Actiaity No.

10

DETERfuIINATION OF IRON IN A FERRIC CHLORIDE SOLUTION

BY PERIVIANCANATE ]ITRATION

One of the most important applications of permanganate titration is the

determination of iron ores such as hematite (Feze), magnetite (Fqoa),
geothite (Fe2O3r11rO), and limonite (2Fe2O3o3HzO). This is done by first
dissolving the iron compounds present in the ore, then reducing the iron (III)
or ferric ions in the solution to iron (II) or ferrous ions, and finally titrating
the ferrous ions to the ferric state with standard permanganate.
Hydrochloric
acid is the best acid for dissolving the ores because of the ability of chloride
ions to tie up the iron in the forrn of complex ions (e.g. FeCl4i FeCl2+, and
FeCl53-; while [n (II) or stannous chloride is normally used for reducing
the
iron (IIf in a sample which has been dissolved. in hydrochioric acid.

In this experiment, the amount of iron (Fe) lMolar weight = 55.g5J in a

sample is to be determined using pernftanganate tihation. However, instead
of using an iron ore, the unknown sample to be used. here is a ferric chloride
solution. This shortens the time of analysis i.vhile making it a lot easier.

Some of the chemical reactions involved are

Fe3+ + 4HCl ---+ FeCla- + 4H+

2FeCla- + Sn++ ----> 2Fe++ + SnC162- + ZCI-

MnOa- + SFe++ + 8H+ Mn++ + 5Fe3+ + 4H2O

-->
PROCEDIIRE:

L. Deliver from a transfer pipet or measuring pipet (recall Figure 14 and

Figure 15, P. 40) triplicate samples of exactly 5.00 mL each (or as specified
by your instructor) into three labeled (L II, m) 25Q-mL beakers or flasks.
 Dilute each sample with 20 mL of distiled water, and add
20 mL of 6 N
HCI.

Heat the acid solutions nearly to boiling. with the beaker

against a white
background, add dropwise 1 N snCl2 solution untii the
solution changes
from yellow to colorless, indicating
that the ferric ions have just been
reduced to ferrous ions. Do not ad.d morc than a drop or
two in excess,
and keep the solution hot during the entire reduction. If
too much SnCl2
is added, add permanganate dropwise until the yellow color refurns;
then
add SnCl2 as before.

A
=. cool completely and without delay add rapidiy 30 mL of Hgcr2 solution
to
the first solution (Triat I) only. A white, silky precipitate should form.
If
there is no precipitate, insufficient SnCl2 has been used; if the precipitate
is at all gray or dark in color, too much snClz has been used. In either
case, the solution shouid be discarded.

5. Allow the above solution to stand for 5 minutes and then transfer the
solution into a clean 500-mL beaker or flask. Rinse the container several
times with distilled water and add the washings into the main solution in
the 500-mL container.

6. Dilute the solution to about 400 mL with cold distilled water, and add 25
mL of MnSOa titrating solution.

7' Titrate the cold solution at once with standard permanganate to a faint
pink color that remains for i.5 seconds or more vrhile the solution is
stirred or swirled. (Be sure to record the initiat buret reading before
titratian!\. When this end point is reached, record the finai buret reading.

8' Then repeat Procedures 4 to 7 using the solutions for Trials Ii and III.

Reference:

Hamiltory L. F. and simpson, s. G., euantitatiae Chemical Analysis, r2*t

Edition, The Macmillan.Companlr New york (1,gT0), pp. ZZfAg.
 53

Actiaity No. i_A

DETERfuIINATION OF IRON IN A FERRIC CHLORIDE

SOLUTION
BY PERfuIANGANATE TITMTION

Error, /o
Rating, %

Deductions, %

Net Rating, /o =

DATA AND RESULTS:

Example

Volume of sample, mL 5.00

Final reading, mL KMnO4 22.61

lnifial reading, mL KMnOa 0.65
Volume, mL KMnOa 21,.96

From Preaious Actiaity:

Normality of KMnO4 = 41467

Calculated Amounts of Fe:

grams Fe 0.1799
milligrams Fe 179.9

Calculated Concentration of Fe:

mg Fe/mL
 54

STATISTICAL EVALUATION OF RESULTS (me

Fe/mL):

Mean, i
Median, M
Standard Deviation, s
Rel. Std. Deviation" RSD (%)
Std. Deviation of the Mezur, S

REPORTED VALUE (mg Fe/mL)

 Actiaity No. 11

DETERJVI I NATION OF JVL\NCAI\ ESE I N PYROL USITE

Another important apptrication of permanganate fitration is the

determination of the percentage of manganese or manganeEe
dioxide in
pyrolusite, the most important ore of manganese which
is principally
manganese dioxide (MnOd. This is usually done by ut indirect
method in
which the manganese dioxide is reduced and dissolved in the presence
of
H2soa by u measured amount of an excess of a reducing agent
such as
arsenious oxide, ferrous sulfate, or sodium oxalate. After
the reduction
Process' the excess reducing agent is determined by tikation with standard
permanganate.

