(18N) Mueller-Mulot, W,, Z. Lebensm.Untersuch.-Forsch..140. 208~. (1969). (19N) Nelson, J. P., Milun, ‘A. J., J . Amer. Oil Chem. SOC., 45,848 (1968). (20N) Niederstebruch, A., Hinsch, I., Fette, Sei&, Anslrichm., 69, 559 (1967). (21N) Pelletier. O., J . Ass. Offic. Anal. Chem., 50, 817 (1967). (22N) Pribela, A., Pikulikova, C., Z. Lebensm.-Untersuch.-Forsch.,139, 219 (1969). (23N) Schmidt, H. E., Fette, Seifen, Anstrichm., 70, 63 (1968). (24N) Zbid., p 159. (25N) Schubert, E., Roland, U., Nahrung., 12, 715 (1968); Anal. Abstr., 18, 1272 (1970). (26N) Slover, H. T., Lehmann, J., Valis, R. J., J . Amer. Oil Chem. SOC.,46, 417 (1969). (27N) Vakil, J. R., Shahani, K. M., J. Dairy Sci., 52, 325 (1969). 128N) Weeks. C. E.. Deutsch. M. J.. J . Ask Ofic. Anal. Chem., 50, 793 (1967). (29N) Wildemann, L., Z. Klin. Chem. Klin. Riochem., 7, 509 (1969); Chem. Abstr., 71, 122462~(1969). (30N) Woodrow, I. L., Torrie, K. M., Henderson, G. A., Can. Znst. Food Technol. J., 2, 120 (1969).
-
’
~
Miscellaneous
(1P) Adda, J., Blanc-Patin, E., Jeunet, It., Grappin, R., Mocquot, G., Pousardieu, B., lticordeau, G., Lait, 48, 146 (1968); Chem. Abstr., 69,95149s (1968). (2P) “Advances in Automated Analysis, Technicon International Congress 1969,” Volume 11, Industrial Analysis, Mediad Inc., White Plains, N. Y., 1970. (3P) “Approved Methods of the AACC,” American Association of Cereal Chemists, Inc., St. Paul, Minn., 1969. (4P) bruemmer, J. hl., Brot. Gebaeck, 22, 241 (1968); Chem. Abstr., 70, 105175j (1969).
(5P) Calzolari, C., Favretto, L., 1nt. Colloq. Chem. Coffee, Srd, 1967, p 257 (1968); Chem. Abstr., 70, 105190k (1969). (6P) Cerma, E., Bruni, G., Coassini Lokar, L., Pertoldi Marletta, G., Rass. Chim.. 20.266 (1968): Chem. Abstr.., 71.. . 11775y (1969). (7P) Ciz, K., Cejkova, V., Listy Cukrov., 84, 104 (1968); Anal. Abstr., 17, 2398 (1969). (8P) Dolby, R. M., N . Z . J . Dairy Technol.. 3. 84 11968): Chem. Abstr.., 70., 46226b’f 1969). ’ ’ (9Pj Engel,-C.’ R., Sawicki, E., Microchem. J., 13, 202 (1968). (1OP) Favretto, L., Favretto Gabrielli, L., Atti Cungr. Qual., 6th, 1967, p 233 (1968): Chem. Abstr.. 72. 77501h I
,
(lip) Gorbach, G., Nahrung, 12, 859 (1968); Anal. Abstr., 18, 1976 (1970). (12P) “Handbuch der Lebensmittelchemie,” Springer-Verlag, New York, 1970. (13P) Herschdoerfer, S. M., “Quality Control in the Food Industry,” Academic Press, New York, 1968. (14P) Joslyn, M. A., “Methods in Food Analysis: Physical, Chemical, and Instrumental Methods of Analysis,” Academic Press, New York, 1970. (16P) Lawrence, B. M., Can. Znst. Food Techno/.J.,2, 20 (1969); Chem. Abstr., 72, 2177y (1970). (16P) Rlohler, K., Looser, S., 2. Lebensm.Untersuch.-Forsch., 140, 149 (1969). (17P) Nakai, S., Le, A. C., J. Dairy Sci., 53,276 (1970). (18P) Newton, J. M., J . Ass. Ofic. Anal. Chem., 52,653 (1969). (19P) “Official Methods of Analysis of the Association of Official Analytical Chemists,” published by the Association of Official Analytical Chemists, Washington, D. C., 1970. (20P) Pierzchalski, T., Mroaowska, A., Chem. Anal. (Warsaw), 13, 367 (1968); Anal. Abstr., 17, 1114 (1969).
