Experiment 1 Preparation and Standardization of Volumetric Solutions

Ph Ch 135 Lab Reviewers
Preparation & Standardization of Volumetric Solutions

FIRST EXAM
ACKNOWLEDGEMENTS
Special thanks to the third year students who willingly gave their time and effort to contribute to the completion of the
compilation of Ph Ch 135 Lab reviewers:
 Donato Legaspi and Frances Ngo for 0.1N Ammonium Thiocyanate VS
 Tanya Adriatico, Janine Asis, and Iris Balutoc for 0.1N Bromine VS
 Ena Naoe and Keith Nieva for 0.1N Ceric Sulfate VS
 Kyna Lim and Kyla Lim for 0.05M Disodium Edetate VS
 Bea To, Loureen Utanes, and James Tronco for 1N Hydrochloric Acid VS
 Daryl Tabud for 0.1N Iodine VS
 Genmar Pasion for 0.1N Oxalic Acid VS
 Abbygail Benemerito and Matthew Que for 0.05M Potassium Iodate VS
 Joshua Chavez, Christine Claros, Keisha dela Cerna, and Kristine Garcia for 0.1N Potassium Permanganate
VS
 Cheli Mendoza for 0.1N Silver Nitrate VS
 Shaynne Demafiles, Christinette Figueroa, Mary France Gonzaga, Darien Rivera, and Chelsea Valdez for
0.01N Sodium Hydroxide VS
 Kristel Serrano and Jarvin Tan for 0.02N Sodium Hydroxide VS
 Jaslyn Alvarez, Nica Aranda, and Dianne Belotindos for 0.05N Sodium Hydroxide VS
 Geovin Uy and Abet Villaluna for 1N Sodium Hydroxide VS
 Imma Olayan, Vienne Pinlac, Nikki Ticman, and Charleen Usacdin for 0.1N Sodium Thiosulfate VS
 Ariane Ramirez and Hanna San Andres for 0.5N Sulfuric Acid VS
 Ara Donayre for 1N Sulfuric Acid VS
 Divina Lucero for 0.05M Zinc Sulfate VS
And to the third year batch representatives, Sharmaine Po and Matthew Que , together with the batch officers for
academics, Genmar Pasion and Daryl Tabud, and other third year students for their unending support.
Prepared by BBB 2011 | Ph Ch 135 Lab, 1st Sem A.Y. 2013-2014

2
TABLE OF CONTENTS
Preparation and Standardization of Volumetric Solutions
0.10 N Ammonium Thiocyanate VS………………………...4

0.10 N Bromine VS……………………...…………………….5
0.10 N Ceric Sulfate VS......................................................7
0.10 N Disodium Edetate VS……………………………...…9
1.00 N Hydrochloric Acid VS………………………………...11
0.10 N Iodine VS………………………………………………12
0.10 N Oxalic Acid VS…………………………………….......14
0.05 M Potassium Iodate VS…………………………………15
0.10 N Potassium Permanganate VS…………………….....16
0.10 N Silver Nitrate VS…………………………………….....18
0.10 N Sodium Hydroxide VS………………………………...19
0.20 N Sodium Hydroxide VS…………………………….…..20
0.50 N Sodium Hydroxide VS………………………..……….21
1.00 N Sodium Hydroxide VS……………………..………….23
0.10 N Sodium Thiosulfate VS……………………………….24
0.50 N Sulfuric Acid VS…………….………………………….26
1.00 N Sulfuric Acid VS….…………………………………….27
0.05 M Zinc Sulfate VS……………..………………………….28

3
Preparation and Standardization of 0.1 N Ammonium Thiocyanate VS
Type of Titration Direct alkalimetry
Type of Reaction Neutralization
Indicator Volumetric precipitation (Volhardt method)
Endpoint Permanent reddish-brown color which does not Indicator is adsorbed to the surface of the
disappear upon shaking particles.
Titration Condition Titration is done in the dark To be discussed in procedure
Temperature must not exceed 25 degrees Higher temperatures tend to bleach the color if
Celcius. the indicator.
Gives a red color with thiocyanic acid, and may
Solution must be free from nitrous acid.
be mistaken for iron (III) thiocyanate
Procedure and RFIS Preparation:
1. Dissolve about 8g of ammonium thiocyanate in 1000ml water, and standardize the solution
as follows.
- A slight amount in excess of ammonium thiocyanate is used since ammonium
thiocyanate is deliquescent.
- Potassium thiocyanate may be used in place of ammonium thiocyanate.
Standardization:
2. Accurately measure about 30mL of 0.1N silver nitrate into a glass-stoppered flask.
- must be done in the dark to prevent the reducing effect of light on the silver nitrate which
might produce elemental silver.
3. Dilute with 50mL of water.
4. Add 2mL of nitric acid and 2 mL of ferric ammonium sulfate TS.

- Concentration of nitric acid should be from 0.5 M-1.5 M since strong nitric acid retards the
formation of the thiocyanato-iron(III) complex.
- The solution is acidified with nitric acid to prevent the hydrolysis that ferric salts undergo in
neutral solutions.
- It also prevents the precipitation of other anions that are soluble in the medium.
- Ferric ammonium sulfate is the indicator. The thiocyanate ion reacts with ferric ammonium
sulfate to form the red ferric thiocyanate.
5. Titrate with the ammonium thiocyanate solution to the first appearance of a red-brown color.
- As the titration process occurs, a white precipitate of AgSCN is observed.
- As endpoint is reached, precipitate becomes flocculent and settles readily.
Chemical Equations AgNO3 + NH4SCN AgSCN↓ + NH4NO 3
Factor 1
Computations Preparation:
4
Wt. of NH4SCN T x VT x
1000
Normality: (after standardization)

N=
4

4
Preparation and Standardization of 0.1 N Bromine VS
Type of Titration Iodometry
Indicator Starch TS (used primarily for iodometric methods due to color change caused by starch-iodo
complex)
Endpoint From dark blue to colorless solution
Titration Condition Use an iodine flask for the standardization procedure.
1. Dissolve 3g Potassium Bromate and 15g Potassium Bromide in water to make 1000mL.
- Indirect generation of bromine circumvents problems associated with the use of standard
bromine solution which lacks stability.
- Potassium bromide may be added in excess to account for the loss bromine vapors as a
source of bromide ions. It is also the cheaper reagent among the two.
Standardization:
1. Accurately measure about 25mL of the solution into a 500mL iodine flask and dilute with
120mL of water.
- The use of a glass-stoppered flask is used to avoid the loss of vapors liberated in the
procedure.
- The stopper should be moistened so it would not be stuck.
- Use the buret to accurately measure the bromine VS.
2. Add 5mL of hydrochloric, insert the stopper in the flask and shake it gently.
- Addition of the acid liberates free bromine (see equation).
- Insert the stopper immediately to prevent the escape of bromine vapors.
- Gentle shaking prevents the build up of pressure in the flask that may cause the stopper
to pop out.
- The solution turns into a transparent yellow solution.
3. Then, add 5mL of potassium iodide TS, again insert the insert the stopper and shake the
mixture.
- This step liberates iodine as bromine oxidizes the iodide ion (see equation).
- The solution turns into a red-orange transparent solution due to the iodine being liberated.
4. Allow it to stand for 5 minutes.

