Dried Ferrous Sulfate
FeSO4·xH2O151.91
Sulfuric acid, iron(2+) salt (1:1), hydrate;
Iron(2+) sulfate (1:1) hydrate
[13463-43-9].
Anhydrous[7720-78-7].
FeSO4·xH2O151.91
Sulfuric acid, iron(2+) salt (1:1), hydrate;
Iron(2+) sulfate (1:1) hydrate
[13463-43-9].Anhydrous
[7720-78-7].DEFINITION
Dried Ferrous Sulfate contains NLT 86.0% and NMT 89.0% of anhydrous ferrous sulfate (FeSO4).
IDENTIFICATION
• A. Identification Tests—General, Iron, Ferrous Salts 
191
and Sulfate 191: Meets the requirements
191 and Sulfate 191: Meets the requirementsASSAY
• Procedure
Sample: 800 mg of Dried Ferrous Sulfate
Blank: Proceed as in the Analysis without the Sample.
Titrimetric system
(See Titrimetry 541.)
541.)Mode: Direct titration
Titrant: 0.1 N ceric sulfate VS
Endpoint detection: Visual
Analysis: Dissolve the Sample in a mixture of 25 mL of 2 N sulfuric acid and 25 mL of freshly boiled and cooled water. Add orthophenanthroline TS, and immediately titrate with the Titrant. Perform a blank determination.
Calculate the percentage of anydrous ferrous sulfate (FeSO4) in the Sample taken:
Result = {[(VS 
VB) × N × F]/W} × 100
VB) × N × F]/W} × 100| VS | = | = Titrant volume consumed by the Sample (mL) |
| VB | = | = Titrant volume consumed by the Blank (mL) |
| N | = | = Titrant normality (mEq/mL) |
| F | = | = equivalency factor, 151.9 mg/mEq |
| W | = | = Sample weight (mg) |
Acceptance criteria: 86.0%–89.0%
IMPURITIES
• Arsenic, Method I 211
211 Test preparation: Transfer 1 g of Dried Ferrous Sulfate to a round-bottomed, 100-mL flask fitted with a glass joint, and add 40 mL of sulfuric acid (1 in 2) and 2 mL of 300 mg/mL of potassium bromide solution. Immediately connect the flask to a condenser having a matching glass joint and a reservoir with a water jacket that is cooled by ice water. Heat the flask gently over a low flame until the solid dissolves, then distill until 25 mL of distillate collects in the reservoir. Transfer this distillate to the arsine generator flask, and wash the condenser and the reservoir with several small portions of water, adding the washings to the generator flask. Swirl to mix, add bromine TS until the color of the solution is slightly yellow, and dilute with water to 35 mL.
Acceptance criteria: NMT 3 ppm
• Limit of Lead
[Note—For the preparation of all aqueous solutions and for the rinsing of glassware before use, use water that has been passed through a strong-acid, strong-base, mixed-bed ion-exchange resin. Select all reagents to have as low a content of lead as practicable, and store all reagent solutions in containers of borosilicate glass. Cleanse glassware before use by soaking in warm nitric acid (1 in 2) for 30 min and by rinsing with deionized water. ]
Ascorbic acid–sodium iodide solution: 100 mg/mL of ascorbic acid and 192.5 mg/mL of sodium iodide
Trioctylphosphine oxide solution: 50 mg/mL of trioctylphosphine oxide in 4-methyl-2-pentanone
[Caution—This solution causes irritation. Avoid contact with eyes, skin, and clothing. Take special precautions in disposing of unused portions of solutions to which this reagent is added. ]
Standard solution: Transfer 5.0 mL of Lead Nitrate Stock Solution, prepared as directed in Heavy Metals 231, to a 100-mL volumetric flask. Dilute with water to volume. Transfer 2.0 mL of the resulting solution to a 50-mL volumetric flask. Add 10 mL of 9 N hydrochloric acid and 10 mL of water. Add 20 mL of Ascorbic acid–sodium iodide solution and 5.0 mL of Trioctylphosphine oxide solution, shake for 30 s, and allow to separate. Add water to bring the organic solvent layer into the neck of the flask, shake again, and allow to separate. The organic layer is the Standard solution, and it contains 2 µg/mL of lead.
231, to a 100-mL volumetric flask. Dilute with water to volume. Transfer 2.0 mL of the resulting solution to a 50-mL volumetric flask. Add 10 mL of 9 N hydrochloric acid and 10 mL of water. Add 20 mL of Ascorbic acid–sodium iodide solution and 5.0 mL of Trioctylphosphine oxide solution, shake for 30 s, and allow to separate. Add water to bring the organic solvent layer into the neck of the flask, shake again, and allow to separate. The organic layer is the Standard solution, and it contains 2 µg/mL of lead.Sample solution: To a 50-mL volumetric flask add 1.0 g of Dried Ferrous Sulfate, 10 mL of 9 N hydrochloric acid, 10 mL of water, 20 mL of Ascorbic acid–sodium iodide solution, and 5.0 mL of Trioctylphosphine oxide solution. Shake for 30 s, and allow to separate. Add water to bring the organic solvent layer into the neck of the flask, shake again, and allow to separate. The organic layer is the Sample solution.
