Detection of Ions in Solutions Using Acid/Base Chemistry: A Quality Control Test

Source: csip.cornell.edu/Curriculum!esources/.../T"annastudent#ersion.doc
Objective: This lab focuses on the detection of ions using titration as an analysis tool.
You will standardize NaOH and HCl solutions so that you know the eact concentration
and then !re!are sa"!les of co""on household ite"s in order to deter"ine the a"ount
of calciu" in Tang
#
$ %g&OH'
(
in %ilk of %agnesia$ etc. You will learn to !re!are
sa"!les of a s!ecified concentration$ learn about acids and bases through the use of
titrations and learn how to detect end!oints using different indicators. You will beco"e
ade!t at "easuring !H with both a !H "eter and indicator !a!er. You will then conduct
)uality control testers and deter"ine if the label on a bottle of over*the*counter !roduct
actually contains the !ercentage of co"!ound that it advertises.
$hat is a Titration%
+ titration is an analytical !rocedure used to deter"ine the concentration of a sa"!le by
reacting it with a standard solution. One ty!e of titration uses a neutralization reaction$ in
which an acid and a base react to !roduce a salt and water.
,n e)uation -$ the acid is HCl &called hydrochloric acid' and the base is NaOH &called
sodiu" hydroide'. .hen the acid and base react$ they for" NaCl &sodiu" chloride'$
which is also known as table salt. The titration !roceeds until the e)uivalence !oint is
reached$ where the nu"ber of "oles of acid is e)ual to the nu"ber of "oles of base.
This !oint is usually "arked by observing a color change in an added indicator.
,n a titration$ the standard solution goes in a buret$ which is a !iece of glassware used to
"easure the volu"e of solvent to a!!roi"ately /.- "0 of accuracy. The solution that
you are titrating goes in an 1rlen"eyer flask$ which should be large enough to
acco""odate both your sa"!le and the standard solution you are adding.
$hat is an Indicator and $hat is it Used &or%
+n indicator is any substance in solution that changes its color as it reacts with either an
acid or a base. 2electing the !ro!er indicator is i"!ortant because each indicator changes
its color over a !articular range of !H values. ,ndicators are either weak acids or weak
bases. 3or ea"!le$ !henol!hthalein is a weak acid &which we will re!resent as H,n'. ,n
a)ueous solution$ the !henol!hthalein dissociates slightly$ for"ing an e)uilibriu".

+n e)uilibriu" occurs when the a"ount of reactants and the a"ount of !roducts are
constant. .hen a syste" is in e)uilibriu"$ it will stay there until so"ething changes the
conditions. + fa"ous 3rench che"ist$ na"ed 0e Chatelier$ develo!ed a way to !redict
how changes in e)uilibriu" affect the syste". 0e Chatelier4s !rinci!le states that when
an e)uilibriu" is disturbed by a!!lying stress$ the e)uilibriu" will shift to relieve the
stress. In an acidic solution$ there is an ecess of H
5
O
6
ions so the e)uilibriu" will shift
to the left and favor the for"ation of H,n$ thus we o'ser(e a clear solution. In 'asic
solution$ there is an ecess of OH
*
ions that react with the H
5
O
6
ions to for" water. This
shifts the e)uilibriu" to the right because water is being for"ed and H
5
O
6
ions are being
re"oved$ thus )e o'ser(e a pin* solution. .e can use this color change to deter"ine
when the end of the titration has been achieved.
Table - lists co""on indicators and the !H range over which they change colors.
Ta'le +: Ta'le of Indicators
Indicator
Color change
inter(al ,p"-
Acid Base
thy"ol blue -.( * (.7 red yellow
"ethyl orange 5.- * 8.8 red yellow
"ethyl red 8.8 * 9.( red yellow
chloro!henol red :.8 * 9.7 yellow ;ed
bro"othy"ol blue 9.( *<.9 yellow =lue
!henol red 9.8 * 7./ yellow ;ed
thy"ol blue 7./ * >.9 yellow =lue
?henol!hthalein 7./ * -/./ colorless ;ed
alizarin yellow -/./ *-(./ yellow green
.easuring p": "o) to Cali'rate a p" .eter
!H is a "easure of acidity or basicity. +n acid has a !H less than <$ a neutral co"!ound
&like water' has a !H near <$ and a base has a !H fro" <*-8. !H can be "easured using
either lit"us &or indicator' !a!er$ which changes color based on the acidity of a solution$
or by using a !H "eter. + !H "eter is a "ore accurate "eans of "easuring !H because
it can be calibrated to "easure one tenth of a !H unit$ whereas the indicator !a!er only
"easures to one !H unit.