- This ensures that the reaction has been completed.
5. Titrate with 0.1 N sodium thiosulfate VS.

- Make sure that the stopper is loosely inserted to prevent the escape of iodine vapors while
titrating.
- Move the stopper back and forth using the handle to allow the liquid to enter the flask.
- The color of the solution lightens as more sodium thiosulfate is added.
6. Add 3mL of fresh Starch TS as the endpoint approached.

- Do this step when the solution is straw-colored (in other words, kakulay niya raw yung ihi
sa umaga).
- Do not remove the stopper when adding starch TS.
- After adding, wash the stopper and lip of the flask thoroughly since some of the titrant are
still there.
- Swirl the solution.
- The stopper may now be removed since the remaining iodine has complexed with starch.
5
7. The endpoint is reached when the solution turns colorless.
- The teacher must be present when doing adding the last drops of titrant the clearly see
the transition.
8. Perform a blank determination.

- In this procedure, iodine is oxidized by bromine.
- However, air may also cause the oxidation of bromine and so, blank determination
is performed to account for this.
Chemical Equations Half-reactions

(2Br- Br2 + 2e-)2
2BrO 3- + 6H+ + 4e- Br2 + 3H2O
4Br- + 2BrO 3- + 6H+ 3Br2 + 3H2O
Complete and Balanced Equation:
5KBr + KBrO 3 + 6HCl  6KCl + 3Br2 + 3H2O
Half-reactions:
Br2 + 2e- 2Br-
I-I2 + 2e-
Br2 + I- 2Br- +I2
Br2 + KI KBr +I 2
Half-reactions:
I2 + 2e- I -
2S2O 32- S4O62- + 2e-
2S2O 32- + I 2 S4O62- + I -
2Na2S2O3 + I 2 2NaI + Na2S4O 6
Factor 2
2
Wt. of Br2 T x VT x
1000
Normality: (After standardization)

2 2 2 2
N=
2

6
Preparation and Standardization of 0.1 N Ceric Sulfate VS
Type of Titration
Direct cerimetry
Type of ReactionReduction-oxidation
Indicator
The ceric solution served as its own indicator.
Endpoint luti n’s ch n e in c l c l less t permanent slight yellow color
Titration Condition
This change in color is most apparent when the temperature of the solution is kept high and the
titration conducted at acidic conditions, and made under bright, white light.
1. Dissolve 42 Gm. of reagent ceric sulfate in about 500 mL of water containing 28 cc. of
sulfuric acid, warming if necessary.
2. When solution is complete, cool, add sufficient water to make 1000 mL., and mix well.
Standardization:
1. Accurately weigh about 0.2 g of sodium oxalate, primary standard, dried according to the
instructions on its label, and dissolve in 75 mL of water.
- because of the possible exchange of water between the atmosphere and the
primary standard, sodium oxalate is dried at 105⁰C for 2 hours to expel any
moisture which may markedly affect the analytical results
2. Add, with stirring, 2 mL of sulfuric acid that has previously been mixed with 5 mL of water,
mix well, add 10 mL of hydrochloric acid, and heat to between 70-75⁰.
2Ce4+ + 2Cl- 2Ce3+ + Cl2
- Sulfuric is added to keep the solution acidic which favors the stability of ceric sulfate.
- A high acidic condition is necessary to prevent the hydrolysis of ceric salts which leads to
the precipitation of ceric hydroxide (hydrated cerium (IV) oxide), a weak base, and other
basic salts.
- Perceric compounds may also form upon the oxidation of cerous hydroxide.
- Among the acids, sulfuric acid is used because ceric salts are most stable in their
solutions.
- Sulfuric acid solutions of ceric sulfate are stable even at boiling temperatures.
- The addition of hydrochloric acid also maintains the acidic titration condition.
- The solution must be heated to 70-75ºC to increase the speed of the reaction.
- The detection of the end point, a slight yellow tint, is easier in hot than in cold solutions
because of an increase in the intensity of the yellow color of ceric ions with a rise in
temperature.
- This permits the end point to be detected without the use of an indic t V el’s .
- However, the solution is not heated up to the boiling temperature because of possible
oxidation of chloride ions, from hydrochloric acid, and liberation of chlorine.
3. Titrate with 0.1 N ceric sulfate to a permanent slight yellow color.

- Since ceric sulfate is standardized against sodium oxalate in hot sulfuric and hydrochloric
solution, the end point is determined without a special indicator or by the potentiometric
method.
- This is because the available oxidation-reduction indicators are oxidized before the
equivalence point is reached.
- Also, ceric salts may only serve as its own indicator if only colorless products are formed.
- Moreover, hydrofluoric acid and fluoride ions are avoided in ceric sulfate titrations because
they decolorize the yellow solution by forming a stable complex with ceric ions.
- Consequently, fluoride decreases the oxidation potential of the ceric -cerous system.
Chemical Equations Half-reactions:
7
(Ce4+ + e- Ce3+)2

C2O42- 2CO 2(g)+ 2e-
Net balanced equation:
2Ce4+ + C2O42- 2Ce3+ + 2CO 2(g)
Balanced Molecular Equation:
2Ce(SO 4)2 + Na2C2O 4 Ce2(SO 4)3 + Na2SO4 + 2CO 2(g)
Factor 2
e 4
Wt of CeSO 4 V
1 1000
Standardization:
2 2 4
Wt of Na2C2O4 V
2 1000
Other Notes Situation: During titration, a white precipitate was observed after every addition of titrant and the
analyte became turbid. The volumetric solution restandardized was said to be contaminated.
Question: What factor/s during the preparation of the volumetric solution could account to the
formation of the precipitate and turbidity of the solution when standardized?
Answer: An insufficient amount of sulfuric acid added during the preparation could have resulted to
the precipitation observed in the solution. Sulfuric acid stabilizes the ceric sulfate solution, hence,
when added in amount lesser than necessary, precipitation of ceric salts may occur.

8
Preparation and Standardization of 0.05 M Disodium Edetate VS
Type of Titration Direct
Type of Reaction Complexation
Indicator Hydroxynaphthol blue
- It is calcium-specific at pH 12-13. It is used since it gives a sharp color change at the end point.
Endpoint Color change from red/pink to blue
MIn- +H2Y2 - ↔ Y2- + HIn2 - + H+
Red Blue
CaIn- +Na2EDTA CaEDTA + NaIn2- + Na+
- Hydroxynaphthol blue serves as calcium indicator which colors the solution blue when
uncomplexed.
- I ll the lciu i ns e tied up s ED c ple , the In c ple c n’t , le din t blue
free indicator.
- CaIn red/pink complex is much less stable than CaEDTA complex.
Titration Condition Basic media, about pH 13
The indicator detects calcium ions at pH 12 – 13.
Procedure and RFIS 1. Accurately weigh about 200 mg of chelometric standard calcium carbonate, previously dried
at 110o for 2 hours and cooled in desiccator.
- Drying ensures the removal of the adsorbed water from the crystals.
- Increasing the temperature will cause the removal of entrapped water from the crystals for
accurate titration.
- The dried chelometric standard calcium carbonate is cooled in a dessicator first before
weighing to prevent water particles to be readsorbed in the calcium carbonate crystals.
- Furthermore, when the weighing is done before it is cooled, the apparent mass of the
sample is lower.
2. Transfer to a 400 mL beaker. Add 10 mL of water and swirl to form a slurry.