(21P) Polzella, L., Boll. Lab. Chim. Prw., 19, 485 (1968); Chem. Abstr., 70, 76487e (1969). (22P) Zbid., p 871. (23P) Ponomarenko, A. A., Plakhotin, V. Y . ,Zzv. Vyssh. Ucheb.Zaved., Pishch. Tekhnol.. 1970, 177: Chem. Abstr.., 73., 86613u (1970).‘ ’ (24P) Prosst, R., Feucht, G., Herrmann, K., Z . Lebensm.-Untersuch.-Forsch., 139, 301 (1969); Anal. Abstr., 19,695 (1970). (25P) Rogers, G. R., J. Ass. O&. Anal. Chem., 53,568 (1970). (26P) Salminen, K., Koivistoinen, P., Acta Chem. Scand., 23, 999 (1969); Anal. Abstr., 18,4367 (1970). (27P) Schultz, G. P. Prinsen, A. J., Pater, A., Rev. Znt. &hoc., 25, 7 (1970); Chem. Abstr., 73, 13192w (1970). (28P) Sloman, K. G., Foltz, A. K., Yeransian, J. A., ANAL.CHEM.,41, 63R (lWlS\. \--_-,-
(29P) Smith, R. F., Rep. Progr. Appl. Chem., 53, 352 (1968); Chem. Abstr., 72, 65435b (1970). (30P) Struhar, M., Nguyen, T. B., Farm. Obz., 36, 549 (1967); Chem. Abstr., 70, 105260h (1969). (3lP) “SchweiaerischesLebensmittelbuch Methoden fuer die Untersuchung und Beurteilung von Lebensmitteln und Gebrauchsgegenstaenden, Bd. 2 (Spezieller Teil),” Schweieerischen Lebensmittelbuch-Kommission (Eidg. Drucksachen- und Materialzentrale:) Bern, Switzerland, 1967; Chem. Abstr., 69, 105228h (1968). (32P) Ulrich, W. F., Food Prod. Develop., 2 , 1 8 (1969). (33P) Zbid., 3, 50 (1969). (34P) Vitathum, 0. G., Znt. CooIZop. Chem. Coffee, Srd, 1967, p 216 (1968); Chem. Abstr., 70, 86336u (1969). (35P) Wolf, W. J., Thomas, B. W., J . Amer. Oil Chem. Soc.. 47. 86 (1970). (36P) Zwaving, J. H., Dikhoff,‘J. HI W., Phurm. Weekbl. Ned., 103, 1399 (1968); Anal. Abstr., 18, 1207 (1970).
Ferrous Metallurgy C . R. Hines and J. R. Dulski, lones & Laughlin Steel Corporation, Graham Research Laboratory, 900 Agnew Road, Pittsburgh, Pa. 75230
T
covers the period from November 1968 to November 1970 and is a continuation of previous reviews (36, 368, 369). The sources of this material were Chemical Abstracts and Analytical Abstracts for the period mentioned. I n introducing this review, it can be pointed out that most of the procedures reviewed are modifications of established procedures, perhaps with more specific applications. However, throughout this review i t is very apparent that atomic absorption has become firmly established as a leading analytical tool in ferrous metallurgy and perhaps in time may even equal or surpass emission spectroscopy as the primary technique of analysis.
