Lab: Hydrate Analysis & Gravimetric Thermal DecompositionCourse level: AP Chemistry

Hydrate Analysis and Gravimetric Reasoning

What you'll be able to do: Determine the formula of a hydrate from heating data and evaluate whether a gravimetric result is trustworthy.

Best after: Empirical and Molecular Formulas, Percent Composition

Introduction

Heating a hydrate drives off its water of crystallisation and leaves the anhydrous salt behind. Two balance readings are therefore enough to determine how many water molecules were bound to each formula unit. This lesson applies the empirical formula method to real laboratory data and asks the harder question of when that data can be believed.

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

Learning objectives

  • Interpret before-and-after heating masses in terms of water lost and anhydrous salt remaining.
  • Determine the value of x in a hydrate formula from gravimetric data.
  • Calculate the percent water in a hydrate and compare it with a theoretical value.
  • Evaluate whether incomplete heating, spattering or rehydration explains a non-integer result.

What a hydrate formula means

In CuSO₄ . 5 H₂O the dot is not multiplication in the usual sense, it records that five water molecules are built into each formula unit of the crystal.

Those waters count fully in the molar mass, so the hydrate (249.68 g/mol) is much heavier per mole than the anhydrous salt (159.61 g/mol). The colour change from blue to white on heating is the visible sign that the water has gone.

CuSO₄ . 5 H₂O

Anhydrous means without water. It is the residue left in the crucible.

Reading the two masses

Mass of water driven off = mass of hydrate minus mass of residue. Mass of anhydrous salt = mass of residue. Every gravimetric hydrate question reduces to those two lines, so write them down before doing any mole arithmetic. Remember to subtract the crucible mass from both readings first.

Let m₀ be the empty crucible mass, m₁ crucible plus hydrate, and m₂ crucible plus dry residue. Then hydrate mass = m₁ − m₀, anhydrous-salt mass = m₂ − m₀, and apparent water mass = m₁ − m₂. The crucible cancels only in the last subtraction. For 30.00, 32.50 and 31.22 g, those quantities are 2.50, 1.22 and 1.28 g respectively. Label all three before choosing the molar masses.

mwater = mhydrate - m_residue

Subtract the empty-crucible reading consistently. Water loss and dry residue must add to the initial sample mass.
Forgetting to subtract the crucible mass is the single most common data-handling error in this experiment.

Finding x

Convert the water mass to moles using 18.02 g/mol, convert the residue mass to moles using the molar mass of the anhydrous salt, then divide moles of water by moles of salt. That quotient is x. For the simple fixed-composition hydrates in this lesson, x is a small whole number. Decide whether a measured ratio supports that integer using the measurement uncertainty; a ratio such as 3.4 should trigger investigation rather than automatic rounding.

The ratio is x = [(m₁ − m₂)/18.02] / [(m₂ − m₀)/M(salt)]. The numerator counts water molecules and the denominator counts anhydrous formula units. Dividing their masses would not count waters because one water molecule and one salt formula unit have different masses. Use the anhydrous formula in the denominator even though the original sample was hydrated.

x = nwater / nanhydrous

Percent water as a cross-check

Percent water = mass of water lost divided by hydrate mass, times 100. Compare it with the theoretical value calculated from the proposed formula. For CuSO₄ . 5 H₂O the theoretical figure is 5(18.02)/249.68 = 36.08 %.

Agreement within the experiment’s uncertainty supports the formula; the acceptable difference depends on balance precision, sample size and the procedure.

Error analysis: which way does the result move?

Incomplete heating leaves water behind, so the measured water loss is too small and x comes out low. Overheating that decomposes the salt itself removes extra mass, so x comes out high. Spattering loses solid and also inflates the apparent water loss. A hygroscopic residue that reabsorbs moisture while cooling in open air lowers the apparent loss. Good practice is heating to constant mass and cooling in a desiccator.

The analysis assumes the only lost material is water and that the residue has the stated anhydrous formula. Spattering violates the first assumption; decomposition can violate both. Incomplete drying and rehydration make the numerator smaller and the apparent salt denominator larger, pushing x down in both ways. Heat gently at first to avoid loss, use the specified temperature, and cool before weighing so a hot crucible does not distort balance readings. Constant mass is necessary evidence of a stable endpoint, but a decomposed residue can also reach constant mass.

Do not just say experimental error. Say which direction the specific error pushes the result, and why.

Connecting back to empirical formulas

This is the empirical formula method with the elements replaced by two components, water and the salt. If you can determine x here, you can determine any empirical formula from mass data, because the reasoning is identical.

Review: Empirical and Molecular Formulas

Use the crucible mass and constant-mass test

A balance often reports crucible plus contents, not the sample alone. Subtract the empty crucible mass from both the initial and final readings; subtract the two sample masses to obtain the water lost.

Heat, cool in a dry environment and reweigh, then repeat until two successive masses agree within the experiment's tolerance. A stable mass supports completion of drying but does not prove the residue has not chemically decomposed.

