Question
It is possible that ores containing basic copper(II) carbonate also contain water of crystallisation.
The formula of these ores would be written as xCuCO3•yCu(OH)2•zH2O.
In this experiment you will heat a sample of a different basic copper(II) carbonate which will thermally decompose as shown.
xCuCO3•yCu(OH)2•zH2O(s) (x+y)CuO(s) + xCO2(g) + (y+z)H2O(g)
You will use your results to determine whether this sample of a different basic copper(II) carbonate contains water of crystallisation.
FA 3 is a sample of a different basic copper(II) carbonate.
(a) Method
●● Weigh the empty crucible with its lid and record the mass.
●● Add all the FA 3 to the crucible.
●● Reweigh the crucible, lid and FA 3. Record the mass.
●● Support the crucible in the pipeclay triangle on top of the tripod.
●● Remove the lid.
●● Heat the crucible gently for about 1 minute and then strongly for about 4 minutes.
●● Replace the lid and allow the crucible to cool.
●● You may wish to start Question 3 while the crucible is cooling.
●● When the crucible has cooled, reweigh the crucible, lid and contents. Record the mass.
●● Calculate and record the mass of FA 3 used, the mass of residue and the loss of mass.
Results
I
II
III
IV
V
VI
[6]
(b) Calculations
(i) Assume the percentage by mass of copper(II) carbonate in FA 3 is 60.0%.
Calculate the mass of copper(II) carbonate present in FA 3.
mass of CuCO3 = …… g
Hence calculate the number of moles of copper(II) carbonate in FA 3.
moles of CuCO3 = …… mol
[1]
(ii) Use your results from (a) to calculate the number of moles of copper(II) oxide formed on heating FA 3.
moles of CuO = …… mol [1]
(iii) Use your answers to (i) and (ii) and the equation on page 5 to calculate the number of moles of copper(II) hydroxide in FA 3.
moles of Cu(OH)2 = …… mol [1]
(iv) Use your answer to (i) to calculate the mass of carbon dioxide produced by the thermal decomposition of the copper(II) carbonate in FA 3.
mass of CO2 = …… g [1]
(v)
Use your answer to (iii) to calculate the mass of water produced by the thermal decomposition of the copper(II) hydroxide in FA 3.
mass of H2O = …… g [1]
(vi) Deduce whether water of crystallisation is present in basic copper(II) carbonate FA 3.
Justify your answer using your results from (a) and your answers to (iv) and (v).
. ……
[1]
(c) (i) The lid was replaced before the crucible was cooled.
Explain how replacing the lid before the crucible was cooled may have increased the accuracy of your results.
. ……
. …… [1]
(ii)
Using the same apparatus, suggest an improvement to the method to increase the accuracy of your results.
. ……
. …… [1]
(iii) A student carried out the method in (a) and obtained inaccurate results.
The student suggested that not all of the copper(II) carbonate in the sample of basic copper(II) carbonate FA 3 had thermally decomposed.
Suggest a chemical test to determine whether the student was correct. Give the expected observations.
Do not carry out this test.
. ……
. …… [1]
[Total: 15]
Qualitative Analysis
Where reagents are selected for use in a test, the name or correct formula of the element or compound must be given.
At each stage of any test you are to record details of the following:
● colour changes seen
● the formation of any precipitate and its solubility in an excess of the reagent added
● the formation of any gas and its identification by a suitable test.
You should indicate clearly at what stage in a test a change occurs.
If any solution is warmed, a boiling tube must be used.
Rinse and reuse test-tubes and boiling tubes where possible.
No additional tests for ions present should be attempted.
3
FA 4 is a solid containing one cation and one anion.
FA 5 is a solution containing one cation and one anion.
Carry out the following tests and record your observations.
(a) (i) Warm (do not boil) a 5 cm depth of FA 5 in a boiling tube. Stop warming the FA 5, add all of the FA 4 and shake the boiling tube.
. ……
Filter the mixture into a second boiling tube. The filtrate will be used in the tests in (ii).
. ……
[2]
(ii) Use a 1 cm depth of the filtrate from (i) in separate test-tubes for each of the following tests.
test observations
Add aqueous ammonia.
Add a 1 cm depth of aqueous potassium iodide, then
add aqueous sodium thiosulfate.
(Rinse the test-tube when you have completed this test.)
Add a 1 cm depth of dilute nitric acid followed by a 1 cm depth of aqueous silver nitrate.
Add a 1 cm depth of dilute hydrochloric or dilute nitric acid followed by a 1 cm depth of aqueous barium chloride or aqueous barium nitrate.
[5]
(iii) FA 6 is a dry sample of the residue obtained by filtration in (i).
test observations
Add a 1 cm depth of dilute nitric acid to all of the FA 6 in its test-tube. Allow the mixture to stand for about 1 minute, then
add aqueous sodium hydroxide.
[2]
(b) (i) From your observations in (a), suggest the identity of the cation and the anion present in the filtrate produced in (a)(i).
cation present in the filtrate ……
anion present in the filtrate ……
[1]
(ii) Write an ionic equation for one reaction in (a)(ii) where a precipitate was formed. Include state symbols.