ALUMINUM
HIS REVIEW
100R
Greatest emphasis was shown in spectrophotometric and atomic absorption methods for determining aluminum in steel, slags, ores, and ferro-alloys. Atomic Absorption. Nitrous oxideacetylene flames are being used exclusively for this determination and detection limits are claimed as low as 0.005%. Methods were presented for analyzing steel and iron (123, 186, 199, 253, 263), slags (111, 288), ores (149,263,288) and ferro-alloys (289). Spectrophotometry. Methods were described or evaluated using eriochrome cyanine (74, 100, 163, 445, 527’), aluminon (104, 121, 333), chlorsulphenol S (dol), chrome aeurol S (529), and 8-hydroxyquinoline (50,126).
ANALYTICAL CHEMISTRY, VOL. 43,
NO. 5, APRIL 1971
Volumetric. A method was described using E D T A titration (10.2). Emission Spectrometry. Methods were described using high frequency plasma torch spectrometry (467, 469) and for determining aluminum in ball bearing steels (11). ANTIMONY
Methods were described for determining antimony in steel and iron using the following techniques: Emission Spectrometry. (40). Polarography. (356). Spectrophotometry. Directly using potassium iodide (52) and after separation by coprecipitation with MnOz (10).
ARSENIC
T h e following techniques were used for determining arsenic in steel and ores: Atomic Absorption. Arsenic was concentrated b y distillation and a hydrogen-argon flame used for analysis
(177). Polarography. (63, 154, 462). X-Ray Spectroscopy. I n steels, after concentration b y precipitation
(73)* Volumetric. T h e standard stannous chloride iodimetric method was used (306). Emission Spectrometry. (386).
task in ferrous metallurgy. With modern steelmaking practices, the rapid determination of carbon for control purposes is being heavily investigated, especially in process analyses (406,628). Procedures presently being used for determining carbon in molten metal include the liquidus arrest method (21, 184,144,150,320) and a n indirect method in which the off-gases from the furnace are analyzed for carbon loss and from the original carbon content and other factors, the carbon concentration in the melt is calculated (48,66, 132,
261 , 499).
The emphasis on spectrophotometric and emission spectrometric methods for determining boron in steel continues; however, neutron activation procedures are being investigated much more. Spectrophotometry. Direct procedures were reported using curcumin (153, 326, 485) and quinalizarin (94). Solvent extraction methods involved the tetrafluoroborate-methylene blue complex (46,49,522). Emission Spectrometry. For direct-reading specirometry, the boron spectral line 1826.4A apparently is being more widely used (243,358, 404).Spectrographic methods were also investigated (193,$46,386). X-Ray Spectroscopy. A method employing proton excitation shows a detection limit of 0.001470 boron in steel
Combustion Technique. For laboratory or production floor analysis for carbon, the combustion technique, in which the solid sample is combusted in oxygen with COz being given off and analyzed by various techniques, is the standard procedure. The combustion of the sample was studied as to the effects of temperature (481,532) and types of fluxes (107,361, 407,533). Evaluation of various commercial instruments (319) and the different techniques of measuring the evolved COz (480)were reported. Methods were described or evaluated using combustion and the following measuring techniques: Manometric. (64,101 , 526). Gas Chromatography. (1 71, 197). Conductometric. (15, 77). Infrared Spectroscopy. (255). Volumetric. (37,237, 408). Emission Spectrometry. Vacuum emission spectrometry, employing spectral lines in the vacuum ultraviolet are still the most prevalent spectrometric techniques for analyzing steels for carbon (84,272,281),but method? were described using the C 2296.89 A line (282) and various cyanogen bandheads in the visible region (274,276,441 , 454,
(211).
455).