- A large container is used for easier washing in the next procedure.
- Formation of slurry ensures all CaCO 3 will not adhere to sides of beaker.
3. Cover the beaker with a watch glass and introduce 2 mL of dilute HCl from a pipet inserted
between a lip of the beaker and the edge of a watch glass.
- HCl solubilizes the calcium carbonate converting it to calcium chloride.
- Covering the beaker is done since CO 2 is produced in the reaction.
4. Wash down the sides of the beaker, the outer surface of pipet and the watch glass with
water and dilute with water to 100 mL.
- Washing ensures all of calcium ions are included in the solution and dilution is done to
achieve less error in titration since high concentration of the metal ion causes a difficulty to
discern the endpoint which may alter the accurateness of the values obtained.
5. While stirring the solution, preferably with a magnetic stirrer, add about 30 mL of the edetate
disodium solution from a 50 mL buret. Add 15 mL of NaOH TS and 300 mg of hydroxy
naphthol blue and continue titration with edetate disodium solution to a blue endpoint.
CaCl2 + Na2EDTA CaEDTA + 2NaCl
- Order of addition is important since if NaOH is added first, Ca(OH) 2 will precipitate thus
making it more difficult to undergo complexation reaction.
- Calcium edetate must first be produced.
- It is buffered to an approximate pH in which it will form a high conditional formation
constant for the metal-EDTA complex to form a sharp end-point
- In this case, the addition of sodium hydroxide T S is used to alkalinify the solution to pH 13.
At this pH, the Ca-EDTA complex will form.
9
- The amount of indicator must not be too many since the intensity of the color of the
solution increases.
- NaOH alkalinizes the solution to about pH 13 to prevent interference of Mg 2+ ions which
can precipitate as Mg(OH)2; since magnesium and calcium both reacts with EDTA at pH 10,
a higher pH is needed to react calcium only and prevent contaminants to react.
- In general to pH titrations, the sharpness of the endpoint is determined by the conditional
formation constant, which increases as pH increases.
- However, when the pH is too high, alkali hydroxides might precipitate out of the solution.
- Thus the analyte must be buffered to the right pH in which the metal-ED c ple ’s
conditional formation constant is large enough to produce a sharp end point.
Chemical Equations Reaction of calcium carbonate with hydrochloric acid:
CaCO 3 + 2HCl  CaCl 2 + H2O + CO 2↑
Reaction of disodium EDTA with CaCl 2:

CaCl 2+Na2EDTA CaEDTA + 2NaCl
Factor No factor.
Molar ratio of EDTA to a metal ion regardless of the charge is in 1:1 ratio.
Wt of EDTA= V
Standardization:
t
V ED

10
Preparation and Standardization of 1 N Hydrochloric Acid VS
Type of Titration Direct acidimetry
Titrant: Prepared Hydrochloric Acid (secondary standard)
Analyte: Anhydrous Sodium Carbonate (primary standard)
Indicator Methyl Red indicating from yellow to light pink color
Endpoint N/A
Titration Condition N/A
1. Dilute 85mL of Hydrochloric Acid to 1000mL.
Standardization:
1. Weigh accurately about 1.5g of primary standard anhydrous sodium carbonate that
previously has been heated at a temperature of about 270 oC for 1 hour.
- In the range of 100-270 degrees Celsius, sodium bicarbonate decomposes quantitatively
based on the equation:2NaHCO 3 Na2CO 3 + CO 2 + H2O
- At temperatures above 300 degrees Celsius, the Sodium Carbonate may decompose to
give the Oxide. (Hamilton and Simpson, 1964, p. 166)
- Use weighing bottle in weighing sodium carbonate; sodium carbonate is hygroscopic, it
absorbs a small amount of moisture from the air; above 50 degrees Celsius or in warm, dry
air effloresces and becoming anhydrous at 100 degrees Celsius. (Soine and Wilson, 1970,
p. 216)
2. Dissolve it in 100mL of water.

- Use boiling water in the preparation and standardization to free carbon dioxide.
- Carbon dioxide being appreciably soluble in water may be present in distilled water.
(Hamilton and Simpson, 1964, p. 155)
3. Add 2 drops of methyl red TS.
4. Add the acid slowly from a buret, with constant stirring, until the solution becomes faintly
pink.
5. Heat the solution to boiling, and continue the titration.
6. Heat again to boiling, and titrate further as necessary until the faint pink color is no longer
affected by continued boiling.
- The carbon dioxide generated as a result of the neutralization reaction renders the solution
acidic and introduces a source of error if not removed.
- After the first end point id reached, the solution is boiled to rid it of CO 2.
7. Each 52.99mg of anhydrous sodium carbonate is equivalent to 1mL of 1N hydrochloric acid

Chemical Equations Na2CO 3+ 2HCl 2NaCl + H2O + CO 2
Factor Hydrochloric Acid: 1
Sodium Carbonate: 2
Computations Pre-lab:
l
Wt of HCl V
1 1000
2
Wt ofNa2CO 3 V
2 1000

11
Preparation and Standardization of 0.1 N Iodine VS
Type of Titration Iodimetry
Titrant: Iodine VS
Titrand: Sodium Arsenite
Type of Reaction Reduction-oxidation
Indicator Starch TS
- used for iodometric and iodimetric methods to detect presence of iodine due to formation of starch-
iodo complex which is colored blue
Endpoint Appearance of blue color.
- formation of starch-iodo complex
- notifies that all arsenite has been consumed
1. Dissolve about 14g Iodine in a solution of 36g of KI in 100mL water.
- 1g of I2 is soluble in 2950 mL water.
- In the presence of KI, solubility is greatly increased because of formation of triiodide ions.
2. Add 3 drops HCl.
3. Dilute to 1000mL.
Standardization:
1. Weigh 150mg As2O3 and dissolve in 20mL 1N NaOH by warming if necessary.
As2O 3 + 6NaOH  2 Na3AsO 3 + 3H2O
- As2O 3 is slowly soluble in cold water and readily soluble in boiling.
- also soluble in alkali OH such as NaOH forming arsenit
- insoluble in acids
2. Dilute with 40mL H2O.
3. Add 2gtt methyl orange TS.

-indicator to test neutrality of titrand
-yellow (basic) to pink (weakly acidic)
4. Follow with diluted HCl until yellow color is changed to pink.