+ !H "eter uses an electrode to "easure the !H of a solution. The electrode is stored in
distilled water in order to kee! it at a neutral !H.
To cali'rate the p" meter:
-. ;e"ove the electrode fro" the distilled water and !lace it in !H 8 buffer$ which is
!ink. %ake sure the electrode is co"!letely covered in buffer and swirl the
solution around.
(. 2et the !H "eter to !H 8 and then rinse the electrode with distilled water to
re"ove any ecess solution.
5. ?lace the electrode in !H -/ buffer &which is blue' and swirl it around in the
solution.
8. 2et the !H "eter to !H -/ and rinse the electrode$ returning it to the distilled
water once you are finished.
The !H "eter should now be calibrated to "easure any !H accurately.
Standardi/ing a Sodium "ydro0ide ,1a2"- Solution
,n a titration$ it is critical to know the eact concentration of the titrant &the solution in the
buret which will be added to the unknown' in order to deter"ine the concentration of the
solution being tested. .e will standardize the @/.- % NaOH solution &the titrant' with
!otassiu" hydrogen !hthalate &AH?$ AC
7
H
8
O
8
H' using !henol!hthalein as the indicator.
AH? is a weak acid and reacts with base in the following way:
To Standardi/e:
-. .eigh @/.7 g of dried AH? &%. B (/8.(5 gC"ol' into an 1rlen"eyer flask and
dissolve in :/*<: "0 of distilled water. ;ecord the a"ount of AH? and water
used.
(. +dd 8 dro!s of indicator into the flask and titrate to the first !er"anent
a!!earance of !ink. Near the end!oint$ add the NaOH dro!wise to deter"ine the
total volu"e "ost accurately.
5. Calculate the concentration of NaOH in the following way:
Calculate Concentration of AH?:
Calculate Concentration of NaOH:
!emem'er: There are +333 m4 in a 4 and +333 mg in a gram.
8. ;e!ort the concentration of NaOH to the class. +n average nu"ber will be
deter"ined to give the "ost reliable value of NaOH concentration. Do not
discard the re"aining NaOH E you will use this for the rest of these e!eri"ents.
Standardi/ing an "Cl Solution
,n a titration$ it is critical to know the eact concentration of the titrant &the solution in the
buret which will be added to the unknown' in order to deter"ine the concentration of
solutions being tested. .e will standardize the @/.- % HCl solution &the titrant' with
sodiu" carbonate &Na
(
CO
5
' using !henol!hthalein as the indicator. Na
(
CO
5
is a base and
reacts with the strong acid HCl in the following way:
To Standardi/e:
-. .eigh @/.( g Na
(
CO
5
into an 1rlen"eyer flask and dissolve it in :/ "0 of boiled$
cooled distilled water. ;ecord the eact a"ount of Na
(
CO
5
used in your
notebook. &The water is boiled to e!el CO
(
fro" the solution.'
(. +dd 8 dro!s of !henol!hthalein to the solution and record the color.
5. Titrate with the HCl until just before the end!oint &when the solution is very light
!ink' and then gently boil the solution to e!el the CO
(
fro" solution that has
been !roduced during the reaction &see e) 8'.
8. Cool the solution to roo" te"!erature and then wash the sides of the flask with a
s"all a"ount of H
(
O to get all of the sa"!le back into solution.
:. 3inish the titration &this will take F1;Y little HCl so go slowG'
9. ;ecord the color of the solution and the volu"e of HCl used.
<. Calculate the concentration of HCl in the following way:
Determination of .agnesium "ydro0ide 5.g,2"-
6
7 Content in .il* of .agnesia
%ilk of "agnesia is a viscous$ "ildly basic "iture that is used to treat u!set sto"ach
and occasionally to !revent consti!ation. +ccording to standards set by the
!har"aceutical industry$ "ilk of "agnesia should contain at least <H %g&OH'
(
by
weight. .e will be doing detective work to see if the !har"aceutical industry is being
truthful in their clai" by deter"ining the weight !ercent of "agnesiu" hydroide in
different bottles of "ilk of "agnesia.
