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Ethylenediamine tetra-ace tic acid and its sodium salts (EDTA ) form a chelated soluble complex when added to a solution of certain metal cations. If a small amount of a dye such as Eriochrome black T is added to an aueous solution containin! calcium and ma!nesium ions at a p" of #$ % $.#& the solution will become wine red. If EDTA is then added as a titrant& the calcium and ma!nesium will be complexed . After sufficient EDTA has been added to complex all the ma!nesium and calcium& the solution will turn from wine red to blue. This is the end point of the titration. Apparatus #. 'urette . ipette *. Erlenmeyer flask +. 'ottle etc. Reagents #. ,tandard EDTA titrant ($.$# ) . Eriochrome black T indicator *. Ammonia buffer solution Procedure #. Dilute m/ of sample (0) to about $ m/ with distilled water in an Erlenmeyer flask. . Add # m/ of buffer solution. *. Add two drops of indicator solution. The solution turns wine red in colour. +. Add the standard EDTA titrant slowly with continuous stirrin! until the last reddish tin!e disappears from the solution. The colour of the solution at the end point is blue under normal conditions. . 1ote down the 2olume of EDTA added (0#).  Calculation Hardness as CaCO3= V1 x S x 1000  mg / L V where& , 3 m! 4a45* eui2alent to # m/ of EDTA titrant  3 # m! 4a45* Hardness as CaCO3= 1000 V1  3 mg / L V

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Ethylenediamine tetra-acetic acid and its sodium salts (EDTA) form a chelated soluble complex when

added to a solution of certain metal cations. If a small amount of a dye such as Eriochrome black T is

added to an aueous solution containin! calcium and ma!nesium ions at a p" of #$ % $.#& the

solution will become wine red. If EDTA is then added as a titrant& the calcium and ma!nesium will be

complexed. After sufficient EDTA has been added to complex all the ma!nesium and calcium& the

solution will turn from wine red to blue. This is the end point of the titration.

Apparatus

#. 'urette

. ipette

*. Erlenmeyer flask

+. 'ottle etc.

Reagents

#. ,tandard EDTA titrant ($.$# )

. Eriochrome black T indicator

*. Ammonia buffer solution

Procedure

#. Dilute m/ of sample (0) to about $ m/ with distilled water in an Erlenmeyer flask.

. Add # m/ of buffer solution.

*. Add two drops of indicator solution. The solution turns wine red in colour.

+. Add the standard EDTA titrant slowly with continuous stirrin! until the last reddish tin!e disappears

from the solution. The colour of the solution at the end point is blue under normal conditions.

. 1ote down the 2olume of EDTA added (0#).

 Calculation

Hardness as CaCO3=

V1 x S x 1000

  mg / L

V

where&

, 3 m! 4a45* eui2alent to # m/ of EDTA titrant

  3 # m! 4a45*

Hardness as CaCO3=

1000 V1

  3 mg / L

V

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TA'/E 56 A758IATE p" 56 ,5E 4551 A4ID, A1D 'A,E,

AT 0A7I59, 4514E1T7ATI51,.

157A/IT:;

1 #1 $.#1 $.$#1 $.$$#1

ATE7IA/

"ydrochloric

acid!;l

---*<. *.< $.*= $.$*=

"4l p" $.## #.$> *

,ulphuric acid !;l +? +.? $.+? $.$+?

",5+ p" $.+ #.#= .$ *

6ormic acid !;l ? +< +.< $.+< $.$+<

"455" p" #.<# #.=? .* .> *.+

/actic acid !;l #>$ ?$ ? $.? $.$?

4*"<5* p" #.=> #.?= .+* .? *.

Acetic acid !;l #$ <$ < $.< $.$<

4"*455" p" .#> .+ .>= *.*= *.>?

T.,... !;l---

>* >.* $.>* $.$>*

1a++5= p" #$. #$.# ?. ?.$#

,oda Ash !;l #$< * .* $.* $.$*

1a45* p" ##.< ##. ###$ ?.>

Ammonia("ydroxide)

1"+5"

!;l *+ #= #.= $.#= $.$#=

p" ##.= ##.? ##.#< #$.<+ #$.#

Trisodium

phosphate!;l ?>.< +?.* +.?* $.+?* $.$+?