- to neutralize basic solution of arsenite
- Note that titration with iodine needs to be in neutral conditions.
- if basic: 2NaOH + I2NaIO + NaI + H2O
- if acidic: starch is hydrolyzed yielding glucose which is a reducing agent
- Neutrality increases reducing power of reducing agent (Na 3AsO 3).
- low H+ thus shifting equilibrium to the right
H3AsO 3 + I2 + H2O  H3AsO 4 + 2I - + 2H+
5. Add 2g NaHCO 3, dilute with 50mL water.

4HI + O 2 2I2 + 2H2O
- pH of titration if maintained by addition of NaHCO 3 through consumption of HI
- NaHCO 3 + HI NaI + CO 2↑ + 2O
- Slso, CO 2 formed saturates atmosphere to minimize O2 concentration thus to avoid
oxidation of excess hydriodic acid(if formed) to iodide which can increase amount of iodine
in titrant (most probably, source of excess hydriodic acid is excessNaI used to dissolve I 2).
6. Add 3mL starch TS.
7. Titrate with Iodine VS until appearance of deep blue color.

12
Chemical Equations Half Reactions:
(Oxidation) AsO 33- + H2O  AsO 43- + 2H+ + 2e-
(Reduction) I2 + 2e- 2I-
AsO 33- + I2 + H2O  AsO 43- + 2H+ + 2I-
Complete Reaction:
Na3AsO 3 + I 2 + H2O  Na3AsO 4 + 2HI
Note that
NaHCO 3 + HI NaI + CO 2↑ + 2O
Thus,
Na3AsO 3 + I 2 + 2NaHCO 3 Na3AsO 4 + 2NaI + 2CO 2 + H2O
Factor Na3AsO 3: 2
As2O 3: 4
-note that 1 mol As2O3 yields 2mol Na3AsO3 and since 1 mol Na3AsO3 produces 2e-,
1 mol As2O3 produces 4 thus factor is 4
I2: 2
NaI:1
Computations Wt I 2 = NT X VT X I dine
2 1000
s2
Wt As2O3= NT X VT X
4 1000
Other Notes  Note the difference between Iodimetry and Iodometry.
 More info on starch-iodo complex formation (amylose, formation of I6): Christian, Analytical
Chemistry, 6th ed. p. 424
 Iodimetry: starch can be added at the beginning of titration; Titration with I 2/I3 -
 Iodometry: Titration of I2/I3 -
 See Harris, Qualitative Chemical Chemistry, 7 th ed. p. 340

13
Preparation and Standardization of 0.1 N Oxalic Acid VS
Type of Titration Direct permanganometry
Titrant: KMnO 4
Analyte: H2C2O 4
Oxidizing Species: MnO 4-
Reducing Species: C2O42-
Indicator Titrant (KMnO 4) is self-indicating
Endpoint Pale pink color which persists for about 15 seconds
- indicative of the complete reaction of all the oxalic acid initially present in the analyte
- pale pink color due to excess of potassium permanganate at the end point (no more oxalic
acid which will react with KMnO 4)
Titration Condition Temperature at end point must not be less than 60°C
- This ssu es th t “t ue” endp int is e ched c plete e cti n between pe n n te nd
oxalate.
- Local excess of permanganate can yield a faint pink color at any temperature even if not in a
reaction with oxalate.
1. Dissolve 6.45 g of oxalic acid in sufficient water to make 1000 mL.
2. Standardize by titration against freshly standardized 0.1 N potassium permanganate.

- Potassium permanganate deteriorates over time and undergoes changes in concentration
Standardization:
1. Measure accurately from a buret about 30 mL of the oxalic acid solution into a conical flask
and dilute with about 200 mL of water.
2. Add 7 mL of sulfuric acid.

- Sufficient acid must be added to keep the hydrogen-ion concentration reasonably constant
throughout the titration, thereby preventing the formation of manganese dioxide and
supplying the hydrogen ions used up in the reduction of the permanganate ion.
3. Heat to about 70°C.

- This hastens the reaction, whic.h slowly occurs at normal temperature.
4. Slowly add the potassium permanganate from a glass-stoppered buret, with constant
swirling.
- If the permanganate is added rapidly, the hydrogen ions may be exhausted locally.
- Brown colloidal manganese dioxide then precipitates as a result.
- Solutions of oxidizing agents should never be titrated from Mohr burets because the
oxidizing agent attacks the rubber and the titer value decreases.
Chemical Equations Half equations:
MnO 4- + 8H+ + 5e- Mn2+ + 4H2O
C2O42-  2CO 2 + 2e-
Molecular Equation:
2KMnO 4 + 5H2C2O4 +3H2SO 4  2MnSO 4 + K2SO4 +10CO 2 + 8H2O
Factor For C2O42-: 2
For MnO 4-: 5
Computations N1V1 = N2 V2

14
Preparation and Standardization of 0.05 M Potassium Iodate VS
Type of Titration Direct iodometry
Oxidizing agent: KIO 3
Reducing agent: KI
Indicator Starch TS
Endpoint Discharge of intense blue coloration
Titration Condition Acidic medium
1. Dissolve 10.7 g of KIO 3, previously dried at 110 oC to constant weight, in water to make
1000 mL.
- To remove moisture, KIO 3 is dried and dessicated.
Standardization:
1. To 15 mL of solution in a 250-mL iodine flask, add 3 gof KI and 3 mL of HCl previously
diluted with 10 mL of water.
- KI is added to form KI3 which will be the source of iodine during oxidation.
KI3<-> KI + I 2
- HCl is added to increase the reducing ability of KIO 3; this can help the reaction to proceed
to completion.
2. Stopper immediately and allow to stand in dark for 5 minutes.

- Iodine flask is used and stoppered immediately to avoid liberation or escape of iodine.
- To prevent deterioration of light-sensitive iodine, it is allowed to stand in the dark.
3. Then, add 50 mL of cold water, and titrate the liberated iodine with freshly standardized 0.1
N sodium thiosulfate.
4. Add 3 mL of starch indicator at the near end of titration, and continue until the discharge of
blue-starch-iodine complex color occurs.
- Starch TS readily detects iodine by the formation of starch-iodo complex.
- Starch TS is only added at the near end of titration because of the reversibility of the color
formation at high concentrations of iodine decreases.
Chemical Equations For the KIO 3 and KI in acidic media:
IO3- + 6H+ + 6e- 3H2O + I-
[2I- I2 + 2e-]3
Net: IO3- + 6H+ +5 I - 3H2O + I2
Balanced Eq:
KIO3 + 6HCl + 5KI  3H2O + 3I 2 + 6KCl
For the Iodine and Na2S2O3:

I2 + 2e- 2I -
S2O32- S4O62- + 2e-
Net: I2 + S2O32- S4O62- + 2I-
Balanced Eq:
I 2 + 2Na2S2O3 2NaI + Na2S4O6
Factor 6
I
Wt KIO 3= NT X VT X
1000
Normality: (After standardization)