+n accurate analysis of "ilk of "agnesia "ust "easure the total %g&OH'
(
both dissolved
and sus!ended in solution. This is tricky because "ilk of "agnesia eists as a white
o!a)ue solution so each sa"!le "ay not be re!resentative of the whole bottle. To "ake
the solution as ho"ogeneous as !ossible$ the bottle "ust be shaken thoroughly.
Direct titration of "ilk of "agnesia is difficult due to the cloudy sus!ension and the fact
that so"e of the solution "ay cling to the sides of the flask$ !reventing co"!lete titration
and altering the "easure"ent of the end!oint. The o!a)ue solution "ay also "ake it
difficult to detect the color change of the end!oint.
3or this reason$ a back titration will be used to "easure the weight !ercent %g&OH'
(
in
"ilk of "agnesia. 1cess HCl will react with all of the %g&OH'
(
to yield a clear solution
and then the ecess unreacted acid will be back titrated with standardized NaOH. The
reactions in this titration are as follows:
8rocedure:
-. Obtain a vial filled with between -*-.: g "ilk of "agnesia and weigh the vial and
sa"!le without the lid on. ;ecord the value.
(. ;inse the contents of the vial into a (:/ "0 1rlen"eyer flask with distilled water
and dilute the solution to :/ "0 total volu"e. 1tra water can be used if "ilk of
"agnesia re"nants re"ain in the vial.
5. +dd a "easured a"ount of HCl &fro" a buret' into the beaker until the solution is
clear and then add an additional -*( "0 HCl to ensure there is an ecess of acid.
;ecord the volu"e of HCl added. &3or a - g sa"!le of "ilk of "agnesia$ this
should be at least 5/ "0 HCl.' %easure the !H of the solution using a !H "eter
or !H !a!er and record the value.
8. +dd 8 dro!s of indicator &what color is the solutionI' and titrate the solution with
standardized NaOH. The titration will go )uickly$ with less than : "0 of NaOH
re)uired. ;ecord the volu"e of NaOH used and the color of the solution.
%easure the !H of the solution again and record the value.
:. ;inse the vial with distilled water and dry in an oven or in a "icrowave for -
"inute. .hen dry and cool$ weigh the vial to deter"ine the actual weight of the
"ilk of "agnesia sa"!le. %ake sure there is no water left in the vialG This will
skew your resultsG ;ecord the weight.
9. Calculate the weight !ercent of %g&OH'
(
in "ilk of "agnesia using the following
e)uation:
Calculate the weight !ercentage of %ilk of %agnesia:
<. ;e!eat with another sa"!le of "ilk of "agnesia fro" a different bottle to see if
the weight !ercent of %g&OH'
(
is consistent fro" sa"!le to sa"!le.
Questions:
-. .ould the weight !ercentage of %g&OH'
(
be higher or lower if so"e of the "ilk
of "agnesia sa"!le got stuck on the sides of the flask and was not titratedI 2how
the thought !rocess for your answer.
(. .as there a consistent a"ount of %g&OH'
(
in each bottle of "ilk of "agnesia$ or
did the values changeI .as the change dra"atic or s"allI
5. How would the weight !ercentage of %g&OH'
(
change if the weight of the sa"!le
was "easured incorrectly &for ea"!le$ the vial was not washed thoroughly or
so"e water re"ained$ changing the weight'I
8. ,f you deter"ined a different weight !ercent of %g&OH'
(
other than @ <H$ what
do you think is the reasonI ,s there so"ething in your deter"ination that went
wrong or are !har"aceutical co"!anies giving us false infor"ationI
Standardi/ing an 9DTA ,ethylenediamine tetraacetic acid- Solution
,n a titration$ it is critical to know the eact concentration of the titrant &the solution in the
buret that will be added to the unknown' in order to deter"ine the concentration of the
solutions being tested. .e will standardize a @/./- % 1DT+ solution &the titrant' by
adding it to a calciu" carbonate &CaCO
5
' solution using hydroyna!hthol blue as the
indicator. 1DT+ is used because it can chelate &bind to a "etal ato" through "any
different bonds' so that it ca!tures and surrounds the calciu" in solution. 1DT+ can
ca!ture the "etal through any of its si donor ato"s$ indicated by boes. ,n this
e!eri"ent$ one "olecule of 1DT+ ca!tures one ato" of calciu".
1DT+
To Standardi/e:
-. .eigh @/.(: g CaCO
5
into a (:/./ "0 calibrated flask and dissolve it in a
"ini"al a"ount of concentrated HCl. Then dilute with distilled water to the
(:/./ "0 "ark. ;ecord the eact a"ount of CaCO
5
used in your notebook.
