0% found this document useful (0 votes)
50 views16 pages

DD Handbook

The document outlines a series of chemistry experiments focused on the synthesis of aspirin from salicylic acid and acetic anhydride, as well as the estimation of ibuprofen and antacid capacity. It includes detailed procedures, calculations, and expected results for each experiment. The aim is to understand the chemical reactions involved and to quantify the yields and effectiveness of the substances used.
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd

Topics covered

  • Ibuprofen estimation,
  • Sodium carbonate,
  • Laboratory equipment,
  • Suction pump,
  • Titration,
  • Chemical analysis,
  • Solvent extraction,
  • Aspirin preparation,
  • Acid-base reactions,
  • Chemical education
0% found this document useful (0 votes)
50 views16 pages

DD Handbook

The document outlines a series of chemistry experiments focused on the synthesis of aspirin from salicylic acid and acetic anhydride, as well as the estimation of ibuprofen and antacid capacity. It includes detailed procedures, calculations, and expected results for each experiment. The aim is to understand the chemical reactions involved and to quantify the yields and effectiveness of the substances used.
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd

Topics covered

  • Ibuprofen estimation,
  • Sodium carbonate,
  • Laboratory equipment,
  • Suction pump,
  • Titration,
  • Chemical analysis,
  • Solvent extraction,
  • Aspirin preparation,
  • Acid-base reactions,
  • Chemical education

Procedure: Reaction:

distilled acetic
Requirements: Theory: Aim:
Salicylic
acid Experiment
Aspirin No. 1
(3)
Chapter 1
(4) (2) (1)
COOH OH anhydride To
water,
a order Nowshaking Add 4150Place 2
glass Heat Salicylic
prepare from
cm -COC-CH,CH, +
Preparations/Estimations
the toadd 150
rod ensure cm or
ofconical g anhydride Salicylic Salicylic
inaspirin
flask 2-3 Acetic cm the acid
for the of
about thoroughon drops [Link]
supplicdthe conicalpresence
flask. acid isfrom
a a Acid (SemesterV)
waterbath 15 of Conc. phenolic
salicylic
anhydride AcetylationH,SO, flask,
powder, of
minutes. mixing,conc. conc.
quantity
water
to H2SO4 accticHzSO acid acid.
about to dryof bath,
and carefully it which
anhydride, gives
50°-60°C ctc.
swirl salicylic
acid Aspirin COOH 0C-CH, on
aspirin.
the constant acetylation
and contents with CH,COOH + conc.
stir in
a H;S04,
with dry with
in
Calculations:Observations:
Results:
Theoretical
yield:(1) Supplied
quantity
(2) (1) (8) (7) (6) (5)
(4) (3) (2) (1) Percentage
yield:(2)
Recrystallise
the Dry waterAllow
:. 138 Yield wateFiler
r.
TheoreticalWeightMelting
Percentage 100 :.g2.608Weight
2gof g product and
of of at and the
g the weigh the shake
of of reaction
ofpoint salicyclic
acisalicyclic
d=
yield yield the
aspirin crude product and the suction
product of the it
product
determineproduct well.
mixture
= = the acid crude
2.608 product = pump
(x) 2.608g.= =
xg. product. Applied
=xgof
aspirin =xg. 180×2180 the using to
g. = 2.608 100 xX 138 and cool
%. = g melting 5
%. of cm' wash Components and
aspirin
point of the add
°C. hot product 50
(Expected
135°C).
of
water. (Drugs
cm
the
of
[Link], with distilled &
Dyes)
dry cold
Estimation:
PartII: Standardisation:
Procedure: lbuprofen
Part I:phenolphthalein
Requtremnents: and Estimation
250 cm standardTheory: Preparations/Estimations
(by Aim: of ExperimnentNo. 2
(4) (3) (2) (1) (2) (1) pipette,c then back
colourless. against
1% Pipette
measuringTransfer
completely.
Ibuprofen alcoholic
Add TbuprofenWeigh colourless. against1%Pipette water. standard Take beaker solution.
buprofen
HCl titration To
the cstimate
phenolpthalcin 15 phenolphthalein 150
0.1IN out e.
etindicator, unreacted
the cmNaOH and [Link] outmeasuring 10 cm IN method)
10flask in 10
cm is the
HCI cm' contents of transfer
a HCI cm conicalalcoholic treated amount
and solution 250 of
distilled Ibuprofen alkali
solution of
indicator. dilute
it cm
solution of flask IN
with
in of Wg indicator. it alcoholic lask, NaOH ibuprofen
to in
it.
and is a
from 150 awith itthe water beakcr. or from 150 a powder, determincdknown
End beaker End dilute
100solution,
the cm'distilled and Add th e cm NaOH cm'
the present
pointburctte
conical stir supplied point conical it distilled
standard cxcess
to 10 burette to
solution
100
[Link] by
to cm will in
wilusing water. 100 adissolve
titrating of the
be flask quantity
of using flask
be cm' measuringwater, HCI alkali
from aand cn standardised from and with in solution, given
the 2 a burette,
drops against like
2 standard
pink drops titrate of pink titrate distilled 100
given flask, NaOH samples.
the cm
to of it to of it 101% a 3
Calculations:
Reactlons:
(4) (3) (2) (1) (2) (1)
The(5)
NaOH+ CH
solution. cm
100Ibuprofen
solution
: diluted Amount Amount
Amount terms
solution=x
cm. solution. (CHhCH-CH:
:. HCl 10 (unused) CH*
1000
Normality cm
cmsample of0.1N CHCH:
of
of of of of the HCl’
IN of AN
A
NHCl A ofdiluted
NNaOH
NaOH=Ibuprofen NaOH NaOH diluted NaCIl
solution
NaOH NaOH +
solution H;0 CH-COOH CH, Applied
206 requircd solution solution
=cm.=Z
=y CH-COONa
H;0 + CH,
g 10 -y
of x cm. solution= solution
Z added Components
lbuprofen. cm. used unused
10
x =AN. required NaOH +
up in
Z terms **0.l
cm by after 10
(Drugs
of 10 x
treatment of cm
A c [Link]
N of
NaoH of Dyes)
the HCI [Link]
in
lbuprofen
stimation
andA;Aim:
.A1 of
xperiment Results:
Preparatiors/Estimations

