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Tiron Dissolution Method Used to Remove and Characterize Inorganic Components in Solls Hideomi Kodama* and G

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Tiron Dissolution Method Used to Remove and Characterize Inorganic Components in Solls Hideomi Kodama* and G 1180 SOlL SCI. SOC. AM. I., VOL. 55, JULY-AUGUST 1991 Wada, K., T. Henmi, N. Yoshinaga, and S.H. Patterson. 1972. Im- Zealand. Aust. J. Soi! Res. 19:185-195. ogolite and allophane formed in saprolite ofbasalt on Maui, Ha- Shoji, S., and Y. Fujiwara. 1984. Active aluminum and iron in the waii. Clays Clay Miner. 20:375-380. humus horizons of Andosols from northeastern Japan: Their Wada, K., and T. Higashi. 1976. The categories ofaluminium- and forms, properties, and significance in clay weathering. Soil Sei. iron-humus complexes in ando soils determined by selective dis- 137:216-226. solution. J. Soil Sei. 27:357-368. Shoji, S., and J. Masui. 1971. Opaline silica ofrecent volcanic ash Wada, K., and Y. Tokashiki. 1972. Selective dissolution and dif- soils in Japan. J. Soil Sei. 22:101-108. ferential infrared spectroscopy in quantitative mineralogical Shoji, S., and J. Masui. 1972. Amorphous clay mineral of recent analysis of volcanie-ash soil clays. Geoderma 7:199-213. volcanic ash soils. Part 3. Mineral composition of fine clay frae- Wada, S.-I., A. Eto, and K. Wada. 1979. Synthetic allophane and tions. J. Sei. Soil Manure Jpn. 43:187-193. imogolite. J. Soil Sei. 30:347-355. Shoji, S., and M. Saigusa. 1978. Occurrence oflaminar opaline silica Wada, S.-I., and K. Wada. 1980. Formation, composition, and strue- in some Oregon Andosols. Soil Sei. Plant Nutr. 24:157-160. ture ofhydroxy-aluminosilicate ions. J. Soil Sei. 31:457-467. Tait, J.M., N. Yoshinaga, and B.D. Mitchell. 1978. The occurrence Wada, S.-I., and K. Wada. 1981. Reactions between aluminate ions ofimogolitein some Scottish soils. SoilSei. Plant Nutr. 24:145-151. and orthosilieic aeid in dilute alkaline to neutral solutions. Soil Tokashiki, Y., and K. Wada. 1975. Weathering implications ofthe Sei. 132:267-273. mineralogy of clay minerals oftwo ando soils, Kyushu. Geoderma Wang, c., and H. Kodama. 1986. POOogenic imogolite in sandy 14:47-62. Brunisols ofEastern Ontario. Can. J. Soil Sei. 66:135-142. Violante, P., and J.M. Tait. 1979. Identification ofimogolite in some Wang, C., JA McKeague, and H. Kodama. 1986. POOogenic im- volcanic soils from Italy. Oay Miner. 14:155-158. ogolite and soil environments: Case study ofSpodosols in Quebec, Wada, K. 1978. Allophane and imogolite. Dev. Sedimentol. Canada. Soil Sei. Soc. Am. I. 50:711-718. 26:147-187. Wells, N., C.W. Childs, and C.J. Downes. 1977. Silica Springs, Ton- Wada, K. 1980. Mineralogical characteristics of Andisols. p. 87- gariro National Park, New Zealand - analyses of the spring water 107. In B.K.G. Theng (00.) Soils with variable charge. New Zea- and characterization of the aluminosilicate deposit. Geochim. land Soc. Soil Sei., Lower Hutt. Cosmochim. Acta 41:1497-1506. Wada, K. 1989. Allophane and imogolite. p. 1051-1087. In J.B. White, J.L. 1971. Interpretation ofinfrared spectra ofsoil minerals. Dixon and S.B. Weed (00.) Minerals in soil environments. 2nd Soil Sei. 112:22-31. 00. SSSA, Madison, WI. Yoshinaga, N., and S. Aomine. 1962. Imogolite in some ando soils. Wada, K., and D.J. Greenland. 1970. Selective dissolution and dif- Soil Sei. Plant Nutr. (Tokvo) 8:22-29. ferential infrared spectroscopy for characterization of "amor- Young, A.W., A.S. Campbell, and T.W. Walker. 1980. Allophane phous" constituents in soils clays. Oay Miner. 8:241-254. isolated from a podzol developed on a non-vitric parent material. Wada, K., and M.E. Harward. 1974. Amorphous clay constituents Nature (London) 284:46-48. of soils. Adv. Agron. 26:211-260. Tiron Dissolution Method Used to Remove and Characterize Inorganic Components in Solls Hideomi Kodama* and G. John Ross ABSTRACT moving these components from crystalline compo- nents and determining their overaJl composition. Treatments using NaOH and Na]COJ have been widely used to In the past 80 yr, a number of chemicaJ dissolution remove poorly crystalline and noncrystalline aluminosUicates and methods have been proposed, modified, and im- hydrous oxides of Si and Al. However, NaOH treatment is orten too proved. Based on chemicaJ reagents used and chemical harsh and Na]COJ treatment is usually too mild and must be ce- reactions involved, these methods can be c1assified peated. Treatment using e)kaline Tiron (4,5-dihydroxy-l,3-benzene- into one or more of the following four categories: (i) disulfonic acid (disodium saltI, CJI.NR]OaSJ wasas effective as aIkaline, (ii) acid, (iii) complexing, and (iv) reducing. acid oxalate in the dissolution of allODbll1llll!..imOl!olite. and ooorly Table 1 shows some major methods c1assifiedin these qystalline bvdrous Fe oxides. In contrast to oxalate, Tiron effec- categories. The extraction capacity and selectivity of tively removed oDaline sUica. and the difference between extracted these dissolution methods are c10sely related to the Si could be used to measure the amount of opaline sUica. Unlike mineral components to be extracted (Kodama and oxalate, Tiron dissolved little mametite. As sJbbsite is partially dis- Jaakkimainen, 1982). For best efficiency, therefore, it solved bv Tiro~ the rates or Al release by gibbsite «214m) dis- solution at different temperatures were used to estimate the gibbsite is essentiaJ to select the dissolution method(s) appro- contents of soil days containing this mineral. Generally, a single priate to the components to be extracted. treatment with Tiron appears to be sufficlent to mildly but effectively Poody crystalline and noncrystaJline inorganic com- clean up sampIes ror x-ray diffraction of crystalline minerals with ponents in soils are mainly hydrous oxide compounds amounts of extracted Si, Al, and Fe indicating the presence and of Si, Al, and Fe (Mn) and hydrous aJuminosilicates quantities or poorly crystalline and noncrystalline aluminosUicates such as allophane and imogolite. Table 2 lists these as weil as hydrous oxides of Fe, Al, and Si, including opaline silica. minerals with some oftheir characteristics. Among the many dissolution methods summarized in Table 1, NaOH, Na2C03, oxaJate, and dithionite-citrate are perhaps most frequently used to remove the hydrous oxide and aJuminosilicate minerals listed in Table 2. Hydroxylamine and Tiron are aJso applied, but less HE CHARACTERIZAnON of poorly crystaJline and T noncrystalline inorganic soil components is of frequently. Since the Tiron method was originally pro- considerable interest in view of their strong influence posed by Biermans and Baert (1977), it has been ex- on the physicaJ, chemical, and biological activities of tensively applied in our laboratory (Wang et al., 1981; soils. ChemicaJ extractions are prerequisite for re- Kodama and Jaakkimainen, 1982; McKeague et al., 1983; Wang et al., 1986; Kodama and Wang, 1989; Land Resource Research Centre, Research Branch, Agriculture Can- Kodama et aJ., 1989). This is because we have found ada, Ottawa, ON, KIA OC6 Canada. LRRC Contribution no. 90- 16. ReceivOO 27 Mar. 1990. .Corresponding author. Abbreviations: AA, atomic absorption; DCB, dithionite-citrate-bi- carbonate; XRD, x-ray diffraction. Published in Soil Sci. Soc. Am. J. 55:1180-1187 (1991). 1181 KODAMA & ROSS: INORGANIC COMPONENTS CHARACfERIZED BY TIRON DISSOLUTION application. The sources of these reference minerals and soil Table 1. Major chemical dissolution methods. sampies are listed in Table 3. The materials to be fraction- Chemical reagents ated were suspended in water and the day fractions (< 2#Lm) used for were separated by a sedimentation method without centrif- Category dissolution Selected references ugation (Jackson, 1968). The pretreatment with H202 to de- Alkaline NaOH Foster (1953) stroy organic matter was applied only to soil sampies, Hashimoto and Jackson (1960) allophane, and imogolite prior to suspension. Fractionated Na2CO. Mitchell and Farmer (1962) Follet et aI. (1965) clay fractions of five soil sampies were saturated with Mg2+ and freeze-dried. The day fractions of other sampies were Acid Ha Deb (1950) not saturated with Mg2+before freeze-drying. For consoli- Segalen (1968) Alkaline plus NaOHlHa dated sampies such as hematite, magnetite, goethite, gibb- acid site, lepidocrocite, opal, and obsidian, the mineral sampies Complexing U.C2O. Chester and Hugbes (1967) were first crushed to sand size and pure mineral grains were H2c.O. Ball and Beaumont (1972) selected by handpicking. (NH.)2C2OJH2c.O. Tamm (1922) After pulverizing by a Spex MixerJMill (Spex Industries, Schwertmann (1959) Metuchen, NJ), powdered sampies were passed through a Na2C2OJH2c.O. Heumi and Wada (1976) c.u.Na20.S. (Tiron) Biermans and Baert (1977) 50-#Lmnylon sieve. When further fractionation was required, Na.P20, McKeague (1967) as in the case of gibbsite, goethite, and hematite, the sampies NH2OH.HClIHa Chao and Zhou (1983) were suspended in water and fractionated using a sedimen- Reducing tation method without centrifugation. The fine-silt (2-5 #Lm) Reducing plus Na,CJisO,lNaHCO,J Mebra and Jackson (1960) and day «2 #Lm)fractions were freeze-dried. All other frac- complexin& Na2S.0. K2C2OJH2C2OJMg Jeffiies (1946) tionated sampies were dried at 60°C in an oven. The ground (NH.)2C2OJH2C2OJ Ducbaufour and Souchier (1966) silicate minerals were prepared by dry grinding for 96 to 180 Na.g.O. h using a mechanical grinder. This procedure was followed to obtain partially noncrystalline specimens of known com- positions (Kodama and Jaakimainen, 1982). Before use, the distinctive merit in this method, inc1uding a high ef- ground sampies were dried overnight at 110°C in an oven. ficiency equivalent to that obtained by a combination Synthetic materials and two ferrihydrite sampies were used of other extraction methods. Therefore, several ex- as obtained or received, since they were already in a fine traction procedures may simply be replaced by a single powdery state. extraction with Tiron. The objective ofthis study was The Tiron method used in this investigation was modified to compare Tiron and other common extraction meth- from the method originally proposed by Biermans and Baert ods on a wide variety of materials.
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