N1V1 = N2 V2
N1 (15 mL) = (0.1 N)(Volume of Titrant)
15
Preparation and Standardization of 0.1 N Potassium Permanganate VS
Type of Titration Direct permanganometry
Indicator Self indicating; Mn7+ is purple while Mn2+ is colorless, a pale pink color therefore indicates an excess
of MnO 4- (Mn7+)
Endpoint Solution turns to a pale pink color that persists for 15 seconds
- It must be observed closely since the color might fade after 15 seconds.
- Oxidizing materials from the surroundings will make the solution turn colorless again.
Titration Condition Acidic
- To obtain Mn2+, neutral solutions will give a product of MnO 2.
60-80°C
- 60°C makes the reaction faster.
- Higher than 80°C will give decomposition.
1. Dissolve 3.3 g KMnO 4 in 1 L H2O.
2. Boil for 15 minutes, stopper flask, let stand for at least 2 days, filter.
- Aqueous solutions of permanganate are unstable.
4MnO 4- + 2H2 ↔ 4 n 2 ↓ + 2 ↑ + 4 -
- The MnO 2 produced acts as a catalyst for further decomposition of permanganate (an
autocatalytic decomposition) and is not as strong as MnO 4- in oxidizing power (Mn4+ instead
of Mn7+).
- The potassium permanganate solution is boiled to hasten the oxidation of reducing
impurities.
- Standing ensures complete oxidation. Filtering removes any MnO 2 that precipitates so the
solution can be stable for a period of time.
3. Filter through fine-porosity, sintered glass crucible.

- Any organic material can reduce Mn 7+, thereby decreasing the concentration of MnO 4-
- In this experiment, any contact with organic materials like filter paper, plastic and rubber
must be avoided.
Standardization:
1. Weigh accurately about 200mg of Na 2C2O 4, previously dried and dissolved in 250ml of
water.
- Sodium oxalate is the best standard to be used because it can be obtained in very pure
conditions.
2. Add 7 ml of H2SO 4.
- It is added to keep the hydrogen-ion concentration constant throughout the titration which
prevents the formation of manganese dioxide.
- H2SO 4 is the preferred acid because it has no action upon MnO 4- in dilute solution, while
HCl may react with MnO 4- to produce chlorine gas.
2 MnO 4- + 10Cl- +16 H+  2Mn2+ + 5Cl2 + 8H2O (Jeffery, 1989, p. 368)
3. Keep the temperature of analyte at around 600-700C.

- This allows the oxalate and permanganate to react fast.
- At the start the loss of pink color will take a few minutes because the reaction between the
two is slow. Elevated temperatures ensure a fast reaction and avoid undertitration.
4. Titrate until endpoint.

- The endpoint is best observed against a white background.
16
- It should only remain for 15 seconds to make sure that the color seen is due to the
endpoint and not the oxidizing materials present in the surrounding.
Chemical Equations Reduction:
MnO 4- + 8H+ + 5e- → n2+ + 4H2O
Oxidation:
C2O42- → 2 2 + 2e-
Net Ionic:
2MnO 4- + 16H+ + 5C2O42- → 2 n2+ + 8H2O+ 10CO 2
Balanced Molecular:
5Na2C2O4 + 2KMnO 4 + 8H2SO 4 → 2MnSO 4 + 5Na2SO4 + K2SO 4 + 10CO 2 +8H2O
Factor KMnO 4 f = 5 for preparation
Na2C2O4 f = 2
KMnO 4 f = 2 for assay
n 4
Wt KMnO4= NT X VT X
5 1000
Standardization:
2 2 4
Wt Na2C2O4= NT X VT X
2 1000
n 4
Wt KMnO4= NT X VT X
2 1000
Other Notes  Boiling the permanganate solution for 15 minutes during preparation significantly decreased the
total volume of the solution, causing the normality to rise. The water lost may be replenished with
water distilled from another potassium permangate solution.
 The excess allotted by the USP (3.3g was stated in the procedure while 3.161g was the
requirement) may not have been completely reduced by the organic impurities from the distilled
water used. This might have contributed to the high normality.
 Potassium permanganate must be kept in glass-stoppered, amber bottles or stored in the dark.
Dust and light decomposes this solution. It should only be handled with inert-material apparatus or
with glass. It can be reduced upon contact with organic substances like rubber.
 This volumetric solution must be standardized from time to time.

17
Preparation and Standardization of 0.1 N Silver Nitrate VS
Type of Titration Di ect tit ti n F j ns’ eth d V lu et ic P ecipit ti n
Titrant: Silver nitrate (AgNO3) VS
Titrand: Sodium chloride
Type of Reaction Precipitation Reaction
Indicator Used Eosin Y TS
Endpoint Change of color of precipitate from white to pink
Titration Condition pH of 2
1. Dissolve about 17.5g of Silver Nitrate in 1000mL of water.
Standardization:
1. Transfer about 100mg, accurately weighed, of reagent-grade sodium chloride, previously
dried at 110o for 2 hours, to a 150-mL beaker.
- Sodium chloride has a purity of 99.9 – 100.0 percent and may be used as a primary
standard.
- Sodium chloride is very slightly hygroscopic; therefore, it is necessary to dry the finely
powdered solid at 110◦ for 2 hours prior to dissolution to correct for absorbed moisture.
2. Add 5mL of acetic acid.

- Acetic acid is added to the solution to prevent a premature endpoint by suppressing the
ionization of eosin, thus, avoiding the displacement of Cl - in the primary adsorbed layer. The
color change is also sharpest in acetic acid solution.
3. Add 50mL of methanol.

- Alcohol, in this case methanol, is added to help keep the precipitated silver chloride in a
colloidal state and thus give sharpness to the color change which occurs in the precipitate
surface.
4. Add about 0.5mL eosin Y TS.
5. Stir, preferably with a magnetic stirrer, and titrate with the silver nitrate solution.
- T itration must be done in a dim environment to prevent photocatalytic degradation of silver
chloride. This is due to the reducing effect of light on silver chloride, producing free silver
which in turn causes a purplish color on the precipitate.
- The F j ns’ eth d uses an adsorption indicator whose color when adsorbed to the
precipitate is different from that when it is in solution. Before the endpoint, the precipitate of
AgCl has a negative surface charge due to the adsorption of excess Cl -. The anionic
indicator, eosin y, is repelled by the precipitate and remains in the solution where it has a
greenish yellow color. After the end point, the precipitate has a positive surface charge due
to the adsorption of excess Ag +. The anionic indicator now adsorbs to the precipit te’s
surface where its color is pink. This change in color signals the endpoint.
- Slow addition of the titrant should be employed with constant stirring to produce a
precipitate with larger particles. In using adsorption indicators, the precipitate formed should
remain highly dispersed, allowing for maximum surface area of adsorption.
Chemical Equations AgNO 3 + NaCl → AgCl↓ + NaNO 3
Factor 1
N= MF =M(1)
Standardization:
18
l
Wt. of NaCl T x VT x
1000
Preparation and Standardization of 0.1 N Sodium Hydroxide VS
Type of TitrationDirect alkalimetry
Indicator Used Phenolphthalein TS
Indication of Endpoint Colorless to very faint, permanent pink solution
pH range: 8.3-10.0
-the range at which phenolphthalein changes from its protonated form to its
deprotonated form; hence, the color change.
Titration Conditions N/A
1. Weigh 1.7g sodium hydroxide in weighing bottles.
- Sodium hydroxide is hygroscopic, and will absorb water upon exposure to air.
2. Dissolve in previously boiled and cooled CO 2-free water to make 2000mL.

