44.1.

16
AOAC Official Surplus Method 906.03i
i
Invert Sugar in Sugars and Sirups

References:

J. Am. Chem. Soc. 28, 663(1906);

26, 541(1907). J. Res. Natl. Bur.
Standards 24, 589(1940).

Munson-Walker General Method

Determination of Reduced Copper

Final Action
Surplus 1989

By Direct Weighing of Cuprous Oxide

31.039

31.037
Reagents
Asbestos.Digest asbestos, amphibole variety
(Caution: See Appendix B: Asbestos), with HC1
(1 + 3) 23 days. Wash acid-free, digest similar period
with 10% NaOH soln, and then treat few hr with hot
alk. tartrate soln, 923.09(A)(b)(alk. tartrate solns that
have stood for some time may be used for this purpose).
Wash asbestos alkali-free; digest several hr with HNO3
(1 + 3); and after washing acid-free, shake with H2O
into fine pulp. In prepg gooch, make film of asbestos 6
mm thick and wash thoroly with H2O to remove fine
particles. If pptd Cu2O is to be weighed as such, wash
crucible with 10 mL alcohol and then with 10 mL ether;
dry 30 min at 100E, cool in desiccator, and weigh.
Other reagents and solns used are described in
923.09(A). Solns may be clarified by neut. Pb(OAc)2
soln, 925.46(B)(d)(never basic Pb(OAc)2). Remove
excess Pb with dry Na oxalate.
31.038
Precipitation of Cuprous Oxide
Transfer 25 mL each of CuSO4 and alk. tartrate solns
to 400 mL beaker of alkali-resistant glass and add 50
mL reducing sugar soln; or if smaller vol. of sugar soln
is used, add H2O to make final vol. 100 mL. Heat
beaker on asbestos gauze over Bunsen burner, regulate
flame so that boiling begins in 4 min, and continue
boiling exactly 2 min. (It is important that these
directions be strictly observed. To regulate burner for
this purpose it is advisable to make preliminary tests,
using 50 mL reagent and 50 mL H2O, before
proceeding with actual detn. Elec. heater may be used
instead of burner.) Keep beaker covered with watch
glass during heating.
Filter hot soln at once thru asbestos mat in porcelain
gooch, using suction. Wash ppt of Cu2O thoroly with
H2O at ca 60E and either weigh directly as CuO,
929.09i
i (See 44.1.17), or det. amt of reduced Cu by
one of methods described in 929.09i
i (See 44.1.17).
Conduct blank detn, using 50 mL reagent and 50 mL
H2O, and if wt Cu 2O obtained is >0.5 mg, correct result
of reducing sugar detn accordingly. Alk. tartrate soln
deteriorates on standing, and wt Cu2O obtained in blank
increases.

Determination

(Use only for detns in solns of reducing sugars of

comparatively high purity. In products contg large amts
of mineral or org. impurities, including sucrose, det. Cu
in the Cu2O by one of methods described in 929.09i
i,
since the Cu2O is likely to be contaminated with foreign
matter.)
Prep. gooch as in 929.09i
i. Collect pptd Cu2O on
matt as in 929.09i; wash thoroly with hot H2O, then
with 10 mL alcohol, and finally with 10 mL ether. Dry
ppt 30 min in over at 100E, cool, and weigh. Obtain wt
invert sugar equiv. to wt Cu2O from 940.39.
Number of mg Cu2O reduced by given amt of
reducing sugar varies, depending upon whether or not
sucrose is present. In table, absence of sucrose is
assumed except in entries under invert sugar and
lactose, where, in addn to columns for these alone,
columns are given for their mixts with sucrose in
specified ratios in the case of lactose adn in specified
amts of total sugar in 50 mL soln in the case of invert
sugar.
(Later Hammon table has replaced original MunsonWalker table, where applicable.)
By Titration with Sodium Thiosulfate
31.040

Reagent

Thiosulfate std soln.Prep. soln contg 39 g

Na2S2O3.5H2O/L. Accurately weigh 0.2-0.4 g pure
electrolytic Cu and transfer to 250 mL erlenmeyer
roughly marked at 20 mL intervals. Dissolve Cu in 5
mL HNO3 (1+1), dil. to 20 or 30 mL, boil to expel red
fumes, add slight excess ssatd Br-H2O, and boil until Br
is completely removed. Cool, and add 10 mL NaOAc
soln (574 g trihydrate/L). Prep. 42 g/100 mL KI soln
made very slightly alk. to avoid formation and oxidn of
HI. Add 10 mL of the KI soln and titr. with Na2S2O3
soln to light yellow. Add enough starch indicator,
922.03(f), to produce marked blue. As end point nears,
add 2 g KSCN and stir until completely dissolved.
Continue titrn until ppt is perfectly white. 1 mL
Na2S2O2 soln - ca 10 mg Cu.
It is essential for Na2S2O2 titrn that concn of KI in
soln be carefully regulated. If soln contains <320 mg

