous Metallurgy I. Light Metals: Aluminum, Beryllium, Titanium, and Magnesium Richard T. Oliver and Ernest P. Cox, Alcoa Research Laboratories, Aluminum Co. o f America, New Kensington, Pa.
T
on nonferrous metallurgical analysis and covers the two-year period from September 1966 through August 1968 as documented b y Chemical Abstracts and Analytical Abstracts. Also, the following journals were surveyed directly for the same period: ANA LYTICAL CHEMISTRY,Analytica Chemica Acta, T h e Analyst, and Talanta. As in the past (178), this review is limited to those analytical methods applied directly to products of the nonferrous metal industry. Many interesting methods potentially applicable to this field are not included because of space considerations. However, some general methods are included, possibly arbitrarily, because they appear particularly useful or novel. Accompanying tables list methods referred to in the discussion along with other methods too numerous to mention individually. Table I shows the light metal materials for which compilations of procedures are available for determining miscellaneous alloying elements and impurities. I n Table 11, arrangement is according to the elements determined. Table I11 lists the elements determined b y atomic absorption in aluminum, aluminum alloys, and hardener alloys, along with conditions and comments relative to their determination. Tables IV and V are similar listings pertaining to the spectrographic and X-ray fluorescence determinations of elements in aluminum alloys. The latter three tables were prepared by Bell, Gaitanis, and Freilino, respectively, of the Analytical Chemistry Division of the Alcoa HIS IS THE TWELFTH REVIEW
Research Laboratories. They represent conditions routinely employed in the respective areas. Many of the instrumental methods included in Table I1 and all of those in Table I are excluded from the general discussion in the text. It was thought that persons interested in these instrumental approaches would benefit. more b y consulting the original articles or abstracts. Aluminum. Poetzl (193) used a differential technique for accurate photometric analysis of high concentrations of aluminum. He stated t h a t precipitation or complexometric reactions can be used t o remove a n accurately defined portion of ions to be determined so t h a t low residual concentration can be determined with high relative accuracy. Aluminum can be determined after partial masking with E D T A and complex formation with ferron. Concentration of the latter is determined photometrically. Results compare well with those of other methods. Tikhonov and Grankina (238) separated microgram quantities of aluminum from titanium b y extracting oxidized titanium cupferrate with chloroform. Aluminum was then determined photometrically (590 mp) with methylthymol blue at a p H of 3 to 3.5. Molot et al. (163) used N-benzolyphenylhydroxylamine (BPH) to separate titanium from aluminum. Chloroform was the extracting solvent. Aluminum was then determined photometrically with pyrocatechin violet (pH 6.0 to 6.3, 580 mp, 10-cm. cell).
Qureshi et al. (199) used paper chromatography to separate aluminum, titanium, and iron quantitatively from each other. Solvent systems reported were 3 : 5 : 2 and 3:4:3 HC02H-HC1Me2C0, respectively. Aluminum was determined photometrically with thiochrome Cyanine-R, titanium with sulfosalicylic acid a t 410 mp and iron with 1, 10-phenanthroline. Results of separations and determinations on synthetic solutions were presented. A complexometric determination of aluminum in titanium alloys b y titration without a buret was reported b y Bondareva et al. (SO). An acid cupferron extraction was used to separate titanium from aluminum. The latter was then titrated a t p H 3 using a “hydrostatic capillary titration” tube. Copper-EDTA and 1-(2-pyridylazo)-% naphthol were used for the indicator and the titration was performed hot. Culp (61) in determining aluminum in an aluminum-titanium binary alloy used lactic acid to mask the titanium while backtitrating an excess of E D T A with bismuth. The indicator was xylenol orange a t pH 5.0 to 5.5 Determination of metallic aluminum in the presence of alumina by an indirect complexometric method was reported by Solodovnikov (226). Metallic aluminum was dissolved in a heated MCuSOd solution. Excess copper was determined by titrating with E D T A using murexide. Alternately, metallic aluminum could be dissolved in ferric chloride and the resulting ferrous ion determined by a redox titration. VOL. 41, NO. 5, APRIL 1969
101R
Table
1.
Methods for Nonferrous Metallurgical Materials
Constituents determined Sc,Co,Hf,Fe Sn,Cd,Zn Ag,Cr,Ce,Cs R b Cu,Ga,Mn da,Co,Cr,~e,Hf,Sb,Sc,dn Zr.Nb.Hf.d'a Variois impurities, review Ti,V Mn,Fe,Ni,Cu,Zn,Ga,Sn,Pb,Bi Fe,di,V,Cr,Ti,Mn,Pb,Mg,Zn,Ga
Material
Al
High purity
Al
Al alloys
A1 salts A403 sinter cake, sinter mixture, etc. abrasives A1F3-NaF Sintered A1 powder
Methods useda References NA NA NA NA MS MS NA NA NA
Mn,Ni,Co,Cu,Fe Cu,Mn,Ga Au,Sb As H ,Mn,W,Co,Cr,Ga,Cu,,In,Cd,kn,hn,bo,Ni,Fe Cu,Zn,Pb,Cd,Ga Pb,Cu,Zn Fe,Mn,Ti,Cu,Mg,Si Cr,Cu,Fe,Ag,Pb,Mn,Co,Ni Zn,Cd,Pb,Cu,Ga Cu,Mg,Zn,Fe Mg,Zn,Fe,Cu,Mn,Pb,Cr,Ni Cu,Mg,Fe,Zn,Cr,Pb,Ni,Mn Ag,Cu,Mg,Zn,Cr,Zr Ni,Mn,Zn,Cu,Fe,Ti Cr,Cu,Fe,Ga,Hf,Mn,Sc,Zn Si,Mg,Cu Si,Mn,Fe,Ti Cu,Mg Mn,Si,Al Al,Cu,hn,Ni La,Fe,Ni,Cu,Mg,Mn,Cr,Zr,Si Ca,Mg,Fe,Ni
P P S S V AA AA AA AA MS NA S S S RO X AA
Na,K,Ca
F
Ca,Fe,Mg,Ti,Zr Composition and vapor pressure
S MS
Cu,Cd,Pb,Zn Mn Cr Mg,Si,Fe,V,Cu,Ti B,Bi,Cd Ga,-
P
de,di,Sn,Tl,Zn,Ca,Eu,kd,Dy,Pb,Gd
S AA B.~.F.c.o NA Ail (mpurities in ppm range MS P Cu,Pb,Cd,Zn,Ni,Co,Fe,Mn Ag,Al,B,Bi,Ca,Ca,Cr,Cu,Fe,Mg,Mn,- S Mo,Ni,Pb,Si,Sn,Ti,V X Al,Si,Fe,U,Th AA Ca,Cu,Mn,Zn NA Review for impurities S Al,Fe,V,Cu,Sn,Cr P Sb,Cu,Pb X Zn,Ni Fe S Cr,V,~r,Nb,Mn,Mg,Al,Si,Ca,Ti Al Si,Ti
Bauxite Be
Mg alloys Ti alloys
Ti slags a AA, atomic absorption; F, flame hotometry; MS, mass spectrogra hic; NA, neutron activation; P, polarographic; R 8 , ring oven; S, spectrographic; voltammetric; X, X-ray.