- Sodium hydroxide reacts with carbon dioxide forming sodium carbonate.
- Production of Na2CO 3 reduces the amount of base present, and increases the amount of
water, resulting to a more diluted volumetric solution.
- Also, a carbonate-bicarbonate buffer will form in the solution and will cause an inaccurate
reading of the endpoint.
- Water must be cooled before addition to sodium hydroxide, because hot alkali solutions
will absorb carbon dioxide more rapidly.
- Evaporation of water is also possible, resulting to a more concentrated solution.
3. Store in tightly capped polyethylene containers

- If stored in glass bottles, concentration of sodium hydroxide will decrease slowly.
- Glass stoppers will freeze due to reaction with the base.
Standardization:
1. Weigh 0.39g potassium biphthalate. Crush lightly and dry at 120 O for 2 hours.
- Crush lightly to increase surface area for drying. Drying results to a purer standard, and
removal of moisture.
- Potassium biphthalate is used because of its high molecular weight (204.222g/mol)
2. From the dried sample, weigh 0.1225g for each trial.
3. Dissolve in 75mL CO2-free water.
4. Add 2 drops of phenolphthalein and titrate.

Chemical Equations KHC8H4O 4 + NaOH KNaC8H4O4 + H2O
Factor 1
Wt NaOH= NT X VT X
1 1000
Standardization:
P
Wt KHP= NT X VT X
1 1000
Other Notes  Solutions of hydroxides naturally absorb CO 2 from the air to precipitate carbonates. This is
unavoidable.

19
Indicator Phenolphthalein TS
Endpoint Colorless to very faint, permanent pink solution
pH range: 8.3-10.0
-the range at which phenolphthalein changes from its protonated form to its
deprotonated form; hence, the color change.
(same as previous)
Standardization:
1. Weigh 0.39g potassium biphthalate. Crush lightly and dry at 120 O for 2 hours.
- Crush lightly to increase surface area for drying. Drying results to a purer standard, and
removal of moisture
- Potassium biphthalate is used because of its high molecular weight (204.222g/mol)
2. From the dried sample, weigh 0.1225g for each trial.
3. Dissolve in 75mL CO2-free water.

- Absorption of CO 2 by a standard solution of Na-/KOH leads to a negative systematic error
in analyses in which an indicator with basic range is used:
CO32- + H3O+ HCO 3- + H2O
Acid indicator: CO 2 + 2OH- H2O + CO 32-
CO32-+ 2H3O+ H2CO 3+ 2H2O
- Effective [ ] of the bases is decreased by absorption of CO 2 = SYSTEMATIC ERROR
- Decrease in [NaOH] will result if stored in glass bottles because of reaction forming
sodium silicates.
4. Add 2 drops of phenolphthalein. Titrate.

Factor 1
Wt NaOH= NT X VT X
1 1000
Standardization:
P
Wt KHP= NT X VT X
1 1000
Other Notes  Solutions of hydroxides naturally absorb CO 2 from the air to precipitate carbonates. This is
unavoidable.

20
Indicator Phenolphthalein
Endpoint Colorless solution turns into faint pink solution
Titration Condition Solutions of titrant and analyte should be cooled to room temp
1. Dissolve NaOH in carbon dioxide-free water.
- Solutions of alkali hydroxides absorb CO 2 when exposed to air; CO 2 lessens the effective
concentration of NaOH.
2OH- + CO 2(g) → 32- + H2O
CO 32- + 2H3O+ → 2CO 3 +2H2O
CO 32- + H3O + → 3 + H2O
-
- Carbonates are avoided when standardizing alkali solutions because intervention with
some titrations happens due to buffering which then results in an unsharp endpoint.
- Carbon dioxide-free water is prepared by boiling water until less prominent bubbling
occurs which means the dissolved gas already evaporated.
- Do not dissolve NaOH while water is hot.
2. Cool the solution to room temp., and filter through hardened filter paper.
- The solution is cooled to room temp because the reaction is very exothermic.
- Filtration can be skipped if no precipitates formed after cooling.
3. Transfer clear filtrate to a tight, polyolefin container, and dilute with carbon dioxide-free
water to 2000 mL
- The solution is preserved in a tightly stoppered bottle fitted, and if possible, with soda lime
tube to protect it from the carbon dioxide of the air.
- P lyethylene b ttle is used since we d n’t w nt unw nted inte cti n between the l ss
and base, producing sodium silic tes; ls , y c use “ eezin .”
Standardization:
1. Weigh potassium biphthalate, previously crushed lightly and dried at 120 degree for 2
hours.
- Analytical grade potassium biphthalate has a purity of at least 99.9%; it is almost non-
hygroscopic.
- Drying ensures the removal of the adsorbed water from the crystals
- Increasing the temperature will cause the removal of entrapped water from the
Crystals.
- Most solids have the tendency to absorb moisture from atmosphere.
- It is crushed lightly since finely divided sample will have more surface area for interaction
with its environment, thus promoting drying.
2. Dissolve potassium biphthalate in 75 ml of carbon dioxide-free water.
3. Add 2 drops of phenolphthalein TS.

- Phenolphthalein is used because the endpoint of this titration is in the alkali region,
between its indicator range, pH 8.9 – 9.8.
- Make sure that only 2 drops of indicator is added to avoid error due to the indicator.
- Phenolphthalein, itself, is a weak acid so it can contribute to the changes in the pH of the
solution.
- Increased amount of phenolphthalein would result to a higher normality factor.
21
4. Titrate produced analyte with the sodium hydroxide solution to the production of a
permanent faint pink color.
- pH range of the color transition is between 8.0-10.0
Factor 1
Wt NaOH= NT X VT X
1 1000
Standardization:
P
Wt KHP= NT X VT X
1 1000
Other Notes  Phenolphthalein or indicators with same pH range are affected by carbon dioxide, cannot be used
at ordinary temperature. With carbonate-free NaOH, phenolphthalein may be employed and
standardization may be effected against potassium biphthalate. It is necessary to remember that
whenever carbonate-free alkali is employed, it is essential that all the water used in the analyses
should be carbon dioxide-free.
 Solutions containing carbonate are not suitable for titration with phenolphthalein as indicator. With
carbonate-free sodium hydroxide, phenolphthalein or indicators with a similar pH range may be
employed. Weak acids like potassium biphthalate use phenolphthalein as indicator. If it is strong
acid, another indicator may be used such as chlorophenol red (color change from yellow to
violet).
 Titrations with the use of standard base solutions usually yield a negative relative error that is
mainly due to carbonate error. To avoid this, a larger amount of NaOH should be weighed
compared to the computed amount. And filter out the carbonates that will precipitate.

