CHEM 163: SYNTHESIS AND ANALYSIS OF A COPPER(II)

COORDINATION COMPOUND
INTRODUCTION
In this multi-week experiment, you will synthesize a compound and then analyze it to determine its
empirical formula. The substance you will prepare is a vividly colored coordination compound of
copper. Based on the reagents used in the synthesis procedure, you can assume that the final
compound contains copperII!, ammonia, sulfate, and water. In your analysis, you goal is to figure out
the mole ratio of each component in the final compound. In other words, you will solve for x, y, z and
a in the formula "ux#$%!y&'(!z ) a$*'. Based on the way the formula is written you can assume that
ammonia and sulfate are acting as ligands and counter-ions, respectively. The water, in contrast, is
water of hydration. That is, it is incorporated into the crystal lattice of the solid compound in a
noncovalent manner, usually by hydrogen bonds, and with a specific stoichiometry.
Synthesis
To prepare your own sample of the coordination compound, you+ll start with solid copperII! sulfate
pentahydrate, "u&'( ) ,$*'. 'nce dissolved in water, the copper ions take on water molecules as
neutral ligands- copperII! ions exist as the hexa.uacopperII! complex ion in a.ueous solution. /fter
adding concentrated ammonia, #$% ligands displace the water molecules covalently bound in the
original copper complex, and a dramatic color change occurs. In your lab report, you will be able to
explain this color change using crystal field theory and the relative energies of copper+s d orbitals in
the two complexes.
The copperII! ammonia complex is a water-soluble ion0 in order to precipitate and isolate the final
product, an ionic compound, you need to decrease the solubility of the compound. / convenient way
of doing this is to add a large amount of ethanol, "$%"$*'$, to the a.ueous solution. 1thanol is
miscible with water but is much less polar, and, as the amount of ethanol in the mixture increases, the
solubility of ionic compounds decreases. /fter the addition of ethanol, your coordination compound
will appear as a crystalline solid, and the synthesis procedure ends with filtration, rinsing, and drying
of the visually stunning product. The next several parts of the lab involve analysis of your copperII!
coordination compound to determine its empirical formula.
Gravimetric Analysis of Sulfate
The amount of sulfate in your product will be determined with a simple gravimetric analysis, a method
that depends on the accurate weighing of a certain sample. 2ou will selectively react the sulfate in the
copperII! compound using an a.ueous solution of leadII! acetate. The entire sulfate in the copperII!
complex sample should precipitate as 3b&'( during this metathesis reaction. /fter careful filtering and
drying of the precipitate, you can use the mass of 3b&'( to calculate the amount of sulfate in the
sample of the copperII! compound.
Volumetric Analysis of Ammonia
2ou will measure the ammonia content of the product with a simple but colorful titration. / standard
$"l solution will be provided to titrate all the ammonia contained in a sample of your copperII!
compound. &ince this is a strong acid-weak base titration, the e.uivalence point occurs at p$ 4 5, and
methyl orange is a good indicator to use. 6ethyl orange changes from orange-yellow to red at the
endpoint of the titration0 however, due to the brightly colored copperII! compounds produced during
the titration you should observe several interesting color changes. The solution starts out deep blue
becomes a blue-green suspension, and then a pea-green suspension when 578 of the $"l has been
SCCC CHEM 163: Synthesis and Analysis of a Copper(II) Coordination Compound, !1"# "3$$%%&'()do*
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added. By the time :,8 of the acid has been added, the suspension is golden yellow. The endpoint
occurs when the suspension becomes a pumpkin-orange solution. / red-orange solution is passed the
endpoint.
Spectrophotometric Analysis of Copper(II)
The last analysis to conduct is by spectrophotometry, that is, the measurement of light and its
interaction with matter. In this situation, you can take advantage of the fact that a.ueous copperII!
ions absorb light in the visible region of the electromagnetic spectrum, as shown in the spectrum
below. #otice that maximum absorbance occurs around ;(, nm, which corresponds to orange light
<igure 9!. To your eye, the solution appears blue because blue light is not absorbed. That is, blue
light is transmitted through the sample, while orange light is absorbed.
#o other species in the copperII! compound not #$%, &'(
*-
, or $*'! absorbs visible light, so the light
absorbed by the entire sample at ;(, nm can be used as a measure of the amount of copperII!
present.= /ccording to Beer+s >aw, there exists a linear relationship between the molar concentration
of a species and the amount of light it absorbs for a specified range of concentration. 2ou can see
evidence of this with your own eyes, without any instrumentation- / copperII! solution with a
molarity of 7.7* 6 appears twice as dark as one with a concentration of 7.79 6. By using a
spectrophotometer, the relationship is .uantitative. ?iven the absorbance of a sample you can
calculate the concentration of copperII!.