In this activity, the % Mn (Morar weight = s4.g4) in pyrolusite is

determined, with Na2C2oa (Morar weight : 134.00) as the reducing
agent.
The chemical equation for the reduction process is

MnO2 (s)+ C2Oa= + 4H+ --+ Mn++ + 2CO2 + 2H2O

For the subsequent titration of the excess red.ucing agent with standard
permanganate, the chemical equation is

SHzCzO+ + 2MnO+- + 6H+ _-* 10COz + 2Mn++ + gH2O

PROCEDURE:

1' Weigh out accurately (by the method of difference) from a weighing
bcttle
into three 400-mL beakers (labeled I, iI, III) kiplicate samples (about
0.10xx
g each) of the manganese ore (previously ground to fine powder and
dried in the oven).

2. Weigh put accurately also (by the method of difference) into the
beakers
containing the ore sampies about 0.35xx g each of pure sodium oxalate
(previously dried). (This amount is approximateiy 0.20
g in excess of the
 56

theoretical amount required to react with 0.10 g of pureMno2 according

to the equation:

MnO2 (s)+ CzO+= + 4H+ -----> Mn++ + 2CAz + 2H2O

3. Pour into each beaker 25 mL of distilled water and 50 mL of 6N Hzso+.

Cover the beaker with a watch glass and warm gently, preferably over a
water bath, until the evolution of COz ceases and the residue is free from
black particles. (Do not let the solution eaaporate to any extent to preaent
the formation of concentrated H2soa which is corrosiae).

4. Finally, slowly and carefully dilute the solution to about 250 mL with
distilled water, heat to just below boiling, and while hof tikate the excess
oxalate with standard permanganate.

5' From the data obtained, calculate the percentage of manganese in the ore
sample.

Reference:

Hamiltoru L. F. and simpson" s. c., euantitatiae chemical Ana1ysis, r1th

Editioru The Macmillan Companlr New york (1.grq, pp.2l4-2J5.
 c/

Actiuity No. 1,1

DETER]VIINATION OF MANCANESE IN PYROLUSITE

Enor, /a
Ratl;ng, %

Deductions, %

Net Rating, /o =

DATA AND RESULTS:

Weighing of pyrolusite sample:

Wt. of bottle with ore sample, g 79.892A
Wt. of bottle with sample minus sample,g 79.7894
Weight of ore sample taken, g 0.1026

Weighing of pure Na2C2Oa:

Wt. of bottle with oxalate, g 36.8674
Wt. of bottle with oxalate - oxalate, g 36.5142
Weight of oxalate taken, g 0.3s32

Final reading, m[, KMnOa 21.M

Ldtial reading, mL KMnOa 0.00
Volume, mL KMnOa 21,.34

From Previous Actiuity:

Normality of KMnO4: IV 0.1,467
Molarity of KMnO4 M 0.029u

millimoies Na2C2Oa
 58

millimoles KMnOa 0.63

millimoles KMnOa in terms of Na2C2O4 1".57
net mmoles = mmoles MnOZ = mmoles Mn 1,.47

Calculated. Percentage:
%Mn

STATISTICAL EVALUATTON OF RESULTS (% rvrr,),

Mean, i
Median, M
Standard DeviatiorL s
Rel. Std. Deviation, RSD (%)
Std. Deviation of the Mean, S

REPORTED vALItE (% vtny

 Actiaitv No. L2

DETERIVIINATION oF THT VOLUMETRIC RATIO oF

IODINE AND THIOSULFATE SOLUTIONS

The reaction between iodine and thiosulfate solutions is another

oxidation-reduction reaction which is of great importance
in analytical
chemistry, parfcularly in volumekic anaiyses. In fact,
the titration of iodine
against thiosulfate or vice versa, is considered as
one of the most accurate of
volumetric processes. Tikation invorving iodine is called
iodimetry (if
iodine is the titrating agent) or iod.ometry (if thiosulfate
is the titrating agent).
In any case, the reaction involved is

12 + 2NazSze ----> 2NaI + Na2SaO6

The usual indicator for iodimetric and iodornetric titrations

is a colloidal
dispersion of starch, which in the presence of iodide ions, give
s a deep blue
color with even fuace amounts of free iodine (Iz). The color is
due to the
formation of adsorption compcunds of complex and variable composition
(iodo-starch complex).

12 + starch ---> iodo-starch complex (deep blue color)

In,'this experiment, the volumetric ratio of the two soiutions,

iodine and.
thiosulfate, is determined by titration. After standardization
of either one of
the solutions, the normality of the other can be caiculated
from this ratio.

PROCEDURE:

I. Preparation of Solutions (0.j. N 12 and 0.1 N NazSzGs)

A. 0.1 N lodine Solution (250 mL)
(Note: Before beginning this part, do procedure 8.1,
bnly) first, to saae time)

1. Weigh out separately on a watch glass (using an ordinary platform

balance) 3.3 grams of iodine (Id crystais and 10 grams of potassium
iodide.
 60

2. Place the 12 and KI in a clean porcelain mortar and kifurate with small
portions of distilled water until all is dissolved. (Trituration
is the
process whereby a sorid is grouncr in contact
with a riquid).

3. Transfer the solution into a 400-mL beaker and

dilute to 250 mL with
distilled water.

A
't. If it is not certain that the iodine has completely dissolved,
filter the
solution through a small wad of glass wool or cotton
using a filter funnel.

