11.1.
28
AOAC Official Method 920.201
Barium in Water
First Action 1920
Final Action
(It is not necessary to look for Ba if sulfate is present in appreciable
amount unless the water contains large amount of bicarbonate or
chloride, which may hold in solution small amounts of both sulfate and
Ba.)
Gravimetric Method
A. Reagents
(a) Ammonium dichromate solution.—Dissolve 100 g of the
SO4-free salt in H2O and dilute to 1 L.
(b) Ammonium acetate solution.—Dissolve 300 g of the salt in
H2O, neutralize with NH4OH, and dilute to 1 L.
(c) Dilute ammonium acetate wash solution.—Dilute 20 mL
(b) to 1 L. (Reaction of acetate solutions should be alkaline rather
than acid.)
B. Determination
Acidify 1–5 L test portion with HCl and con centrate to ca
200 mL. (If precipitate forms, fil ter off and test for Ba.) Add ca
0.5 g NH4Cl, and precipitate Fe and Al with NH4OH. Boil, filter,
and wash. To filtrate, add excess (10 mL) NH4CH3COO solution,
(b), keeping total volume ca 200 mL. Heat to bp, and add, with
stirring, ca 5 mL (NH4)2Cr2O7 solution. Let settle and cool.
De cant clear liq uid through fil ter and wash pre cip i tate by
decantation with dilute NH4CH3COO solution until filtrate is no
longer perceptibly colored (ca 100 mL wash solution).
Place beaker under funnel, dissolve precipitate on pa per with
warm HNO3 (1 + 1), using as little as possible, and wash paper.
Add little more acid to dissolve precipitate in beaker, and then
NH4OH until precipitate that forms no longer redissolves. Heat to
bp; add, with stirring, 10 mL NH4CH3COO solution, (b), and
2 mL (NH4)2Cr2O7 solution; let cool slowly, and wash precipitate
free of chromate with di lute NH 4 CH 3 COO so lu tion by
decantation and filtration. Dry precipitate, ignite moderately to
constant weight, and weigh as BaCrO4. Calculate as Ba, using
factor 0.5421.
References: Morse, “Exercises in Quantitative Chemistry,”
p. 417.
JAOAC 4, 86(1920).
Titrimetric Method
C. Determination
Proceed as in B through “. . . wash precipitate free of chromate
with di lute NH 4 CH 3 COO so lu tion . . . ” (af ter sec ond
precipitation). Dissolve precipitate in ca 10 mL HCl (1 + 1) and
hot water. Wash filter, dilute solution to ca 400 mL, and add ca
50 mL freshly prepared 10% KI solution. Mix carefully and
titrate liberated I2 after 3 or 4 min with 0.1M Na2S2O3. 1 mL 0.1M
Na2S2O3 = 4.578 mg Ba.
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