Objective :

To Oxidise Formic Acid by Hydrogen Peroxide.

Chemicals :

The following chemicals were used as received without further purification; formic acid (99–100 %), ferrous sulfate heptahydrate , ferric sulfate , hydrogen peroxide (30 wt%), and sodium hydroxide .

Methodology :

Fresh solutions of formic acid (0.01 M) mixed with ferric sulfate (0.001 M) or ferrous sulfate (0.001 M) were prepared before the start of each experiment.

experiments were performed in a beaker (250 mL), which was kept at constant temperature. The experiments were started by adding the H2O2 solution (2.0 ml) to the formic acid (0.200 gm ) , total volume was 200 mL). The pH and TDS of the solution was continuously monitored using a pH TDS meter.

24/06/2022

Aim : To study reproduced literature oxidation of Formic Acid using Hydrogen Peroxide in Fenton Reaction.

Preparation:

  1. Take 200 ml Distilled water .
  2. Add 0.135 gm Formic Acid and 0.037 gm FeSO4 .
  3. cheking PH and TDS of solution.

Observation :

Hydrogen Peroxide PH TDS
0.2 gm 1-21100
0.2 gm 1-2950
0.2 gm 1-2900
0.2 gm 1-2750
0.2 gm 1-2700
0.2 gm 1-2500
0.2 gm 1-2400
0.2 gm 2-3300
0.2 gm 2-3350
0.2 gm 2-3300

Conclusion :

From TDS Values it is evident that Hydrogen Peroxide Oxidation resultified in to reduction in ion concentration.

Date : 25/06/2022

Aim : Reapeat of Fenton Oxidation at lower temperature to verify effect of temperature.

Observation:

At room temperature,

Hydrogen Peroxide PH TDS
0.2 gm 1-21100
0.2 gm1-2 950
0.2 gm 1-2900
0.2 gm1-2650
0.2 gm 1-2 500

Conclusion :

From Primary report oxidation at 30 ° seems to be less effective than Fenton Reaction at 45 ° Results are not very significant.

Date : 27/06/2022

Aim : To study effect of time duration of extent of oxidation of Formic Acid.

Observation :

Hydrogen peroxide PH TDS
0.2 gm 1-2 1050
0.2 gm1-2900
0.2 gm 1-2750
0.2 gm 1-2600
0.2 gm 1-2450

Conclusion :

No Significant change Observed.

Date : 28/06/2022

Aim : To study effect of temperature 35° c instead of 45° c and 30° c .

Observation :

Hydrogen Peroxide PHTDS
0.2 gm 1-2 1250
0.2 gm 1-2 1150
0.2 gm 1-2 900
0.2 gm 1-2 750
0.2 gm 1-2650

Conclusion :

No Significant change in extent of oxidation.

Date : 29/06/2022

Aim : To study effect of temperature 40° c instead of 45° c and 30° c .

Observation :

At 40° c ,

Hydrogen PeroxidePH TDS
0.2 gm 1-21150
0.2 gm 1-2950
0.2 gm 1-2850
0.2 gm 1-2750
0.2 gm 1-2700

Conclusion :

No Significant change in extent of oxidation.

Date : 30/06/2022

Aim : To Quantify extent of oxidation un reacted acid gas Titrated agains NaOH .

Preparation:

  1. Take 200 ml Distilled water .
  2. Add 0.135 gm Formic Acid and 0.037 gm FeSO4 .
  3. cheking PH and TDS of solution.
  4. Titrate 20 ml solution against NaOH 0.01 M .
  5. Add Hydrogen Peroxide and checking PH and TDS .

Observation :

PH – 2.62 TDS – 381

At room temperature,

Titration against NaOH = 23.1 ml

Hydrogen peroxide PH TDS
0.2 gm 2.75295
0.2 gm 2.76283
0.2 gm 2.73271
0.2 gm 2.76247
0.2 gm 2.79244

Titration against NaOH= 8.3 ml

Conclusion :

60 % of acid is oxidised at mentioned for N= M reaction conditions i.e. Temperature , room temperature, Time 75 minutes.