5. Finally, transfer the sorution into a crean and, properly-Iabered

bottre and
mix thoroughly. Present to your instructor for approval.

B, 0.1 lf Thiosulfate Solution (250 mL)

l. Boil around 400 mL of distiled water in a 400-mL beaker.

Cover the
beaker and allow to cool (under running water or
in a cool ice-water
bath.)

2. weigh out sn a watch glass (using an ordinary platform

baiance) 6.3
grams of sodium thiosulfate (Na2S2O3rSHzO).

3. Dissolv,€ the thiosulfate in around 200 mL

of the previously boiled
distilled water in a 400-mL beaker. Dilute the resuiting
solution to 250
mL.

Test the acidity of the soiution with lihnus

paper. If it is acid, dissolve in
it solid Na2Co3 (in small increments and not more than 0.025 g) until the
solution is neutral or very slightly alkaline.

Transfer the solutipn in a clean and properly-labeled

bottle and shake
vigorously to ensure homogeneity. Present to your inskuctor for
approval.
 hl

tr. Preparation of starch Indicator solution (50 mL)

The starch solution must be freshly prepared, since on standing

it is
attacked by molds and becomes unsuitable for use. The
50 mL of prepared
solution may be shared by 5 students. Thus, only L sfudent may
need to
prepare the solution for every 5 students. However, one is
not prevented
from preparing his own starch solution.

1
I. Grind out 0.25 g of starch thoroughly in a small mortar with a
small
amount of distilled water untii a smooth paste is formed.

2. Pour slowly into 50 mL of boiling distilled water in a 100 mL

beaker. Boil
for a minute or tr,vo, and decant into a small glass-stoppered and
properly-
labeled bottle. lNote: A Lipovitan or Reil Butt bottle (with
product label
remoaed) can be used as cantainer of your starch solutionl.

Itr. Volumetric Ratio Determination

1. Rinse your acid buret (previously cleaned) two times with

5-mL portions
of the prepared 0.i. N 12 solution. Discard the washings.

2. Do the same for the base buret (previously cleaned) using the
prepared 0.L
N Na2S2Q solution.

3' Fill the acid buret with the iodine solution and the base buret
with the
thiosulfate solution.

4. Adjust the initial readings of both burets to zero or near zero.

5' Run out around 20 mL of the thiosulfate solution into a clean

250-mL
erlenmeyer flaslq dilute with 100 mL of distilled water, and
add 4 mL of
the freshly prepared starch indicator soiution.

6' Titrate the thiosulfate solution with the iodine solution to the
appearance
of the blue color of the iodo-starch complex.
 62

7 ' When the end point is reached, record the final readings of both burets.

8. Do two more trials. Record the results in your answer sheet, and calculate
the ratio of the two solutions. (Nofe; For your conaenience, the second
column of the data table shows results of sample calculations.)

Reference:

Hamilton, L. F. and simpson, s. G,, euantitatiue chemical Anatysis, r1th

Edition, The Macmillan Company, New york (1920), pp.263-265.
 63

Actiaity No, 12

DETER]VIINATION OF THE VOLUMETRIC RATIO OF

IODINE AND THIOSULFATE SOLUTIONS

Instructor's Approaal Signatures for the. Prepared Solutions:

0.1 N 12: ; 0.1 N Na2S2O3:
DATA AND RESIJLTS:

Exampie

Final reading, mL 12 22.21

Inital reading, mL 12 0.1s
Net volumen mL 12 22.46

Final reading, mL Na2S2Ca 20.62

Initial reading, mL Naz5ze 0.11
Net volume, mL NazSzQ 20.51

1,000 mL 12 -
mL NazSzQ? 0.9297
1.000 mL Na2S2Q = ? mL 12 LA76

STAT|STICAL EVALUATTON OF RESULTS (RAT|OS);

Mean Values:
1.000 mL 12 = ? mL Na2S2e mL Na2S2C3
1.000 mL Na2S2Q = ? mL 12 mL 12

Median Values:
1.000 mL = ? mL NazSze
12
mL Na2S2O3
1.000 mL Na2S2Q - ? mL 12
mL 12

REPORTED VALUES:
1.000 mL = ? mL NazSze
12 mL NazSzQ.
1.000 mL NazSzOg - ? mL 12
mL 12
 u
Actiaitv No. 13

STANDARDIZATION OF IODINE SOLUTION

ACAINST ARSENIC OXIDE

In a neuhal solution, iodine reacts quantitatively with arsenite

ion,
AsO33-, oxidizing it to arsenate ion AsO43-,
according to the forward reaction
of the reversible equation

H3AsO3 + Iz + H2O a= H3AsOa + 2I- + 2H+

such reaction is the basis for the standardization

of iodine against arsenic
oxide, Asze (Molar Weight : lg1.g4) as well
as for the iodometric
determination of arsenite. In the standardization
process, the standard
arsenic oxide is converted into arsenite ion
bv dissolving in sodium
hydroxide according to the equation

AszQ + 6OH- --> 2AsO33- + 3H2O

In the presenceof bicarbonate iory FICO3-, which serves to

make the
solution neutral, the arsenite ion is then tih.ated
with iodine to the
appearance of the blue color of iodo-starch
complex. The reaction during
titration is

H3AsO3 + 12 + 2HCO3- H3AsOa + 2I_ + ZCOz + H2O

-->
PROCEDURE:

1' weigh out accurately (by the method of difference) from

a weighing bottle
into three 250-mL erlenmeyer flasks (labeled I, II,
III) tripticate portions of
0'175x - 0'200x g each of pure AszQ which has
been previously dried far 2
hours at 105oC.