3
Table II. Methods for Elements in Nonferrous Metallurgical Materials
Constituent determined Al
Mg
Reagent or method Photometric (high concn) Titrametric (NaF) Eudiometric Titrametric X-ray diffraction Chelometric Atomic absorption Homogeneous ppt Photometric, eriochrome cyanine
(176) (225) (844) (194) (8011 (110) (97)
Ti
Photometric, thiochrome cyanine
(199)
Ti Al-Ti alloy Ti alloys
Photometric, pyrocatechin violet Chelometric Chelometric, hydrostatic capillary titration Photometric, methyl thymol blue Chelometric X-ray fluorescence Electrolytic Neutron activation, on-stream Titrametric, ZnSO,
(163) (61) (SO)
Material Alloys Al salt A1 powder A1203 Alto3 Alloys Be Be
Ti Ti alloys Anodic layers Hall bath Bauxite Bauxite
Al2On
R
R
References (193) (8841
(238) (88) (138) (66) (80%')
(24 1
(Continued) 102 R
0
ANALYTICAL CHEMISTRY
Presence of other reactive metals will cause high results. Alumina. T h e presence of anodic layers of alumina on aluminum was studied b y Lihl et al. (138). A theoretical treatment was presented to show how X-ray fluorescence analyses of aluminum coated with hydrated alumina can be used to find exact composition of the oxide layer and its density. Results showed that the oxide lager converges toward a final composition of A1203 H20 with a corresponding density of 3.1 g per cc. Dewey (66) determined the alumina content of Hall electrolyte b y a potentiometric procedure. The back-EMF (decomposition potential) varied inversely with dissolved alumina content of the electrolyte. A series of potential values were established for ranges of alumina concentrations. The values of dissolved alumina were substantially independent of the anode to cathode spacing of the cell, electrolytic temperature, and resistance in the anode assembly, cathode assembly, and between the molten aluminum layer and the cathode. The results were reported t o agree within 1% of laboratory data. Application of neutron activation to on-stream analysis of aluminum in bauxite and fluorine in fluoride minerals was reported by Rhodes (202). This paper is a review of nuclear techniques for process analysis. Zuda and Jitea (266) studied determination of alumina originating in aluminum powder after the powder was formed. Methods suitable for determination of the original oxide content, formed during manufacture, were unsuitable. Their method calls for dissolution of aluminum powder in sodium hydroxide followed by determination of liberated hydrogen. Total alumina content is found by difference] and the alumina in question is obtained b y subtracting a blank alumina determination on a freshly prepared powder. Dorsey (69) studied hydrous and anhydrous aluminas by using far infrared absorption. The absorption spectra (800 to 835 cm-l) of 15 pure hydrous and anhydrous alumina phases were presented for identification of various forms of alumina. Say and Rase (211) used DTA-TGA to study unreacted alumina trihydrate in silicaalumina catalysts. Their results showed that it was possible to detect and determine aluminum that does not react with hydroxy groups during preparation of catalysts. Beryllium. Dragulescu and Menessy (70) published a review of the analytical chemistry of beryllium. Methods for identifying and determining beryllium and separating i t from foreign ions were reviewed. A comparison of instrumental and radiometric techniques was also included (133 references).
Budanova and Pinaeva (44) determined beryllium in aluminum alloys with beryllon IV (530 mp). Aluminum was masked with EDTA. If beryllon I11 was employed, no masking agent for aluminum appeared effective. Satisfactory results were obtained for alloys containing 0.01 to 0.9% beryllium. Iron, manganese, copper, and nickel did not interfere. E D T A was also used to mask aluminum in the gravimetric determination of beryllium with diketone I (161). A saturated solution of reagent was added to a solution of p H 7 to 8. Titanium did not interfere. For determination of microgram amounts of beryllium in a magnesium-aluminum alloy, Sudo and Ogawa (231) performed separation using a cation exchange resin. E D T A was again used to aid in the separation. If beryllium was greater than O.OOlyo, aluminum was masked with E D T A and beryllium extracted with acetyl-acetone a t a p H of 6. Eristavi et al. (77) also used an ion exchangeapproach to separate beryllium from aluminum in a magnesiumaluminum alloy. They used an anion exchange resin in fluoride form. Beryllium was eluted with 4% N a F (5 ml per min) and determined photometrically. Beryllium and aluminum were separated from magnesium by precipitation with ammonium hydroxide. Stokely (228) determined beryllium in the presence of aluminum b y a solvent extraction separation using trifluoro-2, 4-pentanedione and measured beryllium b y gas chromatography. A detailed investigation of parameters was given. Gagliardi and Likussar (85) used thin layer chromatography to separate beryllium, magnesium, and barium from mixtures. Beryllium was extracted from the plate with ethanol-HC1-HzO (73:12:15:) and determined as the 8-hydroxyquinaldine complex. hiagnesium was extracted with methanol-ethanolHCl-H20 (36:36:13: 15) and determined with Eriochrome Black T. Barium was extracted with methanolHC1-H20 (63: 12:25) and determined with metalphthalein. Bismuth. D’Amore and Corigliano (62) determined bismuth in the presence of aluminum b y a photometric technique using thiocyanate (470 mp) in a thiocyanide medium. Separation of bismuth from aluminum was not necessary nor was separation of bismuth from lead or copper necessary provided that content of bismuth did not exceed O . O l ~ o or O.lyo,respectively. K h e n bismuth content was below these concentrations, a cation exchange separation was used. Boron. Boron in high siliconaluminum alloys was determined photometrically b y Budanova and Gurevich ( 4 3 ) . They used acetylquinalizarin and measured absorbance at 6% mp using a blank prepared from
Table II.
