Practical Skills in Chemistry AS I
- Syllabus
- 2017
- Topic
- —
- Level
- AS
A practical-context problem becomes manageable when you separate what must be found from the chemistry and measurements that can reveal it. Start with the target quantity or decision, then work backwards to the observations and data needed.
| Step | Decision |
|---|---|
| 1. Target | identify the required quantity, comparison or identity |
| 2. Chemistry | select the reaction, relationship or test connecting evidence to the target |
| 3. Design | define what changes, what is measured and what stays controlled |
| 4. Data | specify readings, units, repeats and calculations |
| 5. Check | compare the conclusion with uncertainty and method limits |
If comparing metals by temperature rise, equal moles and equal solution conditions are needed before temperature change can support the comparison. Faster reaction may also reduce heat loss, so reaction rate can affect the measured result even when it is not the target.
Do not begin by naming familiar apparatus. First decide what evidence would answer the stated problem; apparatus is chosen to produce that evidence.
| Variable type | Role | How to state it |
|---|---|---|
| independent | deliberately changed | name the factor and planned values |
| dependent | measured response | name the reading and unit |
| control | could also affect the response | name it and state exactly how it is kept constant |
A fair comparison changes only the independent variable. Controls must be operational: ‘keep temperature constant at 25 °C in the same water bath’ is useful; ‘control temperature’ is not enough. Where samples contain different amounts of water or another component, adjust added quantities so the total relevant amount is equal.
Repeats improve reliability and reveal spread, but they do not replace control variables. An uncontrolled factor can shift every repeat in the same direction.
A data table must preserve what was measured, the units and the precision of the apparatus before any processing is done.
| Feature | Correct practice |
|---|---|
| headings | quantity followed by unit, for example time / s |
| cells | numerical values only; do not repeat units in every cell |
| precision | measurements from the same apparatus use consistent decimal places |
| repeats | keep raw trials visible and place the mean in a separate column |
| anomalies | retain and identify them; do not silently delete them |
Use a graph when the purpose is to show a continuous relationship or obtain a gradient, intercept or endpoint. Use a table when exact values and repeats matter most.
A neat table is not automatically appropriate: headings without units or mixed precision can hide the quality of the measurements.
| Task | Evidence-based response |
|---|---|
| conclude | state the pattern or answer and support it with processed data |
| evaluate results | discuss spread, anomalies, uncertainty and agreement with an accepted value |
| evaluate method | explain how a method feature changes validity, accuracy, precision or reliability |
When an error is directional, trace the whole consequence: identify what is too high or low, show how that changes the calculation, then state the direction of the final result. For example, unreacted ammonia consuming extra acid makes a titre too large and can make the calculated fertiliser content too low.
‘The result is close’ is not an evaluation. Compare the difference with uncertainty or an appropriate scale, and do not claim agreement beyond what the evidence supports.
| Feature | Effect | Useful response |
|---|---|---|
| random variation | readings scatter unpredictably | repeat, identify anomalies and use a justified mean |
| systematic error | readings shift in one direction | correct/calibrate the cause or change the method |
| measurement uncertainty | interval associated with a reading | calculate its size and carry it into the result |
Percentage uncertainty = absolute uncertainty ÷ measured value × 100%. Add percentage uncertainties for quantities multiplied or divided; add absolute uncertainties for quantities added or subtracted. For a difference made from two readings, include the uncertainty of both readings.
A result of 37.52 with 4.5% uncertainty has an absolute uncertainty of 1.69, giving about 35.83–39.21. An accepted value of 39.1 lies inside this interval, so the results are consistent at this uncertainty.
Low percentage uncertainty does not guarantee accuracy: a systematic error can produce precise, tightly grouped results that are all wrong.
| Check | Evidence sought | Improvement pattern |
|---|---|---|
| validity | the method isolates the intended cause | control a confounding variable |
| accuracy | directional loss or contamination is prevented | prevent/correct the named bias |
| precision | instrument resolution supports the reading | use suitable higher-resolution apparatus |
| reliability | variation is measured | repeat and use concordant results or a justified mean |
| completion/purity | reaction, separation or drying is complete | test to constant mass or use a specific endpoint |
Every improvement needs a cause-and-effect link. Rinsing a residue matters because soluble product left on it would dry and add to the measured mass; drying matters because retained water would also add mass. State which measured value changes and why.
Generic advice such as ‘use better equipment’ or ‘be more careful’ is not an evaluation unless it names the limitation and explains how the change affects the result.
| Stage | Requirement |
|---|---|
| axes | independent variable on x; dependent variable on y; quantity and unit on each |
| scale | simple, linear where appropriate, and using at least about half the grid |
| points | small accurate marks; show uncertainty bars only when provided or required |
| fit | best-fit line or smooth curve follows the overall trend, not point-to-point joins |
| extraction | use a large triangle for gradient; read intercept, tangent or line intersection with units |
Describe the relationship first, then support it with a graph feature. An endpoint may be found from the intersection of two best-fit regions; an instantaneous rate comes from a tangent gradient, while an average rate comes from a secant over an interval.