1a*5+ p" #.> #.* ##.+ ##.# #$.?

4austic soda !;l

 

+$ + $.+ $.$+

1a5" p" #*.?* #.?> # ##

 

Caustic Soda l!e"

Take approximately !rams of caustic diluted to $$ ml. 6rom this take $ml and titrate with # 1&

",5+ usin! phenolphthalein as indicator. ercenta!e ,tren!th 3 0 x +$ x #$$; $ x x wt where 0

is the 2olume of ",5+ consumed and wt 3 ;$$ x $ !rams.

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Con#ersion o$ Caustic soda concentrations"

To con2ert a wei!ht of a caustic soda solution to a wei!ht of solid caustic soda& multiply by the @w;w

content and di2ide by #$$.

Example "ow much sold caustic soda should be used in place of # k! of #$$TB caustic soda (@ w;w

3 +=.**)C

Calculation" # x +=.**;#$$ 3 .= k! 1a5" solid.

To con2ert a 2olume of caustic soda solution in to wei!ht of solid caustic soda& multiply the 2olume& in

liters& by the !;l content of the solution.

Example "ow much solid caustic soda should be used in place of # liters of +>.#'e (-=#$!;l 1a5")

caustic solutionC

Calculation" # x =#$ 3 >$! 3 >.k! of 1a5" solid.

,pecific ra2ity and concentration of 4austic ,oda solutions at $4

Specific Gravity and concentration of Caustic Soda solutions at 20C

, 'e TB @B;B ;/

#.$$$ $ $ #.$ #$.<

#.$$ <.= #$ +.<> +>.?

#.#$$ #*.$ $ ?.#? #$#.#

#.#$ #>.> *$ #*.=* #=.?

#.#<$ #?.> * #+.<+ #<?.>

#.#=$ $.? *+ #.+ #>#.>

#.#>$ .$ *< #<.++ #?+.$

#.#?$ *.$ *> #=.* $<.+

#.$$ +.$ +$ #>.< #?.$

#.#$ .$ + #?.<# *#.>

#.$ <.$ ++ $.$= ++.?

#.*$ <.? +< $.?> >.$

#.+$ =.? +> #.?$ =#.

#.$ >.> $ .< >.

#.<$ ?.= *.> ??.$

#.=$ *$.< + +.< *#.?

#.>$ *#. < .< *=.#

#.?$ *.+ > <.+> *+#.<

#.*$$ **.* <$ =.+# <.

#.*#$ *+. < >.** *=#.#

#.*$ *.$ <+ ?.< *><.

#.**$ *.> << *$.$ +$#.<

#.*+$ *<.< <> *#.#+ +#=.

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#.*<$ *>. = **.$< ++?.<

#.*=$ *?.$ =+ *+.$* +<.$

#.*>$ *?.> =< *.$# +>*.

#.*?$ +$. => *<.$$ $$.+

#.+$$ +#. >$ *<.?? #>.$

#.+#$ +.$ > *=.?? *.<

#.+$ +.= >+ *>.?? *.<

#.+*$ +*.+ >< +$.$$ =.$

#.++$ ++.# >> +#.$* ?$.>

#.+$ ++.> ?$ +.$= <#$.$

#.+<$ +.+ ? +*.# <?.<

#.+=$ +<.# ?+ ++.#= <+<.

#.+>$ +<.> ?< +. <<?.#.+?$ +=.+ ?> +<.= <?>.

#.$$ +>.# #$$ +=.** =#$.$

#.#$ +>.= #$ +>.*$ =*$.+

#.$ +?.+ #$+ +?.++ =#.

#.*$ $.$ #$< $.$ ==.+

Finding the strength of Soda Ash

 

Scope"

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This test method co2ers the titrimetric determination of the total alkalinity of soda ash. This alkalinity

is normally expressed as percent sodium oxide (1a 5).

Summar! o$ %est &et'od

Total alkalinity is determined by titration with standard hydrochloric (or sulfuric) acid usin! methyl

oran!e or modi Ced methyl oran!e indicator solution.�

(nter$erences

Alkalies other than soda ash (sodium carbonate) and compounds that consume acid will affect the

accuracy of this test method.

