Experimental Techniques & Chemical Analysis – Identification of Ions & Gases
(a) Carbonate – \$\\mathrm{CO_3^{2-}}\$
Think of carbonate like a “bicarbonate balloon” that bursts when it meets acid.
- Take a small amount of the sample in a test tube.
- Add a few drops of dilute hydrochloric acid (\$\\mathrm{HCl}\$).
- Observe vigorous bubbling – that’s carbon dioxide gas (\$\\mathrm{CO_2}\$) escaping.
- Collect the gas in a test tube inverted over water; the tube will fill with bubbles.
- Optional: Pass the gas through a solution of alkaline silver nitrate – a pale yellow precipitate of silver carbonate (\$\\mathrm{Ag2CO3}\$) confirms the presence of \$\\mathrm{CO_2}\$.
⚠️ Exam tip: Remember the “bubbling” clue – if you see fizzing, you’re likely dealing with a carbonate.
(b) Halides – \$\\mathrm{Cl^-}\$, \$\\mathrm{Br^-}\$, \$\\mathrm{I^-}\$
Halides are like a “silver coin” that turns into a solid when they meet silver ions.
- Acidify the sample with dilute nitric acid (\$\\mathrm{HNO_3}\$).
- Add a few drops of aqua silver nitrate (\$\\mathrm{AgNO_3}\$).
- Observe the formation of a precipitate:
- \$\\mathrm{AgCl}\$ – white, “chalky”
- \$\\mathrm{AgBr}\$ – pale yellow
- \$\\mathrm{AgI}\$ – yellowish‑brown
- Use the colour intensity to differentiate the halides.
📝 Exam tip: Write the equation for each halide: \$\\mathrm{X^- + Ag^+ \\rightarrow AgX(s)}\$ and note the colour change.
(c) Nitrate – \$\\mathrm{NO_3^-}\$
Nitrate is a “silent partner” – it doesn’t react until we give it a push.
- Reduce nitrate with a strip of aluminium foil in acetic acid (\$\\mathrm{CH3COOH}\$). The foil dissolves and releases ammonia gas (\$\\mathrm{NH3}\$).
- Collect the gas in a test tube inverted over water – you’ll see a greenish‑blue colour (due to the bromocresol green indicator).
- Alternatively, add aqua sodium hydroxide (\$\\mathrm{NaOH}\$) to the sample. Nitrate itself is inert, but the presence of ammonia gas indicates nitrate reduction.
🔍 Exam tip: Remember: “Aluminium + acid → NH₃” is the key clue for nitrate.
(d) Sulfate – \$\\mathrm{SO_4^{2-}}\$
Sulfate is like a “silent snowflake” – it only shows up when it meets barium.
- Acidify the sample with dilute nitric acid (\$\\mathrm{HNO_3}\$).
- Add a few drops of aqua barium nitrate (\$\\mathrm{Ba(NO3)2}\$).
- Observe a white precipitate of barium sulfate (\$\\mathrm{BaSO_4}\$).
- Confirm by adding a small amount of hydrochloric acid; the precipitate remains insoluble.
💡 Exam tip: Write the equation: \$\\mathrm{SO4^{2-} + Ba^{2+} \\rightarrow BaSO4(s)}\$ and note the insolubility.
(e) Sulfite – \$\\mathrm{SO_3^{2-}}\$
Sulfite is a “quick‑acting firestarter” that reacts with strong oxidisers.
- Acidify the sample with dilute nitric acid (\$\\mathrm{HNO_3}\$).
- Add a few drops of potassium manganate(VII) (\$\\mathrm{K2MnO4}\$) solution.
- Observe a rapid colour change from green to purple, indicating the formation of potassium permanganate (\$\\mathrm{KMnO_4}\$).
- Confirm by adding a few drops of hydrochloric acid; the purple colour fades.
🚨 Exam tip: Remember the colour shift – green to purple is the hallmark of sulfite reacting with manganate.
| Ion | Key Test | Observations |
|---|
| \$\\mathrm{CO_3^{2-}}\$ | Acid + \$\\mathrm{CO_2}\$ | Fizzy bubbles, pale yellow \$\\mathrm{Ag2CO3}\$ |
| \$\\mathrm{Cl^-}\$, \$\\mathrm{Br^-}\$, \$\\mathrm{I^-}\$ | \$\\mathrm{AgNO_3}\$ | White (\$\\mathrm{AgCl}\$), pale yellow (\$\\mathrm{AgBr}\$), yellowish‑brown (\$\\mathrm{AgI}\$) |
| \$\\mathrm{NO_3^-}\$ | Aluminium + acid → \$\\mathrm{NH_3}\$ | Greenish‑blue gas, no precipitate |
| \$\\mathrm{SO_4^{2-}}\$ | \$\\mathrm{Ba(NO3)2}\$ | White insoluble \$\\mathrm{BaSO_4}\$ |
| \$\\mathrm{SO_3^{2-}}\$ | \$\\mathrm{K2MnO4}\$ + acid | Green → purple, fades with HCl |