To (3) (2) (1)


estimate Amount Normality
of 10
.:.
A
Ncm 10
NaOH x
of Z
is the
amount
[Link] the of cm
solution
dilutcddiluted
2 of
AN
(Alternate
of
present solution NaOH NaOH=
uprofen
a
in solution 206
prescnt the roquired
x10
Method) given (4) 1000
xZ
of in sample (Z) =
xA
i the =
[Link]
given =
e
samples N.

cm
g.
colour. pinkcolourless
to
from bewil point Enindicator.
d phenolphthalcin 1%
of
drops usin2g burctte the fromsolution NaOH [Link] against
titrateit and flaskconical cm' l150 ain itofcm10ouPipette
t (2)
water.
distilled with cn
100 todiluteit and flaskmeasuring standard
100c solution
ain(approximately)
HCl IN of cn10
Take (1)
Standardisation: I:Part
Procedure:
(unused)
H;0 NaCl+ NaOH
’ HCI+ (2)
aci(stomach
d)
2H,0 MgCl+; Mg(OH)
’ 2HCI+ (1)
Reactions:
ctebcaker
. cm250 water,
distilled burctte, pipctte, cm' 10
flask, conical cm150 îlask,measuring
standard cm' indicator,
100 phenolphthalein solution,
1% NaOH
[Link], (approximate)
HCI tablets,
IN Antacid
Requirements:
solution. alkali stanadard
againsta titrated aciisd cxceNN
of solution.
The acistandard
d volume
of
known neutralised
awith Antacid
is pain. rolicve andstomach the in
present acid excess ofneutralise to
used drugs the Antacids are Theory:
antacid. given capacity
aofneutralising acid estimate
the Aim:
To
Drug Capacity
aofNeutralising Acid
Experiment
3No.
=_g=A: A,
sample= the present
inlbuprofen g.
Amount
of (3)
z)
(ylrequired Ibuprofen solution. NaOH NAof
Cm' samplofe solution
of The (2)
solution
(-4) NaOH given Normalofity ()
Results:
7 Pparations/Estimations
antacid Weiof
ght
used acid Amount
of
antacid
of given capacityofNeutralising (5)
Mg(OH)2 NaOH
2= HCl=1 1
observc, reaction,
we the From
Ccm'. 10 cm100 .".
Ccm
=X-y solution
tacid diluted the of cml0 by upused HCI Amount of (4)
AN terms cm. solution
=y NaOH
ofneutralisation
in after unused HCl Amount
of (3)
cm. solution
x = NaOH NA terms
of addcd
in HCl Aount
of (2)
-AN.
M =10x solution HCl given Normality
of
MN. -
10 solution HCl diluted thNormality
e of
Xx0.1
[Link] solution. NaOH
of cm
requiredx solution HCI diluted the of cm10(1)
Calculations:
colour. pink to
rless from be
wil point indicator.
End phenolphthalcin
1%drops
of using2 burette the from solution NaOH [Link]
ainst titrate
it and flask conical ain it of cn10outPipctte (4)
illed with dilute and flameasuring
sk standard water.
cm 100
abeaker
to the contents
of transfer
the and and itCool (3)
completely. antacid given dissolve
the tostir and Wam (2)
solution
it. to standardised
HCI of
cm 10and water distilled of cn 15Add beaker cm250 ain
tacid the quantity
of supplied the or
Wg
transfer ()
Estimation:and Weigh I : Part
Dyer) Components
(Drugs& Applied
8
beakers, cm
S00 cm, 250 tubes,
capillary
Chromat ography hyl pestie,
pag alcohol, Requiretement s: mortar, etc,
extracts, tissue plant strips, paper
pathogens fungi. insects
and especially
herbivores
and many toxic
to are they plants
chemical the flavonoids)
a subcategory as defense
of
inchuding flavonoids, inrole have of anthocyanins (a
radiation (UV)ultraviolet Many DNA. andproteins celdamage
l can that
Flavonoids bl o ck pigmcnts
that pl ant clImportant
ofass
anare photosynthesis.) reactions
wavelengths of light the focritical r
pigmentisand Chlorophyll blu e and red absorbs but light, green reflects
ais animals. interactions
with regulating that
plants rolimportant
in es other havepigCol mentosur-producing beyond
plant kindsdifferent
of thousands of presence Pigments.
be can fruits, of the by accounted
for
andflowerS, lcaves, as
such tissues plant
colours array broad The light. colours found
in
abilities of
to differing have of vari ous reflect and absorb
Different colours. they because col our different appear pigments
many consists
of actually light white that Recall
light. reflects aabsorbs nd thmol
at ecule pi
paper pigby ments natural
Chorophyll). simplyachromatography.
([Link]
,is Theory:A
components
of separate
of Aim:
Chlorophyl) Chromatography
(e. g , To
Paper Pigments by Natural Components
of Separation
of
Experiment
