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LIMIT TEST FOR SULPHATES

 

LIMIT TEST FOR SULPHATES

 

 

AIM: To perform limit test for sulphates in the given sample.

 

APPARATUS REQIURED: Nessler’s cylinder, beaker, pipette, measuring cylinder, glass rods.

 

 

CHEMICALS REQUIRED: BaCl2 solution, BaSO4 reagent, dil. HCl, standard solution of potassium sulphate, distilled water, test sample,

PRINCIPLE: This test is designed for the control of sulphate impurity in inorganic substances. It depends upon the precipitation of the sulphate with barium chloride in the presence of HCl and traces of barium sulphate. The turbidity obtained is compared with standard solution, which contains the known amount of sulphate ions under the same experimental conditions.

SO42- + BaCl2 --------       Dil.HCl-------BaSO₄    +  2Cl^-

PROCEDURE:

 

Preparation of BaSO4 reagent: This reagent must be freely prepared by mixing 10 ml of 25 % solution of BaCl2 and 15 ml of ethanolic sulphate standard solution, which contains 0.10891% K2SO4 in 3% ethanol. K2SO4 has been added to increase the sensitivity of the test. Very small amount of barium sulphate present in the reagent acts as seeding agent for precipitation of barium sulphate. Alcohol helps in preventing super saturation of barium sulphate.

Preparation of test solution:   Dissolve a specified quantity of substance in water or prepare solution as directed by I.P and transfer to Nessler’s cylinder. To this add 2 ml of dilute HCl and make the volume to 45 ml with water. And add 5 ml of BaSO4 reagent. Stir and keep it aside for 5 min.

Preparation of standard solution: Take 1ml of 0.1089% w/v of K2SO4 in Nessler’s cylinder and add 2 ml of HCl and transfer to Nessler’s cylinder and make the volume to 45 ml with H2O. To this add 5 ml of BaSO4 reagent. Stir and keep aside for 5 min. Finally compare the turbidity of two solutions.

SUMMARY:

 

STANDARD SOLUTION	Observation	Inference
Take 1ml of 0.1089 % w/v solution of potassium sulphate in Nessler’s cylinder + 2ml of dilute hydrochloric acid + Dilute to 45 ml in Nessler’s cylinder + 5ml of barium sulphate reagent. Keep aside for 5 min.	The opalescence produced in sample solution is greater than / less than that of standard solution.	The sample passes/ doesn’t pass the limit test for sulphates.
TEST SOLUTION   Take specific weight(1gm) of sample + Add 2ml of dilute hydrochloric acid +Dilute to 45 ml in Nessler’s cylinder + 5ml of barium sulphate reagent. Keep aside for 5 min.

 

 

 

The opalescence produced in the test solution is compared with that produced in standard solution.

 

 

OBSERVATION:

 

 

REPORT: The given sample                  the limit test for sulphates.

 

VIVA QUESTIONS:

 

1.      Write the principle involved in limit test for sulphates.

2.      What forms precipitate in limit test for sulphates?

3.      How barium sulphate reagent is prepared?

4.      The standard solution is prepared with                .

5.      What is the importance of dilute hydrochloric acid in limit test for sulphates?

6.      What is seeding agent?

7.      What is the importance of ethanol in limit test for sulphates?

8.      Write reaction involved in limit test for sulphate.

LIMIT TEST FOR CHLORIDES

 

LIMIT TEST FOR CHLORIDES

 

 

AIM: To perform the limit test for chlorides in the given sample. APPARATUS REQUIRED: Nessler’s cylinders, glass rod, beaker and pipette.

CHEMICALS REQUIRED: Standard Sodium Chloride solution, dilute Nitric acid, 0.1 M Silver natrate solution and Hydrochloric acid.

PRINCIPLE: This test is designed for the control of chloride impurity in inorganic substances. It depends upon the precipitation of chlorides upon reaction with silver nitrate in the presence of nitric acid. The extent of precipitation depends upon the amount of silver chloride formed i.e. on the amount of chloride ions present in the substance. The opalescence produced was compared with a reference standard opalescence having a known amount of chloride impurity.

Cl^- + AgNO3                                  AgCl + NO3-

 

PROCEDURE:

 

em thoroughly a

Take two Nessler’s Cylinders, wash th                                              Dil. HNO3nd then label as STANDARD and TEST

 

Preparation of Standard chloride solution: Accurately weigh 0.05845g of NaCl and dissolve in 100 ml of distilled water. (0.05845% w/v of NaCl).