BISMUTH
A spectrophotometric procedure was reported in which ion exchange chromatography was used to separate interferences and bismuth was determined as the tetraiodobismuthite complex (450). BORON
Neutron Activation. (205, 266,300,
327). CALCIUM
Despite interference problems, atomic absorption spectrometry is being investigated most heavily for determining trace amounts of calcium in steel and larger amounts of calcium in ores and slags. Atomic Absorption. (123, 149, 151,
X-Ray Diffraction. X-ray diffraction mas used t o determine 0.5-1.5% carbon in steel (500). Electron Microprobe. Carbon in steel and a series of carbides were determined quantitatively using the electron microprobe (264). Activation Analysis. Discussions of interferences and chemical separations were presented in activation methods for determining carbon (26,303, 396,397).
206). Emission
Spectrometry.
Steels
(254,451),ores (515). X-Ray Spectroscopy. A non-dispersive method (285). Spectrophotometry. A review of methods for steel (,536). CARBON
Determination of carbon in steel still remains the most important analytical
COBALl
Analytical development in the determination of cobalt in steels centered mainly on spectrophotometric techniques and atomic absorption procedures. Spectrophotometry. (14, 34, 128,
14l,26OJ4SO, 471 , 492). Atomic Absorption. (76,199, 253, 289,391, 393). Polarography. (322). Volumetric. (514). COPPER
Copper is another element for which the analytical development is centering on atomic absorption techniques. Atomic Absorption. (57,11 1 , 123,
186, 199, 253, 257, 289, 391 , 392).
Spectrophotometry. One paper evaluates four reagents for use with different steels (136). Other methods reported used dithiocarbamate (46,371) and oxalic acid bis(cyclohexy1idenehydrazide) (308). Volumetric. K i t h ascorbic acid
(245,247). Polarography. (388). Neutron Activation. (504). HYDROGEN
Sampling of steel for hydrogen determination is troublesome. Methods of taking and storing samples included evacuated silica pipettes sealed with silver chloride (478),storing of samples under a CO, atmosphere (lsl),and the storing of samples under vacuum for several days until a n equilibrium is reached (296). Methods for separating hydrogen from steel for subsequent determination include heating in an inert atmosphere (8, 133, 230, 372, 546), heating under vacuum (284,341, 513,548)and vacuum fusion ( 2 ) . Measuring of the hydrogen is accomplished b y gas chromatography (8, 133, 230, 372, 548), mancmetrically (2,87, Sdl), volumetrically (546),and by mass spectroscopy (513). A spectrographic isotopic method which could determine as little as 1 part per million hydrogen was described
(58)*
1 74,257,288,289,476,484). Volumetric. E D T A Titration (161,
Polarography. (461). Volumetric. E D T A (244,376),
CHROMIUM
LEAD
Although the highlight of a review of the past two years investigations on chromium determination would be the great emphasis on atomic absorption procedures, one novel technique employs gas chromotography to quantitatively determine chromium in steel as low as 0.014% (402). Atomic Absorption. (57,109, 1 1 1,
For determining trace amounts of lead in steel, polarography still appears to be most prevalent method; however, atomic absorption and optical emission spectrometric techniques are being used routinely for low levels of lead. Atomic Absorption. (67,109, 199,
123, 186, 199, 253, 289, 391,392). Spectrophotometry. (268,979).
289). Emission Spectrometry. (39,91). Polarography. (103,156,252).
