Fatima Akintobi Suphate are prepared in the laboratory or Industry. At the same time, 'sulphides' as such has no meaning in exploration as they occur as compounds like PbS, MgS, FeS, and like. These compounds and the associated minerals can be located using gravimetry as they have more density.
Main Takeaway: Quantify sulfate by precipitating it as barium sulfate (BaSO₄), isolating, igniting, and weighing the precipitate; the mass of BaSO₄ yields the sulfate content by stoichiometry.
1. Principle
Under hot, strongly acidic conditions, sulfate ions react with barium ions to form insoluble barium sulfate:
Complete precipitation, digestion, and proper treatment of the solid ensures accuracy1.
2. Reagents & Apparatus
Reagents
Barium chloride solution (~0.05–0.25 M), warmed
Concentrated HCl (to adjust pH ~1–2)
Distilled hot water
Dilute H₂SO₄ wash (~0.1 M) Apparatus
Analytical balance (±0.1 mg)
Ash-free filter paper (e.g., Whatman No. 42)
Porcelain crucibles with lids
Beakers (400 mL) and watch glasses
Hot plate or steam bath
Desiccator and muffle furnace
3. Procedure
Sample Preparation Weigh ~0.4–0.5 g dried solid (or measure known volume of water sample). Dissolve in ~200 mL distilled water; acidify to pH 1–2 with HCl; heat to near boiling.
Precipitation Calculate volume of BaCl₂ solution (stoichiometric amount + 10% excess). Warm both sample and BaCl₂ solutions to near boiling. Add BaCl₂ slowly with vigorous stirring until turbidity ceases; confirm by adding a drop of BaCl₂—no new precipitate should form.
Digestion (Aging) Maintain hot suspension (just below boiling) for ≥1 hour to enlarge crystals and minimize co-precipitation2.
Filtration & Washing Filter rapidly through pre-heated ash-free paper. Wash precipitate with hot distilled water until chloride-free (test filtrate with AgNO₃). Rinse finally with dilute H₂SO₄ to suppress BaSO₄ solubility3.
Ignition & Weighing Transfer filter paper + precipitate to pre-weighed porcelain crucible; ignite at 600–800 °C until constant mass. Cool in desiccator and weigh to ±0.1 mg constancy.
4. Calculations
Let mBaSO4mBaSO4 = mass of ignited BaSO₄ (g). Molar masses: MSO42−=96.06MSO42−=96.06, MBaSO4=233.39MBaSO4=233.39.
For aqueous samples, express concentration as mg SO₄²⁻ L⁻¹ by dividing mSO42−mSO42− (mg) by sample volume (L).
5. Critical Considerations
Acid medium promotes crystal growth and suppresses hydroxide formation. Digestion reduces occlusion of impurities and yields larger, more filterable crystals. Hot washes remove soluble salts; acid wash prevents redissolution. Proper ignition removes filter ash without decomposing BaSO₄. Interferences (e.g., silicates, phosphates, heavy metals) may co-precipitate; preliminary treatment (e.g., removal of Fe³⁺) can be required4.
This step‐by‐step protocol ensures reliable quantification of sulfate via gravimetric precipitation as BaSO₄.
Refer To These References
International Standard ISO 9280:1990(E) – Water quality – Determination of sulfate – Gravimetric method using barium chloride https://cdn.standards.iteh.ai/samples/16932/ca55fcb09b844719ae4683ac144d8678/ISO-9280-1990.pdf
Standard Methods for the Examination of Water and Wastewater, Method 4500-SO4²⁻ C – Gravimetric Analysis with Ignition of Residue https://www.nemi.gov/methods/method_summary/4868/
EPA-NERL Method 375.3 – Sulfate by Gravimetric Determination https://edfhelpdesk.com/sites/default/files/vvl/E375.3.pdf
Indian Standard IS 2317:1975 – Method for Gravimetric Determination of Sulphates https://law.resource.org/pub/in/bis/S02/is.2317.1975.pdf
APHA Method 4500-SO4²⁻ – Standard Methods for the Examination of Water and Wastewater (40 CFR 136.3(a)) https://law.resource.org/pub/us/cfr/ibr/002/apha.method.4500-so42.1992.pdf