Do not force a line through the origin unless the chemistry and data justify it. A best-fit line balances scatter; it need not pass through every point.
Processing converts raw readings into the quantity that answers the practical question: subtract paired readings, select justified concordant values, calculate a mean, then apply the relevant chemical relationship.
| Context | Typical processing |
|---|---|
| titration | final − initial burette readings; mean concordant titre; moles and concentration |
| thermochemistry | ΔT; q = mcΔT; moles; ΔH with sign and kJ mol−1 |
| kinetics | change/time, 1/time as a relative rate, or graph gradient |
| yield/purity | actual/theoretical × 100 or reacting amount/sample amount × 100 |
Carry units through every stage and keep extra calculator digits until the final answer. Check that the sign, scale and trend make chemical sense; a calculation is not analysed until it is interpreted in context.
Do not average all repeats automatically. Exclude a value only with a stated reason such as non-concordance or an identified procedural anomaly.
Significant figures communicate measurement precision. A calculated answer must not imply more reliable digits than the experimental data support.
| Situation | Reporting rule |
|---|---|
| multiplication/division | usually match the input with the fewest significant figures |
| addition/subtraction | usually match the least precise decimal place |
| uncertainty | commonly give one significant figure, or two when useful |
| value ± uncertainty | round both to the same decimal place |
For 24.55 cm3 × 0.1000 mol dm−3, retain guard digits during working and round the final result to four significant figures if those are the limiting measurements. Leading zeros are not significant; trailing zeros after a decimal point are.
Do not round after every step: repeated rounding can shift the final result. Keep guard digits, then round once when the result and its uncertainty are known.
| Idea | Meaning | Evidence |
|---|---|---|
| accuracy | closeness to the accepted or true value | difference from an accepted value, considering uncertainty |
| precision | closeness of repeated measurements to one another | small spread or narrow range |
| repeatability | same method, operator and equipment agree | repeated results under unchanged conditions |
| reproducibility | results agree when operator, equipment or place changes | independent repetition under changed conditions |
A set of temperatures can be tightly grouped but all too low because heat is lost. That set is precise but inaccurate. A wider set whose mean is close to the accepted value may be less precise but more accurate overall.
Instrument resolution contributes to uncertainty, not directly to accuracy. Calibration and systematic effects determine whether readings are centred correctly.
| Job | Suitable apparatus | Why |
|---|---|---|
| fixed accurate volume | volumetric pipette | delivers one calibrated volume precisely |
| variable accurate volume | burette | controlled addition with initial/final readings |
| make a solution to fixed volume | volumetric flask | calibrated total volume |
| approximate volume | measuring cylinder | faster, lower precision is acceptable |
| add dropwise | dropping/teat pipette or burette | small controlled additions |
| collect gas volume | gas syringe | direct volume measurement with limited gas loss |
| measure mass | balance with suitable capacity/resolution | numerical mass reading |
Match the expected value to the apparatus range and the required uncertainty to its resolution. Also consider chemical compatibility, temperature and whether the measurement must be delivered, contained or monitored continuously.
A named ‘pipette’ is not always enough: a volumetric pipette delivers a fixed calibrated volume, while a dropping pipette controls drops but does not measure an accurate volume.
| Technique | Essential control |
|---|---|
| burette | rinse with solution, remove funnel, read meniscus at eye level, record initial and final readings |
| volumetric pipette | rinse with solution, fill to mark at eye level, let drain; do not blow out the calibrated residue |
| volumetric flask | dissolve fully, cool if needed, make to mark dropwise, stopper and invert repeatedly |
| calorimetry | measure mass/volume and initial/final temperature; insulate and mix consistently |
| reflux/distillation | condenser water enters at bottom; reflux returns vapour, distillation collects it |
| filtration/washing/drying | separate the correct phase, remove soluble contamination, then dry before weighing |
Read analogue scales at eye level to avoid parallax and use the bottom of a clear concave meniscus. Record all certain digits plus the justified estimated digit where the scale permits.
Technique must match purpose. Reflux cannot collect a volatile product, and distillation cannot keep volatile reagents in the reaction mixture.
| Property | Meaning | Selection consequence |
|---|---|---|
| range | minimum to maximum value measurable | must include the largest expected value without overflow |
| resolution | smallest change the scale/display can distinguish | finer resolution reduces reading uncertainty |
Choose the smallest suitable range that still covers the expected measurement, because this often gives finer useful resolution. For a single analogue scale reading, uncertainty is commonly about half the smallest division; a digital reading is commonly uncertain by about one final displayed increment unless the instrument information states otherwise. A difference from two readings includes both reading uncertainties.
Measuring about 24.6 cm3 with a 50 cm3 burette is appropriate because the range covers the value and the fine scale supports a small percentage uncertainty. A 100 cm3 measuring cylinder may cover the value but usually resolves it less well.