2' Add 2 mL of 6 N NaoH to each flask, dilute to about 15 mI.' and swirl and
warm the mixture until the oxide has dissolved.
 65

3. Add one dtop of methyl red indicator, then add 6 N HCI dropwise
until
the solution is distinctly acid (red in color), but do not
add more than a
slight excess.

4. Cool, and then cautiously add bicarbonate solution (prepared by

dissolving Z g of NaHCO3 in TS mL distilled water).
Avoid loss by
effervescence by keeping the flask partially covered
with a smail watch
giass during the addition of the entire bicarbonate
sorution.

5. Add 3 mL of starch indicator solution prepared as in previous

$reshly
activity) and wash down the cover glass with a little distilled
water.

6' Rinse and fill your burets with the iod.ine and thiosulfate
solutions.
Adjust and record the initial readings.

7. Titrate the solutions with the iodine solution to the appearance

of the
blue color. Titrate slowly to avoid overrunning the end point.

8. If the end point is overnrn by only a few d.rops, back-titrate with the
thiosulfate solution.

9' when the end point is reached, record the final readings
of both burets.

L0. From the data obtained, carculate the normarity of

the iodine, and from
the preceding volumehic ratio obtained, carcurate the normality
of the
thiosulfate.

Reference:

Hamilton, L. F. and Simpson, S. G., Quantitatiae Chemical

Analysis, 12th
Editioru The Macmillan Company, New York (1,970), pp.267-269.
 66

Actiuitu No, 13

STANDARDIZATION OF IODINE SOLUTION

ACAINST ARSENIC OXIDE

DATA AND RESULTS:

Example

..;;;-;
Wt. of bottle with standard (Aszog) 64.5513
Wt. of bottle with std minus std 64.3623
Weight of standard taken, g 0.1890

Final reading, mL 12 39.29

Initial reading, mL 12 4.49
Volume, mL 12 38.80

Back-Titration:
Final reading, mL Na2S2e L.25
Initial reading, mL Na2S2O3 0.55
Volume, mL Na2S2e 4.70

Ratio (From Preaious Actiaity):

1.000 mL Na2S2O3 = mL 12 1..476

Volume of Na2S2O3 in terms of 12, mL 0.75

Net voiume of 12 mL

Calculated Concentrations:
Normalify of 12 0.1004
Molarity of 12 0.05020

Normality of Na2S2O3 0.1081

Molarily of Na2S2O3 0.1081
 6/

STATISTICAL EVALUATION OF RESU LTS {|\ O RJV1A LIT)') :

Values:
lMean
Mean Normalify 12 N
Mean Normality NazSzQ N

Median Values:
Median Normality 12 N
Median Normality Na2S2O3 N

REPORTED VALUES:
Normality 12 N
Normality Na2S2O3 N
 68

Actiaity No. 14

IODOMETRIC DETERMINATION OF COPPER

IN COPPER OXIDE

one important application of iodometry is the determination of copper

(Cu) lMoiar weight: 63.54] in copper oxide, Cuo. In this method, the copper
oxide is decomposed by nitric acid, after which the resulting cupric ion (Cu++;
is reduced to cuprous ion (Cu+) by the addition of potassium iodide,
precipitating cuprous iodide (Cui), and at the same time liberafing, free iodine
(rd.

2Cu++ + 4I- --+ 2CuI(s) + Iz

The liberated iodine is then titrated with standard thiosuifate.

12 + 2NazSzQ 2NaI + Na2SaO6

-->
Thus, in this case, the end point is the d.isappearance of. the blue color of
the iodo-starch complex"

PROCEDURE:

1. Weigh out accurately (by the method of difference) triplicate portions of

0.25xx - 0.30xx g each eif previously dried copper oxide sample into 2S0-mL
erlenmeyer flasks (labeled I, II, m).

2. Treat with 5 mL of 16 N HNO3 (or slightly more if necessary) to dissolve

the copper oxide. Do this procedure under a hood. If dissolution is slow,
gently warm the mixfure.

3. When the dissolution or decomposition is complete, add 25 mL of

distilled water.
 69

Heat (under a hood!) to remove oxides of nifuogen. Add 5 mL of bromine

water (to oxidize the baces of lower oxides of nitrogen that may still be
present), and heat (under a hood!) until the excess Br2 is expelled.
I

5. Cool, and add 6 N NI-{4CilH dropwise until a blue-green precipitate (of

Cu(OH)z) barely forms and persists on swirling the solution, or until
a
deep blue color [of Cu(NH3)a++ complex] barely forms and persists
on
swirling.

6' In the latter case, gently boit

for 5 minutes or longer to remove rnost of
the excess NHs' (Nofe: Ammonia must be added in slight excess only,
since the excess must be remoaed" by boiling, vthich is tedious).