. …… [1]
(iii) State the type of reaction that occurred in the first part of (a)(iii).
. …… [1]
(c) A student suggested that FA 5 is an acid.
Apart from using an indicator, suggest and carry out a chemical test to determine whether the student was correct.
Record the name of the reagent you used, your observations and your conclusion.
[3]
[Total: 15]
Qualitative Analysis Notes
1 Reactions of aqueous cations
reaction with ion
NaOH(aq) NH3(aq)
aluminium, white ppt. white ppt.
Al 3+(aq) soluble in excess insoluble in excess
ammonium, no ppt.
–
NH4+(aq) ammonia produced on heating
barium, faint white ppt. is nearly always no ppt.
Ba2+(aq) observed unless reagents are pure
calcium, white ppt. with high [Ca2+(aq)] no ppt.
Ca2+(aq)
chromium(III), grey-green ppt. grey-green ppt.
Cr3+(aq) soluble in excess insoluble in excess
copper(II), pale blue ppt. blue ppt. soluble in excess
Cu2+(aq) insoluble in excess giving dark blue solution
green ppt. turning brown on contact green ppt. turning brown on contact iron(II), with air with air
Fe2+(aq) insoluble in excess insoluble in excess
iron(III), red-brown ppt. red-brown ppt.
Fe3+(aq) insoluble in excess insoluble in excess
magnesium, white ppt. white ppt.
Mg2+(aq) insoluble in excess insoluble in excess
off-white ppt. rapidly turning brown off-white ppt. rapidly turning brown manganese(II), on contact with air on contact with air
Mn2+(aq) insoluble in excess insoluble in excess
zinc, white ppt. white ppt.
Zn2+(aq) soluble in excess soluble in excess
2 Reactions of anions
ion reaction
carbonate, CO2 liberated by dilute acids
CO3 2–
chloride, gives white ppt. with Ag+(aq) (soluble in NH3(aq))
Cl –(aq)
bromide, gives cream ppt. with Ag+(aq) (partially soluble in NH3(aq))
Br –(aq)
iodide, gives yellow ppt. with Ag+(aq) (insoluble in NH3(aq))
I –(aq)
nitrate, NH3 liberated on heating with OH–(aq) and Al foil
NO3–(aq)
nitrite, NH3 liberated on heating with OH–(aq) and Al foil
NO2–(aq)
sulfate, gives white ppt. with Ba2+(aq) (insoluble in excess dilute strong acids)
SO42–(aq)
sulfite, gives white ppt. with Ba2+(aq) (soluble in excess dilute strong acids)
SO3 (aq)
2–
Mark scheme
2(a) I Tabulates / clearly lays out all data 1
II Appropriate headings and units for all items listed in the table 1
• mass (empty) crucible (+ lid)
• mass crucible (+ lid) + FA 3 / contents before heating
• mass crucible (+ lid) + contents after heating / residue
• mass FA 3
• mass of residue
• mass loss
Units: / g, (g), in grams.
Use of lid must be consistent.
III All recorded weighings to the same number of dp and all subtractions listed are correct (minimum 1) 1
Examiner checks subtractions then calculates and records the difference between the supervisor’s and candidate’s mass
ratio: mass FA 3 ÷ mass loss (all to 2 dp)
IV Award IV if δ ⩽ ±0.80 1
V Award V if δ ⩽ ±0.60 1
VI Award VI if δ ⩽ ±0.40 1
(Supervisor > 10.00, tolerances are 1.20, 0.90, 0.60; Supervisor > 20.00, tolerances are 2.00, 1.50, 1.00)
2(b)(i) Correctly calculates: mass CuCO3 from mass of FA 3 in (a) 1
60.0 × mass FA 3
=
100
AND
Correctly uses moles CuCO3 = answer/123.5
2(b)(ii) mass residue 1
Correctly calculates: from mass of residue in (a)
79.5
2(b)(iii) Correctly uses: (iii) = (ii) – (i) 1
2(b)(iv) Correctly uses: mass CO2 = n(CuCO3) × 44 1
2(b)(v) Correctly uses: mass H2O = (iii) × 18 1
2(b)(vi) mass loss in (a) – [(iv) + (v)] / comparison of values 1
AND
appropriate comment on presence / absence of water
2(c)(i) prevents absorption of water (vapour) from atmosphere 1
2(c)(ii) heat to constant mass / heat for longer to ensure all CO2 and H2O driven off 1
OR
increase the mass (of FA 3) (to reduce % error)
2(c)(iii) add (named) acid AND fizz / effervescence / bubbling / gas gives white ppt with limewater (means student correct) OR no fizz 1
indicates all CuCO3 decomposed
OR
reheat residue AND pass any gas through limewater which turns milky (means student correct) OR limewater does not turn
milky indicates all CuCO3 decomposed
FA 4 is Cu2O(s); FA 5 is H2SO4(aq); FA 6 is Cu powder