Assay of Ferrous Fumarate Conical Flask

Principles Involved 500 mg ferrous fumarate

Type of titration: Direct cerimetry with preliminary
treatment and blank Dilute HCl
Heat to boiling determination
SnCl2 in HCl (dropwise, excess)
Cool to room temp
Type of reaction: Redox reaction
Titrant used: 0.1 N Ceric sulfate MgCl2
Indicator: Orthophenanthroline TS
Endpoint: red (ferroin) to pale blue (ferrin) solution
Water

Pharmaceutical/Medical Use Dilute H2SO4

1. Used as haematinic (stimulates the production
of red blood cells or increases the amount of H3PO4
hemoglobin in the body)
2. Used in the treatment of Iron deficiency anemia O-phenanthroline TS

3. For the prevention of iron deficiency in Red Titrate

0.1 N Ce(SO4)2
pregnancy

Schematic Diagram Faint/Pale Blue Solution

Procedure + RFIS + Discussion

1. Conical flask
 used in order to limit exposure to atmospheric
oxygen that may oxidize the ferrous ion to ferric
ion via the ff reaction:
4Fe2+ + O2 + 4H+  4Fe3++ 2H2O
2. Dilute HCl
 Dissolve ferrous fumarate and to liberate fumaric
acid in the sample
FeC2H2(CO2) + HCl → FeCl2 + C2H2(CO2H)2
 Ferrous salts are more prone to oxidation in
neutral or basic solutions
 Dilute solution is used since Ce (IV) solutions
are unstable if the HCl concentration is more
than 1 M
3. Heat to boiling + SnCl2 in HCl (dropwise,
excess)
 Heat to boiling to increase the rate of
formation of fumaric and to remove
dissolved O2 and CO2 from the analyte
 SnCl2 in dilute HCl
o Pre-reducing agent that reduces any
Fe3+ in the analyte to Fe2+
o Add in excess to ensure that all the
iron in the solution is in the reduced
state Fe2+
4. Cool + HgCl2
 HgCl2 is added to remove excess SnCl2
which can consume some of the titrant
because of its identity as a reducing agent
PH CH 135-IPB AALA, JUDAN, ORDONEZ
 Sn2+ + 2HgCl2 →Sn4+ + Hg2Cl2 + 2Cl Volume of 0.1 N Ce(SO4)2
5. H2O + Dilute H2SO4 + H3PO4 + O- = Vactual – Vblank
phenanthroline TS = 18.90 mL – 0.75mL
 Dilute H2SO4 and H3PO4 - acidify the = 18.15 mL
analyte and to complex with any possible
Fe3+ Amount of C2H2FeO4:
 Phosphoric acid - prevent oxidation of Cl- 1L 0.1≡. Ce ( SO 4 ) 2 1≡. C 2
which is a possible interference in the assay
18.15 mL Ce ( SO 4 ) 2 x x x
1000 mL 1 L Ce ( SO 4 ) 2 1≡. Ce
 The indicator is a complex of Fe2+ with = 0.3084 g C2H2FeO4
1,10-phenanthroline; the Fe2+ component of
the indicator can be oxidized by ceric sulfate % w/w C2H2FeO4:
to indicate the endpoint of the titration
g of C 2 H 2 FeO 4
6. Blank determination ¿ x 100
g of sample
 Accounts other variables that may interfere
in the assay, specifically any Fe2+ 0.3084 g
¿ x 100
consumed by the reagents added 0.3512 g
= 87.81 %
Chemical Equation Involved
References
2+
Oxidation: Fe → Fe + e3+ - Bothara, K. (2007). Inorganic Pharmaceutical Chemistry
Reduction: Ce4+ + e- → Ce3+ (9th ed.) Pune: Nirali Prakashan, p.11-7
Net: Fe2+ + Ce4+→ Fe3+ + Ce3+
Molecular: FeC4H2O4 + Ce(SO4)2 → Fe2(SO4)3 + Knevel, A. M., & DiGangi, F. E. (1977). Jenkins’
Ce2(C4H2O4)3 Quantitative Pharmaceutical Chemistry (7th ed.) New
York: McGraw-Hill Book Company, p. 170.
Factor: 1 (since 1 e- is released, and the oxidation state
of iron changed from 2+ to 3+) National Institutes of Health (n.d.). NCI Drug Dictionary:
Ferrous fumarate. Retrieved on October 16, 2017
Sample Computations from
Prelab Computation: https://www.cancer.gov/publications/dictionaries/cancer-
drug?cdrid=755248
MW (reagent )
wt .=NT x VT
f
g
169.9013
mol
wt .=0.1 N x 0.03 L
1
¿ 0.5097 gof Ferrous fumarate
Postlab Computation:

% AI = ¿ ¿

Word Problem:

The amount of Ferrous Fumarate in a 0.3512 g sample

was determined by a redox titration with Ce(SO 4)2.
Titration to a faint blue end point with
orthophenanthroline TS required 18.90 mL of 0.1 N
Ce(SO4)2. The blank solution required 0.75mL of the
titrant. Report the content of the tablet as % w/w
C4H2FeO4. What can you say about the quality of the
sample?

PH CH 135-IPB AALA, JUDAN, ORDONEZ