POST LAB

QC1-Prelims
Ms. SHARMAINE S. NARCISO, RPh
 DIFFERENT LABORATORY APPARATUS,
REAGENTS, AND GLASSWARES
› Burette
1. Mohr Burette
–Rubber tube + pinchcock
2. Geissler Burette
–Glass stopper
 QUALITATIVE-QUANTITATIVE ANALYSIS
› ALSO KNOWN AS ANALYTICAL CHEMISTRY
/ WET CHEMISTRY METHOD
 TITRIMETRIC METHOD
› VOLUMETRIC ANALYSIS
› The VOLUME of a solution of known
concentration consumed during an
analysis is taken as a measure of
the amount of AI in a sample.
 QUALITATIVE-QUANTITATIVE ANALYSIS
EQUIVALENCE POINT
-THE POINT IN A TITRATION AT WHICH
THE QUANTITY OF TITRANT IS EXACTLY
SUFFICIENT FOR STOICHIOMETRIC
REACTION WITH THE ANALYTE.
 QUALITATIVE-QUANTITATIVE ANALYSIS
ENDPOINT
-THE POINT IN A TITRATION AT WHICH
THERE IS A SUDDEN CHANGE IN A
PHYSICAL PROPERTY, SUCH AS
INDICATOR COLOR, PH, CONDUCTIVITY,
OR ABSORBANCE. USED AS A MEASURE
OF THE EQUIVALENCE POINT.
QUALITATIVE-QUANTITATIVE ANALYSIS

ACCURACY PRECISION
- refers to the closeness of a - refers to the closeness of two
measured value to a or more measurements to each
other.
standard or known value.
QUALITATIVE-QUANTITATIVE ANALYSIS

 Strength in grams per milliliter solution

or the weight of a substance chemically
equivalent to 1 ml of a standard solution.
QUALITATIVE-QUANTITATIVE ANALYSIS
INDICATOR
INDICATOR
PH RANGE ACID BASE

MALACHITE
0-2.0 YELLOW GREEN
GREEN

METHYL ORANGE 3.4-4.4 PINK YELLOW

METHYL RED 4.2-6.2 RED YELLOW

BROMOTHYMOL
6-7.6 YELLOW BLUE
BLUE
PHENOLPHTHALEI
8-10 COLORLESS PINK/PURPLE/RED
N
QUALITATIVE-QUANTITATIVE ANALYSIS

PRIMARY STANDARD SECONDARY

–HIGHLY PURIFIED
COMPOUND USED STANDARD
– NOT NECESSARILY PURE
AS A REFERENCE BUT EXACT
MATERIAL IN CONCENTRATION IS
TITRIMETRIC KNOWN
ANALYSIS.
–PROPERTIES:
QUALITATIVE-QUANTITATIVE ANALYSIS

NORMALITY VS MOLARITY
QUALITATIVE-QUANTITATIVE ANALYSIS

 ONE IN WHICH THE ANALYTE IS

TREATED WITH TITRANT, AND THE
VOLUME OF TITRANT REQUIRED FOR
COMPLETE REACTION IS MEASURED.
 QUALITATIVE-QUANTITATIVE
QUALITATIVE-QUANTITATIVE ANALYSIS
ANALYSIS

 A MEASURED EXCESS OF THE

STANDARD SOLUTION IS ADDED TO THE
SAMPLE TO ACCOMPLISH A DESIRED
REACTION AND THE EXCESS IS THEN
TITRATED WITH ANOTHER STANDARD
SOLUTION.
ACIDIMETRY
Preparation and standardization of 1N
HCl
TITRANT ANALYTE INDICATOR ENDPOINT

ANHYDROUS GOLDEN
SODIUM YELLOW TO
CARBONATE SALMON
PINK
ALKALIMETRY
Preparation and standardization of
1 N NaOH
TITRANT ANALYTE INDICATOR ENDPOINT

NaOH Colorless
to
Permanent
Pink color
 WHAT IS THE WHAT IS THE
SIGNIFICANCE OF SIGNIFICANCE OF
WHY DO WE NEED TO
WEIGH NAOH
ADDING BARIUM DISSOLVING
PELLETS IN EXCESS? HYDROXIDE IN KHC8H4O4 IN
YOUR NAOH CARBON DIOXIDE
SOLUTION? FREE WATER
CONTAINER TO BE USED: STOPPERED BOTTLE WITH SODA-LIME TUBE (TO
PREVENT IT FROM CO2 IN THE AIR)

REMEMBER:
SOLUTIONS WHICH CONTAIN CARBONATE ARE NOT
SUITABLE FOR TITRATION WITH Pp TS AS INDICATOR SINCE
CARBONATE WON’T YIELD ACCURATE ENDPOINT.
Mo TS IS USED INSTEAD, AND THE RESULTS ARE THE SAME
AS IF ALL THE SODIUM AR PRESENT AS HYDROXIDE.
EXPERIMENT NO. 3
ASSAY OF SODIUM
BICARBONATE TABLETS
 ASSAY OF SODIUM BICARBONATE
TABLETS
TITRANT ANALYTE INDICATOR ENDPOIN
T
NaHCO3 Methyl red

Direct Acidimetric Titration

Experiment No. 4
ASSAY OF ACETIC ACID
CONTENT OF VINEGAR
 ASSAY OF ACETIC ACID CONTENT
IN VINEGAR
TITRANT ANALYTE INDICATOR ENDPOIN
T
NaOH phenolphthalein

