Test Method of Liquid Top Flux –

GETFLUX A

Date : 21.11.2018
 LIQUID FLUX

CHARACTERISTICS METHOD

APPEARANCE VISUAL

SPECIFIC GRAVITY BY HYDROMETER

ZINC CHLORIDE
METHOD – 1
(% W/W)

TOTAL CHLORIDE
METHOD – 2
(% W/W)

AMMONIUM CHLORIDE
METHOD – 3
(% W/W)

SODIUM CHLORIDE METHOD – 4

(% W/W)
 METHOD - 1

DETERMINATION OF ZINC CHLORIDE

Apparatus:
100 ml Beaker.
250 ml Beaker
250 ml Conical Flask.
250 ml Volumetric Flask
1000 ml Volumetric Flask.
50 ml Burrette.
25 ml Pipette.
100 ml cylinder.

Reagents;
EDTA Solution (0.0575(M))
Ammonia - Ammonium Chloride Buffer Solution
Erichrome Black-T Indicator
Sulphuric Acid

Preparation of Reagents:

 :
EDTA Solution (0.0575(M))
Weight exactly 21.41 gm of Ethylenediamine Tetraacetate(EDTA) and
dissolve in 600 ml of demineralised water and take to 1000 ml with demineralised
water.
Factor of EDTA = Weight taken
21.41
 Ammonia – Ammonium Chloride Buffer:
Weight 55 gm of Ammonium Chloride and dissolve in 500 ml of
demineralised water.
Add 350 ml conc.Ammonia Solution and take to 1000 ml with demineralised
water.

 Erichrome Black – T Indicator:

Dissolve 1 gm of Erichrome Black –T and 10.0 gm of Hydroxylamine
Hydrochloride
In sufficient methyl alcohol to produce 250 ml..
Procedure :

Take near about 3 gm sample and dissolve in demineralised water and add
0.5 ml Sulphuric Acid and volume make up to 250 ml. Take 25 ml solution in
a conical flask and add 50 ml demineralised water and also add 25 ml
Ammonia – Ammonium Chloride Buffer .Titrate with 0.0575(M) with Erichrome
Black – T indicator.

Calculation : Burrete Reading X F X 7.837

Weight Taken
 F = Factor of 0.0575(M) EDTA

METHOD - 2

DETERMINATION OF TOTAL CHLORIDE

Apparatus:
100 ml Beaker.
250 ml Beaker
250 ml Conical Flask.
250 ml Volumetric Flask
1000 ml Volumetric Flask.
50 ml Burrette.
10 ml Pipette.

Reagents;
Silver Nitrate Solution(0.1(N))
Calcium Carbonate
Potassium Chromate Indicator

Preparation of Reagents:

 :
Silver Nitrate Solution (0.1(N))
Weight exactly 16.987 gm of Silver Nitrate and dissolve in 500 ml of
demineralised water and take to 1000 ml with demineralised water.

Factor of Silver Nitrate = Weight taken

16.987

 Potassium Chromate Indicator:

Dissolve 12.5 gm of Potassium Chromate in demineralised water to produce
250 ml..
Procedure :

Take near about 3 gm sample and dissolve in demineralised water and

volume make
up to 250 ml. Take 10 ml solution in a conical flask and add 2-3 gm Calcium
Carbonate with 50 ml demineralised water .Titrate with 0.1(N) Silver Nitrate
with
Potassium Chromate as indicator.

Calculation : Burrete Reading X F X 8.865

Weight Taken

F = Factor of 0.1(N) Silver Nitrate

 METHOD - 3

DETERMINATION OF AMMONIUM CHLORIDE

Apparatus:
Heating Mantle.
Two Naked R.B. Flask with Condensor
Addition Funnel.
Glass Bend Collector with Funnel.
Still Head with Fixed Thermometer Pocket
500 ml Beaker, 250 ml Beaker.
500 ml Volumetric Flask.
25 ml Pipette.
1000 ml Volumetric Flask
100 ml cylinder.
250 ml Conical Flask
Reagents;
Sodium Hydroxide Solution (1.0(N))
Sulphuric Acid Solution (1.0(N))
Oxalic Acid Solution 1.0(N)
50% Sodium Hydroxide Solution
Methyl Red Indicator.
Phenophthalein Indicator.