ANALYTICAL CHEMISTRY, VOL. 43, NO. 5, APRIL 1971
102 R
MAGNESIUM
Atomic absorption, because of its great sensitivity for magnesium, is now being used routinely by a large number of laboratories for determining magnesium in iron, ores, and slags. Volumetrically, EDTA titration is used almost exclusively. Atomic Absorption. (123, 149, 151, 186, 199, 257, 288, 290, 357, 476). Emission Spectrometry. ( 5 9 ) . Volumetric. (161, 206, 277). Spectrophotometry. (30,334). MANGANESE
Atomic Absorption. Manganese has been determined in a wide range of alloys, slags, and ores over a wide concentration range with atomic absorption techniques (57, 111, 123, 149, 184, 186, 199, 253, 257, 288, 289, 391, 392, 509). Neutron Activation. Both a direct method and a chemical separation technique were described for trace manganese concentrations (335). Spectrophotometry. A detection of 0.0002% manganese was achieved (305). Volumetric. A titration with ascorbic acid was described (246) and various electrometric techniques were used for determining trace amounts of manganese (124, 189, 479, 486). MOLYBDENUM
Spectrophotometry. Thiocyanate was used in the automated direct determination of steel (60) and also after solvent extraction (495). Chromotropic acid was used directly (489) and N , N'-diphenylthiocarbamohydroxamic acid (314) and Rezarson (302) were used with solvent extraction. Atomic Absorption. Molybdenum is being determined routinely b y atomic absorption in many laboratories. I n almost all cases, an additive such as a chloride salt is added to the solution to overcome interferences (83, 110, 111,186,199,253,382). Emission Spectrometry. High frequency plasma torch (468) a n d visual spectroscopic methods were described (351). Volumetric. Coulometric ( 5 ) . Precipitation of PbhfOO, with a n excess of lead and back titration of lead (165). Polarography. (53, 367). Neutron Activation. With chemical separation (287, 336). NICKEL
Spectrophotometry. T h e dimethylglyoxime method was used in steels (233, 581), stainless steels (188), and ores (429). Atomic Absorption. Nickel is another element being routinely de102 R
*
termined in a large number of laboratories by atomic absorption techniques (76, 109, 111, 123, 186, 199, 253,289,391,393). Polarography. (457, 547). NIOBIUM
Spectrophotometry. Reagents used for determining niobium in steels include chlorsulphenol S (105, 414, 519, 520), xylenol orange (413), bromopyrogallol Red (390), catechol violet (315), tichromin (531), and 4-(2-pyridylazo) resorcinol or acid chrome violet K (24). Emission Spectrometry. A flame emission method after solvent extraction was described (117). Polarography. ( 7 , 44). NITROGEN
Methods for determining nitrogen in steel were reviewed (120, 194) and comparisons of chemical and fusion methods were made (2998,460). A unique method for determining metallurgically dissolved nitrogen in steel involved extraction of the nitrogen with hydrogen with the nesslerization of the resulting ammonia (99). Fusion Techniques. For either vacuum or inert gas fusion, it is recommended that a Mg0-lined crucible be used to eliminate the interference of graphite (152). Inert Gas Fusion. (196, 231, 420, 421,539). Vacuum Fusion. (1, 248, 299). Spectrophotometry. T h e indophenol method was automated (530), Nessler's reagent was used in a n acid dissolution method (297), and bis(pyrazo1inone) was recommended as superior to Kessler's reagent (236). Isotopic Dilution. (360). M a s s Spectrometry. (510). Emission Spectrometry. (449). Polargraphy. (438). NONMETALLIC INCLUSIONS
The interest in the isolation and identification of nonmetallic inclusions in steel increased greatly during the past two years. Instrumental approaches, such as the electron microprobe (55, 69, 176, 178, 202, 214, 265, 295, 417, 418, 446,523, 537) and the quantitative microscope (127, 130, 399) are being used heavily for the identification and even the quantitative determination of inclusions. Chemical and electrochemical methods are still the predominant methods for isolating the nonmetallic inclusions. Some of the methods and the types of inclusions isolated by the methods are as follows: Halogen-Organic Solvent. Oxides (216, 222, 238, 304, 339, @ l ) , nitrides (470)' Electrolysis. Carbides (218, 220,
ANALYTICAL CHEMISTRY, VOL. 43, NO. 5, APRIL 1971
221, 340, 535), oxides (21?', 269, S79, 491, 497'), nitrides (326), and sulfides (310, 406). Schemes were offered using combinations of chemical and electrochemical treatment to determine oxides (292, 498, 542), oxides and nitrides (291), and complete analyses of boron nonmetallic inclusions (521) or rare earth inclusions (88, 250). Although the isolation techniques tend to identify the anions, the specific cations must be determined from the isolated residues. Methods which were investigated included: Spectrophotometry. (116, 270). Emission Spectrometry. (95, 487). Infrared Spectroscopy. (190, 21 5, 21 9,223). Atomic Absorption. ( I 08, 422). Differential Thermal-Emuent Gas Analysis. (28, 29). OXYGEN
