37.1.
39
AOAC Official Method 910.03
Tartaric Acid (Total)
in Fruits and Fruit Products
Bitartrate Method
First Action 1910
Final Action
A. Apparatus
Device for filtering at 0°.—Use apparatus similar to that
described in 941.09E(d) (see 34.1.09).
B. Removal of Pectin
Take sample prepared as in 920.149 (see 37.1.07) with titratable
acidity ca 3 mL 1 N acid and solids content £20 g. Designate as x, mL
alkali required to neutralize sample. Adjust volume of sample to ca
35 mL by evaporation or by addition of H2O, add 3 mL 1 N H2SO4,
and heat to 50°. Transfer adjusted sample to 250 mL volumetric
flask, rinse with 10 mL hot water, and finally with alcohol; cool,
dilute to volume with alcohol, shake, and let stand overnight if
necessary, until pptd pectin separates, leaving clear liquid. Transfer
to centrifuge bottle, add 0.2 g filter-aid, shake vigorously,
centrifuge, and decant through retentive paper (cover funnel with
watch glass). Pipet 200 mL filtrate into centrifuge bottle.
If sample contains alcohol, esters of organic acids may be present,
and saponification is necessary. Adjust volume to 35 mL, add x +
3 mL 1 N KOH, heat to ca 60°, and let stand overnight. Add x + 6 mL
1 N H2SO4, transfer to 250 mL volumetric flask, and proceed as
above.
C. Determination
(Caution: See Appendix B, Hydrogen Sulfide.)
To solution in centrifuge bottle add vol. Pb(OAc)2 solution,
943.03 (see 37.1.40), equal to x + 3 mL, or if saponification was
made, x + 6 mL, and 0.2 g filter-aid; shake vigorously 2 min and
centrifuge. Test supernate with few drops of the Pb(OAc)2 solution
and if ppt forms, add additional Pb(OAc)2 solution, shake, and again
centrifuge. Decant and let drain thoroughly by inverting bottle
several minutes. To material in centrifuge bottle add 50 mL 80%
alcohol, shake vigorously to disperse ppt, add 150 mL more 80%
alcohol, shake, centrifuge, decant, and drain.
To Pb salts in centrifuge bottle add ca 150 mL H2O, shake
thoroughly, and pass in H2S to satn. Unsatn is indicated by presence
of partial vac. obtained by stoppering bottle, shaking, and observing
partial vac. when carefully removing stopper. Transfer to 250 mL
volumetric flask, dilute to volume with H2O, and filter through
folded paper. Transfer 100 mL clear filtrate to 250 mL I flask, tared
with 2 or 3 glass beads. (Harvard trip balance sensitive to 0.1 g is
convenient.) Evaporate on gauze over flame to ca 30 mL, remove
from flame, add second 100 mL aliquot, and evaporate to 19 ± 0.5 g.
Neutralize with 30% KOH solution, 1 drop at time, using phthln, and
add one drop alkali in excess. Add 2 mL HOAc and 0.2 g filter-aid
(Celite 545 is satisfactory), and slowly, with agitation, add 80 mL
95% alcohol. Cool in cracked ice-salt mixture, shake vigorously
2 min, place in refrigerator, and hold overnight at 0°.
Cover filtering disk, A, with thin layer of asbestos and place over
it thin layer of filter-aid. Place cracked ice in outer funnel, wash
filter mat with ice-cold alcohol, and let stand few minutes to cool
filter thoroughly. Swirl flask to suspend filter-aid and ppt, and filter
at 0°, sucking mat dry. (Use filtrates and washings for L-malic acid
determination.) Wash stopper with ca 15 mL ice-cold alcohol,
letting wash liquid run into pptn flask. Stopper and shake to wash
flask well. Stirring rod bent at 45° angle 2.5 cm from end helps in
washing inside of filter tube. Conduct wash liquid completely
around inside of filter tube and suck dry. Wash flask and filter tube
with two 15 mL portions ice-cold 80% alcohol. While filtering, keep
flask cold with cracked ice. Remove ice from outer funnel and
transfer ppt and glass fiber filter to pptn flask with boiling CO2-free
H2O. Heat almost to bp and titrate with 0.1 N alkali, using phthln.
1 mL 0.1 N alkali =
0.015 g tartaric acid
Tartaric acid/0.64 = tartaric acid in sample taken
References: Bull. Soc. Chim. 7, 567(1910); 11, 886(1912).
JAOAC 8, 637(1925); 13, 103(1930); 36, 266(1953).
Method was modified as follows: Replace “asbestos pad” with “glass fiber
filter.”
Revised: March 1996
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