Methods for Elements in Nonferrous Metallurgical Materials (Continued)
Constituent determined
B
Be
Bi
Material Bauxite Aluminate solutions A1 powder A1203-Si02 catalyst A1 A1 alloys A1 alloys Hydrous AlzO3 A1 A1-Si alloys Al-Mn-B alloy General General A1 A1 A1 3Ig-A1 alloy AI-RIg-Be alloys Al-hIg hIg, A1 hlg-A1 alloys All Ti Be-Rlg-Ba A1 A1 alloy Al, Be
C
Be
Ca
Al-Mg-Ti Be
Cd
Mg hlg Ti, Al, Be A1 A1 A1 All Mg Al, blg Be salts General
co Cr
cs cu
A1 A1 A1 products A1 A1 AI, Rfg A1 A1 A1 A1-Ti alloys Al, Ti
AI-Cu alloy A1 A1 A1
Al-Cr-Ni alloys Mg
F Ga
AlFa Al, A1203 A1 A1
Ge Ai3 AU c1
A1 All general A1
Ti A1 A1 Ti alloy Ti
Reagent or method Neutron activation Titrametric
References
Gasometric DTA-TGA Review Photometric Gravimetric Infrared Mass spectrometry Photometric, acetylquinalizarin Titrametric Microdiffusion, titrametric Review Gas chromatography Photometric Photometric, beryllon IV Photometric, chlorphosphonazo R Photometric, arsenazo I Photometric, beryllon I1 Photometric after ionx sepn. Photometric after ionx sepn. Gravimetric, diketone I Photometric, 8-hydroxyquinaldine Photometric Photometric, thiocyanate JV-Benzoyl-S-phenylhydroxyalamine GC, conductometric Ionx sepn. Photometric after solvent extraction Photometric, azo-azoxy BN Chelometric Gravimetric Ionx sepn., polarographic Chelometric, EGTA Radiotracer, dithizon sepn. Gravimetric] diphenylthiophosphoric acid Photometric, bromobenzthiazo Voltammetry, hanging Hg drop Gravimetric, quinoylphosphoric acid Chelometric Photometric, tribenzylamine Photometric Mass spectrometry Atomic absorption Potentiometric Chelometric Photometric Atomic absorption Photometric Photometric, bis-cyclohexanone oxalyldihydrazone Chelometric Photometric, RIDCAI. X-rav fluorescence PolaGographic Atomic absorption Photometric, 2,2’-bicinchoninic
agents Activation analysis, extractionphotometric Photometric, rhodamine B Photometric, xglenol orange Photometric, phenylazo-benzoylthiazole cmpd. Activation analysis Voltammetry, paraffin-C electrode Voltammetry, paraffin-C electrode Photometric, SnC12 Voltammetry, hanging Hg electrode (Continued)
VOL. 41, NO. 5, APRIL 1969
103R
Table 11.
Methods for Elements in Nonferrous Metallurgical Materials (Continued)
Constituent determined
Material
Nt
Be
os
Tic14 A1 A1
Reagent or method AgNOs titration, external indicator paper GC Thermal conductivity Apparatus Manometric Hot extraction, manometric Vacuum diffusion, manometric Vacuum sublimation, GC D2 exchange; uv or ir Vacuum extraction Spectrographic Discussion of chemistry Hollow cathode discharge Gravimetric, 1,6-diaminohexane Activation analysis, extractionphotometric Polarographic Chelometric titration Atomic absorption X-ray fluorescence Atomic absorption Photometric, 1,lO-phenanthroline Photometric, thio 1 colic acid Photometric NH,&!!N Photometric, thiocyanate Chelometric, ionx sepn. Polarographic X-ray fluorescence Spectrographic Redox Solvent extraction, photometric Oscillopolarographic titration Voltammetry, handing Hg electrode Ionx sepn., titration of LiOH Chelometric or photometric, titan yellow Photometric, a phenylazo cmpd. Chelometric, mixed indicator Activation analysis Atomic absorption Polarographic Fluorometric, oxine Photometric, congo red Photometric, Eriochrome Black T Mg oxine, iodometric Gravimetric Electrographic X-ray diffraction Atomic absorption Photometric, 8-hydroxyquinaldine Atomic absorption Photometric, O-nitrophenylfluorone i3rtrographic otometric, 4-(2-pyridylazo)resorcinol Photometric, indophenol Photometric, Nessler’s reagent Isotope dilution Coulometric titration Manometric Review (2,38,66,67, Activation analysis
Al, Ti Be, Mg, A1 Be Be Be Mg, Ti Ti Ti Ti Ti Tic14 Alios
Activation analysis Radioactive microtitration Activation analysis Activation analysis Activation analysis Activation analysis Reduction melting Activation analysis Activation analysis Fusion, coulometric Manometric Spectrographic
Ti He H
Hz0 HI
DI
In
Fe
Pb Li Mg
Mg Mn Ni Nb
Be0 A1 alloys A1 Al alloy melts Al Al, A1 alloys Magnox A180 Be0 Be Ti Ti, Mg, A1 Ti Al Al A1 Mg alloys Mg Al Al A1 Ti Al Nonferrous alloys A1 A1 A1 Ti Ti concentrates A1 alloy Al alloys Be salts A1-Li alloys Al A1 A1 A1 A1 Duraluminum Al. Ti ~ g - alloy ~ i Be-Mg-Ba Raw materials Raw materials Mg alloys Mg powder A1 Be- Al-Mg Al-Cr-Ni alloys Ti, TiCh
Nb, Ta
Pd
104 R
3 Ti
ANALYTICAL CHEMISTRY
84,87,210) (107)