The ever increasing need for rapid oxygen detemination was shown by the great number of investigations into determining oxygen in molten metals. Several patents were granted for apparati for performing this determination (67, 143, 145, 456) and many other investigations were reported (129, 135, 140, 312, 316, 354, 365, 366, 452, 466, 544)* For determination of oxygen in solid steel, sampling (72, 96, 195, 262, 385) and standards (85) remained points of investigation. Reviews of the various methods of analysis were presented (149, 168, 294). Vacuum Fusion. (93, 138, 167, 191, 21 0 , 224, 394,437,463, 464). Inert Gas Fusion. (13, 42, 98, 137, 192,212,409,505). Neutron Activation. (90, 146, 209, 227,286,324, 338,494). Emission Spectrometry. (43, 75, 122,448). Infrared Spectroscopy. I n e r t gas fusion is used and the resultant C02 is measured by infrared absorption (106, 459). Spectrophotometry. A unique method was described for determining oxygen in cast iron in which excess metallic aluminum was added to molten iron in a special chill mold. All of the FeO is reduced to stable -41203. The acid-insoluble aluminum is determined with eriochrome cyanine R and the oxygen calculated (86). PHOSPHORUS
Spectrophotometry. Variations of the molybdenum blue method were used for determining phosphorus in iron and steel (293), iron ores (68),high alloy steels (119, 180, 363, 428), and ferro-alloys (432, 538). Polarography. A method is pro-
posed which is especially suited for the range 0.0005-0.005% P (444). Neutron Activation. Chemical separation is used (444)-
interferences and high limit of detection (377, 378, 502, 505). SPECTROSCOPY
RARE EARTHS
Spectrophotometry. Arsenazo was used for the determination of total rare earths in steel (271, 400) and for determining cerium in nonmetallic inclusions (160). Cerium was also determined in iron and steels using 8hydroxyquinoline (157), the peroxide complex (344, 443), and orthotolidine (51, 54) Polarography. T o t a l rare earths were determined in a method involving precipitation as oxalates (549, 550). Cerium was determined after separation with ion exchange (175) and by A uoride precipitation (54). Gravimetric. Procedures were described for determining lanthanum (lid), scandium (115),and yttrium and hafnium (113). SELENIUM
Volumetric. A method was described in which selenium is determined iodometrically after being separated by extraction (475). X-Ray Spectroscopy. For trace selenium contents, a precipitation procedure was described in which the selenium is collected on millipore filter and determined by X-ray spectroscopy (6). SILICON
Several unique methods were reported for determining silicon in steel. A differential thermal analysis procedure uses the difference in temperature variations between a standard and the sample when both are treated with hydrofluoric acid (412). A gas chromatographic procedure was reported which measures Sic14 which forms when the steel is treated with chlorine a t 600 OC (442). For control analysis in cast iron production, the thermoelectric procedure is proving very rapid (251, 501, 517, 518). The method was also used for determining silicon in ferrochromium (226). Atomic Absorption. (125, 149, 186, 288, 289). An atomic fluorescence procedure was compared to atomic absorption (249). Spectrophotometry. (31, 278, 280, 41 0, 41 5 ) . Volumetric. Procedures based on the titration of KzSiFe with sodium hydroxide were described as being rapid enough for process control (342, 389, 403). Polarography. (17 ) . Neutron Activation. All the procedures are limited by t h e aluminum
Auger Spectroscopy. A new technique in ferrous metallurgy, Auger Spectroscopy, was used to study grain boundries (364) and surface segregation in steels (170). Atomic Absorption. Atomic absorption spectroscopy has now arrived a t a point where it is an integral part of chemical laboratories in ferrous metallurgy. The general use of the technique in ferrous metallurgy was described and reviewed (198, 427). Schemes of analysis of steel by dissolution of the sample were presented (76, 111, 123, 186, 199, 253, 337, 391, 392) and even the newer technique of direct analysis of the solid sample was investigated (57). Other materials which can be analyzed by atomic absorption procedures include ferrosilicon (289), ores (109, 149, 25267, 288), and slags (257, 288). Mass Spectroscopy. Spark source mass spectroscopy has not come to a point of being a routine laboratory instrument in ferrous metallurgy, but it is proving to be a valuable aid in determining trace amounts of impurities in iron and steel. One method reported used isotope dilution (570) while others employed the spark source with solid samples (118, 321, 419, 606, 611, 512, 54O,641). Mossbauer Spectroscopy.