Beer+s >aw is applied most accurately when a calibration graph is used. To do so, several solutions of
known concentration the standards! are prepared, and the absorbance of each is measured. /s shown
below on a sample calibration graph, a plot of absorbance /! vs. concentration molarity! will result
in a straight line, and the e.uation of this line can be determined by linear regression.
?iven a copper solution of unknown concentration, you can measure the absorbance of the unknown,
and then use the calibration graph to determine the molarity. <or example, using the calibration graph
in <igure *, if an unknown solution has an absorbance of 7.(,9, the concentration of the copper can be
calculated using the e.uation of the line.
=max also occurs at ;;, nm and @5,7 nm.
SCCC CHEM 163: Synthesis and Analysis of a Copper(II) Coordination Compound, !1"# "3$$%%&'()do*
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<igure 9
/bsorbance &pectra of
Aissolved "u&'(
A Bater
! 7.7C 6 #$%D7.7C 6 #$(
E
C 9 6 #$%
Figure 2
<inally, once the mass percentages of ammonia, copper and sulfate have been determined, the mass
percentage of the remaining component, water, is calculated by subtraction of the known percentages
from 9778.
PROCEDURE
General Notes
This lab will take about three lab periods to complete. 2ou and your instructor will work
together to plan a schedule for conducting all the parts of the experiment.
Feep your data well organized- There are several parts of this lab, and you may be collecting
data for more than one part at a time. /lso, note that you will write descriptive observations for
several parts, in addition to collecting .uantitative data in data tables.
Gespect significant digits in the recording of data and the calculations with that data.
Part I Synthesis of the Copper(II) Coor!ination Compoun!
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SCCC CHEM 163: Synthesis and Analysis of a Copper(II) Coordination Compound, !1"# "3$$%%&'()do*
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y H *.C%;!x E 7.797:!
7.(,9 H *.:5x E 7.77* max
7.(,9 H *.CCx E 7.79: min
max x H max I"u
*E
J H 7.9,; 6
min x H min I"u
*E
J H 7.9(, 6
Linear Regression Analysis of Absorbance of
Standardized Aqueous Cu(II) Solutions at 645 nm
0.000
0.100
0.200
0.300
0.400
0.500
0.600
0.700
0.800
0.00 0.10 0.20 0.30
Concentration ()
A
b
s
o
r
b
a
n
c
e
Standard Absorbance
Linear (Standard
Absorbance)
y = 2.93(6)x 0.010(8)
9. Beigh out 97 grams of copperII! sulfate pentahydrate "u&'( ) ,$*'! to the nearest centigram,
and record the actual mass used. Gecord your observations of the original compound+s appearance.
3lace the crystals in a *,7 m> beaker.
*. /dd about 97-9, m> of water to the solid and then, in a hood, add *7 m> of 9, 6 #$%
concentrated ammonia.! &tir to dissolve the crystals, carefully holding the beaker up to the light to
see whether crystals still remain.
%. 'ver a period of 9 minute, slowly add *7 m> of C,8 ethanol to the solution. &tir and cool to room
temperature. Gecord your observations of any change that occurs.
(. In a beaker prepare a %7 m> solution from 9, m> of concentrated ammonia and 9, m> of C,8
ethanol. 6ix well and set aside.
,. &et up a vacuum filtration apparatus using a vacuum flask, three pronged clamp, tubing, Buchner
funnel, and ring stand. >ay flat a circle of filter paper in the Buchner funnel, and moisten it with water
so that it lies flat and covers all the holes in the funnel. "onnect the apparatus to the vacuum nozzle
yellow handles! and turn on the suction. "arefully pour your reaction mixture into the funnel,
swirling the slurry of li.uid and solid as you go so that you transfer as many of the crystals as possible
into the funnel. If a significant amount of crystals stay behind you can retrieve them by scraping or by
using some of the filtrate mother li+uor!, in the filter flask, to rinse the crystals free. It is okay to
carefully disconnect the filtration apparatus to remove some filtrate, and then reassemble it all to
continue filtering.
