3.4.

14
AOAC Official Method 920.10
Sulfur in Plants
Sodium Peroxide Method
Final Action
(Caution: See Appendix B, safety notes on sodium peroxide.)
A. Preparation of Solution
Place 1.52.5 g sample in ca 100 mL Ni crucible and add 5 g
anhydrous Na
2
CO
3
. Mix thoroughly, using Ni or Pt rod, and moisten
with ca 2 mL H
2
O. Add Na
2
O
2
, ca 0.5 g at time, mixing thoroughly
after each addition, and continue until mixture becomes nearly dry
and quite granular (ca 5 g Na
2
O
2
). Place crucible over S-free flame
or electric hot plate and heat carefully, stirring occasionally, until
contents are fused. (If material ignites, determination is worthless.)
After fusion, remove crucible, let cool somewhat, and cover
hardened mass with more Na
2
O
2
to depth of ca 5 mm. Heat gradually
and finally with full flame until fusion again takes place, rotating
crucible occasionally to bring any particles adhering to sides into
contact with oxidizing material. Continue heating 10 min after fusion
is complete. Cool somewhat, place warm crucible and contents in
600 mL beaker, and carefully add ca 100 mL H
2
O. After initial
violent action ceases, wash material out of crucible, make slightly
acid with HCl (adding small portions at time), transfer to 500 mL
volumetric flask, cool, dilute to volume, and filter.
B. Determination
Dilute aliquot of prepared solution to ca 200 mL with H
2
O and
add HCl until ca 0.5 mL free acid is present. Heat to bp and add 10
mL 10% BaCl
2
solution dropwise with constant stirring. Continue
boiling ca 5 min, and let stand 5 h in warm place. Decant through
ashless paper or ignited and weighed Gooch. Add 1520 mL boiling
H
2
O to precipitate, transfer to filter, and wash with boiling H
2
O until
filtrate is Cl-free. Dry precipitate and filter, ignite, and weigh as
BaSO
4
. Weight precipitate 0.1374 = S.
References: USDA Bur. Chem. Bull. 105, p. 151; 116, p. 92; 137,
p. 30.
CAS-7704-34-9 (sulfur)
Copyright 1998 AOAC INTERNATIONAL