Chemical ReactionsLaboratory AnalysisContent level: Core 26 min

Lab Skills: Gravimetric Analysis and Redox Titration

What you'll be able to do: Analyse gravimetric and redox titration data, including percent composition and sources of experimental error.

Introduction

Two classical techniques turn the ideas in this unit into numbers on a lab bench: weighing a precipitate, and titrating with permanganate. Both are only as good as the technique, so understanding how errors propagate matters as much as the arithmetic.

These are recommended, not required. You can start this lesson at any time.

Learning objectives

  • Outline the steps of a gravimetric determination
  • Calculate percent composition from precipitate mass
  • Perform a redox titration calculation using a permanganate standard
  • Predict the direction of error caused by a procedural mistake

Lesson

The gravimetric idea

If an ion can be precipitated completely as a compound of known formula, then weighing that dry solid measures how much of the ion was present. The method needs no calibration curve and no standard solution, only an accurate balance and patient technique.

Ba²⁺(aq) + SO²⁻(aq) → BaSO(s)

Procedure that protects the result

Add a slight excess of precipitating agent to drive the reaction to completion, digest the mixture so crystals grow larger and filter more cleanly, wash the solid to remove adsorbed spectator ions, then dry to constant mass. Drying to constant mass, weighing repeatedly until the reading stops falling, is the step that proves the water is gone.

Constant mass is evidence, not a formality. A single weighing cannot show that drying is complete.

From precipitate mass to percent composition

Convert the precipitate mass to moles, use the formula to find moles of the ion of interest, convert that to a mass, then divide by the original sample mass. The gravimetric factor is simply this chain expressed as a single multiplier.

percent = (mass of analyte / mass of sample) × 100

Permanganate titration

In acidic solution, MnO is reduced to the almost colourless Mn²⁺ while the analyte is oxidised. Because the purple colour disappears as it reacts, the first drop of excess titrant leaves a faint persistent pink, so no separate indicator is required. Sulfuric acid is used to acidify, because hydrochloric acid would itself be oxidised.

MnO + 8 H + 5 e → Mn²⁺ + 4 HO

Thinking about error direction

For any mistake, ask whether the measured quantity ends up too high or too low, then follow it through the calculation. A precipitate that is not fully dried weighs too much, so the reported percentage is too high. A burette rinsed with water instead of titrant delivers dilute titrant, so more volume is needed and the calculated analyte appears too high.

Never memorise error outcomes. Trace the affected measurement through the calculation each time.

Key ideas

Definition
Gravimetric analysis

Quantitative analysis based on measuring the mass of a pure isolated product.

Definition
Constant mass

Repeated drying and weighing until successive masses agree, showing all solvent has gone.

Definition
Self-indicating titrant

A titrant whose own colour change marks the endpoint, as permanganate does.

Rule
Excess precipitant

A slight excess of the precipitating agent ensures the analyte is removed completely.

Key concept
Error direction

Trace each procedural fault to whether the measured value becomes too high or too low.

Equation
Percent composition

percent = (mass of analyte / mass of sample) × 100

  • mass of analyte = mass of the target species calculated from the precipitate
  • mass of sample = mass of the original impure sample

Worked examples

Worked example 1

A 1.000 g sample containing sulfate is dissolved and treated with excess BaCl, yielding 0.750 g of dry BaSO. What is the percent sulfate by mass?

Try it first: Decide what the weighed solid tells you about moles before converting anything.

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    Worked example 2

    A 25.00 mL sample of Fe²⁺ solution requires 18.60 mL of 0.0200 M KMnO in acid to reach the first persistent pink. What is the iron concentration?

    Try it first: Recall how many electrons permanganate accepts, since that sets the ratio.

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      Worked example 3

      In the gravimetric experiment above, the student removes the filter paper before the precipitate reaches constant mass. What effect does this have on the reported percent sulfate?

        0 of 4 steps revealed.

        Common mistakes

        Using hydrochloric acid to acidify a permanganate titration.

        Why it's wrong: Chloride is itself oxidised by permanganate, consuming extra titrant.

        Check instead: Acidify with sulfuric acid, which is not oxidised.

        Treating the precipitate mass as the analyte mass.

        Why it's wrong: The solid includes the counter-ion added during precipitation.

        Check instead: Convert to moles, apply the formula ratio, then convert back to the analyte mass.

        Assuming a spilled sample always lowers the reported percentage.

        Why it's wrong: The direction depends on which measurement was affected and where it appears in the calculation.

        Check instead: Trace the specific quantity through each step of the arithmetic.

        Weighing the precipitate once and calling it dry.

        Why it's wrong: Residual solvent adds mass that is indistinguishable from product.

        Check instead: Dry and reweigh until two successive masses agree.

        Practice this skill

        No practice questions are available for this topic yet. You can still practice the whole unit.

        What you should now know

        Gravimetric analysis determines an unknown amount by converting it quantitatively into a pure, dry, insoluble solid and weighing it. Redox titration determines it by measuring the volume of an oxidising agent consumed, with permanganate acting as its own indicator. In both, the calculation runs from the measured quantity through moles and the mole ratio to the analyte, and every procedural fault can be traced to whether it makes the measured quantity too high or too low.

        • Gravimetric analysis weighs a pure dry precipitate to measure an ion
        • Dry to constant mass before recording a precipitate mass
        • Convert precipitate mass to moles, then to analyte mass, then to percent
        • Permanganate is self-indicating and is acidified with sulfuric acid
        • Trace every procedural error to whether the measurement is too high or too low

        Sources and further reading

        This lesson is original Chem Help content. No external sources were adapted.