“silumin” free of boron. Sample was dissolved in a 1:5:4mixture of sulfuric, phosphoric, and nitric acids. Xakashima et al. (171) described a simple and rapid method for determination of 1 to 10% boron in aluminum-manganeseboron alloys. Aluminum and manganese were completely precipitated using oxine without adsorption of boron. Excess oxine was removed b y addition of magnesium chloride. After interfering substances were further removed mannitol was added, boron was titrated with standard sodium hydroxide. A microdiffusion technique for separation of boron as trimethylborate was presented b y Umland and Janssen (246). After separation, boron was determined photometrically using carminic acid. Cadmium. Dialkyl and diaryldithiophosphoric acids were used for detection and determination of cadmium in the presence of aluminum and magnesium. Busev and Shishkov (50) reported t h a t diphenyldithiophosphate can be used t o precipitate cadmium quantitatively. T h e precipitate was dried at 80 to 90 “ C to a constant weight. Alternately, reaction of the complex in chloroform with copper sulfate (giving a yellow color) can be used for photometric determination of cadmium. Pribil and Vesely (196) suggested that cadmium can be determined in the presence of aluminum, zinc, lead, and iron using an EGTA titration. Aluminum and iron were masked b y triethanolamine, while lead and zinc were masked with sodium hydroxide. Separation of cadmium and zinc from aluminum by a strongly basic anion exchange resin in the chloride form, prior to their polarographic or complexometric determination, was reported b y Simek (221). Aluminum passed through the column while cadmium and zinc were retained. Zinc was eluted with 0.001.V HC1 and cadmium with 0.01 N acetic acid. The method is suitable for determination of 0.004% zinc and 0.0002~o cadmium in the presence of a lo4- to lO5-fold excess of copper, nickel, or aluminum. The hanging mercury drop electrode was used to concentrate microgram quantities of cadmium and lead in beryllium compounds. lower limits of determination for cadmium and lead are in the 1 O - * M range. Calcium. Gorbenko and S a d e z h d a (90) compared volumetric and photometric methods for determination of calcium and pointed out t h a t beryllium, even a t low concentrations, interfered in all of them. They recommended t h a t calcium could be separated from beryllium by a solvent extraction using azo-azoxy B N . Adter extraction, calcium was backextracted with 0.l.V HCl and either titrated complexometrically using murexide as
indicator or determined photometrically with glyoxalbis-(2-hydroxyanil), depending on whether calcium content in the sample was higher or lower than 50 pg respectively. The same authors (91) recommended the extraction procedure for determination of calcium in magesium at the 0.001% level. An ion exchange separation of calcium from magnesium, aluminum, and other elements was reported by Strelow and Van Zyl (229). Magnesium was separated from calcium b y eluting with 3V HCl containing 60% ethyl alcohol from a column of AG-5OW-X 8 cation exchange resin. Calcium was eluted with 3.1.1 HC1 or 2 N H S O s . Separations were sharp and quantitative. Up to 10 mmol of magnesium can be separated from 0.01 mmol of calcium or vice versa on a 60-ml column. Aluminum and titanium (in the presence of peroxide) accompany the magnesium. Carbon. Determination of free, combined, a n d absorbed carbon in beryllium was reported by Postma a n d Walden (195). Combined carbon was determined b y converting beryllium carbide t o methane and sweeping t h e gas into a gas chromatograph. Free carbon was filtered f r o m dissolved beryllium sample and ignited to carbon dioxide, a n d t h e gas was swept into a conductometric cell containing barium hydroxide. Absorbed carbon (as COz on the surface of the metal) was separated from beryllium b y heating the sample in an inert atmosphere and sweeping the gas into the conductometric cell. Cesium. Determination of cesium in t h e presence of aluminum a n d magnesium was accomplished b y Serebrennikova et al. ($13) using a potentiometric approach. T h e method was leased on precipitation of cesium as CssTeIa, dissolving the precipitate with sodium hydroxide and titrating the free iodide formed with a silver nitrate solution. The method could be used for analysis of cesium containing materials in the absence of rubidium. Chromium. Several enrichment techniques for determination of chromium in bauxite a n d red muds a n d aluminum were rcported by Klug a n d Metlenko ( 1 2 2 ) . Bauxite and muds were fused with sodium hydroxide and sodium peroxide. Aluminum was dissolved in a nitric-sulfuric acid mixture. Chromium in t h e latter was oxidized with peroxide. Prior t o photometric determination of chromate with o - dianisidine, S,S- dimethyl - p - phe nylenediamine, or 3, 3'-dimethylnaplithidine, impurities were separated b y extraction with cupferrate into chloroform, ferric iron being used as a carrier; b y extraction of 8-hydrosyquinolinates at p H 3.5 to 4.2 into chloroform, with ferric iron as a carrier; or by passing the solution through an anion exchange resin
Table II. Methods for Elements in Nonferrous Metallurgical Materials (Continued)
Constituent determined Material P Nonferrous alloys A1 Pu Al K A1 Rare earths A1 Al-Y Y La Al
?
