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84-011 ACID AH4OIVIuH.

OXALATE extractable Fe and Al (Mn and Si if desired)

1. Application

1.1 This method is applicable to the determination of amorphous

inorganic Fe and Al and organic complexed Fe and Al from soils.
It attacks most silicate minerals and goethite and hematite only
slightly, but it dissolves magnetite and finely divided,
easily-weathered silicates such as olivine to a considerable
extent.

2. Apparatus

2.1 Disposable culture tubes (16 x 125 mm)

2.2 Eppendorf pipette and disposable tips

2.3 Repipet dispensing bottles (accuracy 15, reproducibility 0.1%)

2.4 End-over-end shaker (40 - 50 rpm)

2.5 Atomic Absorption Spectrophotometer (Model 1200 Varian Techtron)

2.6 Centrifuge (IEC Low Speed)

3. Reagents

3.1 Acid oxalate extracting solution

A. 0.2 M Ammonium oxalate (NH4)2 C2O4.H2O: Dilute 28.3 g

of ammonium oxalate to 1 liter in a volumetric flask with
distilled water.

B. 0.2 M Oxalic acid (H2C204.2H20): Dilute 25.2 g of oxalic

acid to 1 liter in a volumetric flask with distilled water.

cm Extracting solution: Mix 700 mL of A and 535 mL of B, check pH

and adjust to 3.0 by adding either A or B.

3.2 Sodium chloride (2000 ug/mL): Dilute 5.084 g of sodium chloride

to 1 liter in a volumetric flask with distilled water.

3.3 Certified atomic absorption standards + 1%.

4.Procedur-e

4.1 Extraction

4.1.1 Weigh 0.250 g of soil ground to pass a 35 mesh sieve into a 15

mL disnosable test tube.
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4.1.2 Use a repipet dispensing bottle and add 10 mL of the acid oxalate I_

solution and stopper the tube tightly.

4.1.3 Place the tubes in an end-over-end shaker and shake for four (4)
hours (the extraction has to be done in the dark).

4.1.4 Centrifuge the tubes for 20 minutes at 510 G and decant the clear
centrifugate into a suitable container (disposable scintillation
vials, handiclean) and store for analysis within a few days.

4.2 Determination

4.2.1 Dilute the extracts (1 mL of extract and 4 mL NaCl solution) to

give a convenient concentration.

4.2.2 The matrix of the standard solutions should also contain the same
concentration of acid oxalate extracting solution as the dilutions
and Na at 2000 pg/mL to suppress interferences.

4.2.3 Extracts containing suspended material should be filtered.

4.2.4 An air-acetylene flame is suitable for the determination of Fe and

Mn, and a nitrous oxide-acetylene flame for Al.

4.2.5 Calorimetric methods can be used to determine Fe, Al and Si if

desired (McKeague ed. 1978).

5. Calculations

5.1 % Fe, Al, Mn = ug/mL in final sol'n x extractant (mL) x dil x 100
wt. of soil (mg) x 1000

5.2 For 0.250 g of soil, 10 mL of extractant, 5 x dilution and 12.0

pg/mL of Fe determined

% Fe q 12.0 x 10 x 5 x 100
250 x 1000

= 0.24

6. Precision

6.1 In the LRRI analytical service lab, the coefficients of variation

at Fe levels of 2.7% and Al at levels of 1.2% were 4.5% and 5.0%
respectively.

7. References

7.1 Baril, R. and Bitton, G. 1967. Anamalous values of free iron in

some Quebec soils containing magnetite. Can. J. Soil Sci. 47,261.

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7.2 Blume, H.P. and Schwertmann, U. 1969. Genetic evaluation of

profile distribution of aluminum, iron, and manganese oxides. Soil
Sci. Sot. Am. Proc. 33, 438-444.

7.3 McKeague, J.A. and Day, J.H. 1966. Dithionite and

oxalate-extractableFe and Al as aids in differentiating various
classes of soils. Can. J. Soil Sci. 46, 13-22.

7.4 Schwertmann, W. 1964. The differentiation of iron oxide in soils

by a photochemical extraction with acid ammonium oxalate. Z.
Pflanzenernahr Dung. Bodenkunde, 105, 194-201.

7.5 Schwertmann, U. 1973. Use of oxalate for Fe extraction from

soils. Can. J. Soil Sci. 53, 244-246.

7.6 Webber, M.D., McKeague, J.A., Raad, A.T., DeKimpe, C.R., Wang, C.,
Haluschak, P., Stonehouse, H.B., Pettapiece, W.W., Osborne, V.E.
and Green, A.J. 1974. A comparison among nine Canadian
laboratories of dithionite -, oxalate -, and
pyrophosphate-extractableFe and Al in soils. Can. J. Soil sci.
54,293~298.
 Notes

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