4No.
antacid given capacioftyNeutralising
(3)
consumcd
(C) solution solution. NaOH [Link] of cn
antacid diluted the of cm10 (2)
N. solution
(4) HCl given Normalofity ()
Results:
antacid
W
Weigof
ht
10C xC10
9 Preparationg/Estimations
amount
ol the and have you sample of
type Depending
the on load ncxt
applying
the before dry fully paperis the until wailoading,
t cach After
4-(probably
6). extract of
loads several upply need
to wil you paper,
the pigments
on concentrate
the to
order cxtract,
In of
load another
withrepcat then papcr, completely
the on dry extract
to the Allow
fibers. paper the absorbed
into isitaspaper the onto tube
lary the ofout move wilextract chromatography
The paper. your
oriof
gin the ontcapillary
o the of
end the Dab [Link] the up
grate extract
to thcAllow solids.) the from away run fraction
to liquid
the allow slightly
to mortar your tilt this,minimise [Link]
the clog wil which tissue plant fragments
of contain may extract
(your extract. your portion
of liqud the into tubecapillary aDip
chromatogram: the onto extract the Load 3:Step
consistency. paste-like avoida solution but
rated highly createa to goal
is You [Link] dark very
illiliters
of few crcatea nccessary
to tissuc)
as plant ethanol (or adding
ntinue solution. ipigments
nto threlcasc
e pestle
to completely
wiath
grind and tissue plant the cthanol to amount
of small Add
aflowers).
leaves
or few (a
mortar o
inatinterest tissuc
of plant the Place
extract: plant yourPrepare Step
2:
paper
[Link] Preparation
of 2.2: Fig.
migratofion paper. the pigments
up
with
the interfere fingertips
can from oils possible
-
litle
as as them touch tocaro taking edges, the papers by the Handle
rigin. the is this cnd- one from cm 2-3 about strip thacross)
e way
not (but across line pencil fine Drinstructor,
awa your suggested
by the
ionsall following strips chromatography
into paper the Cut
chromatography
papers: Prepare Step
1:
Procedure:
Dyes) (DrugsComponents
& Applied
pigments differeni spectra
for known tcompared
he to could
bespectrum
resultant spectrophotometer.
The the using spectrum absorption
mcasuring
is andethanol as
suchsolvent, another dissolving
in it
chromatography
paper
by the from pigment (remove)a elute could we
example, Formcthod. another byassayit and paper the from removeit
physically topigment
is identity
a of determine
the to way One
methods. variety
of identificd
aby becan separated,
they Pigments
are
the Once another. one fromseparate visibly to
themallowing paper
atography the up
ratesdifferent move
at pigments
wil different
result, solvent).
aAs chosen solubilitics
our in different (e.g,properties
physical and shapes, sizes, different havepigments Different
tography: Paper Isolated
by Pigments ldentifying
notebook. your indata your
alRecord
l isolated. youpigments the identity
of the about provided)
reference instructor
(or your Consult tested. solvent
chromatography
each pigment
in cach fobelow)
r (described Rfvalue Calculate
the
pigments: yourIdentify St6:
ep
time). overa fade wil (thcy observe youpigments the label
and trace then dry,chromatogram
air to the Allow front. solvent the
location
of the mark quickly pencil
to chromatogram.
aUsc thremove
e
pape, the oftop the from cm2-3 within front
is solvent the When
results: your recordchromatogram
and the Stop 5:Step
source) ignition other spark,
or flame, any clear of kzp
possible
and as
much as
fumes inhaling
the avold to
care Takeinhaled. Langerous
if
becan flammable
and highly solvent etherlacetone
s petroleum (Warning:
The
chromatography
paper) the pigment
up ansolvent
d movement
of
theobserve frequently
to chromatogram the Check solvent. the
origin
in submcrgc
the towant chromatogram
not doyou your origin
on
the below solvent
is the of
level the that sure Make down. end origin
the provided
with container solvent the into strip paper your Place
solvent:
chromatography chromatogram
the in the Set 4:
Step
prepare chromatograms) the
al exiract
to same the tissue.
Use plant given a
lolested
r should
be solvents
omatography which know you let instructor
