2.5.

05
AOAC Official Method 955.06
Potassium in Fertilizers
Flame Photometric Method
Final Action
Surplus 1986

2.110

2.1082.113, 14th ed.

(Caution: See 51.007.)
2.108

Reagents and
Apparatus

(a) Ammonium oxalate soln.Dissolve 40 g

(NH4)2C2O4 in 1 L H2O.
(b) Methyl red indicator.Dissolve 0.2 g Me red in
100 mL alcohol.
(c) Dilute nitric acid.(1 + 10).
(d) Anion exchange resin.REXYN 203(OH)
(Fisher Scientific Co.); Duolite A-7 or Duolite A-41
(Diamond Shamrock, 1100 Superior Ave, Cleveland,
OH 44114); permutit S-100 (Permutit Co., E49
Midland Ave, Paramus, NJ 07652); or equiv.
(e) Potassium nitrate or potassium chloride.
Recrystallize reagent grade salt twice from H2O and
dry 5 hr at 105E.
(f) Ion exchange column.Made from 30 cm length
of std wall glass tubing, 2.5 cm od; one end closed by
1-hole No. 4 rubber stopper thru which is inserted 2way stopcock or glass tubing connected to rubber
tubing and compressor clamp. Do not let stopcock
tubing protrude above stopper. Choose stopper large
enough so that there is no space between stopper
vertex and column wall. Alternatively use glass
chromatgc tube 300 19 mm id with stopcock or
valve at bottom to control flow rate (such as SGA
Scientific Inc. No. C4225).
Place glass wool plug in bottom of tube, close
valve, and add H2O to ht of 10 cm. Transfer portion of
resin to
200 mL beaker and suspend in H2O. Transfer slurry to
column and adjust ht of packed resin to 20 cm,
draining
excess H2O until 2.5 cm head remains. Regenerate
resin after 10 successive aliquots have passed thru.
For Na, regenerate after 5 aliquots have passed thru.
2.109

NaOH twice, decanting NaOH soln after final

treatment. Add 2 L H2O to resin, stir few min, let
resin settle, and decant wash H2O. Repeat 34 times.
Resin is now in free base form. Regenerate to nitrate
form by treating 3 times with HNO3 (1 + 19), in same
manner as with NaOH soln. Wash resin with H2O
until pH of washings is $2 by backwashing in column
or by stirring and decanting in large beaker. Store
resin under H2O in stoppered bottle.

Preparation of Resin

Place ca 450 g resin in 4 L beaker and add 2 L 5%

NaOH. Stir 30 min with elec. stirrer. Let resin settle,
and decant NaOH soln. Repeat treatment with 5%

Preparation of Solution

(a) Mixed fertilizers and potassium-magnesium

sulfate.Weigh 1.5058 g sample into 250 mL vol.
flask (500 mL flask if sample contains >30% K2O),
add
125 mL H2O and 50 mL (NH4 )2 C2 O4 soln, and boil 30
min. Cool, dil. to vol., mix, and pass thru dry filter.
(b) Potassium chloride and sulfate.Dissolve
1.5058 g in H2O and dil. to 500 mL.
2.111

Preparation of Standard Curve

Dissolve 1.2931 g KNO3 (or 0.9535 g KCl) in H2 O

and dil. to 500 mL (1000 ppm K). Prep. std solns by
diln to cover range 080 ppm K at intervals #10 ppm,
adding appropriate amt LiNO3 if internal std
instrument is to be used. Prep. std curve of emission
against concn, adjusting instrument so that 50 ppm K
gives reading near mid-scale. Atomize portions of std
solns until readings for series are reproducible.
2.112

Determination

(a) Mixed fertilizers, potassium sulfate, and

potassium-magnesium sulfate.Transfer 10 mL aliquot
of sample soln to 250 mL beaker. Add 1 drop Me red
and neutze with HNO3 (1 + 10). Adjust H2 O level in
column to top of resin and quant. transfer aliquot to
column. Open stopcock to give flow rate of 2
drops/sec, collecting effluent in 250 mL vol. flask.
Wash aliquot into resin with 23 small portions H2 O.
Collect 5075 mL effluent; then open stopcock and
collect addnl 100 mL by pouring H2O onto column,
making certain that H2O level does not fall below top
of resin bed. Dil. to vol. and mix (if internal std
instrument is used, add
required amt LiNO3 before dilg to vol.). Atomize
portions of sample several times to obtain reliable av.
reading for each soln. Det. ppm K from std curve.
(Temp. of std and sample solns must not differ by
>2E.) Calc. % K2O as follows:
030%: ppm K/2 = %K2O
>30%: ppm K/1 = %K2O
(b) Potassium chloride.Proceed as in (a) but omit
neutzn and resin treatment.

2.113

Instrument and Procedure

Performance Test

Weigh 1.5058 g K acid phthalate (primary std;

%K2O
= 23.0) and transfer to 250 mL vol. flask. Add ca 0.5 g
(NH4)2HPO4 and proceed as in 2.110(a), beginning "...
add 125 mL H2O ..."
Refs.: J. Agric. Food Chem. 3, 48(1955). JAOAC 41,
533(1958); 51, 857(1968).
CAS-7440-09-7 (potassium)
AOAC INTERNATIONAL