Date : 1/07/2022

Aim : To study Oxalic Acid Oxidation under Fenton Conditions.

Preparation :

  1. Take 200 ml Distilled water.
  2. Add 0.180 gm Oxalic Acid and 0.037 gm FeSO4.
  3. Checking PH and TDS .
  4. Add Hydrogen Peroxide and checking PH and TDS .

Observation:

At room temperature,

Hydrogen Peroxide PH TDS
0.2 gm 1.941228
0.2 gm 1.961219
0.2 gm 1.951218
0.2 gm 1.96 1205
0.2 gm 1.97 1198
0.2 gm 1.981194
0.2 gm 1.971192
0.2 gm 1.971184
0.2 gm 1.971181
0.2 gm 1.971178

Conclusion :

No Oxidation evident from quantitative estimation of un reacted acid by titration.

Date : 02/07/2022

Aim : To verify results of Oxalic Acid Fenton Reaction.

Observation :

At room temperature ,

PH = 1.94 TDS = 1350

20 ml solution titrate against NaOH 0.01 M = 29.5 ml

Hydrogen Peroxide PH TDS
0.2 gm 1.911426
0.2 gm 1.901419
0.2 gm1.901414
0.2 gm 1.901412
0.2 gm 1.901402
0.2 gm1.901399
0.2 gm 1.901397
0.2 gm 1.901390
0.2 gm1.901385
0.2 gm 1.901382

20 ml titrate against NaOH = 29.6 ml

Conclusion:

No Oxidation evident from quantitative estimation of un reacted acid by titration.

Date : 02/07/2022

Aim : To oxidised Formic Acid at room temperature in 75 minutes using Hydrogen Peroxide.

Preaparation :

  1. Take 200 ml Distilled water.
  2. Add 0.135 gm Formic Acid , 0.180 gm Oxalic Acid and 0.037 gm FeSO4.
  3. cheking PH and TDS of solution.
  4. Titrate 20 ml solution against NaOH . Record results.
  5. Adding Hydrogen Peroxide and checking PH and TDS.
  6. Titrate 20 ml of Solution against NaOH record results .

Observation :

20 ml Titrate against NaOH = 50.7 ml

Hydrogen peroxide pH TDS
0.2 gm 1.90 1502
0.2 gm 1.881501
0.2 gm 1.861495
0.2 gm 1.871493
0.2 gm 1.871489

20 ml Titrate against NaOH = 55.3 ml

Conclusion :

No reaction evident may be due to presence of Oxalic Acid.

Date : 04/07/2022

Aim : Verification on results of oxidation of Formic Acid in presence of Oxalic Acid.

Observation:

20 ml Titrate against NaOH = 62.2 ml

Hydrogen Peroxide pHTDS
0.2 gm 1.921513
0.2 gm 1.921504
0.2 gm 1.911498
0.2 gm 1.911493
0.2 gm 1.911486
0.2 gm 1.911479
0.2 gm1.911473
0.2 gm 1.911470
0.2 gm 1.911564
0.2 gm 1.911460

titrate against NaOH = 62.2 ml

Conclusion :

No Oxidation evident from quantitative estimation of un reacted acid by titration.

Date : 05/07/2022

Aim : Oxidation of calcium formate under Fenton Condition .

Preparation:

  1. Take 200 ml Distilled water in beaker .
  2. Add 0.135 gm of Formic Acid and 0.074 gm of calcium Hydroxide.
  3. Add FeSO4 0.037 gm .
  4. Cheking PH and TDS.
  5. Add Hydrogen Peroxide in solution.
  6. Cheking PH and TDS.
Hydrogen peroxide pH TDS
0.2 gm 4.33460
0.2 gm 4.34461
0.2 gm 4.35462
0.2 gm 4.37463
0.2 gm 4.38464

Conclusion:

No conclusion could be Draw as TDS changes to small .

