Disodium Salt Tests For Detecting Fe%

SODIUM IRON (III) ETHYLENEDIAMINETETRAACETATE, TRIHYDRATE

Prepared at the 53rd JECFA (1999) and published in FNP 52 Add 7 (1999),
superseding specifications prepared at the 41st JECFA (1993), published in
FNP 52 Add 2 (1993). Evaluated as safe for use in supervised food
fortification programmes at the 53rd JECFA (1999)

SYNONYMS Ferric sodium edetate, sodium iron EDTA, sodium feredetate

DEFINITION
Chemical names Sodium [[N,N'-ethanediylbis[N-(carboxymethyl) glycinato]] (4-)] ferrate(1-);
sodium [(ethylenedinitrilo) tetraacetato]ferrate(1-); Sodium iron (III)
ethylenediaminetetraacetate
C.A.S. number 15708-41-5
Chemical formula C10H12FeN2NaO8 · 3H2O
Structural formula
Formula weight 421.09 (trihydrate)
Assay Not less than 12.5% and not more than 13.5% iron, calculated on the basis
of the trihydrate. Not less than 65.5% and not more than 70.5% EDTA,
calculated on the basis of the trihydrate.
DESCRIPTION Light yellow coloured powder that is relatively stable and unaffected by
storage
FUNCTIONAL USES Nutrient supplement
CHARACTERISTICS
IDENTIFICATION
Solubility (Vol. 4) Soluble in water
Test for iron (Vol. 4) Passes test
Test for sodium (Vol. 4) Passes test
PURITY
pH (Vol. 4) 3.5 - 5.5 (1 in 100 soln)

Water-insoluble matter Not more than 0.1%
Weigh accurately 5 g of sample and transfer into 100 ml water. Stir until
dissolved. Place a filter paper (1 µm porosity, maximum) in a Gooch
crucible (3.5-4.0 cm) and seat the paper by applying vacuum while washing
with water. Dry the crucible at 175o for 15 min, cool in a desiccator, and
weigh. Pour sample solution through the crucible and wash with three
successive 10 ml portions of water. Dry the crucible at 110o for one hour.
Cool in a desiccator and weigh the crucible. Calculate as percentage.
Nitrilotriacetic acid Not more than 0.1%

See description under TESTS
Arsenic (Vol. 4) Not more than 1 mg/kg

Test 3 g of the sample as directed in the Limit test (Method II)
Lead (Vol. 4) Not more than 1 mg/kg

Determine using an atomic absorption technique appropriate to the
specified level. The selection of sample size and method of sample
preparation may be based on the principles of the method described in
Volume 4, “Instrumental Methods.”
TESTS
PURITY TESTS
Nitrilotriacetic acid Mobile Phase Add 10 ml of a 1 in 4 solution of tetrabutylammonium

hydroxide in methanol to 200 ml of water, and adjust with 1 M phosphoric
acid to a pH of 7.5 ± 0.1. Transfer the solution to a 1000-ml volumetric flask,
add 90 ml of methanol, dilute with water to volume, mix, filter through a
membrane filter (0.5-µg or finer porosity), and degas.
Ammonium hydroxide blank solution Add 0.5 ml of ammonium hydroxide to

a 10 ml volumetric flask. Dilute with water to volume.
Stock Standard Solution Transfer about 100 mg of nitrilotriacetic acid,

accurately weighed, to a 10-ml volumetric flask, and add 0.5 ml of
ammonium hydroxide, and mix. Dilute to volume, and mix.
Standard Preparation Transfer 1.0 g of the sample to a 100-ml volumetric

flask. Add 100 µl of the Stock Standard Solution, dilute with water to
volume, and mix. Sonicate, if necessary, to achieve a complete solution.
Test Preparation Transfer 1.0 g of the sample to a 100-ml volumetric flask.