E& La Y
La sc Re Rh Ru Sb Si
Na S Te Th Sn
Ti
Ti
U
v Zn
Zr, Hf Zr
Reagent or method References Indirect atomic absorption (119) Photometric, Molybdophaaphoric (181,814,SW) acid X-ray fluorescence (86) Photometric, dinitrohydroxyazo (46)
Chelometric Chelometric Oxine extraction-photometric, methyl thymol blue Al Gravimetric A1 Chelometric Photometric, xylenol orange -41, Mg Al-La Separation technique Chelometric Al, Mg Al, M g Photometric, thiourea X-ray fluorescence Be-Rh alloys Spectrographic AlzOa Atomic absorption A1 A1-Mg Activation analysis A1 Photometric Photometric, nonreduced molybdoAll Be silicate A1-Si Resistivity Differential Dhotometric Ti products Ti Spectrographic Nonferrous alloys Indirect atomic absorption A1 Activation analysis A1 Flame photometry Activation analysis Mg Tic14 Redox, photometric Al-base alloys X-ray fluorescence Activation analysis A1 Photometric A1 Amperometric titration, A1 methylene blue Photometric, phenylfluorone All Ti Titrametric, K8Fe(CN)s General Photometric, dimercaptcGeneral thiopyrone Photometric, diacetoxynaphA1 alloys thalene Photometric, chromotropic acid AI-Cr catalyst Chelometric A1-Ti alloy Activation analysis A1 Polarographic A1 Chelometric A1 A1 Polarographic A1 Photometric, thiochrome cyanine R Chelometric, ionx sepn. A1 Gravimetric, cupferron General Photometric, salicylohydroxamic Buaxite acid A1 Amperometric titration, methylene blue Photometric, arsenazo I11 A1 Al-U Coulometric Al, A1 alloys Photometric, BPHA Al Photometric, pyrogaIlol deriv. A1 Spectrographic Redox titration TiCl, Photometric A1 A1 Polarographic A1 Ionx sepn., polarographic A1 Atomic Absorption hlg alloys Titration, K4Fe(CN)6 Al, hlg Spectrographic Ionx sepn., chelometric AI A1 Photometric, 3-cyano-1,5-bis-(2hydroxy-5-sulphophenyl) formazan A1 alloys Photometric, arsenazo I11 A1 Atomic absorption Al, Mg Photometric, stilbazogall I1 hlg, A1 alloys Photometric, zirconin Ti Photometric, arsenazo I11 and 12 others
(88) (40)
(941' (119)
(138) (136) (209) (49) (7s) ($411 (181)
(249) (164,221) (i2,23,mIr8) (133) (2611 (48) (130)
(867) (198) (169) (64.170l
VOL. 41, NO. 5, APRIL 1969
105R
Table 111.
Elements Determined b y AA in Aluminum, Aluminum Alloys, and Hardener Alloys
Achievable Analytical ranges Hardener Conventional alloys, alloys, nominal upper ranges," % limits, % Fe cu 31n hlg Cr Ni
Zn Ti
0.001-10.0 0.001-10.0 0.001- 5.00
0.000-20.0 0.001-1.00 0.001-5.00 0.000-10.0 0.02-0.5
50.0 25.0 10.0
3.0
Conditions Line A
Slit, min
Oxidizer
2483.3 3247.5 2794.8 2852.1 3578.8 2320.0 2138.6 3642.7 2117.0 6707.8 2246.1 2348.6 5890.0 4226.7 2230 6 2288 0
0.3
Air Air Air Air Air Air Air
1.o 1.o
3.0 0.3 0.3
3.0 0.3 1.0
N20
Flame Fuel
Condition
Interfering elements
CzHz CzHz C2Hz C2Hz CzH2 C2Ht CzHz CJL C2Hz CzH2 Hz CiHi C;Hi C;H; C2Hz CzHz
Oxidizing Oxidizing Oxidizing Reducing Reducing Oxidizing Oxidizing Reducing Oxidizing Oxidizing Reducing Reducine Oxidizini Reducini Oxidizing Oxidizing
None None None Alb None None None None None None None None None Aib None None
Pb 0.000-1.0 Air 0.000-2.0 3.0 Air Li 0.000-20.0 1.0 Air Sn 3.0 NqO 0.000-0.5. Be 0.000-0. O h d 0.3 Air Na 0.000-0.0sd Ca 1.0 Air 0 001-1 .oo Bi 0.3 Air 0.000-1.00 Cd 1 .o Air a Range limits expressed as 70concn. Upper "nominal ranges" can be extended to 20% or greater if care in technique is exercised. b Addition of lanthanum removes aluminum interference in air acetylene flame. Analyses performed in NZO-GHt flame do not have ail aluminum interference; however, at low concentrations of magnesium or calcium, its noise is objectionable. c This upper nominal range applies to special alloys rarely encountered. d Sodium and calcium are present as impurities.