Preparation of standard Solution:

 

Take 1 mL of NaCl solution and transfer into Nessler’s cylinder and add 10 ml dilute Nitric Acid and make up the volume up to 50 mL with distilled water then add 1 mL of silver nitrate solution. Stir well with a glass rod and keep it aside for 5 min.

 

 

Preparation of Test Solution:

 

Weigh a specified quantity of test sample and transfer into Nessler’s cylinder and add 10 ml dilute Nitric Acid and make up the volume up to 50 mL with distilled water then add 1 mL of silver nitrate solution. Stir well with a glass rod and keep it aside for 5 min.

SUMMARY:

 

STANDARD SOLUTION	Observation	Inference
In a Nessler’s cylinder Chloride std. solution (25ppm Cl) 10ml taken. Add 5ml water + 10 ml of dil.HNO3.
Dilute to 50 ml in Nessler’s cylinder + 1 ml of 0.1 M AgNO3 solution.
Stir & allow to stand for 5 min.   Observe the opalescence	The                opalescence produced in sample solution is greater than / less than that of standard solution.	The sample passes/ doesn’t pass the limit test for chlorides.
TEST SOLUTION
Specified substance (1gm) + 10 ml of water + 10 ml of dil.HNO3.
Dilute to 50 ml in Nessler’s cylinder + 1 ml of 0.1 M AgNO3 solution.
Stir & allow to stand for 5 min.
Observe the opalescence

 

The opalescence produced in the test solution is compared with that produced in standard solution.

 

 

OBSERVATION:

 

 

 

REPORT: The sample_              limit test for chlorides.

Dostarlimab Drug

  Dostarlimab, The Drug That 'Cured' Cancer During Trials.

 

As many as 18 rectal cancer patients were given the Dostarlimab drug in prescribed dosages every three weeks for six months.

 A study has found that a drug named Dostarlimab has helped treat rectal cancer. This has been described as a "first time in history"kind of result in cancer treatment with the disease simply vanishing in patients after the experimental treatment.

Here are 10 things to know about Dostarlimab, the drug that cured cancer during trial:

1. The clinical trial comprised a group of 18 patients. All of them were battling rectal cancer at the Memorial Sloan Kettering Cancer Center in Manhattan, US.

2. In all patients, rectal cancer was locally advanced. This means the tumours had spread within the rectum and in some cases, to the lymph nodes, but not to other organs.

3. The drug named Dostarlimab was administered to the patients for a period of six months. The medicine was given in prescribed dosages every three weeks for the said period.

4. At the end of the trial, cancer was checked for and remained undetected through physical exam, endoscopy, positron emission tomography or PET scans or MRI scans. 

5. According to New York Times, the medicine costs nearly $11,000 or ₹ 8.55 lakh per dose.

6. Dostarlimab works by "unmasking" cancer cells, which in turn helps the immune system identify and destroy them.

7. The rectal cancer study was inspired by a clinical trial conducted by Dr. Luis A. Diaz Jr. of Memorial Sloan Kettering Cancer Center led in 2017.

8. The patients involved in the clinical trial had undergone previous treatments to manage their cancer, including chemotherapy, radiation, and invasive surgery. Post the trial, they were able to be taken off painful chemotherapy and radiation sessions.

9. Patients showed a complete absence of significant post-treatment complications as well as any signs of recurrence of cancer in the patients until 25 months from the end of the trial.

10.The study was sponsored by the drug company GlaxoSmithKline.

SYNTHESIZE BENZYL ALCOHOL FROM BENZALDEHYDE

TO SYNTHESIZE BENZYL ALCOHOL FROM BENZALDEHYDE

Reference: Vogel's textbook of practical organic chemistry revised by B.  S.  Furniss, a.  J  Hannaford, P.  W.  G.  Smith, A.  R.  Tatchell, Fifth Edition, ELES, 1989, page no - 1029.

 Requirements:

Apparatus - Beaker, Conical Flask, Round Bottom Flask, Water Bath Vessel, Reagent Bottle, Separatory Funnel, Funnel, Measuring Cylinder.  Pipette, Condenser, Stirrer, Spatula, Etc. 

 Chemical: - Potassium Hydroxide, Ice, Benzaldehyde, Ether, Sodium Metabisulphite, Sodium Carbonate, Anhydrous Magnesium Sulphate. 

Instrument - Rotary Evaporator, Hot Air Oven, Vacuum pump.  Melting Point Apparatus. 