wil Your lesting bewil you
solvent
chromatography chromatogram
cach for prepareI lo
necl wil You (Note:
completely
dry. sample
is your until step3 proceed
to not minutes).
Do
(2-10 dry sample
to r
the fominutes sevcral take may it it, in
water
Preparalions/Esamations
pignents Rfvalueof ()
Results:
cmfront
in solvent origin to fromdistance
cm pigment
in oritogin fromdistance value Rf
manzal. refercnce recorded ain values known pigment to
nown our colour
of and value Rfthe match then can Again, we
avels. chronatography
solvent thdistance
e the relative
to travels
gment distancea representing the ratio valuae, Rf calculate
the to is
ethodalternative manul.
An reference appropriate scarching
anin by
Dyes) (DrgsComponents
& Applied
stirring. constant with waterdistilled in
of cm10nitrite
sodium oflgof solution to
adda and 5°C solution the Cool (2)
obtaincd. solution
is clear until warmit beaker
and cm250
water distilled
ain ofcm25 carbonate
and sodium anhydrous
acid,
of1.g0 sulphanilic supplied
quantity
of the or gPlace2 (1)
Procedure:
Orange
lIl -Naphthol
No,sN-N HOSN-NCI
Coupling )
NaOH
OH
OH
Sulphanilic
acid
o,SN-NCI 05C NH, -
HCI NaNO,+
Diazotisation
Reactions:
ctc. ovenelectric icrushed
ce, thermometer, bcaker, cm
s0
NaCl, NaCO,, anhydrous solution, NaOH l0% B-Naphthol
in water,
distilled solution, HCl conc. NaNO,, Sulphanilic
acid, Requirements:
Orange
Il. get meditoum
alkaline p-naphthol
in withcoupled whiisch diazonium
salt gives
(0C at
HCI and NaNO, diazotisation
with Sulphanilic
on
acid Theory:
sulphanilic
acid. from Orange
ll prepare To Ain:
Sulphanilic
Acid from OrangeII
Work Project
Chapter2
orange
lI xgof orangeII of
3.791g
xgproduct crude Weiof ght
yiPercentage
eld: (2)
-3.791g
173 sulphanilic
aci=d of2g :.
x2328
orange
II of
=328g sulphanilic
acid ofg173
Theoretical
yield: (1)
Calculations:
xg. product= the Yiof
eld (2)
quantity= Supplied (1)
Observations:
product. dricd
the weigh and 80°C oven
at electric anproduct
in the Dry (10)
solution. saturated
salt
litde wiath washit and pump, suction the product
at the Filter (9)
[Link]
is until ice in
cool then and hour Ifor air the incool solution
to the Allow (8)
dissolves. untilit warm and chloride
itto sodium Add5gof (7)
dissolved. has solid
the all until mixture the heat mintes, 10
atter and wll Stir (6)
paste.
lline aas
separates
out dye the andread1ly place takes
pl1ng $°C. and between0temperature maintaining
the
sulphanilic
acid diazotised suspension
of mixed well
stirring
the constant with inpour and $°C solution
to this Cool (5)
beaker. cm 100 ain
tion NaOH 10% ofcm
B-naphthol
10in ofDissolve
2.g0 (4)
icrushed
ce. of g
and HCI conc.
15 2.5
ofcm'containing beaker cm250 inato
g constar1t with andslowly solution resulting the Pour (3)
Components
es) (Drugs& Applied 14
is itdye, and fibrebetween interactions typcs various knowing
of
(Fabrics):
By Fibres particular applcable
to Dyes Types
of
cotton
fibres, unmerceriscd than dyes
aflinity
for inercascs
the almercerisation.
so This is
called treatmcnt
procedure lengthwisc.
This shrink cannot they and luster like silk
of
acquire fibres cottontreatmcnt, this Afler swollen. them make which
pressure alkali
under concentrated with treatcd arefibres Cotton
Mercerisation:
CH,OH
OH H
H OH H
/OH
H H
CH,OH OH H
basic. noracidic neither are
uniCellulose
ts hydrophilic. highly fibre the make which unitsbiglucose
groups
of side argroups
e alcoholic secondary anprinary
d Iinkage,
ether bridgesof With [Link] chains
of arranged linearly of
-up made are uniCellulose
ts unitscellulose
. pure ofisfibre Cotton
Cotton:
polyester. and nylon like fibressynthetic
are fibresmanmade
other while wool, and silk cotton, arenative fromobtained Fibres
Fibres: of
Types
fabric. cotton given adye To
Aim:
(Cotton) Fabric Dyeing
of
Percentage
yicld (3)
yield-3,791g. Theoretical (2)
product
(*) the Weiof
ght ()
Results:
%.
3.791
x100 X 100g ..
15 Work Prfect
16 Applied Components (Drugs &Dyes)
possible to guess appropriate dye for the particular types of fibre as
indicated below:

Types of Fibre (Fabric) Type of Dyes


(1)Cotton Direct and vat dyes.
(2) Wool Acid, basic, mordant and reactive dyes.
(3) Silk Acid, basic and mordant dyes.
(4) Polyesters Disperse dyes.
(5) Polyacrylonitile Cationic dyes.
(6) Polypropylene Selected disperse dyes.
Basic Operations of Dyeing Process:
Various methods are utilised for dyeing purposes according to the
requiremnents. They are:
(1) Preparation of the fibres
(2) Preparation of the dye bath
(3) Application of the dye
(4) Finishing.
Methods of Dyeing:
Following methods of dyeing are used:
(1) Direct dyeing
(2) Vat dyeing
(3) Mordant dyeing
(4) Disperse dyeing
(5) Formation of dye on the fibres
(6) Dyeing of the wool with acid dyes
(7) Dyeing with reactive dyes.
dyeing of
Of the above, the first and second methods are used for
cotton fabrics.
(1) Direct dyeing:
decide the
Absorptive power of the fibre and nature of the dye
variations in the conditions of dyeing.
ProjetWork 17

(1) The dye bath is prepared by dissolving dye in distilled water.


(2) A small quantity of sodium sulphate (Na,SO4) and sulphuric
acidacetic acid (H,SOJCHCOOH) are added to it. Stir it
well.

(3) The cotton fabric is introduced in this bath. And the


temperature ismaintained at 60°C.
(4) A small quantity of common salt (NaCl) or Glauber's salt
(NazSO4) is added to the bath, heat the bath to boiling for
sometime.
(5) Coolthe bath and remove the dyed cotton fabric. Rinse with
cold water and then dry it.
(2) Vat dyeing:
(1) Prepare the dye bath by adding vat dye in the form of paste
and dispersing agent is water that contains caustic soda
(NaOH) and sodium bydrogen sulphide (NaHS).
(2) Vat dyeing is partly carried out by continuous process. Cotton
fabric is saturated with vat liquor and then it [Link] to fix
the leuco compound to the fabric.
(3) The cloth is allowed is pass through a bath which contains
oxidising agent like chromatic acid and acetic acid or
perchlorate.
(4) The colour generates which is soaped, rinsed thoroughly with
water and finally dried.
cotton fabrics].
[Note: Vat dyes offer excellent fastness and are used invariably for

You might also like