in the chloride form. Chromate was eluted with 0.005X HCl. Sensitivity for each method was 0.01 pg of chromiumper ml. Accuracy is within =+=77&. Fasolo et al. (79) used tribenzylamine to extract between 1 and 300 ppm of chromate in NHCl into chloroform. hbsorbance of the extract was measured a t 355 mp (up to 30 ppm) or 458 mp (up to 300 ppm). Separation was also used for determination of chromium in aluminum alloys b y neutron activation. Cobalt. Johnson and PIPellor (113) used a n E D T A titration t o determine 30 to 100 pg of cobalt in aluminum foil, Cobalt was separated from aluminum b y an anion exchange resin (Cl-form). Aluminum was eluted with HCl and cobalt with water. PAX was used as the indicator and a 1:1 acetone solution was employed. The end point was determined photometrically. Copper, Corbett (60) used formation of a deep yellow color (432 mp) between copper and 5-hydroxy-3methyl-5-(D-arabinotetrahydrosybutyl) thiazolidine-2-thione as the basis of a method for determination of copper in aluminum. Copper in nonferrous metals and alloys at concentrations between 0.003 to 10% was determined b y Rohde (203) using biscyclohexanone oxalyldihydrazone. A blue complex (595 nip) was formed a t p H 9 in the presence of ammonium citrate, a sodium borate buffer, and a slight excess of sodium hydroxide. Beyer and Likussar (27) used morpholinium morpholineN-dithiocarbamate (438 mp) to determine O . O l ~ ocopper in pure aluminum. Fluoride. Fluoride was determined in aluminum fluoride by use of wide line nuclear magnetic resonance (80). 106 R
ANALYTICAL CHEMISTRY
T h e sample was fused with sodium carbonate, dissolved in water, acidified to remove excess carbon dioxide, and concentrated to 100 ml. T h e limit of detectability was 2 mg per ml. Gallium. Photometric determination of gallium with organic reagents such as diphenylcarbazone, hematoxylin, Eriochrome Black T, alizarin S, morin, quercetin, and quinalizarin was studied by Bashirov et al. (19). From this work a method for photometric determination of gallium with diphenylcarbazone in metallic aluminum, alumina, alunite, and slag from an aluminum factory was developed. A prior extraction of gallium with acetone from 6LV HC1 was necessary. Gold and Silver. Lovasi and Tomcsanyi (144) employed anodic stripping voltammetry for determination of gold and silver in high purity aluminum. T h e relative error did not exceed 5% and the lower limit of sensitivity vias 0.5 ppm. Chloride. Polarographic determination of microgram amounts of chloride in titanium was reported by Flidlider and Kharchenko (81). Sample was dissolved in a nitric-sulfuric acid mixture and the vapors were absorbed After in 0.1:V sodium hydroxide. absorbate was treated to expel oxides of nitrogen and p H was adjusted between 2 and 3, a film of HgCl was deposited polarographically a t f 0 . 0 5 V vs. a S-Hg2S04-mercury electrode. The film was then dissolved cathodically. The range of usefulness of the method was 5 X loT6to 5 X lO-'N chloride. Helium. Gas chromatography was used b y Hibbits (103) to determine helium in neutron-eradiated beryl-
lium oxide. Sample was heated under reflux with a sulfuric-phosphoric acid mixture in a n atmosphere of argon. Liberated helium was transferred t o a gas-sampling bulb. Activated charcoal was used to separate helium from other volatile species except about 10% of any hydrogen present. Recovery of helium b y this method ranged from 94 to 103%. Hydrogen. Predominant methods for determination of hydrogen were vacuum extraction and manometric (Table 11). However, one article is worthy of elaboration. Hardie and Turner (99) presented a discussion of physical chemistry of the interaction of hydrogen. Observations and experimental results were reported on mechanical effects associated with hydrogen in dissolved and combined form in titanium and magnesium and their alloys. Problems in processing nonferrous metals due to hydrogen effects associated with porosity and individual contributions related to copper, aluminum, and their alloys were reviewed. Smythe and Whateley (223) evaluated three methods for determination of water in beryllium oxide. I n the first of these, a mixture of the sample with dry KCN (as internal standard) was ground under specified conditions in an atmosphere of dry nitrogen, and further ground after a few drops of hesachlorobutadine were added, extinction of the resulting mull was measured between rock salt plates a t 3300 em-* and a t 2050 cm-1. X calibration graph was prepared from mixtures of beryllium oxide and beryllium hydroxide. The second method was based on the exchange of DzO; the third method-to a
mixture of 0.01 N-methanesulfonic acid, 2,2-dimethoxypropane1 and carbon tetrachloride in a stoppered flask was added 1 g of sample. After a 24-hour period, ir spectrum of the supernatant liquid was recorded from 1600 cm-l to 1900 cm-'. A 0.1-mm calcium fluoride cell was used. The DzO exchange method was considered the most accurate and sensitive. Indium. A separation of indium from aluminum based on precipitation of I n ( O H ) , by l16-diaminohexane was reported by Korenman and Chelysheva (125). Hydroxides of aluminum, zinc, a n d cadmium were not precipitated. Indium was determined chelometrically, a s were aluminum and total zinc plus cadmium. Iron. Babatchev (16) separated iron and titanium from aluminum using a n ion exchange resin and then determined individual elements chelometrically. Iron I11 and titanium I V were determined simultaneously by titration with E D T A a t 55 "C and p H 1.5 t o 2 in the presence of peroxide. Sulfosalicylic acid was used as indicator. Iron was titrated separately in an aliquot without peroxide. Solution containing titanium peroxide complex was passed through a cation exchange column whereby aluminum alone was retained after elution of iron and titanium with water. Aluminum was then eluted with 3N HCl and determined chelometrically by backtitaration of an excess E D T A with zinc acetate a t p H 4.8 (xylenol orange indicator). Dichromate and vanadate were used to determine total iron in a titanium concentrate without preliminary separation of titanium. Interference by titanium \vas eliminated by oxidation to titanium IV or conversion to a fluoride complex. Lead. A method employing a n ac oscillopolarographic titration was successfully applied to determination of lead in white metal and aluminum alloys (116). Potassium chromate (0.1.U) was used as the titrant in 0.1M ammonium acetate. T h e end point was indicated by disappearance of the cathodic wave for lead. Lithium. Hourquin et al. (108) reported on determination of lithium in aluminum-lithium binary alloys. Sample was dissolved in sulfuric acid and solution allowed to pass through a column packed with IRA-400 resin which had been pretreated with E D T A . Aluminum and associated sulfate were removed. Next, solution was passed through a second column packed with the same resin in hydroxide form to remove sulfate associated with lithium ions. The effluent contained lithium hydroxide and was titrated with standard acid. Magnesium. Si1 and hlitra (219) determined magnesium in aluminummagnesium alloys. Aluminum was