7. Add 20 mL of 6 N HCzH3e2 cool under running water (or in a cool ice-

water bath) and add 3 grams of KI dissolved in a little distilled water.

8' Rinse and fill the corresponding buret with thiosulfate soiution. Adiust
and record the initial reading.

9. Titrate the resulting solution in Proced.ure 7 with the standard thiosulfate

solution until the brownish color of the iiberated iodine is nearla
destroyed.

10' Add 3 mL af freshly prepared starch indicator solution, and abou t

2 g of
potassium thiocyanate, KCNS. (Nofe; The KCNS preuents the
adsorption of iodine (by cuprous iodide) by
forming the aery insolubte
cupraus thiocyanate from the less insoluble cuprous iodid.e, thus
eliminating the cuprous iodide).

L1" Continue the titration with the stanclard thiosulfate, this

trme dropu:ise
until the blue coior of the iodo-starch complex disappeqrs f.or at least 15
sec (end point).

12. when this end point is reached, record the final buret reading.
 70

13. From the data obtained, and from the normarity

of the standard
thiosulfate solution, calculate the percentage of copper in the
copper oxide
1 sample.

Reference:

Hamiltoru L. F. and Simpson, S. G., Quantitatiue Chemical Analysis,

IZth
Editioru The Macmillan Company, New York (1,970), p. ZTB.
 71,

Actiaity No. L4

IODOMETRIC DETERfuIINATION OF COPPER

IN COPPER OXIDE

Ettor, %

P.attng, %

Deductions, %

Net Rating, fr =

DATA AND RESULTS:

Wt. of bottle with CuO sample, g 28.4064

Wt. of bottle with sample minus sample,g 28.L246
Weight of CuO sample taken, g 0.2818

Final reading, mL Na2S2G3 30.65

Initial reading, mL Na2S2e 0.19
Volume, mL Na2S2O3 34.46

From Preuiaus Actiaitu:

Normality of Na2S2O3 :

Calculated Percentage:
%Cu 74.24
 Fr4
IL

STATISTICAL TVALUATION OF RESULTS (% cu\:

Mean, I
Median, M
Standard Deviation, s
Rel. Std. Deviation, RSD (%)
Std. Deviation of the Meao S

REPORTED VALUE (% Cu)

F
 Actiaity No. 15

DETERMINATION OF CHLORINE IN A SOLUBLE CHLORIDE

(Mohr Method)

The Mohr Method for the determination of chlorine (C1) lMolar Weight:
35.45] is a direct titration method, and uses the formation of a secondary
precipitate (AgzCfr+) to detect the equivalence point. In this method, the
amount of chlorine in a soluble chloride sample (added with 1 mL of s%
K2GOa as the indicator solution) is determined by titration with standard
AgNO3 soiution, precipitating the chloride as AgCl (in a neutral or nearly
neutral solution).

Cl- + Ag* --> AgCl(s) Titration Reaction

analyte titrant white ppt.

Here, the end point is the formation of a red precipitate of Ag2Croa

which forms only when all the Cl- ions in the sample has been precipitated as
AgCl.

Cro+= + Ag* Ag2GOa(s) End Point Reaction

-,>
indicator o(cess titrant red ppt.

In this activity, the standard silver nitrate solution is to be prepared

directly from pure AgNO3 (crystals), as described in Part I. Thus, there is no
more need to standardize the prepared solutiory since the acfual
concentration can be calculated from the weight of pure AgNO3 crystals used,
and the volume of the solution.

PROCEDURE:

I. Direct Preparation of standard silver Nitrate solution

[Nate: Due to the high cost of AgNO3, it ztill be issued to the student at a
limited and manitored arnount (around L g per stud.ent). Each stud.ent
should check out the AgNO3 crystals contained in a weighing bottle or
film
container, making sure the excess is returned immediately to the instructor
after zoeighing the desired amount. Your instructor should
ffix
his signature
 74

as proof of the return in the appropriate space in your data sheet. Deduction
,.will be imposed for failure ta returnll

1' Thoroughly clean a 50-mL volumetric flask with detergent

solution.
Wash with tap water and rinse at least five times
with distilled water.

2' weigh out accurately (by the method of difference) from

a weighing bottle
(or film container) 0.85xx grams of pure
AgNo3 crystals into a clean and
dry paper container (folded at 4 sides). Record the weights
in your data
sheet. (Note: Make sure your actuar weight of AgNe
crystars is exactly
0.85xx, where x could be any number. Deductian
will be imposed for
weights outside the required weightl)

3' Transfer the accurately rveighed crystars into the cleaned 50-mL
volumekic flask without anv waste.

4' Add around 25-mL of chloride-free distilled water and stir or

swirl until
all the crystals has dissorved. (Nofe; Test the ,,chlorid.e-freeness,,
of your
distilled water, To do this, take a small portion of it, and add
a drop of
A8NO3 solution. If no precipitate
forms, your distilled water is chloride-
free). {
5' Dilute the solution with the chloride-free distitled water to
the 50-mL
mark, stopper, and shake to ensure homogeneity.