Principle: Refer experiment for synthesis of benzoic acid from benzamide’-

Figure 07  A typical assembly for purification of liquids by simple distillation at atmospheric pressure

Procedure:

       I.            Dissolve 29 g of potassium hydroxide in 27 ml of water in a beaker or conical flask, and cool the solution to about 20C in ice water.  Pour this solution in 250ml reagent bottle and add 32g (30 ml, 0. 3 mol) of pure benzaldehyde.  (ork bottle and shake it vigorously until it has been converted into thick emulsion and allow the bottle to stand overnight.

    II.            Add just sufficient water (about 105 ml) to dissolve the potassium benzoate which but comed poar this mixture into a separatory funnel, rinse reagent bottle with about 30 ml of ether and add this ether to the solution in the funnel.

 III.            Shake the solution in order to thoroughly extract the benzyl alcohol with the ether, separate the lower aqueous solution and carry out further extractions each with about 25 ml of ether.

 IV.            Combine the ether extract and distil the ether from a water bath (rotary evaporator) until the volume is about 25 ml.

    V.            Cool and shake the ether solution twice with 5ml portions of saturated sodium metabisulphite solution in order to remove any benzaldehyde which may be present. 

 VI.            Separate the ethereal solution wash it with 10ml of 10% sodium carbonate solution to ensure complete removal of bisulphite, then with 10ml of water and dry with anhydrous magnesium sulphate or anhydrous sodium carbonate.

VII.            Remove the ether on a water bath and distil the residual liquid from an air bath.  Replace the water condenser by and air condenser or empty the water completely from the condenser jacket.

VIII.             Collect the benzyl alcobol at 204-207 C. Pure compound boils at 205.5 C. The yield is 13g (86.5%).

  Reagent Preparation:

Sodium carbonate solution (10% w / v) - Dissolve 10g of sodium carbonate in sufficient water to produce 100 ml

Result:-                    

Synthesize Bezoic Acid from Benzaldehyde.

Experimant No 06 :-  To Synthesize Bezoic Acid from Benzaldehyde.

Reference: Vogel's Textbook of practical organic chemistry revised by B.  S.  Furniss, a.  J  Hannaford.  P.  W.  G.  Smith, A.  R.  Tatchell.  Fifth Edition.  ELBS.  1989.  page no - 1029. 

Requirements:

Apparatus - Beaker, Conical Flask, Water Bath Vessel, Reagent Bottle, Separatory Funnel, Funnel.  Measuring Cvlinder.  Pipette, Stirrer, Spatula, Etc

Chemicals - Potassium Hydroxide, Ice, Benzaldehyde, Ether, Sodium Metabisulphite, Sodium Carbonate, Hydrochloric Acid.  Instrument - Hot Air Oven.  Vacuum Pump, Melting Point Apparatus. 

Principle: maticaldehydes do not contain alpha hydrogen atomseg.  Formaldehyde and bonatachar under the influence of strong aqueous or al ammeous or alcoholic alkali undergoes simultaneous oxidation and on yielding the alcohol and corresponding carboxylate salt.

                                                                           

This dismutation or disproportionation reaction is known as the Cannizzaro reaction.  The mechanism of the reaction involves the production of the anion (1) which may transfer a hydride ion to a carbonyl carbon atom in another aldehyde molecule.  The reaction is completed by a proton transfer toyield the carboxylate anion and the alcohol.

The reaction is illustrated here by the conversion of benzaldehyde into benzoic acid and benzyl alcohol. 

Reaction:-

Procedure:

I.                   Dissolve 29 g of potassium hydroxide in 27 ml of water in a beaker or conical flask, and cool the solution to about 20C in ice water.  Pour this solution in 250ml reagent bottle and add 32g (30 ml, 0. 3 mol) of pure benzaldehyde.  Cork bottle and shake it vigorously until it has been converted into thickemulsion and allow the bottle to stand overnight.

II.                 Add just sufficient water (about 105 ml) to dissolve the potassium benzoate which formed.  Pour this mixture into a separatory funnel, rinse reagent bottle with about 30 ml of ether and add this ether to the solution in the funnel. 

III.             Shake the solution in order to thoroughly extract the benzyl alcohol with the ether, separate the lower aqueous solution and carry out further extractions each with about 25 ml of ether.  Save the aqueous solution.

IV.              Add this aqueous solution into a mixture of 80 ml of concentrated hydrochloric acid and 80 ml of water and about 100 g of crushed ice. 

V.                Filter the precipitated benzoic acid at the pump, wash it with little cold water, drain and recrystallize from boiling water.

VI.              The yield of benzoic acid (colorless crystal), m.  p 121 ° C, is 13.  5 g (79%)

Result:-