Moss-
bauer spectroscopy, a relatively newly developed technique, is being investigated for use in ferrous metallurgy. Several investigators are using Mossbauer for studying corrosion of steel (92,204, 523), and for determining both the chemical composition and iron content of ores (148, 424). Other uses include determining residual austenite in steels (507), the identification of phases in steel (81), and the identification of surface compounds in steel (47267). One report discusses the possible uses of Mossbauer in ferrous metallurgy (158). Neutron Activation. hlthough neutron activation has been used primarily for determining oxygen in steel, some investigations have used chemical separations in developing schemes of analysis for steel and iron (f 6,482).
Optical
Emission
Spectrometry.
Because of its speed and relatively good accuracy, optical emission spectrometry still remains the most important control analysis technique in ferrous mettallurgy. Kow, with the use of computers, the time of analysis has been even further reduced to make the technique even more valuable. Several reports on the general use of emission
spectrometry were presented (240, 24248, 258,348,394,447,525). Sampling, one of the most important tasks in control analysis by emission spectrometry, was investigated for steel (9, 7 l ) , and cast iron (228). Remelting of steel chips in an arc or induction furnace is proving to be a valuable aid in the spectrographic laboratory (70, 112, 181, 229, 518, 458). Solution techniques are another method of overcoming sampling problems (27, 256, 398). Besides carbon and low alloy steel analysis, emission spectrometry was applied to the analysis of irons (25, 47, 159, 283, 3529, high alloy steels (147, S l l ) , and slags (62, 125, 172, 200, 203, brs, s i s , 3 4 5 , 3 4 r , 387,440, 488,499). New techniques investigated involved the plasma jet (179), hollow cathodes (483), a laser beam (32673),and the use of cellophane tape to limit the spot size to 50 micions for inclusion analysis (139). The direct spectrographic analysis of molten iron and steel was also reported (56).