6' Finally, fransfer into a crean, properry-Iabeled., and preferably

dark bottle,
and present to your instructor for approval.
[Nofe; A Lipovitan or Red
Bull battle knith product label remoaed) can be used as container
of your
AgNO3 solution.l

II. Determinafion of Chlorine

1' Weigh out accurately (by the method. of difference) into

two clean 250-mL
erlenmeyer flasks (or momentarily into two paper
containers) duplicate
samples of about 0.10xx g each. Record the weights
in your laboratory
 ......-

notebook. (Note; Due to the high cast of AgNog, you are req.uired to do
only duplicate
- trials, instead of the usual triplicate,)
\

2. Dissolve each weighed sample contained in the flasks in 50 mL of

chloride-free distilled water.

J. Test the solution with lihnus paper to make sure that it is neutral or
nearly so. (If it is too acidic, add solid CaCO3 until it remains in excess as a
suspension. The suspension does not interfere with the end point).

4. Add 1 mL of 5% KzCfi+ indicator solution.

5. Rinse and fill your acid buret with the standard AgNo3 solution. Adjust
and record the initial reading.

6. Tihate the solution (Trial I) (against a white background and away from
direct sunlight or sbong fluorescent light) with the standard AgNo3, with
constant side-to-side agitation of the flask until the yellow color of the
suspension is converted to a reddish color (end point)"

7- When the end point is reached, record the final reading of the buret.

\ 8. Repeat Procedures 6 and 7 for Trial trI after taking the initial buret reading.

g' From the data obtained, calculate the percentage of chlorine (Cl) in the
sample.

Reference:

Hamilton, L. F. and simpson, s. G., euantitatirse chemical Analysis, lzfh

Edition, The Macmillan Company, New york (rgz0), pp.292-29s.
 /o

Actiuity No. 15

DETERJV1INATION OF CHLORJNE IN A SOLUBLE CHLORIDE

(Mohr Method)

Error,/o :
Ratsng, % :
Deductions, % :

Net Rating, % =

Instructor's Approaal Signatures Jor the Return af the Excess AgNO3 Crystals
and for the Prepared AgNO3 Solution:

Return of Excess AgNO3 Crystals: ; 0.1 N AgNO3:

DATA AND RESULTS:

Example

Weighing of Std. AgNO3 crystals:

Wt" of bottle with std. AgNOe g 11.8868
Wt. of bottle with std minus strl, g 11.4342
Weight of std. AgNO3 taken, g 0.8526

Calculation of Normality of AgNO3 Solution:

Volume of AgNO3 solution, mL 50.00
Normaiity of AgNO3solution 0.1004

Weighing of Unknawn Chlorid.e Samltle:

Wt. of bottle with sample, g, 14.58/.6
Wt. of bottle with sample minus sample, g 14.4779
Weight of sample taken, g 0.1067
'<" \
/t
/ 77

/
Titration Data:
Final reading, mL AgNO3 17.35
Initial reading, mL AgNO3 0.62
Volume, mL AgNO3 1,6.73

Calculated Percent Chlorirce:

%cr

STATISTICAL EVALUATION OF RESULTS (% CT'l,

Mean, *
Standard Deviation, s
Rel. Std. Deviation, RSD (%)
Std. Deviation of the Mean, S

REPORTED VALUE {% CI)

AIPIPIENIDITCIES
 Appendix 1

MTINC SCALE FOR ANALYSIS OF UNKNOWN SAMPLES

BASED ON PERCENT ERROR

Enot Ratins Vo Enar Ratins Vo Error

0.0 - 0.1 100 0.5 -.r.0 95 10.0 - 15.0 45
0.1. -0.2 99 1.0 - 2.0 90 15.0 - 20.0 4A
0.2 - 0.3 98 2.0 - 3.0 85 20.0 - 25.0 JC

0.3 - 0.4 97 3.0 - 4.0 80 25"0 - 30.0 30

0.4 - 0.5 96 4.0 - 5.0 75 > 30.0 z3

5.0 - 6.0 70

6.0 - 7.0 65

7.0 - 8.0 60
'.. 8.0 - 9.0 55

9.0 - 1"0.0 50
',:.'. .'. , ,
 80

Appendix 2

LIST OF OFFENSES AND CORRESPONDINC DEDUCTIONS

A. Attendance
-2
oLa te beyond 30 min
-10
r ljnexcused absence -10
B. Perfonnance
. No laborator n/not weari -10
-3
nruo& etc. ..... -5
-5

: !l*s*siH :l-'y i" ns#:s-"steg -5

-10
o Failure to submit answer notebook after
-10
. Using the issued labora manuai du rlonnance. -10
C. Calculations
-10
o$ iqg recalculation -5
. Late calculation -10
e$y' icant fi -0.5
D. Results
-5
:zsP"mElk_?
o!{ answer but no recalc.
E. Im r Laboratory Behaviors
-_---
n--,:
- uurlng 7 t -
' LflU: eatrng inside laboratory, throwing wastes into sink" leiving
,'visitors,,,
faucet on a{ter use, entertaining etc. -J
.t.. aft*
class
-3
t
,1

81

Appendix 3

LABORATORY ORIENTATION SESSION

Student's and Instructor's Guide

Check-up of Certificate of Regiskation (CoR) by Instructor, and Class

Cards Submission by Students

rts. Laboratory Manual Issuance to

Sfudents: inclividual or by group
depending on the number of laboratory manuals available. A minimum
rental fee is charged for each manual, to be collected bv the instructor
upon issuance of the manua!.

tmportant Notes on the Laboratory Manual:

1. LOSS OF MANUAL: The manual is stricfJy lor rent only, not for sale!
Thus, if the manual is iost at the end of the semester, the student should
replace it with a photocopied version (clear copy) which is bound, with
title page printed on the cover. Before binding, the student should show
the photocopied version to his instructor /or approual. The instructor
should evaluate the acceptability and completeness of the copies to be
bound.

