QUALITY CONTROL
Weighing by difference- employed when
Lower meniscus- clear/colorless
Sa line- colored
Introduction:
Analytical Chemistry
Qualitative- identify the unknown
Quantitative- determine the amt of
substance
Methods of Quantitative Analysis
1) Volume of Analysis-vol. of std. consumes/
reacted
2) Physicochemical Methods
a. Instrumental techniques
i. Chromatography- TLC
ii. Spectrometry- UV vis
iii. Electrometry
iv. Refractomery
v. Polarimetry
3) Gravimetric analysis- mass or wt. of
solid/ppt
4) Special Method- specific for a substance
Volumetric Anaylsis (Titrimetry)
vol. of standard = vol. of analyte
Types:
Neutralization- acid & base; forms salt+
water
Precipitation (Precipitimetry)- form ppt;
insol solid; use of precipitating agent
Complexation (Complexometric)-
determine amt or test metals, ligands,
chelates; uses polyvalent ions
Oxidation-reduction gain & loss of e-;
change in oxidation number
Analytical Balance
Specifications:
Accuracy- nearest to the true value
Precision
Capacity- largest amt the balance can
weigh
Sensitivity- smallest amt the balance can
weigh
Readability- mg or g
Techniques in weighing
1. Direct- weight empty container- tare- add
the sample- desired weight
2.
the substance is hygroscopic
Titration
- Actual process of adding or making a
standard react with your analyte using a
burette
o Titrant: the standard; in the burette
o Analyte: the sample/ substance you are
analyzing
o Indicator: substance that changes color
when endpoint has been reached
o Endpoint: the point at which equal amt of
std & analyte have reacted; actual
o Equivalence or stoichiometric point: based
on balanced chemical equation; calculated
theoretically
Standard: solution of known concentration
o Primary standard- chemically pure solids
o Primary standard solution- prepared from
a primary standard
o Secondary standard solution- determined
from a primary standard solution
Standardization
- Primary standardization: uses 1o standard
to standardize a solution
- Secondary standardization
Types of Titration
1. Direct- analyte reacts with a titrant
A + T P
2. Indirect- aside from the titrant, you add
another substance because the analyte
cannot react directly with the titrant
A + R IP
IP + T P
3. Residual/ Back titration- analyte is not
very reactive
xss
A + P
T
xss
+ T2 P
T
Classification of Reagent
1. Technical/ Practical grade: only for
cleaning
2. Reagent grade: high grade (for labs)
3. Primary standard: chemically pure solid;
used for reaserch ; meets USP
requirements
4. Specific use: made solely for a particular
research
5. Specific use: made solely for a particular
research

Blue: bases; weak acid

Red: acid; strong acids
Expt 1:
Preparation & Standardization of * NaOH pellets- hygroscopis
Hydrochloric Acid Soln *Solution- exothermic
PRINCIPLE: Primary standardization/ Direc * amberflint bottle
titration
ENDPOINT: Salmon Molarity:
Reagents: NaOH
HCl Sample/ analyte ( mL x M)NaOH= (mL x M)HCl x RR HCl
Methyl orange Indicator
Anhydrous Na2CO3 Primary standard
Normality:
Na2CO3 + 2HCl > 2NaCl + H2O + CO2 ( mL x N)NaOH= (mL x N)HCl x

*colorless flint bottle Expt.3

Assay of Aspirin
Molarity: PRINCIPLE: Residual/ Back titration
Na 2CO 3 ENDPOINT: disappearance of light pink/
mL x M= mL x M x RR HCl colorless
Reagents:
Na 2CO 3 Aspirin Sample/ analyte
mmol = mL x M x RR HCl Phenolphthalein Indicator
Standard HCl T2 / back titrant
solution
mg Na 2CO 3
Standard NaOH Excess Titrant/ T1
MW = (mL x M) x RR HCl
solution

mg Rxns: Actual determination

HCl 1) Neutralization
MW
MHCl= x RR Na 2CO 3
mL

Normality: + NaOH > + H2O

MeqsNa2CO3= meqsHCl
wt .( g) ASA+ NaOH > Sodium acetylsalicylate + H2O
MW /h x 1000 = mL x N
2) Saponification

wt .(g)
NHCl = MW /h x 1000
mL(HCl)
+ NaOH > +

Expt. 2
Preparation & Standardization of Sodium
Hydroxide Soln Sodium acetylsalicylate + NaOH > Sodium salicylate +
Sodium acetate
PRINCIPLE: Secondary standardization/
ENDPOINT: Light pink 3) Excess NaOH
Reagents: NaOH + HCl > NaCl + H2O
Sodium hydroxide Sample/ analyte
Phenolphthalein Indicator Rxns: Blank determination
Standard HCl Primary standard 1) NaOH + HCl > NaCl + H2O
solution soln

NaOH + 2HCl > NaCl + H2O

 wt . (g)of pure ASA
% ASA= x 100
wt .vol. of sample
Molarity:

Normality:
Precipitation/ Precipitimetry/
Argentometry/ Saturation

Standard solutions:
AgMO3, KSCN, NH4SCN
Indicators:
Colored ions: Ferric alum/ FeNH4(SO4)2 Expt.5
Colored secondary ppt: K2CrO4 Assay of Ammonium Chloride
Colored absorption product:
PRINCIPLE: Residual titration ( Volhards)
Dichlorofluorescein
ENDPOINT: Flesh color (supernatant liquid)
Eosin
Reagents:
Y.T.S.
NH4Cl Analyte
TEE
( tetrabromo phenolphthalein ethyl ester) AgNO3 soln XSS titrant/ ppting
agent
Methods: Conc. HNO3 Prevent silver to ppt
1) Thiocynate- direct/ indirect; uses ferric as carbonate,
alum phosphate, etc
2) Volhards- residual; uses ferric alum KSCN Back titrant/ ppting
3) Mohr- determine Br, Cl, CN ions; uses agent
K2CrO4 Ferric alum / Indicator
4) Fajan- absorption production indication
FeNH4(SO4)2
Expt. 4
Rxns:
Preparation and Standardization of
NH4Cl + AgNO3 > AgCl + NH4NO3
Potassium Thiocynate Solution ( KSCN) (excess) (white ppt)