Date : 06/07/2022

Aim : Oxidation of calcium formate under Fenton Condition.

Observation :

20 ml Titrate against NaOH = 9.6 ml

Hydrogen Peroxide pH TDS
0.2 gm 4.06469
0.2 gm 4.07470
0.2 gm 4.07471
0.2 gm 4.08472
0.2 gm 4.09472

20 ml Titrate against NaOH = 7.6 ml

Conclusion :

Titration for quantitative of make is not helpful . Hence no conclusion could be derived.

Date : 06/07/2022

Aim : Oxidation of Formic Acid in presence of calcium oxalate .

Preparation:

  1. Take 200 ml Distilled water.
  2. Add 0.135 gm Formic Acid , 0.180 gm Oxalic Acid and 0.037 gm FeSO4.
  3. cheking PH and TDS of solution.
  4. Add 0.148 gm of calcium Hydroxide.
  5. Titrate 20 ml solution against NaOH . Record results.
  6. Adding Hydrogen Peroxide and checking PH and TDS.
  7. Titrate 20 ml of Solution against NaOH record results .

Observation:

At room temperature,

20 ml Titrate against NaOH = 15.1 ml

Hydrogen Peroxide pH TDS
0.2 gm 3.94505
0.2 gm 3.99502
0.2 gm 4.05498
0.2 gm 4.15494
0.2 gm 4.29482

20 ml Titrate against NaOH = 9.4 ml

Conclusion:

After Addition of equimolar quantity of a lime to oxalic acid . Fenton resulted in oxidation of Formic Acid. 40 % Formic Acid Oxidised compare to 60 % in absence of Oxalic Acid .

Date : 07/07/2022

Aim : To study effect of pH on Fenton Oxidation of Formic Acid.

Preparation:

  1. Take 200 ml Distilled water in a beaker .
  2. Add 0.135 gm of Formic Acid and 0.037 gm of FeSO4.
  3. checking PH and TDS of solution.
  4. Adjusting pH by adding HCL .
  5. Checking PH and TDS of solution.
  6. Titrate 20 ml against NaOH and record pH and TDS.
  7. Adding Hydrogen Peroxide in solution
  8. Checking PH and TDS of solution
  9. Titrate 20 ml solution against NaOH and record results.
Hydrogen Peroxide pH TDS
0.2 gm 1.902000
0.2 gm 1.891993
0.2 gm 1.861995
0.2 gm 1.881986
0.2 gm 1.921980

20 ml Titrate against NaOH before adding Hydrogen Peroxide = 51.9 ml

20 ml Titrate against NaOH after adding Hydrogen Peroxide = 50 ml

Conclusion:

If Solution is not ionised it can’t be Oxidised.

Date : 07/07/2022

Aim :

To study effect of pH on Fenton Oxidation of Formic Acid.

Preaparation :

  1. Take 200 ml Distilled water in a beaker .
  2. Add 0.135 gm of Formic Acid and 0.037 gm of FeSO4.
  3. checking PH and TDS of solution.
  4. Adjusting pH by adding Sulphuric acid .
  5. Checking PH and TDS of solution.
  6. Titrate 20 ml against NaOH and record pH and TDS.
  7. Adding Hydrogen Peroxide in solution
  8. Checking PH and TDS of solution
  9. Titrate 20 ml solution against NaOH and record results.

Observation :

20 ml Titrate against NaOH= 77.2 ml

Hydrogen Peroxide pH TDS
0.2 gm1.752000
0.2 gm 1.722000
0.2 gm 1.722000
0.2 gm 1.712000
0.2 gm 1.712000

20 ml Titrate against NaOH = 72.1 ml

Conclusion :

If Solution is not ionised it can’t be Oxidised.

08/07/2022

Aim : To find out oxalic and formic acid levels and pH at which oxalic acid neutrilized.