22
Preparation and Standardization of 1 N Sodium Hydroxide VS
Indicator Phenolphthalein (pH range: 8-10)
- The reaction involves a weak acid (KHP) and a strong base (NaOH) so the expected
equivalence point will be slightly above pH 7.
Endpoint From colorless to very faint pink
Procedure and RFIS 1. Weigh 80g (amount was modified from USP) NaOH pellets in a beaker covered with
watchglass.
- Sodium hydroxide is very deliquescent and rapidly absorbs moisture.
- Sodium hydroxide also reacts rapidly with atmospheric carbon dioxide and produces
sodium carbonate.
2. Dissolve NaOH pellets in CO 2 free water.

- Atmospheric carbon dioxide is readily absorbed by water and forms carbonic acid.
- This may affect the results since the reaction involved is a neutralization reaction-the
carbon dioxide free water must be cooled to room temperature first before dissolving the
sodium hydroxide because hot alkali solutions rapidly absorb carbon dioxide.
3. Transfer 54.5mL of the clear filtrate to a tight polyolefin container.

- A polyolefin container is used to store the solution because containers with glass stoppers
are liable to freeze or leech in the neck of the bottle.
4. Dry Potassium biphthalate at 120 o for 2 hours

- KHP is heated to remove adsorbed moisture. It is heated to a temperature of 120oC since
it is stable on heating up to 135 oC.
5. CO2 free water is used to prevent formation of sodium carbonates (weaker base); leads to
more titrant volume lower NF
- After drying, put in dessicator to prevent uptake of moisture.
6. Cool Co2 free water because sodium hydroxide pellets are exothermic, to proceed
solubilization. Preferably dissolve in an ice bath.
7. KHP crushed lightly for uniform heating
8. Few drops of indicator because phenolphthalein is weak acid, may interfere with result
larger volume of titrant, lower NF.
Chemical Equations KHC8H4O 4 + NaOH  KNaC8H4O4 + H2O
Factor 1
Wt NaOH= NT X VT X
1 1000
Standardization:
P
Wt KHP= NT X VT X
1 1000

23
Preparation and Standardization of 0.1 N Sodium Thiosulfate VS
Type of Titration Iodometry
Indicator Primary reaction: Self indicating;
- Yellowish green color is due to chromium (III) ions whose formation indicates that the titration
is near its endpoint.
- This first endpoint signals addition of starch see RFIS no. 7.
Starch TS
- Blue strach-iodo complex is formed and as it reacts with Na 2S2O3, loses its blue color.
Endpoint Blue to yellowish green
Dark blue to light blue
Titration Condition Acidic Media (see RFIS no.3)
Procedure and RFIS 1. Accurately weigh about 210 mg of primary standard potassium dichromate (previously
pulverized and dried according to the instructions on its label, if necessary) and dissolve in
100 mL of water in a glass stoppered, 500 mL iodine flask.
2. Swirl to dissolve the solid, remove the stopper.
3. Quickly add 3 g of potassium iodide, 2g of sodium bicarbonate, and 5 mL of hydrochloric

acid.
- Hydrochloric acid is added to ensure that reaction proceeds in the right pH.
- All iodometric titrations are made in either neutral or acid solution for iodine reacts with
alkalies to form hypoiodite and iodide:
I2+2OH- IO - + I - + H2O, 3IO - IO32- + 2I -
- Excess KI is added to keep the free iodine in solution as KI3.
4. Insert the stopper gently in the flask, swirl to mix, and allow to stand in the dark for exactly
10 min.
- The solution is allowed to stand in the dark since light accelerates the hydrolysis of iodine
by causing decomposition of hypoiodous acid 2HIO  2H+ +2I- + O 2.
5. Rinse the stopper and the inner walls of the flask with water.
6. Titrate the liberated iodine with the sodium thiosulfate solution until the solution is yellowish
green in color.
7. Add 3 mL of starch TS.

- Starch should not be added until just prior to the end point, when the iodine color is
beginning to fade.
- Otherwise, there is a tendency to formation of a reddish color which is not readily
discharged at the end point.
8. Continue the titration until the blue color is discharged.
9. Perform blank test.

- Potassium iodide sometimes contains appreciable amounts of potassium iodate as an
impurity.
- In the presence of acid, iodine would be liberated (IO 3- + 5I- + 6H+ 3I2 + 3H2O) -- if a
blue color is obtained with starch, determine the volume of thiosulfate required to discharge
the color, this volume must then be subtracted from the volume required in the
standardization titration.
24
Chemical Equations Primary Standard (K2Cr2O7) and KI [in acidic media]

Red: Cr2O 72- + 14H+ + 6e- 2Cr3+ + 7H2O
Ox: 6I- 3I2 + 6e-
Net: Cr2O 72- + 14H+ + 6I-  2Cr3+ + 3I2 + 7H2O
Balanced: K2Cr2O7 + 14HCl + 6KI 2CrCl 3 + 3I 2 + 7H2O
Liberated iodine and titrant (Na 2S2O 3) –titration proper

Red: I2 + 2e- 2I-
Ox: 2S2O 32- S4O 6- + 2e-
Net: I2 + 2S2O3- 2I- + S4O6-
Balanced: I 2 + Na2S2O3NaI + Na2S4O 6
Factor 6
Computations NT : {WtK2c r2O7/ [MWK2Cr2O7 /(fx1000)]} / VT

25
Preparation and Standardization of 0.5 N Sulfuric Acid VS
Indicator Methyl red
pH range: 4.2-6.2
- Titration of weak base with strong acid uses methyl red as indicator since the equivalence point
is lower than pH 7 and coincides within the pH range of methyl red.
Tromethamine can also be used as indicator.
Endpoint Yellow to pink.
Pink color should not be affected by boiling.
Procedure and RFIS 1. Add slowly, with stirring, 30 mL of sulfuric acid to about 1020 mL of water, allow to cool to
25° C.
2. Heat the anhydrous sodium carbonate to 270ºC for an hour.

- to ensure that moisture is driven off
- to facilitate the conversion of sodium bicarbonate to sodium carbonate, since sodium
bicarbonate is more acidic than the carbonate
3. Weigh 1.5 g anhydrous sodium carbonate using weighing bottles.

- Since sodium carbonate is hygroscopic and to prevent its reaction with CO 2.
4. Dissolve it in 100 ml of water, and add 2 drops of methyl red TS.
5. Add the acid slowly from a buret, with constant stirring, until the solution becomes faintly
pink.
6. Heat to boil the solution once it turns pink, then titrate again.
- Heating is to get rid the solution of CO 2 that was produced in the reaction, CO 2 if not
driven off will render the solution acidic.
7. Heat again to boiling, and titrate further as necessary until the faint pink color is no longer
affected by continued boiling.
Chemical Equations Na2CO3 + H2SO4 → Na2SO4 + H2SO4 + CO2
Factor 2
Computations For preparation:
Wt (g) = N x V x MW
f
Wt of primary standard = NT x VT x MWprimary standard
f primary standard
Other Notes  Indic t s sh uldn’t be used in e cess. he cidic n tu e ethyl ed, i dded in e cessive
amounts, could affect the amount of titrant needed to react with the analyte.
 The pink solution will lose its color when heated, even before it starts to boil. Even so, continue
heating until the solution boils to make sure all carbon dioxide has been driven off.