Large range is not automatically better. Capacity beyond what is needed can come with coarser resolution and a larger percentage uncertainty.
| Step | Decision |
|---|---|
| identify hazard | name the harmful property of the substance or procedure |
| identify exposure | state the route and scale by which harm could occur |
| assess risk | judge likelihood and severity in this method |
| control | choose a specific change that reduces likelihood or consequence |
| dispose | specify management of reactive, metal-containing or organic waste |
Use the control that matches the hazard: a fume cupboard for harmful vapour, small quantities and no flame for volatile flammable liquids, gloves plus careful transfer for corrosive liquids, a water bath for flammable solvents, and secure clamping/slow heating for hot glassware. Wear eye protection and a laboratory coat throughout.
A hazard label describes an intrinsic property; risk depends on the procedure, amount and exposure. ‘Wear goggles’ alone does not manage inhalation, pressure or fire hazards.
| Species | Test | Positive observation |
|---|---|---|
| CO32−/HCO3− | add dilute aqueous acid; pass gas into limewater | effervescence; limewater turns milky/cloudy |
| SO42− | acidify, then add barium chloride solution | white precipitate |
| NH4+ | add NaOH(aq) and warm | NH3 turns damp red litmus blue and gives white fumes with HCl |
| O2 | insert a glowing splint | splint relights |
| NO2 | observe gas and test damp indicator | brown gas with acidic pH |
| H2O | anhydrous CuSO4 or cobalt chloride paper | white→blue or blue→pink |
| Cation | Flame colour |
|---|---|
| Li+ | crimson red |
| Na+ | yellow |
| K+ | lilac |
| Ca2+ | brick/orange-red |
| Sr2+ | crimson red |
| Ba2+ | apple green |
| Mg2+ | no characteristic visible flame colour |
Use a clean wire in a non-luminous flame and prevent contamination. A test result is the complete combination of reagent/conditions and observation, not a colour alone.
Acidify the sulfate test before adding barium ions so carbonate does not give a misleading barium carbonate precipitate. Never identify an ion from an unqualified precipitate colour.
| Feature | Reagent/conditions | Positive observation |
|---|---|---|
| C=C | bromine water, shake | orange/brown/yellow→colourless |
| alcohol –OH | dry sample with PCl5 | steamy/misty HCl fumes |
| aldehyde | warm with Benedict's/Fehling's solution | blue solution gives brick-red Cu2O precipitate |
| primary/secondary alcohol oxidation | warm with acidified K2Cr2O7 | orange→green; product evidence is still needed |
| carboxylic acid | add carbonate/hydrogencarbonate | CO2 effervescence; gas turns limewater milky |
| halogenoalkane halogen | warm with aqueous AgNO3 in ethanol | AgCl white, AgBr cream, AgI yellow precipitate |
Choose tests that discriminate between plausible structures, include a valid negative control where useful, and interpret results together. Dry conditions matter for PCl5 because water also produces HCl; warming and stated reagents matter for oxidation and aldehyde tests.
One positive test identifies a functional feature, not necessarily the whole molecule. Dichromate colour change alone does not distinguish an aldehyde, ketone or carboxylic-acid product.
| Context | Core measurements | Processing and method check |
|---|---|---|
| molar mass | mass and moles from reaction/gas data | stoichiometry; completion and product identity |
| titration | pipetted volume and concordant titres | mean titre→moles→concentration; endpoint and glassware uncertainty |
| thermochemistry | mass/volume and temperature change | q=mcΔT→ΔH; heat loss and incomplete reaction |
| simple kinetics | time plus concentration, volume, mass or colour measure | rate/change or gradient; mixing, temperature and endpoint |
Write the chemical relationship before substituting numbers, convert all units, use the measured limiting quantity, and state the final unit and sign. Then evaluate the result by tracing the largest uncertainty or directional loss through the calculation.
For titration, subtract initial from final burette readings, average concordant titres, convert cm3 to dm3, calculate moles from n=cV, use the equation ratio, then divide by the sample volume. Each step must preserve units and stoichiometry.
A correct numerical answer does not validate the method. Concordance checks precision; indicator choice, transfer, reaction completion and contamination can still affect accuracy.
| Stage | Inorganic crystal preparation | Organic liquid preparation |
|---|---|---|
| react | use correct stoichiometry; complete reaction without avoidable excess contamination | choose reagent, conditions and reflux where volatile material must be retained |
| separate | filter insoluble excess/impurity if present | use separating funnel or distillation according to phases/volatility |
| purify | concentrate to saturation, cool to crystallise, filter and wash | wash organic layer, dry with anhydrous agent, distil a narrow boiling fraction |
| finish | dry crystals without decomposition | collect dry product and minimise evaporation/transfer loss |
| assess | percentage yield and purity evidence | percentage yield, boiling range and suitable chemical test |
Link each technique to the material removed or retained. Heating a salt solution to dryness can trap impurity or decompose product; concentrating then cooling forms larger crystals. In an organic preparation, reflux promotes reaction without losing vapour, while later distillation separates the volatile product.
High yield is not proof of purity: retained solvent, water or soluble impurity can increase measured mass. A pure but incompletely recovered product can have low yield.