X-Ray and Electron Microprobe. X-ray spectrometry is proving to be a dependable and versatile technique in ferrous metallurgy (80, 374, 425). Because of its inherent excellent repeatability, it is used extensively for the determination of major components in stainless steels (185, 201, 434), iron ores (164, 235, 329, %0), ferroalloys (516, 545), and slags (259). With improvement in X-ray tubes and crystals, the technique is now being used to determine minor constituents in steel and irons (328, 453), even sulfur and phosphorous ( 4 , 1 2 ) . For solid samples, sample prepaiation was shown to be very important (201) and the technique can be applied to solutions (155, 426) and powders (164, 235,259,329,330). I n general analytical schemes for steels and stainless steels, matrix effects are severe and must be considered. Many laboratories use calibration curves prepared from standards of like matrices; however, the mathematical treatment of data for absorption and enhancement effects is extensively used (12,41,185,~ 9 , 3 3 1434,455). , Although X-ray fluorescence is the predominant technique used, primary X-rays from radioisotopes (436) or a n electron beam source (301) are also employed. The electron microprobe, although still not generally a quantitative instrument, has been used to determine chromium and tungsten in steels (411). Reviews on the use of the instrument in steel research and development were presented (232,Sf 7 ) . The microprobe has also been used to analyze cast irons (439) and to determine the concentration and distribu-
ANALYTICAL CHEMISTRY, VOL. 43, NO. 5, APRIL 1971
103 R
tion of alloying elements in oxide scales (624)* SULFUR
Combustion. T h e use of zirconium oxide was recommended in analyzing pig iron to prevent sample loss during combustion (183). For detection of the SO2 formed after combustion, methods using pararosaniline (169) and methyl vioIet (4Q6)were evaluated. Volumetric. T h e evolution sulfur technique was used with the liberated H2S being determined volumetrically with the iodineazide reaction (22) and with mercuric acetate and dithizone (380). Gravimetric. A barium sulfate gravimetric procedure for determining sulfur in ferrovanadium was described in which interferences are eliminated by ion exchange chromatography (508). Emission Spectrometry. T h e effect a n d minimization of elongated sulfide inclusions on the emission spectrometric determination of sulfur in steel was discussed (61). M a s s Spectrometry. Mass spectrometry was used t o study desulfurization during melting procedures (234, 643). Polarography. (353). TANTALUM
Spectrophotometry. An investigation of three reagents, pyrogallol, pyrocatechol, and malachite green showed the latter to be the most selective and sensitive (534). X-Ray Spectroscopy. A solution X-ray technique was described in which the tantalum is separated by precipitation and redissolved in tartaric acid (384).
for concentrations greater than O.OOl%, other techniques are generally being investigated. Spectrophotometry. (lQ, 33, 78, lO4,162,56QJ361,475). Polarography. (226, 356). Neutron Activation. (416 ) . Emission Spectrometry. (38). Volumetric. (876). Atomic Absorption. (109, 111, 186, 199, 288,289). TUNGSTEN
Spectrophotometry. Colorimetric methods were described for determining tungsten in steels (275, 433, 474) and ferroalloys (207,208). Polarography. (383). X-Ray Spectroscopy. Using a platinum target (3) and a tungsten target (490). VANADIUM
For the determination of vanadium in steels and slags, the emphasis is on spectrophotometry with a variety of reagents, and atomic absorption spectroscopy. Spectrophotometry. (23, 35, 89, 97,166, 182, 267, 343). Atomic Absorption. (109, 111, 186, i 8 r J i 9 9 ,253,288). Polarography. (465). ZINC
Spectrophotometry. (423). Polarography. ( 7 9 ) . X-Ray Spectroscopy. ( 8 2 ) . Atomic Absorption. (67, 123, 186, 199). ZIRCONIUM
Spectrophotometry. A turbidimetric method using stannous chloride was described (309) and a colorimetric procedure with Bismuth01 I1 (307) was presented. Atomic Absorption. (32, 186).
Spectrophotometry. Three methods involving t h e use of xylenol orange were described (215,241, 332). X-Ray Spectroscopy. For zirconium determination as low as 0.002%, a method was described in which zirconium is precipitated with phenylarsonic acid and the precipitate, collected on millipore filter, is analyzed by X-ray spectroscopy (65).
TIN
LITERATURE CITED
Spectrophotometry. Variations of the phenylfluorone method were described for determining tin in ferroalloys (173) and steels (18, 20). Volumetric. T h e iodimetric method was used to determine as low as 0.001% tin in iron ore (472). Atomic Absorption. (263, 289).
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TELLURIUM
TITANIUM
For determining trace amounts ( < 0 . 0 0 1 ~ ~of) titanium in steels and slags, polarography and neutron activation techniques are being used, and 104R
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