Practical Skills in Chemistry AS I

Syllabus
2017
Topic
Level
AS

Learning objectives

3P1—Solving practical-context problemsSolve problems set in a practical context and apply scientific knowledge to practical contexts.3P2—Controlling variablesIdentify and state how to control variables to improve experimental validity.3P3—Presenting dataPresent data in appropriate ways.3P4—Evaluating results and conclusionsEvaluate results and draw conclusions.3P5—Uncertainties and errorsRecognise and evaluate measurement uncertainties and errors.3P6—Evaluating an experimental methodComment on the method used for an experiment.3P7—Plotting and interpreting graphsPlot and interpret graphs.3P8—Processing and analysing dataProcess and analyse data using appropriate mathematical skills.3P9—Significant figuresUse appropriate numbers of significant figures based on the experimental data.3P10—Accuracy and precisionConsider the accuracy and precision of data.3P11—Selecting laboratory apparatusRecognise a range of laboratory apparatus and select appropriate apparatus for a particular scenario.3P12—Using apparatus and techniquesUnderstand how to use the apparatus and techniques appropriate to this specification.3P13—Range and resolution of apparatusConsider the range and resolution of apparatus.3P14—Health and safetyIdentify health and safety issues and explain how they may be managed.3P15—Tests for ions and gasesRecall and interpret observations relating to tests for ions and gases in Units 1 and 2.3P16—Tests for organic functional groupsRecall and interpret observations relating to tests for organic functional groups in Units 1 and 2.3P17—Measurements and data in Units 1 and 2Manipulate data and evaluate experimental methods and techniques for measurements in Units 1 and 2, including molar-mass calculations, titrations, thermochemical investigations and simple kinetics experiments.3P18—Preparing inorganic and organic compoundsEvaluate experimental methods and techniques for preparing inorganic or organic compounds in Units 1 and 2.

Turn a practical problem into a testable plan

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.

Control variables so one cause can be tested

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.

Present measurements so the evidence is readable

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.

Separate a conclusion from an evaluation

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.

Use uncertainty to judge a measured result

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.

Evaluate a method by tracing each failure mode

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.

Plot a graph that can support a measurement

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.

Process data without losing its experimental meaning

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 mol1^{-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.

Report only the precision supported by the data

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 cm3^3 × 0.1000 mol dm3^{-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.

Accuracy and precision answer different questions

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.

Choose apparatus from the measurement job

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.

Use apparatus so the reading means what you think it means

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.

Match apparatus range and resolution to the task

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 cm3^3 with a 50 cm3^3 burette is appropriate because the range covers the value and the fine scale supports a small percentage uncertainty. A 100 cm3^3 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.

Turn a chemical hazard into a specific risk control

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.

Identify ions and gases from reagent plus observation

Species Test Positive observation
CO32_3^{2-}/HCO3_3^- add dilute aqueous acid; pass gas into limewater effervescence; limewater turns milky/cloudy
SO42_4^{2-} acidify, then add barium chloride solution white precipitate
NH4+_4^+ add NaOH(aq) and warm NH3_3 turns damp red litmus blue and gives white fumes with HCl
O2_2 insert a glowing splint splint relights
NO2_2 observe gas and test damp indicator brown gas with acidic pH
H2_2O anhydrous CuSO4_4 or cobalt chloride paper white→blue or blue→pink
Cation Flame colour
Li+^+ crimson red
Na+^+ yellow
K+^+ lilac
Ca2+^{2+} brick/orange-red
Sr2+^{2+} crimson red
Ba2+^{2+} apple green
Mg2+^{2+} 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.

Use chemical tests as converging organic evidence

Feature Reagent/conditions Positive observation
C=C bromine water, shake orange/brown/yellow→colourless
alcohol –OH dry sample with PCl5_5 steamy/misty HCl fumes
aldehyde warm with Benedict's/Fehling's solution blue solution gives brick-red Cu2_2O precipitate
primary/secondary alcohol oxidation warm with acidified K2_2Cr2_2O7_7 orange→green; product evidence is still needed
carboxylic acid add carbonate/hydrogencarbonate CO2_2 effervescence; gas turns limewater milky
halogenoalkane halogen warm with aqueous AgNO3_3 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_5 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.

Connect Unit 1 and 2 measurements to the final quantity

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 cm3^3 to dm3^3, calculate moles from n=cVn=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.

Evaluate a preparation by yield, purity and safe separation

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.