;. 'nce all the mother li+uor has been sucked out of the crystals, use the solution you prepared in step
( to wash the crystals. Turn the aspirator off, make sure the vacuum is broken, and pour about 97 m>
of the ammonia-ethanol mixture into the funnel. Kse the smooth end of a fire-polished glass rod to
break up all clumps of solid, dispersing the crystals evenly in the solution. Be careful not to tear the
filter paper. Turn on the aspirator to remove the li.uid. Gepeat this two more times with the remaining
amounts of ammonia-ethanol mixture. In the same manner, wash the solid twice with 97 m> portions
of C,8 ethanol. <inally, wash the solid twice with 97 m> portions of acetone.
5. /t this point your crystals should be nearly dry. 2ou may continue rinsing with acetone if you feel
that the product is still wet with solvent. <inally, leave the aspirator on and pull air through the crystals
for about , minutes. Break up the crystals and lightly press them against the funnel so that the entire
sample becomes well dried. Gecord the appearance of your product at this point. Aoes it appear
homogeneousL
:. "eigh a large #atch glass and empty the crystals on to it, now weigh the watch glass and
compound. "over with a tissue and leave the sample in your drawer to continue drying until the next
lab period.
C. Bhen you return to lab make sure the final product is dry of all solvent. Gecord its mass to the
nearest centigram. /lso record the crystals+ appearance and note any heterogeneity to the sample.
SCCC CHEM 163: Synthesis and Analysis of a Copper(II) Coordination Compound, !1"# "3$$%%&'()do*
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PA$% II Analysis of Pro!uct
A& Gravimetric Analysis of Sulfate
9. To the nearest 7.9 milligram, weigh about 9 gram of your dry coordination compound in a 977 m>
beaker. Gecord the actual mass of the sample. 'btain a piece of filter paper for use in &tep (, and
record its mass to the nearest 7.9 milligram.
*. Aissolve the crystals in about 97 m> of ; 6 nitric acid.
%. 'btain about ,-; m> of 9 6 leadII! acetate. /dd it dropwise to the solution of your compound and
record observations of any changes that occur. "ontinue to add leadII! acetate until the precipitation
is complete-; m> of leadII! acetate may be sufficient. "heck for completeness- 9! allow the
precipitate to settle to the bottom of the beaker leaving a clear solution above the solid, *! add one
drop of leadII! acetate on the beaker wall, allowing the drop to run down the glass and into the
solution, and %! watch carefully for more precipitation as the leadII! acetate hits the clear solution.
The lack of precipitation after the addition of drops of leadII! acetate signals the completion of the
reaction.
(. "ollect all the precipitate and measure the mass accurately in the following manner. <irst, filter the
precipitate by gravity filtration. Kse a conical funnel and the filter paper you weighed in &tep 9, folded
in half once, then again. 'pen up the filter paper and gently push it into the funnel, using some water
to get the paper to adhere to the funnel and stay in place. The entire filtration process may take some
time- fill the funnel half full with the slurry, wait for it to drain, and repeat until all the reaction
mixture has been transferred to the filter. Bhile waiting for gravity to do its part, you can set up the
second trial of this part or work on any other part of this lab.
,. <or your results to be accurate, you must be absolutely sure that the entire sulfate has been
precipitated. "heck the filtrate for unreacted sulfate by adding a few more drops of leadII! acetate. If
more precipitate forms in the filtrate, you should add 9 m> of the leadII! acetate and refilter.
;. <or accurate results, you must also be sure that you have collected all the precipitate on the filter
paper, and that it is not contaminated with other substances. Kse small volumes of water to rinse out
any solid remaining in the original reaction beaker. <inally, rinse the solid and the filter paper with
additional amounts of water. Gecord your observations of the solid and the filter paper, during the
rinsing, and realize that appearance indicates when all copper-containing compounds have been rinsed
free. >ast, rinse the precipitate with about 97 m> of acetone.
5. ?ently remove the filter paper with the wet precipitate and place on a watch glass, where the solid
can continue to dry until the next lab period. Feep in mind that wet filter paper tears very easily, and
you do not want to lose any of your precipitate.
:. Gepeat steps 9-5, for a second trial.
C. Bhen the two samples are completely dry, record the mass of the solid and filter paper together, to
the nearest 7.9 milligram.
97. 2ou may choose to do a third trial of this analysis.
SCCC CHEM 163: Synthesis and Analysis of a Copper(II) Coordination Compound, !1"# "3$$%%&'()do*
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'& Volumetric Analysis of N()
9. To the nearest 7.9 milligram, weigh out about 9 gram of your compound, and record the actual
mass. Aissolve it in about %7 m> of deionized water in an 1rlenmeyer flask.