Check the residue's appearance and the plausible hydrate ratio alongside the mass data. Moisture reabsorption during open-air cooling makes the final mass too high and the calculated water ratio too low.

Key ideas

Definition
Hydrate

An ionic compound whose crystal includes a fixed number of water molecules per formula unit.

Definition
Water of crystallisation

The bound water represented after the dot in a hydrate formula; it counts in the molar mass.

Rule
Lost mass is water

For a well-behaved hydrate, mass lost on gentle heating equals the mass of water driven off.

Rule
x must be a whole number

For the simple fixed-composition hydrates here, use uncertainty and the proposed salt identity to assess a small integer x; do not force an unsupported noninteger result to the nearest whole number.

Assumption
Only water leaves

The method assumes the anhydrous salt is thermally stable at the temperature used. Salts that decompose break this assumption.

Equation
Hydrate coefficient

x = (mwater / 18.02) / (manhydrous / Manhydrous)

  • x = moles of water per mole of anhydrous salt, a whole number
  • mwater = mass lost on heating, in g
  • manhydrous = mass of residue after heating, in g
  • use when = before and after heating masses are supplied
  • limits = assumes complete dehydration and no decomposition of the salt
Equation
Percent water in a hydrate

% H₂O = mwater / mhydrate x 100 %

  • mhydrate = mass of the hydrate before heating, in g
  • use when = cross-checking a determined formula against a theoretical percentage
  • limits = crucible mass must already be subtracted from both readings

Worked examples

Worked example 1

A 4.98 g sample of hydrated copper(II) sulfate is heated to constant mass, leaving 3.18 g of white residue. Determine x in CuSO₄ . x H₂O.

Try it first: Which of the two masses is the water, and which is the salt?

    0 of 4 steps revealed.

    Worked example 2

    A student determines x = 3.4 for a hydrate expected to be the tetrahydrate. Give the most likely cause and its direction.

    Try it first: Does an x that is too low mean too much or too little mass was lost?

      0 of 3 steps revealed.

      Worked example 3

      An empty crucible is 30.00 g; with hydrated MgSO₄ it is 32.50 g; after heating it is 31.22 g. Find x in MgSO₄·xH₂O. Use M(MgSO₄) = 120.37 g/mol.

      Try it first: Remove the crucible mass from both measurements.

        0 of 3 steps revealed.

        Common mistakes

        Common mistakes and better checks
        MistakeWhy it's wrongCheck instead
        Dividing the residue mass by the molar mass of the hydrate.The residue is the anhydrous salt, so using the heavier hydrate molar mass understates its moles and inflates x.Match each mass to the substance it actually is before choosing a molar mass.
        Using total crucible-plus-sample readings as the sample masses.Both masses are then too large by the same amount, which distorts the mole ratio even though the difference is unaffected.Subtract the empty crucible mass from every reading first.
        Reporting x = 4.6 as the answer.A hydrate has a fixed whole number of waters per formula unit, so a non-integer is evidence of experimental error.Round to the nearest whole number and explain the deviation, or identify the error if it is large.
        Explaining a deviation only as experimental error.It gives no chemical information and does not account for whether x came out high or low.Name the error and state which direction it pushes the measured mass loss.
        Treating the residue mass as the water lost.The two are swapped, so the calculated ratio is inverted and x is far from any sensible value.Write mwater = mhydrate - m_residue explicitly before calculating.

        Scroll horizontally if needed to read all columns.

        After the lesson · Question bank

        Independent practice

        Work through new problems on your own. The lesson's quick checks and worked examples stay above if you need to review a step.

        12 topic questions across 3 difficulty levels.

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        What you should now know

        Subtract the crucible mass, convert the apparent water loss and residue to their separate mole amounts, then assess the water-to-salt ratio. Inferring a hydrate requires a stable, correctly identified residue and evidence that only water was lost; constant mass and a plausible integer ratio support the assignment without proving it alone.

        • Subtract the empty crucible from both combined mass readings.
        • x is moles of water lost divided by moles of anhydrous salt.
        • Compare the proposed integer ratio and percent water with experimental uncertainty.
        • Incomplete drying or rehydration lowers x; spattering or decomposition can raise the apparent water loss.
        • Constant mass does not by itself establish that the residue has the correct composition.

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        Sources and further reading

        • Chemistry 2e, Section 3.1: Formula Mass and the Mole Concept
          Paul Flowers, Klaus Theopold, Richard Langley, William R. Robinson, et al. · OpenStax, Rice University · Chapter 3.1 · pp. Section 3.1 (web edition)
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          Recorded attribution / license claim (applicability unverified): Adapted from "Chemistry 2e" by OpenStax, Rice University, licensed CC BY 4.0. Changes were made.

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        • General Chemistry bookshelf (LibreTexts)
          LibreTexts, University of California, Davis
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