Blank: To a 50-mL volumetric flask add 10 mL of 9 N hydrochloric acid, 10 mL of water, 20 mL of Ascorbic acid–sodium iodide solution, and 5.0 mL of Trioctylphosphine oxide solution. Shake for 30 s, and allow to separate. Add water to bring the organic solvent layer into the neck of the flask, shake again, and allow to separate. The organic layer is the Blank, and it contains 0 µg/mL of lead.
Instrumental conditions
Mode: Atomic absorption spectrophotometry
Analytical wavelength: 283.3 nm
Lamp: Lead hollow-cathode
Flame: Air–acetylene
System suitability
Samples: Standard solution and Blank
Suitability requirements: The absorbance of the Standard solution and the absorbance of the Blank are significantly different.
Analysis
Samples: Standard solution, Sample solution, and Blank
Concomittantly determine the absorbances of the Blank, Standard solution, and the Sample solution. Use the Blank to set the instrument to zero.
Acceptance criteria: The absorbance of the Sample solution does not exceed that of the Standard solution (NMT 10 ppm).
• Mercury
[Note—Carry out this test in subdued light, because mercuric dithizonate is light sensitive. ]
Hydroxylamine hydrochloride solution, Standard mercury solution, Dithizone extraction solution, and Diluted dithizone extraction solution: Prepare as directed in Mercury 261, Method I.
261, Method I.Control solution: Mix 3.0 mL of Standard mercury solution, 30 mL of nitric acid (1 in 10), 5 mL of 250 mg/mL of sodium citrate solution, and 1 mL of Hydroxylamine hydrochloride solution.
Test preparation: Dissolve 1 g of Dried Ferrous Sulfate in 30 mL of nitric acid (1 in 10) with the aid of heat, on a steam bath. Cool quickly by immersing in an ice bath, and pass through a fine-porosity filter that previously has been washed with nitric acid (1 in 10) and water. To the filtrate, add 20 mL of 250 mg/mL of sodium citrate solution and 1 mL of Hydroxylamine hydrochloride solution.
Analysis: Adjust the Control solution to a pH of 1.8 with ammonium hydroxide and the Sample solution to a pH of 1.8 with sulfuric acid. Separately transfer the solutions to separators. Treat the Sample solution and the Control solution in parallel as follows.
Extract with two 5-mL portions of Dithizone extraction solution and 5 mL of chloroform, pooling the chloroform extracts in a second separator. Add 10 mL of hydrochloric acid (1 in 2), shake, allow the layers to separate, and discard the chloroform layer. Wash the acid extract with 3 mL of chloroform, and discard the washing. Add 0.1 mL of 20 mg/mL of edetate disodium solution and 2 mL of 6 N acetic acid, mix, and add slowly 5 mL of ammonium hydroxide. Close the separator, cool it under cold running water, and dry its outer surface. Remove the stopper, and pour the contents into a beaker. Adjust the Sample solution and the Control solution to a pH of 1.8 in the same manner as before, and return the solutions to their respective separators. Add 5.0 mL of Diluted dithizone extraction solution, shake vigorously, and allow the layers to separate. Using Diluted dithizone extraction solution as a color blank, compare the colors developed in the chloroform layers of the Sample solution and the Control solution.
Acceptance criteria: The color developed by the Sample solution is not more intense than that developed by the Control solution (NMT 3 ppm).
• Insoluble Substances
Sample: 2.0 g of Dried Ferrous Sulfate
Analysis: Dissolve the Sample in 20 mL of freshly boiled dilute sulfuric acid (1 in 100), heat to boiling, and digest in a covered beaker on a steam bath for 1 h. Filter through a tared filtering crucible, wash thoroughly, and dry at 105
.
.Acceptance criteria: The weight of the insoluble residue does not exceed 1 mg (NMT 0.05%).
ADDITIONAL REQUIREMENTS
• Packaging and Storage: Preserve in well-closed containers.
Auxiliary Information— Please check for your question in the FAQs before contacting USP.
| Topic/Question | Contact | Expert Committee |
|---|---|---|
| Monograph | Huy T. Dinh, M.S. Scientific Liaison 1-301-816-8594 | (DS2010) Monographs - Dietary Supplements |
USP35–NF30 Page 3182
Chromatographic Column—
Chromatographic columns text is not derived from, and not part of, USP 35 or NF 30.