*. /dd 97 drops of methyl orange indicator, and titrate with the standard $"l solution provided for the
class. Aon+t forget to record the actual molarity of the standard $"l solution for your dataM! Geview
the description of the titration in the introduction of this experiment, so you know what progression of
colors to expect. Gemember that the disappearance of the precipitate is the clearest indicator of the
e.uivalence point, though the colors will help you know when the end point is approaching.
%. Gecord the results of your titration, and conduct a second trial. "heck to see if your two trials agree
within 98. 2ou can+t simply compare the final volumes of $"l used0 instead, divide the volume of
$"l by the mass of compound titrated for each trial. If these values agree within 98 for the two trials,
you don+t need to conduct a third trial. 'therwise, titrate a third sample.
C& Spectrophotometric Analysis of Copper(II) Ion
9. Geview the instructions for using the &pec-*7 spectrophotometers. /dNust the wavelength to ;(,
nm and allow the lamp to warm up.
*. 3repare 2 sets (*+ *,) of five standard solutions using the volumes in Table 9 as a guide. 3repare
these solutions in 2 x , clean, dry, and labeled test tubes. Be sure to mix the solutions well using a
pipet but do not remove the pipet. The copperII! stock solution and the nitric acid solution will be
available in self-zeroing burets. Be sure to record the actual volumes used, in your data tables, to the
proper number of significant figures.
Table 9- &tandard &olutions for &pectrophotometric /nalysis
&ample #umber Oolume of &tock "u
*E
&olution m>! Oolume of 9 6 $#'% m>!
7, 7+ 7.77 97.77
9, 9+ *.77 :.77
*, *+ (.77 ;.77
%, %+ ;.77 (.77
(, (+ :.77 *.77
4'ant%tat%0e&y prepare only two solutions of your own compound using the amounts shown in Table *
as a guide.
Table *- &olutions of the "oordination "ompound for &pectrophotometric /nalysis
&ample #umber 6ass of "ompound g! Oolume of 9 6 $#'% m>!
, /bout 7.9* 97.77
; /bout 7.*( 97.77
#ote- Aepending on time-constraints, your instructor may have you work with another student,
sharing data for the absorbance values of the standards. If so, it is important that you use the same
&pec-*7 as the other student0 the absorbance readings in your calibration curve and for your samples of
compound should all come from the same instrument.
SCCC CHEM 163: Synthesis and Analysis of a Copper(II) Coordination Compound, !1"# "3$$%%&'()do*
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%. Talk to the instructor about properly using the &pec *7. 'btain two matched cuvettes. Bith nothing
in the cuvette holder adNust the left knob such that the spectrophotometer reads 78 transmittance. Kse
one cuvette filled with deionized water to adNust right knob such that the spectrophotometer reads
9778 transmittance. Kse the other cuvette to record the absorbance values at ;(, nm of samples 7-(
and repeat these measurements with a freshly prepared set of standards, 7+-(+. 6easure the absorbance
of samples , and ; after each standard set has been measured.
CALCULATIONS
To calculate the formula of the coordination compound you synthesized, you will first use simple
stoichiometric calculations to determine the mass 8 of every component sulfate, ammonia, copper,
and water!. Then you will use the percent composition of the whole compound to calculate mole ratios
of the empirical formula0 that is, the su-scripts in the formula. $ere are some formulas and other
things to remember-

mass %=
mass of component
total mass of compound
100%

) 2ou will have two or three trials from the gravimetric analysis of sulfate. "alculate mass 8
&'(
*-
for each of the trials, and then a final average with standard deviation. If you have more than two
trials and one is an obvious outlier, you may choose to drop the problematic value, but you should note
this in your lab report or talk with your instructor about it.
) The mass of the precipitate collected in the gravimetric analysis is not pure sulfate, of course.
Kse the formula of the precipitate to convert grams of precipitate to grams of sulfate.
) Kse the stoichiometric ratio between ammonia and $"l in a simple neutralization reaction to
calculate the amount of #$% in your compound. 2ou don+t have to write a balanced reaction in which
$"l is reacting with the whole copper compound.
) <or the spectrophotometric data, calculate an average absorbance value for each standard and
unknown / H -logT H -log8TD977!. "onstruct a calibration graph as described in the introduction
and on page (7 and use it to calculate the molarity of copper in each of the two solutions of your
unknown, separately. <or each solution, use molarity and volume to calculate moles, and then grams
of copper in the sample.
) The mass 8 of water is determined by subtraction when the other three percentages are known.
) 'nce you have the mass 8 of every component, you can derive the empirical formula. If
needed, review your "$16 9;9 notes and text for a refresher. Gemember to round each coefficient to
integer values in your final formula.
