Free sulphuric acid content analysis

1) Shall Weigh 5-10 gm Sample (W) of PTSA / DDBSA / DDNSA OR Other grade

2) Shall add about 150 ml DW and 0.5 to 2 ml conc. HCL and put the beaker on

hot plate. Then add 15-20 ml 10% BaCl2 by measuring cylinder into the

beaker.

3) Shall digest the solution for 40-60 minutes at 90-100 deg C temperature

4) Shall weigh sintered G-4 crucible and note down the weight as W1 gms above

filter the digested solution using vaccum pump.

5) Shall add 20-25 ml D.M into the bucket and transfer it in the crucible

[ensuring no adhered ppt. remains in the beaker]

6) Shall wash the residue in the crucible with hot DW till filtrate show no

turbidity when tested with drops of HNO3 and 0.5 ml silver nitrate solution

7) Shall put the crucible in an oven kept at 115+/-10 drg C for 30-45 minutes.

Then cool the crucible in desiccator to room temperature.

8) Shall weigh the crucible and note down the weight as W2 gms

9) Shall calculate sulfate content using following formula –

PTSA monohydrate

% free H2S04=[(W2-W1) x98x100] ¸ [Wx233.28]=[(W2-W1)x42] ¸ W

Where, W1=Weight of empty crucible in gms, W2=Weight of crucible +ppt in gms

W= Weight of sample taken in gms

10) Shall note down the result and use the data for further reference

Assay of PTSA/ DDBSA

Shall Calculate % Assay of PTS Acid on monohydrate basis using following

formula

A=[(Total acidity - Free H2SO4)] X 190 ¸ 49

Where, A= %PTSA Assay on Monohydrate basis,

Shall Calculate %Assay of PTS Acid on monohydrate basis corrected to

moisture using following formula

B=[Ax100] ¸ 100-[(Ax (total moisture%-9.47) ¸ 100]

Where B=%PTSA Assay Corrected to moisture content

Shall note down the result and use the data while preparing an analytical report.

The H2SO4 reacts with the BaCl2 to produce BaSO4 precipitate . The precipated BaSO4 is then weighed and

calculated as H2SO4 in the product , with the related Calculation given in MOA . The reaction is as under

H2SO4 + BaCl2 ----> BaSO4 + 2HCl

MW -------> 98.08 208.23 233.38 72.92

MW of H2SO4 / MW of BaSO4 x 100 = 42 (Factor)