2. CARE oF MAI{\AL: LJpon issuance of manual, the instructor

together r,vith the sfudent evaluates the overall stafus or condition of the
manual with respect to various defects, such as dir! writings on pages,
tom pages, missing pages, damaged pages, etc. The insftuctgr writes his
observations in the Manual Evaluatiorl Page (Appendix 7). At the end of
the semester, the sfudent should refurn the manual in the same
condition as indicated by the inskuctor. Additional damage inflicted by
the student due to careiessness is subj{ct to fine and/or d.eduction.

C. After issuance of laboratory manuals, the insku.ctor elaborates/explains to

the sfudents (but first, the instructor let the students read, by turn and
paragraph by paragraph) he following ltopics found on the indicated pages
of the manual:
 87

Page
1. FOREWORD TO THE STUDENT v1
2. RECORDING LABORATORY DATA x
3. GENERAL RULES FOR USE OF BALANCES xii

Notes:
1". Students who missed the Orientation Session will be required to copy
(in their own handwriting) the above topics into their procedure
Notebook.

2. The instructor has the option to give a quiz on the topics discussed.
abovq during the next laboratory session.

D. REQUIREMENTS

1. Procedure Notebook, Lesson plan type non-spring, thir:r, to be

coaered with transparent cellaphane.
2. Data/Results Notebook, Lesson plan Wpe, non-spring, thiru to be
coaered with transparent cellaphane.
3. Laboratory Gown (apron-type is not allowed!)
4- Laboratory accessories: rag, match, liquid detergent (to be checked
every meeting when needed)
5. 2 pcs. L-liter bottles (with screw cap), or dextrose bottles with caps
(needed starting with Act. No.4)
6. 1 pc. black film container
7. 1 pc. Lrtility tray (plastic)
8. 'l'pc. Red BuIl or Lipouitan
bottle product label removed
9. 1, dozen rubber bands

10" 1 ro11 31A-in masking tape (for labeling prepared solutions)

11. 60 pcs. weighing papers ( from 10 pcs. long size bond paper cut into 6
equal portions per bond paper)

Notes for Part E and F:

The laboratory manual issued to the students is intended
for home use
only. Students are nat allowed. to use it in the laboratory. Thus, you are
required to transfer its aontents anto your corresponding laboratory
 83

natebooks (DatalResults Notebook and praced.ure Notebook), accord.ing

to the guidelines described in parts E and E,

E. GUIDELINES for Preparing the Data/Results Notebook

1- Number al| right hand pages first, on upper right corner, starting
with front page as page L.

2. on pages 2 and 3, copy the LIST oF ACTNITIES (found in pages viii-

ix of the laboratory manual), from Activity L to 15, in the same
tabular format as in the manual. usE DouBLE SPACING
ALWAYS. And use the right hand pages of yaur notebook only.

3. On page 4, copy the Answer Sheet of Activity No. 1 in same format.

usE DOUBLE SPACING ALwAys. And use the fight hand pages 0f
your notebaok only.

4. Copy the Answer Sheets of the next activities into the succeeding
pages of your Data/Results Notebook. usE DOUBLE spAcING
ALWAYS. And use the right hand pnges of your notebook only,

5. All Answer Sheets from Act. 1

to L5 must have been copied into the
Data/Results Notebook during the first two weeks/weekends of the
semester. After this period, the ansTuer notebook can no longer be
brouqht home. It should be submitted to the instructor after each
laborptory period. students who bring home their laboratory
notebook will be penalized with deductions from their radngs
(unless given consent by the inskuctor).

6. Left hand page$ of the Data/Results Notebook should be reserved for

alJ calculations..,
 84

F. GUIDELINES for Prepari"ng the Procedure Notebook

1. CoPy the procedure (except the figures) for the current activity into
the procedure notebook in the same format as in the manual. usE
DOUBLE SPACING ALWAYS.

2. Copying of the procedure must be done at home, and not during the
laboratory period.

3" Be 6ure to copy each procedure in advance of the scheduled

performance of the activity. For example, if the current activity is
No. 3, then you must have copied No. 4 already.

4. only Procedure Notebooks (not the Laboratory Manua1) can be used

during the laboratory period. The issued Laboratary Manual is for
home use anly. Anybody cau.ght using the laboratory manual
during the performance ,f 6n actiz.tity ruill be penalized with
d eduction.

5. No student will be allowed to perform the current activity without

his Procedure Notebook containing the said activity.