Reagents

# "ydrochloric (or ,ulfuric) Acid (#.$ 1)Frepare in accordance with ractice E $$ (recordtemperature of solution when standardiGed).

odi Ced ethyl 5ran!e Indicator ,olution or ethyl 5ran!e Indicator ,olutionF,ee ractice E�

$$. ##.* Bater& carbon dioxide-free (freshly boiled and cooled).

Procedure

#. Bei!h& to the nearest $.# m!& +.+ H;- $.# ! (1ote #) of the sample and transfer to a $$-m/

conical ask. Add #$$ m/ of water and swirl to dissol2e the sample. 9se of the spec Ced wei!ht of�

sample reuires a #$$-m/ buret for titration and is recommended. If a $-m/ buret is used& the

sample wei!ht should be hal2ed to . !. Add * drops of modi Ced methyl oran!e indicator solution�

. Titrate this solution with standard #.$ 1 acid to a !ray end point.

*. 7ecord the 2olume to the nearest $.$ m/ and temperature of the acid used. 4orrect the acid

normality for any difference from the standardiGation temperature by use of the factor D1;4

$.$$$* between $ and *$4. Add the correction when the temperature of use is below and subtract

when abo2e the temperature of standardiGatiGed.

If desired& $.# @ methyl oran!e indicator solution may be used.

FThe analyst should end the titration at the same shade of color as was used for the end point in the

standardiGation of the acid.

Calculation

4alculate the total alkalinity as percent sodium oxide

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,odium 5xide Bt@ 3)A x * + 0030,,0- x 100/*

where

A 3 acid reuired for titration of the sample& m/&

' 3corrected normality of the acid& and

B 3 sample used& !.

Alternati2ely& calculate the alkalinity as sodium carbonate as follows

sodium car.onate t 3 #.=#$# x 1a5 wei!ht @

If actual sodium carbonate content is desired& the sodium bicarbonate content must be determined

separately as

sodium car.onate (actual)& @ 3 A -(' 8 $.<*$>)

where

A31a45* & @ and

'3 1a"45*& @ .

7ef 4ourtesy http;;en.bliJoil.com;9ser6iles;9ploads;E*?.D6

Anal!tical met'ods

H2O2 concentration

eneral remar4s

This method describes the determination of hydro!en peroxide concentration in an aueous solution.

Be recommend that each sample is processed at least twice.

Procedure

lace approx. $ ml 1 sulfuric acid (",5+ & . mol;l ) in a flask and add an exactly wei!hed

sample of the "5 containin! solution. 9se an analytical balance (four decimal di!its). A syrin!e

could be used to add the "5 sample. In this case& the syrin!e has to be rinsed thorou!hly before

use. 4alculate the amount by wei!hin! the filled syrin!e before and after addin! a few drops to the

flask.

6or all procedures only deioniGed or distilled water should be used.

Titrate the sample with $. 1 potassium perman!anate solution ($.$ mol;l) while mixin! 2i!orously.

If usin! 2isual;manual titration& titrate until a pale pink coloration persists for a while. If usin!automatic titration euipment& the end point could be determined potentiometrically 2ia a redox

electrode.

1ote otassium perman!ante solutions must be standardiGed re!ularly.

4alculation

The content of hydro!en peroxide in the solution is calculated as follows

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The result !i2es the concentration of hydro!en peroxide in the solution expressed in wei!ht percent (!

"5;#$$ ! solution)

Sta.ilit!

eneral remar4s

This method describes the determination of hydro!en peroxide stability in an aueous solution. A

sample of hydro!en peroxide is stored at ?< 4 for #< hours. This treatment leads to a certain loss of

hydro!en peroxide content. The percenta!e loss of content !i2es the decomposition rate of the

sample.

The content of "5 before and after the treatment is analyGed with potassium perman!anate in

acidic medium.

4lean euipment and a clean workplace alon! with hi!h purity of the rea!ents are essential for this

analytical method. The flasks should be dedicated to this procedure. 5therwise& unreliable results

could be obtained. Be recommend that each sample is processed at least twice.

Procedure

Each of three flasks of #$$ ml 2olume is filled with exactly $ ml (pipette) of the hydro!en peroxide

sample. To a2oid losses by e2aporation& the flasks are co2ered (e.!. with a condenser cap)& but not

closed ti!htly. 5ne of the flasks is used to determine the initial hydro!en peroxide content. This one is

stored at room temperature. The two other flasks are stored in a water bath for #< hours at ?< 4.