Add 100 µl of Ammonium hydroxide blank solution and dilute with water to
volume, and mix. Sonicate, if necessary, to achieve complete solution.
Chromatographic System (see High-Pressure Liquid Chromatography, in

General Methods (Guide to JECFA Specifications), FNP 5/Rev. 2 (1991)).
The chromatograph is equipped with a 254-nm detector and a 4.6-nm × 15-
cm column that contains 5- 10-µm porous microparticles of silica to which is
bonded octylsilane (Zorbax 8 or equivalent). The flow rate is about 2 ml/min.
Chromatograph three replicate injections of the Standard Preparation, and
record the peak responses as directed under Procedure. The relative
standard deviation is not more than 2.0%, and the resolution factor between
nitrilotriacetic acid and sodium iron EDTA is not less than 4.0.
Procedure Separately inject equal volumes (about 50 µl) of the Standard

Preparation and the Test Preparation into the chromatograph, record the
chromatograms, and measure the responses for the major peaks. The
retention times are about 3.5 min for nitrilotriacetic acid and 11.9 min for
sodium iron EDTA. The response of the nitrilotriacetic acid peak of the Test
Preparation does not exceed the difference between the nitrilotriacetic acid
peak responses obtained from the Standard Preparation and the Test
Preparation.
METHOD OF Iron
ASSAY Dissolve the sample (approx. 0.5 g accurately weighed) in distilled water (40
ml) in an iodine flask. Add concentrated hydrochloric acid (20 ml) mix, add
potassium iodide (3 g) and then allow to stand for 5 min.
Titrate the liberated iodine with standardised 0.1 M sodium thiosulfate, using
starch solution as indicator. Avoid vigorous mixing during the titration.
Perform a blank, omitting the sample.
where
Ts = sample titre in ml
Tb = blank titre in ml
0.05585 = atomic weight of iron × 10-3
M = molarity of sodium thiosulfate
W = sample weight (g)
EDTA
Reagents
(1) 0.25 M calcium acetate solution, standardized - Weigh and transfer 44.0
g reagent grade calcium acetate monohydrate to a 1 L volumetric flask; add
water to dissolve and fill to the mark. Weigh accurately 2.0 to 2.1 g of
reagent grade EDTA acid into each of three 250-ml conical flasks. Add 150
ml water and adjust to pH 11-12 (pH paper may be used) with 50% sodium
hydroxide solution. Add about 30 mg of hydroxynaphthol blue indicator and
titrate with calcium acetate to a sharp red endpoint.
(2) Triethanolamine, reagent grade. (3) Hydroxynaphthol Blue indicator. (4)

50 % sodium hydroxide solution.
Procedure
Accurately weigh 0.8 - 1.0 g of sample into a 250-ml beaker. Add 75 ml of
distilled water to dissolve. Adjust the pH to 9.0 by dropwise addition of
triethanolamine. Then adjust to pH 12.5 - 13.0 by addition of 50% aqueous
NaOH. The solution should be clear and colourless. Add about 30 mg
hydroxynaphthol blue indicator and titrate with 0.25 M calcium acetate
solution to a red endpoint.

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SODIUM IRON (III) ETHYLENEDIAMINETETRAACETATE, TRIHYDRATE

SYNONYMS Ferric sodium edetate, sodium iron EDTA, sodium feredetate

C.A.S. number 15708-41-5

Chemical formula C10H12FeN2NaO8 · 3H2O

Formula weight 421.09 (trihydrate)

FUNCTIONAL USES Nutrient supplement

Solubility (Vol. 4) Soluble in water

Test for iron (Vol. 4) Passes test

Test for sodium (Vol. 4) Passes test

pH (Vol. 4) 3.5 - 5.5 (1 in 100 soln)

Nitrilotriacetic acid Not more than 0.1%

Arsenic (Vol. 4) Not more than 1 mg/kg

Lead (Vol. 4) Not more than 1 mg/kg

Nitrilotriacetic acid Mobile Phase Add 10 ml of a 1 in 4 solution of tetrabutylammonium

Ammonium hydroxide blank solution Add 0.5 ml of ammonium hydroxide to

Stock Standard Solution Transfer about 100 mg of nitrilotriacetic acid,

Standard Preparation Transfer 1.0 g of the sample to a 100-ml volumetric

Test Preparation Transfer 1.0 g of the sample to a 100-ml volumetric flask.

Chromatographic System (see High-Pressure Liquid Chromatography, in

Procedure Separately inject equal volumes (about 50 µl) of the Standard

(2) Triethanolamine, reagent grade. (3) Hydroxynaphthol Blue indicator. (4)

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