2
Cu, at completion of titrn 4.2-5 g KI should have been
added for each 100 mL totl soln. If greater amts of Cu
are present, add KI soln slowly from buret with const
agitation in amts proportionately greater.
31.041

Determination

Wash pptd Cu2O, cover gooch with watch glass, and

dissolve the Cu2O with 5 mL HNO
(1+1) directed
3
under watch glass with pipet. Collect filtrate in 250 mL
erlenmeyer roughly marked at 20 mL intervals, and
wash watch glass and gooch Cu-free. Proceed as in
929.09i
i, beginning, ...boil to expel red fumes, ...
Obtain wt reducing sugar equiv. to wt Cu from 940.39.
Refs.: JAOAC 12, 38(1929); 18, 83(1935). J. Am.
Chem. Soc. 57, 845(1935). Anal. Chem. 21, 975(1949).
By Titration with Potassium Permanganate
31.042

Reagents

(a) Potassium permanganate std soln.Approx.

0.1573N, and contg 4.98 g/L. Prep. and stdze as in
940.35, using 0.35 g Na oxalate.
(b) Ferric sulfate soln.Dissolve 135 g
FeNH4(SO4)2.12H2O or 55 g anhyd. Fe2(SO4)3 in H2O,
and dil. to 1 L. Det. Fe2(SO4)3 in stock supply by strong
ignition to Fe2O3. Titr. 50 mL Fe2(SO4)3 soln, acidified
with 20 mL 4N H2SO4, with MnnO4 soln, and use this
titer as 0-point correction.
(c) Ferrous phenanthroline indicator.Dissolve
0.7425 g o-phenanthroline.H2O in 25 mL 0.025M
FeSO4 soln (6.95 g FeSO4.7H2O/L).
31.043
Determination
Filter the Cu2O thru gooch, and wash beaker and ppt
thoroly. Transfer asbestos pad to beaker with glass rod.
Add 50 mL Fe2(SO4)3 soln and stir vigorously until
Cu2O is completely dissolved. Examine for complete
soln, holding beaker above eye level. Cu2O must be
quant. transferred; if necessary, immerse crucible in
soln and make sure adhering Cu2O is dissolved. remove
crucible with glass rod and wash with H2O. Add 20 mL
4N H2SO4 and titr. with std KmnO4 soln. As end point
approaches, add 1 drop ferrous phenanthroline
indicator. At end point, brownish soln changes to green.
Obtain wt reducing sugar equiv. to wt Cu from 940.39.

By Electrolytic Deposition from Nitric Acid Solution

31.044
Determination
Decant hot soln, 929.09i
i, thru asbestos mat in
gooch, and wash beaker and ppt thoroly with hot H2O.
Transfer asbestos mat from crucible to beaker with
glass rod and rinse crucible with 14 mL HNO3 (1+1),
letting rinsings flow into beaker. After Cu2O dissolves,
dil. to 100 mL, heat to bp, and continue boiling ca 5
min to remove oxides of N. Cool, filter, transfer to 250
mL beaker, and dil. to 200 mL. Add 1 drop 0.1N HC1
and mix thoroly.
For electrolysis use cylindrical electrodes of Pt
gauze, ca 4 and 5 cm diam., resp., and ca 4.5 cm high,
thoroly cleaned, ignited, cooled in desiccator, and
weighed. Insert electrodes in Cu soln so that surface of
cathode clears anode by $5 mm and both electrodes
almost touch bottom of beaker. Cover with split watch
glass to avoid loss by spattering. Electrolyze with
current of 0.2-0.4 amp of beaker and watch glass with
H2O, thus raising level of soln and exposing new
surface of cathode; if new surface shows deposit of Cu,
electrolysis is not complete.)
Without interrupting current, slowly lower beaker
and at same time wash electrodes with stream of H2O.
Immediately immerse electrodes in another beaker of
H2O and break current. (Siphon can be used for
washing, adding H2O as soln is removed. Diplacement
of HNO3 soln is complete when current ceases to flow.)
Rinse cathode with alcohol and dry few min in oven at
100E. Cool in desiccator and weigh.
Electrolyte may be stirred by rotating anode or mech.
stirrer. In this case, current may be increased to 1-2
amp, thus shortening time required for complete
deposition of Cu to ca 1 hr.
If extreme care is taken to avoid spattering, Cu2O can
be dissolved by letting HNO3 flow down walls of
crucible. Keep crucible covered as much as possible
with small watch glass. Collect filtrate in beaker, and
wash watch glass and tip of pipet with jet of H2O.
continue as above, beginning ...dil. to 100 mL,...
Obtain wt reducing sugars equiv. to wt Cu from 940.39.
Refs.: JAOAC 23, 558(1940). J. Res. Natl. Bur.
Standards, 22, 697(1939);RP1213.
CAS-8013-17-0 (invert sugar)
AOAC INTERNATIONAL

Refs.: J. Res. Natl. Bur. Standards 15, 493(1935); 19,

691(1937); RP 1057.