SCCC CHEM 163: Synthesis and Analysis of a Copper(II) Coordination Compound, !1"# "3$$%%&'()do*
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C(./ 01) 2a- $eport Format
Synt,e"%" an# Ana&y"%" of a C'(II) Coo!#%nat%on Co$.o'n#
The partially #or!3processe! report will consist of the following C sections exact order is worth
points!. "or!3processe! sections are in -ol!.
9. %itle ,op of pa-e- 3rovide the experiment title in YOUR own words do not use the manual+s
title!, the date the experiment was performed, and your name first followed by your partner+s
name.
*. Intro!uction an! Purpose Ksing YOUR own words, interest the reader in the investigation
and explain what is being determined, -enerally how the investigation is conducted, and why
this determination is important in the greater sense. A0o%# .&a1%a!%"$ /y %t%n1 %nfo!$at%on
t,at %" not yo'!")
%. Proce!ure Kse the following reference-
>oftus, ".0 "abasco-"ebrian, T.0 Bick, A. P>aboratory 6anual for "$16 9;%Q spring *79*
1dition, Aepartment of "hemistry, &eattle "entral "ommunity "ollege, pp LLL
Include the relevant page numbers for the investigation. If you change a given procedure, you
must outline, briefly, exactly what was done differently. Bebsites may be referenced simply,
such as www.google.com. 2ou must also put in when the website was last updated.
(. $esults
1mbed a properly labeled table with units showing, for each trial, a! the mass of compound,
the mass of 3b&'(

E filter paper and the mass of the filter paper, b! the mass of compound and
the volume of L 6 $"l, and c! the mass of compound and the calculated concentration of
"u
*E
.
1mbed and complete a table similar to that below into your document.
&pecies &'(
*-
#$% "u
*E
$*'
Trial 9 8! %;.7;
Trial * 8! %C.5*
6ean8! %5.:C
&tdev8! *.,C
6eanstdev!8! %:%!
1mbed an absorbanceDconcentration table for each sample in each trial clearly showing original
absorbances and corrected absorbances
1mbed an excellent and properly formatted plot of absorbance vs. concentration standard
curve!.
6ake sure that a >I#1&T table is embedded and print the line e.uation with errors on your
plot.
SCCC CHEM 163: Synthesis and Analysis of a Copper(II) Coordination Compound, !1"# "3$$%%&'()do*
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,. "alculations- &how ./E detailed representative calculation significant digits important! each
for 8&'(
*-
, 8#$%, and 8"u
*E
. &how the calculations of the remaining water percentage and
empirical formula.
;. Conclusion (follo# -asic grammar an! spelling rules)- &tate the empirical formula of your
coordination compound.
5. 4iscussion If there are any uncertainties in your conclusion state these and explain alternative
possibilities. Be sure to calculate the 8 relative error only not the 8 relative uncertainty!.
2ou will need to consult other resources cite them! to determine the actual formula.
'bservations are crucial for supporting any alternative formula due to an impurity or
unexpected compound formation.
&) Post32a- 5uestions To be announced.
$) 0a1 2ata: Atta*h at the 3a*4 of your report a 5ero#ed *opy of 6a3 Staff si-ned ra1 data from
your note3oo4)
(o# to /a6e a Proper Stan!ar! Curve
9! /verage the two 9 6 $#'% blank absorbance readings.
*! &ubtract the average 0 / (N7) -lan6 a-sor-ance from each of the standard absorbance
readings 9-( /#A each 9 6 $#'% blank.
%! 2ou should have 97 data points to construct the standard curve * x (, "u
*E
solutions plus *,
9 6 $#'% solutions!
(! /dd a trendline and calculate slope and intercept with errors using a linest analysis.
Gecall that BeerRs >aw / H bc! has the y-intercept e.ual to zero. 2our line might be close to zero but
close to zero is still non-zero.
SCCC CHEM 163: Synthesis and Analysis of a Copper(II) Coordination Compound, !1"# "3$$%%&'()do*
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8ncertainty in
D
( 5(
D
) ((
D
n (
(
%
5
%
5

+ + = 0
m
s
y

=
5
%
5
%
) ( ( ) (( n D
9ou #ill calculate the uncertainty in : for each un6no#n
If you ha! run four trials of ;&2;;; g of compoun! use
the value of < in place of 0 for the first term of the s=uare root&
SCCC CHEM 163: Synthesis and Analysis of a Copper(II) Coordination Compound, !1"# "3$$%%&'()do*
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