PRINCIPLE: Direct titration AgNO3 + KSCN > AgSCN + KNO3

(excess) (white ppt)
ENDPOINT: Flesh color (supernatant liquid)
Reagents: wt . of pure NH 4 Cl
KSCN Titrant %NH4Cl=
x 100
wt of Sample
AgNO3 soln Analyte/ standard
Conc. HNO3 To remove red color
that would interfere Molarity:
with endpoint
Ferric alum / Indicator
FeNH4(SO4)2

Rxns:

AgNO3 + KSCN > AgKSCN (white ppt) + KNO3 Normality:

_FeNH4(SO4)2 + _KSCN > _ Fe(SCN)3 +

_K2SO4 + (NH4)2SO4
(flesh color)
Molarity:
mnKSCN= mnAgNO3
KSCN
mL x M= mL x Mx RR AgNO 3 Complexation/ Complexometry/
Complexometric
Normality:
Ex: Test for metals Water hardness Mg, Ca,
meqskscn=meqsAgNO3
mL x N = mL x N K ions
Complex: formed when a molecule reacts with wt .( g)
a metal ion (N x mL)CaCO3 = MW /h x 1000
Chelate: resulting complex when a combining
molecule contains 2 or more groups
*weight in 1.0mL only (aliquot)
EDTA- Ethylene diamine tetraacetic acid *EDTA reacts in 1:1 ration with any metal ion,
( Standard) thus h is always 1

REDOX Reactions
Iodimetry- iodine as titrant

Y - Iodometry- iodine in thesample-

liberating iodine
or
Indicator: STARCH- from arrowroot
MW: 372. 24 g/n Iodo-starch complex (dark blue)
Expt.6
Preparation and Standardization of EDTA
Soln

PRINCIPLE: Complexation
ENDPOINT: clear blue solution
Reagents:
EDTA Titrant/ acid burette
CaCO3 Primary standard/ Expt. 7
analyte Preparation & Standardization of Sodium
Conc. HCl Enchance solubility of thiosulfate Soln
CaCO3 PRINCIPLE: Redox/ Iodometry
Ammonia buffer Maintain pH at 10; Initial endpoint: Pale yellow
pungent ENDPOINT: disappearance of blue color
Eriochrome black Indicator
*boil to sterilize water bc Na2S2O3 is not stable
T / EBT
NaOH Enhance solubility of Reagents:
EDTA in water Na2S2O3 Analyte/ base burette
MgCl2 Source of Mg ion; KIO3 Primary standard/ acid
sharpens the endpoint Starch T.S. Indicator
Na2CO3 Prevent acid catalyzed
*EBT- binds with metal to form a RED complex hydrolysis
*pH 10- the pH at which EDTA reacts rapidly & KI Hasten dissolution
quantitatively
Rxns:
Rxs: *chage in oxidation number
*reativity factor is based in the loss or gain of
MgY- + CaEBT > CaY2- + EBT + Mg2+ electrons
(red complex) (blue)

CaCO3 + 2HCl > CaCl2 + CO2 + H2O

(boiled to remove CO2)

Molarity:
mL x MCaCO3 = mmolEDTA x RR IO3- + 5 I- + 6 H+ > 3 I2 + H2O
wt .(mg)
mL x M= MW x RR

Normality:
GEROA- gains e- - reduced- oxidizing
agent
 LEORA- loses e- - oxidized- reducing I2 Analyte
agent Starch T.S. Indicator

Rxns:
2 Na2S2O3 + I2 > 2 NaI + Na2S4O6 2 Na2S2O3 + I2 > 2NaI + Na2S4O6

Molarity:

Molarity: 1I2
wt .(mg) (mL x M)i2 = (mL x M)na2so3 x RR 2 Na2 SO3
(mL x M)NA2SO3 = ( MW )KIO3 x
I2 Na 2 SO 3
KIO 3 RR x I2
Normality:

meqsi2 = meqsna2so3
Normality: (N x mL)i2 = (N x mL) na2so3
wt .( g)
(mL x N)NA2SO3 =(
MW /h x 1000 KIO3 Expt.9
Assay of Ascorbic Acid in commercially
available tablets

PRINCIPLE: Redox/ Bromination

Initial endpoint: Faint straw yellow/ golden
yellow
ENDPOINT: disappearance of blue color
Reagents:

Na2S2O3 Back titrant

KBrO3 Titrant1
KI Analyte
Expt. 8 Starch T.S. Indicator
KBr
Preparation & Standardization of
Iodine Soln KBr- Potassium bromide
KBrO3- Potassium bromate
PRINCIPLE: Redox/ Iodometry/ Secondary
standardization Standardizations:
Initial endpoint: Faint straw yellow/ golden 1)
C6H8O6 + Br2 > C6H6O6 + 2Br - +
yellow 2H+
ENDPOINT: disappearance of blue color
Reagents: 2) BrO3- + 5Br- + 6H+ > 2Br- + I2

Na2S2O3 Titrant/ Primary 3) 2I- + Br2 > 2Br- + I2

standard
4) 2S2O32- + I2 > 2I- > 2I- + S4O62-