After that& all flasks are cooled to $ 4 and filled up to the #$$ ml mark with distilled or deioniGed

water. 1ow& the hydro!en peroxide content of these heated and unheated samples is determined. 6or

this& the titration method with potassium perman!anate is applied (see abo2e).

Calculation

The decomposition rate of the hydro!en peroxide sample is calculated as follows

pH #alue

eneral remar4s

This method describes the determination of the apparent p" 2alue of hydro!en peroxide. The

measurement is carried out directly in the sample. A !lass electrode and a common p" meter with a

resolution of $.$# p" units is used.

Procedure

The p" euipment must be calibrated for acidic p" ran!es usin! two different& well-defined standard

p" solutions. 4alibration has to be repeated before e2ery series of measurements.

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Determination of the apparent p" of the hydro!en peroxide sample is carried out directly in the

sample. The 2alue !i2en by the p" meter represents the final result.

Determination of the strength of sodium hypochlorite

Sodium H!poc'lorite" (1a54l) E Bt *.

5etermination o$ acti#e c'lorine in Commercial Sodium H!poc'lorite"

Acti2e 4hlorine is not liberated as such from alkaline hypochlorite bleach liuors.

The effecti2e amount of 4hlorine liberated by acidification of hypochlorite solution is defined by the

euation as below.

1a54l H KI H ",5+ I H 1a4l H K,5+ H "5

1a,5* H I 1aI H 1a,+5<

Procedure"

ml of concentrated hypochlorite is diluted to #$$ ml with distilled water.

ipette #$ml of the abo2e solution in to a $$ ml conical flask containin! about $$ ml distilled water

and $ml otassium Iodide solution ( approximately #<< !;l)

Add $ml dilute (#$@) ,ulphuric acid and titrate with $.#1 ,odium Thiosulphate until the solution is

pale yellow color.

Add ml starch solution (soluble starch #@ w;w) and continue titration until the blue color formed is

dischar!ed. /et the Titre 2alue be A ml of $.#1 ,odium Thiosulphate.

Calculation"

# ml $.#1 ,od. Thiosulphate 3 $.$$* !ram acti2e chlorine

ram;liter Acti2e 4hlorine 3 $.$$* x A x #$$$ x #$$;(#$ x )

Standardisation o$ Sodium %'iosulp'ate"

1a,5*. "5 ol Bt +>.#> !;mol E. Bt +>.#>

,tandard ,olution <.$ !ram of Thiosulphate is dissol2ed in $ ml of D.D.water (Alkaline proof)

=.p".

6or alkaline proof& we ha2e to add some phenolphthalein indicator and add $.#1 1a5" lye until pink

colour appears.

(odometric con#ersion ta.le"The table below pro2ides easy con2ersion of titres to ,odium "ypochlorite or acti2e chlorine content of 

bleach liuor when a #$ml sample of the liuor has been titrated with $.#1 ,odium Thiosulphate

solution.

Volume of 01NNa2S3O4

Active Chlorinecontent of 100%

Active Chlorinecontent of 26% conc

Active Chlorine g/l

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conc olution olution

1 0!22 0!"" 0!3#

2 0!4# 1!$6 0!$1

3 0!6$ 2!64 1!06

4 0!0 3!#2 1!42

# 1!13 4!40 1!$$

6 1!3# #!2" 2!13

$ 1!#" 6!16 2!4"

" 1!"0 $!04 2!"4

2!03 $!2 3!1

10 2!26 "!"0 3!##

11 2!4" "!6" 3!0

12 2!$1 10!#6 4!26

13 2!3 11!44 4!61

14 3!16 12!32 4!$

1# 3!3 13!20 #!32

16 3!61 14!0" #!6"

1$ 3!"4 14!6 6!03

1" 4!06 1#!"4 6!3

1 4!2 16!$2 6!$4

20 4!#2 1$!60 $!10

 

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• Textile Testin!

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• 6ind the stren!th of caustic soda

• 6ind the stren!th of ,oda Ash

• 6ind the stren!th of "ydro!en eroxide

• 6ind the stren!th of ,od."ypoclorite

• 6ind the stren!th of acids L sod.bicarbonate

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Testing Strength of Acetic acid, Hydrochloric acid , Sulphuric acid and

Oxalic acid -1

Standardisation o$ Sulp'uric Acid ol Bt ?>.$> L E. Bt +?.$

+? !rams;litre of ",5+ !i2es #1 acid.

