Combine Year 12 anion tests with transition-metal and ammonium tests. Use separate aliquots and record evidence that actually distinguishes the candidates.
A useful test must answer a specific question
Qualitative analysis identifies species from reproducible reactions. Work on small labelled portions of the unknown, record starting appearance, add reagent a little at a time and then in excess when that distinction matters. A fresh aliquot prevents reagents from one test creating false positives in another.
Distinguish observation from inference. “A pale-blue precipitate forms and dissolves in excess ammonia to a deep-blue solution” is an observation sequence; “Cu²⁺ is present” is its interpretation. Write both when asked. One observation may fit more than one ion, so combine independent evidence.
This topic develops PAG4 skills. Wear the required eye protection, use the specified small quantities and follow laboratory risk assessments for corrosive reagents, ammonia and metal-ion waste. Heating a sample requires appropriate handling; do not identify gases by directly inhaling them.
Choose an acid that does not supply the ion being tested
For carbonate, add dilute acid and pass the evolved gas through limewater; effervescence plus limewater turning milky supports CO₂. For sulfate, use an acidified fresh aliquot and barium ions; a white BaSO₄ precipitate supports sulfate. Acidification removes carbonate that could otherwise form white BaCO₃.
For halides, acidify a fresh portion with dilute nitric acid and add silver nitrate. HCl would introduce chloride and could create a false AgCl result. Use ammonia to distinguish the precipitates rather than relying on subtle colour differences alone. Do not use sulfuric acid to prepare a sulfate-test aliquot.
| Ion | Reagent/sequence | Observation |
|---|---|---|
| CO₃²⁻ | Dilute acid, then limewater gas test | Bubbles; limewater turns milky |
| SO₄²⁻ | Dilute HCl then BaCl₂, or compatible nitrate reagents | White precipitate |
| Cl⁻ | Dilute HNO₃ then AgNO₃; dilute NH₃ | White AgCl, dissolves in dilute NH₃ |
| Br⁻ | Dilute HNO₃ then AgNO₃; concentrated NH₃ | Cream AgBr, dissolves in concentrated NH₃ |
| I⁻ | Dilute HNO₃ then AgNO₃; NH₃ | Yellow AgI, insoluble in dilute/concentrated NH₃ |
Release ammonia from ammonium with an alkali
Add aqueous NaOH to a separate portion and warm gently as directed. Ammonium ions react to release ammonia, which turns damp red litmus blue. The paper must be damp for the gas to dissolve and establish alkaline conditions; avoid touching it with alkaline solution splashes.
NH₄⁺ + OH⁻ → NH₃ + H₂O shows proton transfer. Ammonium is the conjugate acid and hydroxide removes a proton. Do not confuse this gas test with adding aqueous ammonia as a reagent to precipitate transition-metal hydroxides.
Use both the initial precipitate and excess-reagent behaviour
The same initial hydroxides form with small amounts of NaOH or ammonia. The excess tests distinguish copper and chromium from iron and manganese. Look promptly because Fe(OH)₂ and Mn(OH)₂ can change colour through air oxidation. Chromium–ammonia ligand replacement may develop slowly under the specified conditions.
A green initial precipitate alone is not enough to distinguish Fe²⁺ from Cr³⁺. Solubility in excess NaOH supports chromium; iron(II) hydroxide remains. A blue precipitate becoming a deep-blue solution in excess ammonia strongly supports copper(II) among this required set.
| Ion | Initial hydroxide | Excess NaOH | Excess NH₃ |
|---|---|---|---|
| Cu²⁺ | Pale blue | Insoluble | Deep-blue solution |
| Fe²⁺ | Green; browns in air | Insoluble | Insoluble |
| Fe³⁺ | Orange-brown | Insoluble | Insoluble |
| Mn²⁺ | Off-white/pale; darkens | Insoluble | Insoluble |
| Cr³⁺ | Grey-green | Green solution | Purple/violet complex under suitable conditions |
Worked interpretation: combine cation and anion evidence
An original unknown gives a grey-green precipitate with NaOH that dissolves in excess to a green solution. A separate acidified sample gives a white precipitate with barium chloride. The cation evidence supports Cr³⁺ and the anion evidence supports SO₄²⁻. For a simple salt containing only those ions, charge balance gives Cr₂(SO₄)₃.
Explain why the alternatives fail: Fe²⁺ can give green hydroxide but it does not dissolve in excess NaOH in this scheme. A white barium precipitate without prior acidification would be less decisive because carbonate is an alternative. These tests do not establish a hydration number or prove the absence of every trace impurity.
For a second illustrative sample, white AgCl dissolving in dilute ammonia and copper’s characteristic ammonia sequence support CuCl₂, assuming a simple salt. Use separate portions; putting HCl into the halide aliquot would destroy the value of the chloride inference.
Quick checks
Original Finesse questions. Reveal the indicative worked solutions after attempting each question; these are not official OCR A mark allocations.
Q1. Why use nitric acid rather than hydrochloric acid before silver nitrate?Show answer
Hydrochloric acid supplies Cl⁻ and could create AgCl even if the unknown contained no chloride. Nitric acid acidifies without introducing a tested halide.
Q2. A green precipitate is insoluble in excess NaOH and browns on standing. Which required ion is most likely?Show answer
Fe²⁺. Fe(OH)₂ is green, remains insoluble in excess NaOH and can oxidise in air. Cr(OH)₃ would dissolve in excess NaOH, so the excess test is decisive.
Q3. Write the ionic equation for the sulfate test and describe the observation.Show answer
Ba²⁺(aq) + SO₄²⁻(aq) → BaSO₄(s). A white precipitate forms in the appropriately acidified aliquot. An equation alone does not state the observation.
Q4. Why can damp red litmus touching the NaOH solution invalidate an ammonium test?Show answer
The alkali itself turns red litmus blue. Keep the damp paper in the evolved gas without solution contact so the observation supports ammonia rather than direct contamination.
Q5. A sample gives yellow silver precipitate insoluble in ammonia and a rust-brown hydroxide insoluble in excess alkali. Suggest a simple salt formula, then identify a chemical caveat.Show answer
The separate test patterns suggest I⁻ and Fe³⁺, giving a formal charge-balanced FeI₃ composition. However Fe³⁺ can oxidise iodide, so a stable aqueous sample containing only those unchanged ions is chemically problematic. Recheck the sample and observations rather than forcing a formula from two tables. This transfer question links qualitative analysis to redox.
Sources
Sources and examiner guidance (reviewed 6 October 2026)
- OCR A H432 specification — version 3.1 — 5.3.2, printed pp. 52; outcomes and additional guidance, with relevant Module 1 practical skills.
- Chemrevise — OCR A 5.3.2 — Pages 1–2; secondary coverage cross-check. Lesson explanations, data and questions are original Finesse material.
- OCR H432/01 mark scheme — June 2025 — Q21(a)(ii); printed pp. 28. Question-specific evidence, not universal marking rules.
- OCR H432/01 examiner report — June 2025 — Q21(a)(ii); printed pp. 45. Read with the corresponding question context.
- OCR H432/01 question paper — June 2025 — Q21(a)(ii); context for the assessment references, not reproduced questions.
Finesse Tuition is not endorsed by AQA or Chemrevise. All explanations and examples here are our own.