(. Calculate the concentration of CaCO
5
in the following way:
5. Transfer (:.// "0 &"easured with a calibrated !i!ette' into a (:/ "0 1rlen"eyer
flask and dilute with an e)ual volu"e of water.
8. +dd - % NaOH to raise the !H to -( &"easure with a !H "eter or !H !a!er'. ,f
the !H dro!s below !H -( during the titration$ add additional NaOH.
:. +dd 8*7 dro!s of hydroyna!hthol blue indicator to the solution and record the
color.
9. =egin adding 1DT+ until the color change is observed. ;ecord the color of the
solution and the volu"e of 1DT+ necessary to achieve this change.
<. Calculate the concentration of 1DT+ in the following way:
Determination of Calcium in Tang
:
'y Bac* Titration
Tang
#
is an orange drink that serves as an orange juice substitute$ and astronauts drink
Tang
#
because it is easy to trans!ort to s!aceG Tang
#
boasts that it is a Jgood source of
calciu"K des!ite containing only a fraction of the "ini"u" daily re)uire"ent of Ca
(6
.
To test the "anufacturer4s clai"$ we will deter"ine the a"ount of calciu" in Tang
#

through the use of a co"!leo"etric titration.
+ co"!leo"etric titration is a ty!e of titration where a co"!le is for"ed between an
analyte and a titrant. The analyte is the ion you are testing for$ here Ca
(6
. The titrant is
the 1DT+ that was !reviously standardized. During the course of the titration$ the 1DT+
will ca!ture one "olecule of Ca
(6
and bind to it$ for"ing a colored co"!le.
During the forward titration$ each "olecule of 1DT+ will ca!ture one "olecule of Ca
(6
.
.hen all of the Ca
(6
is co"!leed$ the solution will change color and you will observe
the end!oint. To check yourself$ you will add additional 1DT+ to the solution and
!erfor" a back titration. Now there is ecess 1DT+ floating in solution but no Ca
(6
to
bind to it. =y adding CaCO
5
$ the 1DT+ can bind to the new source of Ca
(6
$ which leads
to the net color change when all of the Ca
(6
has found an 1DT+ "olecule.
The color change at the end!oint will be hard to see due to the orange nature of the Tang
#
solution$ so it will be necessary to !erfor" a back titration. The !H "ust be "aintained
at !H -($ which is where the indicator hydroyna!hthol blue is effective.
8rocedure:
&or)ard Titration:
-. %easure between -5*-8 g of Tang
#
into a (:/./ "0 volu"etric flask. 3ight the
te"!tation to drink the Tang
#
G ;ecord the eact weight you "easured. Dilute to
the line on the flask with distilled water.
(. %easure (:./ "0 of the Tang
#
solution &using a calibrated !i!ette' and !lace it
into an 1rlen"eyer flask. +dd an additional :/ "0 of distilled water to the flask.
5. +dd -/*(/ dro!s of hydroyna!hthol blue indicator.
8. +dd - % NaOH until the !H of the solution is -(. &%easure the !H with a !H
"eter or !H !a!er.'
:. Titrate with the 1DT+ solution until you observe the end!oint. ,t is critical that
you record the volu"e of 1DT+ usedG ;ecord the color change.
Bac* Titration:
9. +dd an additional 8*: "0 of 1DT+ to your solution and record the added
volu"e.
<. Titrate the solution with CaCO
5
of a known concentration until you observe a
color change. ;ecord the volu"e of CaCO
5
used and the color of the solution.
Calculate the a"ount of Ca
(6
in Tang
#
:
,f the end!oint was reached accurately in the direct titration$ both calculations should
give you the sa"e value for the a"ount of Ca
(6
in Tang
#
.
Questions:
-. Do you think this is a large a"ount of calciu"I ,s this "ore or less than the
a"ount of calciu" found in "ilkI
(. ,f you overshot the first end!oint &added too "uch 1DT+'$ would you calculate
"ore or less calciu"I
This material was developed through the Cornell Science Inquiry Partnership program (http://csip.cornell.edu), with
support from the National Science Foundations raduate Teaching Fellows in !"#$ %ducation (!"#$) program
(&% ' ($)#*#) and ' **+*,#-) and .ornell /niversit0. 1n0 opinions, findings, and conclusions or recommendations
e2pressed in this material are those of the author(s) and do not necessaril0 reflect the views of the NSF.