Direct Alkalimetric Titration

EXPERIMENT NO. 5
ASSAY OF ASPIRIN
 ASPIRIN (ACETYL SALICYLIC ACID)
 Contains nlt 99.5% and
nmt 100.5% of C9H8O4.
 MW = 180
TITRANT ANALYTE INDICATOR ENDPOIN0T

0.5 ASPIRIN PHENOLPHTHALE DISAPPEARANC

H2S04 IN E OF PINK
/ 0.5 COLOR
HCl
 ONE IN WHICH AN EXCESS OF STANDARD
REAGENT IS ADDED TO REACT WITH ANALYTE.
THEN THE EXCESS REAGENT IS TITRATED
WITH A SECOND REAGENT OR WITH A
STANDARD SOLUTION OF ANALYTE.
 BLANK TITRATION
 AN ANALYSIS OF A SAMPLE
WITHOUT THE ANALYTE OR
ATTRIBUTE, OR AN ANALYSIS
WITHOUT A SAMPLE.
 SIGNIFICANCE OF ADDING
NAOH IN THE SAMPLE:
- TO NEUTALIZE ANY FREE ACID FORMED
BY THE HYDROLYSIS OF ASA AND TO
NEUTRALIZE THE CARBOXYL GROUP OF
ASA.
C6H4OCOCH3COOH + H20
C6H4OHCOOH + CH3COOH
C6H4OCOCH3COOH + NaOH
C6H4OCOCH3Na + H2O
 ON BOILING WITH STANDARD SODIUM
HYDROXIDE SOLUTION, ASPIRIN IS
HYDROLYZED INTO SALICYLIC ACID AND
ACETIC ACID.
 THE LIBERATED ACID REACTS WITH
SODIUM HYDROXIDE TO FORM SODIUM
SALT.
 ALSO, TO REMOVE CARBONATE PRESENT
SINCE THE INDICATOR USED IS Pp TS.

SIGNIFICANCE OF BOILING THE SOLUTION

OF ASPIRIN BEFORE TITRATION
EXPERIMENT NO. 6
DOUBLE INDICATOR TITRATION
 Double Indicator Titration

Solution 1 (NaOH + Na2CO3) Solution 2 ( NaHCO3 + Na2CO3)

20 ml water 20 ml water

2 gtts of Pp TS 2 gtts of Pp TS

Titrate with HCl Titrate with HCl

Endpoint : Disappearance if pink color Endpoint : Disappearance if pink color

2 gtts of Mo TS 2 gtts of Mo TS

Endpoint : Salmon color Endpoint : Salmon color

 DOUBLE INDICATOR TITRATION
TITRANT ANALYTE INDICATOR ENDPOINT
HCL SOLUTION
1
SOLUTION
2

NaOH + HCl ---------- > NaCl + H2O

Na2CO3 + HCl -------- > NaHCO3 + NaCl
NaHCO3 + HCl ------- > NaCl + CO2 + H2O
 Pp Mo
NaOH + HCl - NaCl + H2O
Na2CO3 + HCl - NaHCO3 + NaCl NaHCO3 + HCl -NaCl
+ CO2 + H2O

v1 > v2 = NaOH, Na2CO3

Pp Mo

Na2CO3 + HCl -
NaHCO3 + NaCl NaHCO3 + HCl -NaCl + CO2 +
H2O
NaHCO3 + HCl -NaCl + CO2 + H2O
v1 < v2 = Na2CO3, NaHCO3
 Percentage assay : NaOH,
Na2CO3
% NaOH = (mL HCl Pp - mL HCl Mo) x N HCl
x meq
------------------------------------- x 100
wt of sample
% Na2CO3 =2 (ml HCl Mo) X N HCl X meq
------------------------------------- x 100
wt of sample
 Na2CO3, NaHCO3
% Na2CO3 =2 (ml HCl Pp) x N HCl x meq
------------------------------------- x 100
wt of sample
% NaHCO3 = (mL HCl Mo - mL HCl Pp) x N HCl x
meq
------------------------------------- x 100
wt of sample
Reagents:
Reagents Hydrochloric acid
› Clear, colorless solution
› Highly corrosive
› Strong mineral acid
› Aka Muriatic acid, Spirits of salt
› Contains nlt 36.5% and nmt 38% by
weight.
› Preserve in tight container
› MW = 36.46
› Strong monoprotic acid
Reagents:
Reagents Sodium Hydroxide
› Highly caustic metallic base
› Hygroscopic
› Aka Caustic soda
› Contains nlt 95% and nmt
100.5% of total alkali
› MW = 40
› Preserve in tight container
› Strong base
Reagents:
Reagents Acetic Acid
› Colorless liquid
› Component of vinegar
› Weak acid
› Contains nlt 36% and nmt
37% by weight.
› MW = 60
› Weak acid
Indicators: Phenolphthalein
› C20H14O4
› Often used in titrations, it
turns colorless in acidic
solutions and pink in basic
solutions.
› Colorless = acidic = pH< 8
› Pink = basic = pH > 8
› Purple in strong solution
› Used as laxative (withdrawn)
› Carcinogenic
› MW = 318
Indicators:
Indicators Methyl Orange
› In an acid it is reddish and
in alkali it is yellow
› Mutagenic property
› C14H14N3NaO3S
› MW = 327
› Has a pKa of 3.47 in
water at 25 degrees
Celsius
“ IF MY MIND CAN
CONCIEVE IT, MY
HEART CAN BELIEVE
IT, I KNOW I CAN
ACHIEVE IT! ”
-JESSE JACKSON