G. ISSUANCE of Glasswares and Lockers

These items will be issued on a permanent basis for the entire semester.
Stock Room rules should be shictly followed by the students to safeguard
the items in the locker. These items are the responsibilily of all the
students using the locker

End of Orientation
 85

Appendix 4

COURSE OUTLINE

Course No. Chem 28

Description Quantitative Analytical Chemish.y (Lecfure)
Credit 3 units (3 hours per week lecture)
Textbook Skoog, D. A., West, D.M., ancl Holier,F.I.,
Analytical chemistry, zth Edition, saunders
Fund.amentals ,f
College
Publishing, Philadelphia, pennsylvania, U. S.A.,
1.996.
References Christian, D, Analytical
" G. Chemistry,Sth EditiorU Iotrn
Wiley and Sons, Inc., New york, Lgg4.
c Day, R. A. and underwood A.
L., euantitati,e Analysis,
6th Editior; Prentice Hall, New Jersey, 1,gg'. (Reprinted
by
jMC Press,lnc., Quezon City)
r Hamilton, L" F. and Simpson, S. G.,
euantitatioe
Chemical Analysis, 12th Editioru Collier_Macmillan Ltd.,
London, 1,971.
o Harris, D"c.,
euantitatiae Chemicnl Anarysis.4th Editioru
W. H. Freeman and Company, New york, tggl.

Topics :

I. INTRODUCTION

1.1 RoIe of analytical chemisky

1,.2 Classification of quantitative methods of analysis (gravimetric
methods, volumetric methods, instrumentar methods)
1.3 Classification of analyses
1,.4 Steps in quantitative analysis

It SIGNIFICANT FIGURES

2.L Uncertainty
2.2 Significant figures
 86

2.3 Rules to determine the number of significant figures

2.4 significant figures in calculated results (additiorr, subtraction,
multiplication, division)
2.5 Logarithms and significant figures
2.6 Rounding data and results from chemical computations

ru. EVALUATION OF ANALYTICAL DATA

3.1 Errors in chemical analysis (mean, median, precision, acquacy/

absolute ertart relative- error)
3.2 Types of errors (indeterrninate, determinate, gross)
3.3 ' sources of systematic errors (instrurnental, methodic, personal)
3.4 Constant and proportional.errors
3.5 Detection of systematic errors
3.6 Sources of random errors
3.7 Distribution of experimental data
3.8 Statistical keahnent of random errors
3.9 Absolute deviation
3-10 Relative deviation lpercent (%), parts per thousand (ppt)]
3.1L Standard deviation (single determinatiory mean)
3.12 Reliability of s (sample standard deviation; pooled standard
deviation)
3.13 other ways of expressing precision of samples of data
3.1.4 Confidencelimits
3.15 Detection of gross errors (e-tests, other tests, treahnent of
outliers)
3.16 Least-squares method
3.L7 Correlation coefficient

IV. GRAVIMETRIC METHODS OF ANALYSIS

4.1, Gravimetric factors and caiculations

4.2 Properties of precipitates and precipitating agents
4.3 Drying and ignition of precipitates
4.4 Application of gravimekic methods
4.5 Gravimetric problems
 FIRST DEPARTMENTAL EXAM:
Topics I, Il, III, and IV

V. TITRIMETRIC (VOLUMETRIC) METHODS OF ANALYSF

5.1 Aspects of votrumelric titrimetry (standard solution, equivalence

poinf end point primary standard)
5.2 volumetric calculations (molarity, nclrmality, percent (%), parts
per rnillion (pp*), parts per billion (ppb), density, specific
gravity)
5.3 Gravimetric titrimetrv

VI. ACID-BASE TITRATIONS

6.1 Solutions and indicators for acid/base tikations

6.2 Buffer solutions
6.3 Titration curves: stuong acids with shong bases (HCl vs. NaOH)
and vice versa, weak acids with r,veak bases (HCzHgGZ vs. NFb)
and vice versa, salt of weak acid (conjugate base) with strong acid
(NaCN vs. HCi).
6.4 Acid/base indicators
6.5 Polyfunctional acids / bases (descriptive)
6.6 Titration curves for polyfunctional acids/bases (descriptive)
/d
o./ Applications of neutralization titrations
6.8 Doubl e-indicator titrafi ons

SECO},ID DEPARTMENTAL EXAM:

Topics V and VI

VII. REDUCTION-OXIDATION TITRATIONS

7.1 Redox indicators

7.2 Auxiliary reducing/ oxidizing agents
7.3 Applications of standard reductants
7'.4 Applications of standard oxidants: permanganate, dichromate,
and iodine solutions
 88

7.5 Specialized oxidants: potassium bromate, periodic

acid, and Karl
Fischer reagent

VM. PRECIPITATION AND COMPLEXA,TION TITRIMETRY

8.1 Argentometric titrations (Mohr method., volhard method,

Fajans method), apprications of silver nitrate sorutions,
probiems
8.2 Compiex-formation reaclions (Hamilton Reference):
cyanide
determination by Liebeg Method, determination of
cyanide-
halide mixtures" EDTA titrations, indicators of EDTA
titrations.

THJRD DEPARTMENTAL EXAM:

Topics VII and VIII

COMPREHE]VSIYE FINAT DEPARTMENTAT EXAM:

'lopics I ta VIII

June/ ?004