NFL Water 200 ml + 0.100 gm

lime pH TDS
100 mg 1.64 8400
100 mg 1.758250
100 mg 1.896650
100 mg 2.19 5400
100 mg 2.78 4450
100 mg 3.40 3850
100 mg 4.02 3800
100 mg 7.674000
100 mg 10.564350
100 mg 11.344700

Conclusion :

At pH 3-3.5 TDS starts increasing hence concluded that calcium formate is generate at pH 3.5

09/07/2022

Aim : To study oxidation of Formic Acid using Hydrogen Peroxide at pH 3-3.5

hydrogen Peroxide pH TDS
0.6 gm 3.334250
0.6 gm 3.334150
0.6 gm 3.334200
0.6 gm 3.334550
0.6 gm 3.334000

Conclusion:

At pH 3.5 , No oxidation of Formic Acid evident NaOH required for reaction remain practically same .

11/07/022

Aim : To study oxidation of Formic Acid using Hydrogen Peroxide .

1 ml Titrate against NaOH 0.01 M = 16.3 ml

Hydrogen PeroxidepH TDS
1.5243.127150
1.5243.106900
1.5243.066400
1.5243.016250
1.5242.936800

1 ml Titrate against NaOH 0.01 M = 18.4 ml

Conclusion :

No oxidation formic acid Acid evident NaOH required for reaction remain practically

CONCLUSION :

Oxidation of Formic Acid and formaldehyde before biological treatment was problematic due to

  1. Higher requirement of Hydrogen Peroxide.
  2. Oxidation of phenolic compounds.

Hence the Other option of treating formate typically calcium formate consumption was took on priority.

Aim : To Study TDS Conductivity change on oxalic acid and lime reaction .

Requirements : Oxalic Acid, pH TDS meter , Distilled water, lime .

Preparation :

  1. Take 200 ml Distilled water.
  2. Add 1 gm of Oxalic Acid and check pH and TDS .
  3. Add lime 100 mg and check pH and TDS
  4. Repeat this step till pH range 7 .
lime ( mg ) pH TDS
1001.707850
1001.716300
1001.855400
1002.024150
1002.243250
1002.321950
1002.711100
1009.43800

Conclusion :

With errors pH as well as Conductivity followed expected pattern. Lowest Conductivity was Observed above pH 7 .

Aim : To Study effect of calcium hydroxide reaction with formic acid .

Requirements : beaker , volumetric flask , spatula, Distilled water, formic acid, pH TDS meter.

Preparation:

  1. Take 200 ml Distilled water in a beaker .
  2. Add 1 gm Formic acid .
  3. Check pH and TDS of solution.
  4. Add lime and record pH and TDS of solution.

Observation:

lime ( in mg ) pH TDS
2003.251222
2003.602000
2004.454750
504.626050
505.007000
5010.735800

Conclusion:

Formic acid reacts with lime then calcium formate is form remain formic acid eeactwith agin hence pH decreases and increases .

Aim : To estimate amount of Oxalic Acid in oxalic acid formic acid mixture.

Requirements : beaker , volumetric flask , spatula, Distilled water, formic acid, pH TDS meter , oxalic acid.

Preparation :

  1. Take 200 ml Distilled water in beaker.
  2. Add 1 gm of Formic Acid and 1 gm of Oxalic Acid.
  3. Check pH and TDS of solution.
  4. Add lime and check pH and TDS of solution.

Observation:

Lime ( mg ) pHTDS
3001.739950
3002.275850
502.635500
202.765200
202.855750
202.935000
203.034800
203.164700
203.345400
503.585000
2004.165100

Conclusion :

Lowest Conductivity deep for the first time represents amount of Oxalic Acid in mixture.

COD of LQ 602 water = 193800

CONCLUSION:

RO Reject water has high TDS and We did analysis and possible treatment. Some gummy mass not calcium salt was isolated but could not be characterized. Treatment with oxalic acid has very limited success.

The method for determination of Oxalic Acid and formic acid on quantitative scale was developed by using pH and TDS meter . Dilution was an alternative approach but was not successful.

GC analysis of Formic Acid and total acidity by pH titration could not be an option.