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Skills

Chemical Synthesis and Characterisation

8 weeks · 0 milestones

Plan and execute (or rigorously analyse) a chemical synthesis: document the procedure (reagents, quantities, reaction conditions, safety precautions), isolation methodology, percentage yield calculation, and full characterisation data (melting or boiling point, spectroscopic data including at least one of NMR, IR, or MS). The proof is the lab notebook record or equivalent documentation plus characterisation data with comparison to published literature values. For students without lab access, the accessible alternative is a rigorous comparative analysis of characterisation data from ChemSpider, Cambridge Crystallographic Data Centre (CCDC — free for academic use), or SDBS for a named literature compound — documenting each characterisation value, comparison to the reference, and what discrepancies would indicate about purity or identity. Reviewed by a chemist who challenges the characterisation interpretation, specifically asking about discrepancies between measured and reference values and what they indicate about the sample.

Milestone map

Milestone map

3 milestones

Plan synthesis route and complete safety assessment

1–2 weeks

Design a synthesis route for a specific organic or inorganic compound and complete a comprehensive safety and risk assessment before any experimental work. Accessible alternative: if physical laboratory access is unavailable, select a published reaction and design a computational analysis of spectroscopic properties and reaction mechanism using free open databases — the proof standard is identical for both routes.

Proof required

Submit your synthesis route (step-by-step reaction scheme with reagents, conditions, and expected intermediates), a COSHH or equivalent safety assessment listing all hazardous substances and control measures, and a brief justification for why this route was chosen over alternatives.

What gets checked

  • Synthesis route names specific reagents and conditions at each step — not 'add reducing agent' but 'add NaBH4 (1.2 equiv) in MeOH at 0°C'
  • Safety assessment identifies hazards for each named reagent and product — not a generic lab safety statement
  • Route justification addresses why an alternative approach was not preferred — demonstrates genuine understanding of the chemistry

Common mistakes

  • Writing a synthesis plan without completing the safety assessment first — the safety assessment must precede any experimental work
  • Choosing a synthesis without considering the characterisation step — the route must produce a product that can be characterised with available equipment

Resources

Foundationstart here

Depthgo deeper

Masteryfor the dedicated

What a verifier looks for

  • Ask the submitter to explain why each reagent was chosen — can they name the functional role of each component?
  • Ask what the key hazard is for this synthesis and how it is controlled — confirms the safety assessment was genuinely completed.
  • Ask what would happen to the yield or selectivity if the temperature or solvent were changed — tests whether they understand the chemistry or just followed a procedure.

Execute synthesis and collect characterisation data

1–4 weeks depending on synthesis complexity

Perform the synthesis following the planned route, recording all observations in a lab notebook as they occur. Characterise the product using at least two methods — physical properties plus at least one spectroscopic method. Accessible alternative: analyse authentic spectroscopic data from SDBS or NIST WebBook, documenting how spectral features are interpreted and what they confirm about structure.

Proof required

Submit your lab notebook record showing the procedure as actually performed (including deviations), raw characterisation data (spectra or physical measurements), and an initial interpretation of what the data confirms about product identity and purity.

What gets checked

  • Lab notebook includes actual observations and any deviations — not a rewritten procedure presented as a lab record
  • Characterisation data is raw or minimally processed — actual spectra, melting point range, or measurement outputs
  • Initial spectral interpretation names specific peaks and assigns them to structural features — not 'the IR confirmed the product' but 'the broad O–H stretch at 3300 cm⁻¹ is consistent with the carboxylic acid product'

Common mistakes

  • Not recording deviations as they occur — a lab notebook with no deviations is suspicious; real synthesis always involves adjustments
  • Characterising only by melting point or physical appearance — single-method characterisation is insufficient for product identity claims

Resources

Foundationstart here

What a verifier looks for

  • Ask the submitter to interpret a specific peak in their spectrum — can they assign it to a structural feature?
  • Ask about a deviation from the planned synthesis — how did they decide to handle it?
  • Ask what the characterisation data does NOT tell them about the product — good analytical chemists know the limits of each technique.

Write lab report and present mechanism with Q&A

1–2 weeks to write and schedule review

Complete a full lab report covering the reaction mechanism, experimental results, yield and purity assessment, and comparison against reference data. Present to an organic or physical chemist for a Q&A that probes understanding of the reaction mechanism and characterisation data interpretation.

Proof required

Submit your complete lab report (3–5 pages: introduction with mechanism, experimental procedure, results with annotated spectra, discussion of yield/purity/mechanism, and conclusion) plus a Q&A record showing mechanism or characterisation challenges from the reviewer and your responses. The reviewer must be named and their chemistry background stated.

What gets checked

  • Mechanism section shows the electron-pushing mechanism for the key step — curly-arrow notation showing electron movement (hand-drawn is fine)
  • Yield is calculated correctly and the discussion addresses why the yield was lower than theoretical if applicable
  • Q&A record includes at least one challenge to the mechanism or spectral interpretation — not just confirmation that the experiment was performed

Common mistakes

  • A mechanism section that describes what happened without showing why — 'the hydroxyl group attacks the carbonyl' without arrow-pushing does not demonstrate mechanistic understanding
  • A reviewer who only checks that the procedure was performed correctly — the Q&A must include at least one mechanistic challenge

Resources

What a verifier looks for

  • Ask the submitter to draw the curly-arrow mechanism for the key transformation during the review — cannot be prepared in advance.
  • Ask why the specific conditions used control selectivity or yield — tests whether they understand the chemistry beyond procedure-following.
  • Verify the reviewer has organic or physical chemistry training — a biology or materials science reviewer may not probe mechanism at the appropriate depth.

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