precipitated with hexamine in a nearly neutral solution. A colored species was formed between magnesium and congo red which had a n absorption maximum at 550 mp. Beer's law was obeyed up to 2.4 pg. per ml. 8-Hydroxyquinoline-&sulfonic acid was used as a fluorometric reagent for determination of magnesium in the presence of calcium (186). Interferences from iron, chromium, aluminum, and titanium were eliminated by hydroxide precipitation or extraction with dithiocarbamate. Manganese. Determination of micro amounts of manganese in beryllium by extraction with diethyldithiocarbamate and photometry with 8hydroxyquinaldine was reported b y Motojima and T a m u r a (166). T h e manganese - diethyldithiocarbamate complex was extracted into benzene, then reacted with 8-hydroxyquinaldine. T h e latter was done t o take advantage of the fact t h a t the second reagent has a molar extinction coefficient for manganese which is 2l/2 times that of the first one. Absorbance measurements were made a t 400 mp. Niobium and Tantalum. A relatively convenient method for determination of traces of niobium in titanium and titanium tetrachloride was described by Yagnyatinskaya and Nazarenko (259). Niobium was separated by extraction with a solution of tribenzylamine in chloroform from 11M HCl. Determination was completed photometrically with orthonitrophenylfluorone. Sensitivity of the method was niobium in titanium and 2 x 10-570 niobium in titanium tetrachloride. Silicylfluorone and a coprecipitator dissalicylaldianisidine were suggested for concentration of low amounts (3 to 100 pg) of niobium and tantalum (261). Precipitation was performed in 3N HC1 under which conditions aluminum and magnesium do not interfere. Titanium will be coprecipitated within 2 to 9% of the amount present. Precipitate was calcined a t 700 to 800 "C and products were weighed as oxides and determined spectrographically. Niobium was determined in aluminum alloys by complexing with 4-(2-pyridy1azo)-resorcinol in the presence of oxalate and tartrate (76). The complex exhibited a maximum absorbance at 540 mp or 520 mp with molar extinction coefficients of 23,300 and 28,000, respectively. I n the presence of tartrate, the molar extinction coefficient could be increased by increasing acid concentration to 7.551 in HC1. Nitrogen. Bundy and Goode (46) used indophenol blue for determination of nitrogen in beryllium without distillation. Maximum absorbance was a t 630 mp and Beer's law was obeyed for 0 to 50 pg N in 50 ml. Sen-
sitivity of the method was 0.002 pg N per cm2. As little as 4 ppm nitrogen was detectable in a 100-mg beryllium sample. A coulometric titration was used by Yoshimori et al. (260) to determine nitrogen in metallic titanium. Sample was dissolved with acid and ammonia separated by Kjeldahl distillation process, followed by coulometric titration using electrolytically generated
BrO -1.
Table IV. Quantometer Range and Limit of Detection Parameters for Analysis of Aluminum and Aluminum Alloys
w
Element Si Fe CU Mn Mg Cr Ni Zn Ti V Pb Sn B Be Na Ca Bi Ga Zr Cd co
Max, 14.0 4.50 22.0 2.0
11 .o
Std dev at
o.ooo~o
0.00011 0.00014 0.00010 0.00010 0.00002
3.0
0.00010 3.0 0.00010 10.0 0.00026 0.50 0.00010 0.00010 0.50 1.0 0.00027 1.0 0.00018 0.10 0.00003 0.30 0.00001 0.10 0.00002 0.00001 0.10 0.00022 1.0 0.10 0.00011 0.30 0.00010 0.00010 4.0 0.00006 0.10 Li 1.5 0.00010 1.5 0.00004 Ag a Highest concn provided for. Table V. X-Ray Fluorescence Limits of Detection for Aluminum Metal Primary source, Ag target Exposure time, 100 sac
Element Si
Fe cu Mn
2
Ni Zn Ti
v
Pb Sn B Be Na Ca Bi Ga Zr
Cd
co
PPm 6 1 1 1 10 1 1 1 1 1 2 4
N.D.a N.D. N.P.b 4 1 1 0.5 le lC
Wavelength KlY KLY Ka Ka Kff KCY Ka Ka Ka Ka La La
KCY La
Ka
Ka Kff KLY
Id Ka Not detectable. * Not practical in metal. c Estimated value. * Estimated value using Cr target. a
VOL. 41, NO. 5, APRIL 1969
107R
Oxygen. See Table 11. Phosphorus. Indirect sequential determination of phosphorus and silicon b y atomic absorption spectrophotometry was reported b y Kirkbright et al. (119) using a n amplification procedure. Phosphomolybdic acid was formed and selectively extracted away from silicate and excess of molybdate reagent into isobutyl acetate. T h e 12 molybdate ions associated with each phosphate and silicate ion were determined b y direct atomic absorption spectrometry in isobutyl acetate and butanol phases inoa nitrous oxide acetylene flame at 3132 A. With this procedure 0.8 to 1 ppm of phosphorus and 0.08 to 1.2 ppm of silicon can be determined in the same solution. Alternately, molybdenum in molybdic acid can be determined by a kinetic method employing catalytic oxidation of potassium iodide by peroxide (214). Pakalns (181) described a method where phosphorus was extracted as molybdophosphoric acid at p H 0.3 to 0.45. The solution contained sulfuric acid, tetrafluoroborate, or HFHClOd with iso-BuOAc, and absorbance of the reduced species was measured at 725 mp. Sydakov et al. (232) used safranine molybdophosphate reduced by ascorbic acid to determine phosphorus. The reduced species was extracted by a mixture of chlorobenzene with acetophenone or by isobutylmethlyketone. Absorbance of the organic phase was measured at 785 mp. Potassium. Potassium can be determined in the presence of aluminum (249) b y first extracting aluminum with 8-quinolinol in chloroform, then photometrically measuring potassium with dinitrohydroxyazo a t 640 mp. Rare Earths. Cvarova et al. (249) made a comparative investigation of known methods for separating lanthanum and showed that methods based on extraction of hydroxyquinoline complexes a t different p H values, or using tributylphosphate in the presence of potassium nitrate do not ensure quantitative separation. Precipitation of lanthanum as t h e oxalate gives complete separation from aluminum, but hinders further chelometric titration of aluminum because of the need to destroy large amounts of oxalate ion. The most suitable method for separating the two is to precipitate lanthanum hydroxide with a freshly prepared sodium hydroxide solution. A procedure for determination of lanthanum aluminate solution was presented. Yttrium and lanthanum were determined in aluminum alloys using separation of aluminum by oxine extraction (115). Rare earths were then determined photometrically with methyl thymol blue (610 mp). I n another paper (190), yttrium was determined 108 R