Strengt' %esting o$ Sulp'uric Acid"

Bei!h accurately about # !ram of the acid and transfer to a conical flask with D.D.Bater. Add

phenolphthalein indicator and titrate a!ainst $.1 1a5" to a permanent pink colour.

@ of ",5+ 3 (0ol. of 1a5" x 1 of 1a5" x +?) ; (Bt of Acid x #$)

,tandard 1orms 3 ?<.@ to ?>@ w;w.

Acetic Acid Strengt' %esting" ol Bt <$.$ E.Bt <$.$ 6reeGin! oint#<.< and 'oilin!

oint##>4

Bei!h accurately about $. !ram of the sample and transfer to a conical flask usin! D.D.Bater. The

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@ of Ac5" 3

(0ol. of 1a5" x 1ormality of 1a5" x <$) ; (Bt of acid x #$)

,tandard 1orms ?< to ?>@ w;w

 

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esting Strength of Acetic acid, Hydrochloric acid , Sulphuric acid and

Oxalic acid -3

Potassium Permanganate" ol Bt #>.$+ B.Bt 3 *#.<#reparation of ,tandard solution *.#<# !ram of K15+ in $$ ml of D.D.water boiled for *$ minutes

and made up to # litre !i2es $.#1 solution.

Determination of the stren!th of K15+ $ ml of $.#1 5xalic acid H $ ml of #1 ",5+ are heated

to a warm temp. and titrated a!ainst K15+.

0#1# 3 01 1#3 01 ($.# 8 $);burette readin! of K15+

Oxalic Acid Strengt' %esting" ol Bt#<.$= E.Bt <*.$

Bei!h about $. !ram of the acid and transfer to a conical flask containin! $ ml of distilled water.

Dissol2e the acid completely and titrate a!ainst $.1 1a5" usin! phenolphthalein as indicator.

@ of "554-455"."5 3 (0ol of 1a5" x 1 x <*); (wt of acid x #$)

,tandard 1orms 3 ?+ to ?>@ w;w.

Strengt' o$ Sodium *icar.onate" 1a"45*

About # !ram of the sample accurately wei!hed is dissol2ed in distilled water and made up to $ ml.

a $ ml of the solution is titrated a!ainst $.#1 "4l usin! phenolphthalein as indicator and the readin!

noted as :.

Take another $ ml of the solution and titrate a!ainst $.#1 "4l usin! methyl oran!e as indicator and

the Titre 2alue be 8.

4aluculation

@ of ,od.'icarbonate 3

O(8 P :) x $.$$>+ x #$$ x 1ormality of "4l)Q;wt of sample in $ml

,tandard 1orms ?+ to ?>@.

Strengt' o$ Citric acid " E Bt =$ eltin! oint#*4

Bei!h accurately $. !ram of the sample and dissol2e in $ ml of distilled water. Add phenolphthalein

indicator and titrate a!ainst $.1 1a5" to a permanent pink color.

4alculation

@ of acid 3 (0ol of 1a5" x 1 x =$);(Bt of acid x #$)

,tandard 1orms ? to ?>@ w;w.

,tren!th Testin! of "ydro 4hloric Acid ol Bt 3 *<.+<

Bei!h accurately $. !ram of the acid and transfer to a conical flask with D.D.water. Add

phenolphthalein indicator and titrate a!ainst $.1 1a5" to a permanent pink colour.

4alculation

@ of "4l 3

(0ol of 1a5" x 1ormality of 1a5" x *<.) ; Bei!ht of "4l x #$

,tandard "ydrochloric acid stren!th will be ? to *

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%ri Sodium P'osp'ate E Bt >

About !rams of dried sample ( heated to #$$4 for hours)& accurately wei!hed is dissol2ed in $

ml of distilled water. Add . !ram of common salt (2acuum salt) and after to #4& the solution is

titrated to a distinct red color with #1 "4l& usin! methyl oran!e as indicator.

4alculation

@ of T.,.. 3 (0ol of "4l 8 1ormality of "4l x >);(Bt of the sample x #$)