26
Preparation and Standardization of 1 N Sulfuric Acid VS
Indicator Methyl Red with transition interval of pH 4.2-6.2.
- It is used for weak base titrated against strong acid.
Endpoint From yellow to faint pink color
Titration Condition The reaction should occur at 25 degrees Celsius.
The analyte which is the anhydrous sodium bicarbonate should be dissolve in a carbon dioxide- free
water.
Procedure and RFIS 1. Concentrated sulphuric acid should be added to water and not the other way around.
- The reaction is exothermic and will cause great hazard if done the other way around.
2. The analyte which is the sodium bicarbonate should be heated in the oven at 270 degrees
Celsius for one hour.
- It is done to ensure the removal of moisture content and convert the remaining NaHCO 3
into Na2CO 3.
3. The analyte should be weighed on a weighing bottle.

- The anhydrous sodium carbonate is a hygroscopic substance thus placing it in a weighing
bottle will prevent its uptake of moisture from air.
4. The analyte should be dissolve in a carbon dioxide- free water.

- It is done to prevent the reaction of carbon dioxide with sodium carbonate causing the
formation of unwanted reactant which is the sodium bicarbonate.
5. At first observation of endpoint, the titrand should be heated on boiling until it becomes
colorless. Titrate and heat again if necessary until the titrand does not change in color upon
heating.
- Heating is done to remove the carbon dioxide from the reaction of sulphuric acid and
sodium carbonate in the titrand solution.
- The carbon dioxide causes the color change at first observation because phenolphthalein
is greatly affected by this by-product.
- It is a technique that will distinguish the theoretical endpoint from the pseudo-endpoint
caused by the carbon dioxide.
Chemical Equations H2S04 + Na2CO3 Na2SO4 + H20 + CO2
Factor 2
Computations Wt (g)= NT X VT X MW
2 X 1000

27
Preparation and Standardization of 0.05 M Zinc Sulfate
Type of Titration Direct complexometric titration
Type of Reaction Complexation
Indicator Dithizone TS
- restricted at pH 4.6 (pH where zinc complexes with dithizone)
Endpoint From purplish green to rose pink
Titration Condition pH 4.6
Procedure and RFIS 1. 0.05 M edetate disodium VS
- analyte
2. Add, in the order given, acetic acid-ammonium acetate buffer TS, alcohol, and dithizone
TS.
- The order of addition ensures maintainance of pH at 4.6 and solubilisation of dithizone and
formation of colored complex with alcohol.
Titrate with the zinc sulphate solution to a clear, rose pink color.
3.
- endpoint
Chemical Equations Na2EDTA + ZnSO 4ZnEDTA + Na2SO 4
Factor 1
Computations M 1V1 = M 2 V2

28

Experiment 1 Preparation and Standardization of Volumetric Solutions

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Preparation & Standardization of Volumetric Solutions

Prepared by BBB 2011 | Ph Ch 135 Lab, 1st Sem A.Y. 2013-2014

0.10 N Ammonium Thiocyanate VS………………………...4

Prepared by BBB 2011 | Ph Ch 135 Lab, 1st Sem A.Y. 2013-2014

3. Dilute with 50mL of water.

4. Add 2mL of nitric acid and 2 mL of ferric ammonium sulfate TS.

Normality: (after standardization)

Prepared by BBB 2011 | Ph Ch 135 Lab, 1st Sem A.Y. 2013-2014

4. Allow it to stand for 5 minutes.

5. Titrate with 0.1 N sodium thiosulfate VS.

6. Add 3mL of fresh Starch TS as the endpoint approached.

8. Perform a blank determination.

Chemical Equations Half-reactions

Normality: (After standardization)

Prepared by BBB 2011 | Ph Ch 135 Lab, 1st Sem A.Y. 2013-2014

3. Titrate with 0.1 N ceric sulfate to a permanent slight yellow color.

Prepared by BBB 2011 | Ph Ch 135 Lab, 1st Sem A.Y. 2013-2014

Prepared by BBB 2011 | Ph Ch 135 Lab, 1st Sem A.Y. 2013-2014

2. Transfer to a 400 mL beaker. Add 10 mL of water and swirl to form a slurry.

Reaction of disodium EDTA with CaCl 2:

Prepared by BBB 2011 | Ph Ch 135 Lab, 1st Sem A.Y. 2013-2014

2. Dissolve it in 100mL of water.

3. Add 2 drops of methyl red TS.

5. Heat the solution to boiling, and continue the titration.

7. Each 52.99mg of anhydrous sodium carbonate is equivalent to 1mL of 1N hydrochloric acid

Prepared by BBB 2011 | Ph Ch 135 Lab, 1st Sem A.Y. 2013-2014

2. Add 3 drops HCl.

2. Dilute with 40mL H2O.

3. Add 2gtt methyl orange TS.

4. Follow with diluted HCl until yellow color is changed to pink.

5. Add 2g NaHCO 3, dilute with 50mL water.

6. Add 3mL starch TS.

7. Titrate with Iodine VS until appearance of deep blue color.

Prepared by BBB 2011 | Ph Ch 135 Lab, 1st Sem A.Y. 2013-2014

2. Standardize by titration against freshly standardized 0.1 N potassium permanganate.

2. Add 7 mL of sulfuric acid.

3. Heat to about 70°C.

Prepared by BBB 2011 | Ph Ch 135 Lab, 1st Sem A.Y. 2013-2014

2. Stopper immediately and allow to stand in dark for 5 minutes.

For the Iodine and Na2S2O3:

Normality: (After standardization)

3. Filter through fine-porosity, sintered glass crucible.

3. Keep the temperature of analyte at around 600-700C.

4. Titrate until endpoint.

Prepared by BBB 2011 | Ph Ch 135 Lab, 1st Sem A.Y. 2013-2014

2. Add 5mL of acetic acid.

3. Add 50mL of methanol.

4. Add about 0.5mL eosin Y TS.

2. Dissolve in previously boiled and cooled CO 2-free water to make 2000mL.

3. Store in tightly capped polyethylene containers

2. From the dried sample, weigh 0.1225g for each trial.

3. Dissolve in 75mL CO2-free water.

4. Add 2 drops of phenolphthalein and titrate.

Prepared by BBB 2011 | Ph Ch 135 Lab, 1st Sem A.Y. 2013-2014

2. From the dried sample, weigh 0.1225g for each trial.

3. Dissolve in 75mL CO2-free water.

4. Add 2 drops of phenolphthalein. Titrate.

Prepared by BBB 2011 | Ph Ch 135 Lab, 1st Sem A.Y. 2013-2014

2. Dissolve potassium biphthalate in 75 ml of carbon dioxide-free water.

3. Add 2 drops of phenolphthalein TS.

Prepared by BBB 2011 | Ph Ch 135 Lab, 1st Sem A.Y. 2013-2014

2. Dissolve NaOH pellets in CO 2 free water.