0
ANALYTICAL CHEMISTRY
photometrically with xylenol orange a t p H 5 to 5.5 in the presence of sulfosalicylic acid which strongly masks lanthanum. The sum of the two was determined using arsenazo 111. The method was applied to aluminum and magnesium alloys. Yttrium and aluminum in a yttriumaluminum garnet crystal were determined chelometrically by Grosskreutz etal. (96). Crystals were decomposed by a borate-carbonate fusion and dissolved in dilute sulfuric acid. Sulfosalicylic acid and urotropine were added to complex aluminum. Yttrium was titrated with E D T A using xylenol orange. The sum was determined by a backtitration employing zinc sulfate and dithizone. Scandium was determined in the presence of aluminum by first extracting it as the diantipyrylmethane-nitrate complex (263). Dysprosium was determined in aluminum alloys (253) by separating it as the hydroxide precipitate, redissolving it and reprecipitating with oxalic acid. The precipitate was dried and weighed as the oxide. Bruck and Lauer (41) determined dysprosium in aluminum by a method similar to that discussed above for yttrium and aluminum (96). A general chelometric method for rare earths was presented by hlilner and Gednasky (159). Aluminum was masked with acetylacetone; cerium and lanthanum were titrated chelometrically using xylenol orange as the indicator. Silicon. A study of the solubility of silicon in dilute aluminum-silicon alloys by low temperature resistivity measurement was reported by KovacsCsetenyi, Vassel, and Kovacs (128). The samples contained 0 to 0.4% silicon and were previously heat treated for 1 hour at 100 to 600 OC. Tikhonov and Chernsheva (2%') used a differential spectrophotometric approach for determining silicon in products of the titanium industry. The method was stated to be suitable for determining 20 to 50% silicon in 0.3 to 0.4 gram of the sample. The method is based on the measurement at 850 mp of the reduced molybdic acid blue color. Sulfur. Sulfur was determined in titanium tetrachloride by a method based on the oxidation of the sulfur compounds to sulfate and the subsequent reduction to sulfide with chromium in the presence of phosphoric acid (265). The sulfides were absorbed in cadmium acetate and determined iodometrically or photometrically using dimethyl-p-phenylenediamine. Tin. A general titrimetric method for determination of tin was reported b y Basinska and Wisniewski @ I ) . T h e solution containing 0.01 to 0.9 gram of SnClz was made alkaline so t h a t i t would be 2.5 t o 831 in potassium hydroxide at the end point,
and titrated with illKaFe(CN)s using alizarin yellow R as indicator. Aluminum and zinc did not interfere. Zhivopistsev et al. (264) used antipyrinyl- [4 - (benzylmethy1amino)phe nyl] - 4 dimethylaminophenylmethanol in a n acid solution containing ammonium thiocyanate for determination of tin in aluminum alloys. Extinction of the complex is maximum a t 600 mp. Titanium. Titanium in a n aluminum-chromium catalyst was determined b y a method based on reaction of titanium with chromotropic acid (55). T h e complex was formed at a p H of 2.9 to 3.2 and absorbance was measured at 465 mp. Samples were fused with pyrosulfate to render them soluble. Chromotropic acid is not a very stable reagent and Asmus and Kurzmann (9) recommended that diacylated chromotropic acid be used. Their paper presents data for determination of titanium in aluminum alloys. Horiuchi and Ichijyo (106) determined titanium in the presence of aluminum b y a chelometric procedure. Two methods were given. I n the first, aluminum and titanium (in the presence of peroxide) were determined b y backtitration of an excess of E D T A with bismuth using methyl thymol blue as indicator. A second titration was performed using sulfosalicylic acid to mask aluminum, I n the second method, zinc was used as the backtitrant and aluminum was masked with triethanolamine or ammonium fluoride. Uranium. For determination of microgram quantities of uranium in aluminum, Kuroha et al. (231) extracted the uranium-arsenazo I11 complex form butyl alcohol in t h e presence of diphenylguanidine. SOdium fluoride and boric acid were added to prevent interference of aluminum. Maximum absorbance of the complex was 660 mw. 4 s a n alternate approach the measurements were performed fluorometrically. Vanadium. Chemistry of reaction between vanadium and S-benzoly-ATphenylhydroxylamine was studied b y Sawada et al. (909). They made use of this reagent for photometric determination of uranium in aluminum and aluminum alloys. Vanadium was determined in titanium tetrachloride by an osidation-reduction titration (2.42). The method differentiates among various valence states of vanadium--vis., 111,IV, and V. Determination of vanadium IV was based on ability of potassium dichromate to oxidize vanadium selectively to the + 4 state in a 4W sulfuric acid solution. Excess dichromate was determined by titration with a ferrous salt. Zinc. Potassium hesncynnoferrate I1 was used to titrate zinc in mngnesium alloys (23s). Zinc mas extracted as the thiocyanate complex and back-
-
extracted with 6M HCI. T h e zinc was titrated a n d a n aqueous ethanol solvent with methanolic 3,3’-dimethylnaphthidine as indicator. Zirconium. Dedkov et al. (64) made a comparison of 13 reagents for photometric determination of zirconium. Of these they concluded t h a t arsenazo I11 was t h e best reagent with respect to sensitivity, selectivity, a n d independence of p H . Kurbatova a n d Feofanova (1.90) used 3-cyano1,5- bis(2 - hydroxy - 5 - sulphophenyl) metric reagent for determination of zirconium in aluminum alloys. Maximum absorbance was at 680 mp. Iron and aluminum were removed b y a n ion exchange separation using the acid form of a strong cation resin. Burriel-Marti and Alvarez-Herrero (48) also employed a cation exchange separation to determine zirconium in aluminum. After separation, both zirconium and aluminum were determined chelometrically. LITERATURE CITED
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