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43.1.05 (c) Ground mustard or mustard flour.

Ignite as in (a) and heat


AOAC Official Method 941.12 30 min at 550C. Leach ash with hot H2O, filter, and wash
Ash of Spices thoroughly. Transfer paper and contents to ashing dish, dry, and heat
Gravimetric Methods in furnace 30 min. Remove dish, let cool, add 510 drops HNO3,
First Action 1941 evaporate to dryness, and heat in furnace 30 min. Repeat HNO3 and
Final Action heating treatment until residue is white. Add filtrate, evaporate to
A. Determination dryness, and heat in furnace 30 min. Cool, and weigh as in (a).
(a) Most spices.Weigh ca 2.000 g test portion Pt in flat-bottom Reference: JAOAC 24, 667(1941).
dish. Place dish in entrance of open furnace so that sample fumes off
without catching fire. Then ash 30 min at 550C, break up ash with B. Ash Insoluble in Acid
several drops H2O, evaporate carefully to dryness, and heat in furnace Boil residue from A in 25 mL HCl (2 + 5) 5 min, covering dish
30 min. If previous wetting showed ash to be C-free, remove dish to with watch glass to prevent spattering; collect insoluble matter on
desiccator containing fresh, efficient desiccant [H2SO4 or anhydrous Gooch or ashless filter, wash with hot water until washings are
Mg(ClO4)2 is satisfactory], let cool to room temperature, and weigh acid-free, ignite until C-free, cool, and weigh.
soon. If first wetting showed C, repeat wetting and heating until no
specks of C are visible; then heat 30 min after disappearance of C. If C C. Calcium in Ash
persists, leach ash with hot H2O, filter through quantitative paper, Ignite 24 g test portion as in A, digest with hot HCl (2 + 5),
wash paper thoroughly, transfer paper and contents to ashing dish, evaporate to dryness, moisten dry residue with dilute HCl, and again
dry, and ignite at 550C until ash is white. Cool dish, add filtrate, evaporate to dryness to make SiO2 insoluble. Treat residue with
evaporate to dryness on steam bath, and heat in furnace 30 min. Cool, 510 mL HCl, add ca 50 mL H2O, let stand on water bath few
and weigh as previously. minutes, fil ter, and wash in soluble res i due with hot water.
(b) Nutmeg, mace, ginger, and cloves.Proceed as in (a), but Determine CaO in combined filtrate and washings as in 910.01 (see
heat at 600C. 3.3.02).

2006 AOAC INTERNATIONAL

2005 AOAC INTERNATIONAL

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