Preparation of Reagents:

 :
Oxalic Acid Solution (1.0(N)
Weight exactly 63.0 gm of Oxalic Acid and dissolve in 500 ml of
demineralised
water and take to 1000 ml with demineralised water.

 Sodium Hydroxide Solution (1.0(N) :

Weight 40 gm of Sodium Hydroxide and dissolve in 500 ml of demineralised
water.
and take to 1000 ml with demineralised water.
Standardisation : Pipette out 25 ml of the oxalic Acid (1.0(N)) solution into a
250 ml
Conical Flask.Add 2-3 drops of phenolphthalein indicator solution into it &
titrate
with 1.0(N) Sodium Hydroxide solution until pink colour is obtained.
Calculation : Exact Normality /Factor = _____ 25__________
Burrette Reading

 Sulphuric Acid Solution (1.0(N) :

In a beaker take 500 ml of water .Add slowly with constant stirring about 27
ml of Sulphuric Acid (98%).and take to 1000 ml with demineralised water.
Standardisation : Pipette out 25 ml of the above solution into a 250 ml Conical
flask
 . Add 2-3 drops of phenolphthalein indicator solution into it & titrate with
1.0(N)
Sodium Hydroxide solution until pink colour is obtained.
Calculation :Exact Normality /Factor = Burrette Reading X Factor of Sodium
Hydroxide
25

 Sodium Hydroxide Solution (50%):

Weight 500 gm of Sodium Hydroxide and dissolve in demineralised water.
and take to 1000 ml with demineralised water.

 Phenophthalein Indicator:
Dissolve 0.1 gm of Phenophthalein in 20 ml of Methyl Alcohol demineralised
water to produce 250 ml.

 Methyl Red Indicator:

Dissolve 0.025 gm of Methyl Red in 125 ml Methyl Alcohol and dilute to 250
ml. with
Water.

Procedure :

Take 25 ml. sample in Two naked R.B. Flask and add 50 ml. D.M.
water and also add 150 ml. 50% Sodium Hydroxide Solution drop by drop by
addition funnel. Distilled out the vapour and 200 ml. liquid by Condenser
which added with extra Glass Bend Collector with Funnel in 500 ml. beaker
where 100 ml. 1.0(N) Sulphuric Acid and 100 ml. D.M. water and 2-3 drops
Methyl Red Indicator stored (If the color is change Red to Yellow then add
extra quantity of 1.0(N) Sulphuric Acid). Collect total solution and volume make
up to 500 ml. Volumetric Flask. Take 25 ml. from this solution and add 50
ml. D.M. water.Titrate with 1.0(N) Sodium Hydroxide using Methyl Red
Indicator.

Calculation : (A1 X F1  B1 X 500/25 X F2) X 53.5 X 100

1000 X 25 X Sp.Gravity of the sample

Where A1 = Required quantity of 1.0(N) Sulphuric Acid

F1 = Factor of 1.0(N) Sulphuric Acid
B1 = Required quantity of 1.0(N) Sodium Hydroxide
F2 = Factor of 1.0(N) Sodium Hydroxide
 METHOD - 4

DETERMINATION OF SODIUM CHLORIDE

Apparatus:

Muffle Furnace (800C)

Reagents;

Hydrochloric Acid.

Procedure :

Weigh near about 3 gm. Sample in a Silica or Platinum Crucible and

add 5
ml. conc. Hydrochloric Acid . Ignite at 800C about 2 hrs. After ignite if the
Residue is yellowish then again add Conc. Hydrochloric Acid and also ignite
at 800C until colourless Residue. Weigh the Residue.

Calculation : Weight of the Residue X 100

Weight Taken