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Method 1:

1. Add 9.5 mL of Methanol to each flask

2. Now add the following amounts of toluene (Concentration 1000mg L-1) to each flask

  • Flask 1 - 100µL (Toluene)
  • Flask 2 - 80µL (Toluene)
  • Flask 3 - 60µL (Toluene)
  • Flask 4 - 40µL (Toluene)
  • Flask 5 - 20µL (Toluene)

3. Make each flask up to the mark (10mL) with methanol

4. Put stoppers into the necks of the flasks and mix by inverting them 6 times

5. Inject 1µL of solution into the chromatograph and record the peak area

6. Repeat this process for all 5 flasks and record the results accordingly

7. Now run the unknown sample through the chromatograph once.

Results for method 1

Flask No.

Volume of Toluene added / mL

Peak Area of Toluene

Toluene Concentration mg L-1

1

100

59.6229

10

2

80

53.9481

8

3

60

44.7381

6

4

40

26.5328

4

5

20

12.7134

2

Unknown

 

32.5719

4.8553

 Method 2 - Using internal standard (Ethylbenzene)

1. Add 100µL Ethyl benzene (Concentration 1000mg L-1) to each flask & mix thoroughly

2. Run each solution through the chromatograph as (Method 1 Step 5) & record the results.

3. Now add 100µL ethyl benzene to the unknown, mix, inject and record the result.

4. Choose anyone of the standards & inject it a further 4 times & record the results

Results for method 2 (Steps 1 to 3)

Flask No.

Area of Toluene

Area of Ethylbenzene

Area of Toluene

Area of Ethylbenzene

1

65.6147

45.3774

1.4460

2

53.7759

71.4809

0.7523

3

38.3167

72.7725

0.5265

4

27.0729

75.4286

0.3589

5

12.5096

52.0932

0.2401

Unknown

34.1252

36.0508

0.9466

Results for method 2 (Step4 the repeated sample)

Sample (A, B or C)

Retention Time / min

Peak Area

 

1

3.000

68.6642

2

2.992

45.6637

3

2.992

45.6637

4

3.000

75.1459

5

3.092

41.9748

Mean value

 

55.4225

Questions to be answered

1. Using Excel, construct a calibration graph of concentration vsarea ratio for your results from Method 2, print it off and calculate the concentration in mg L-1 of toluene in the unknown sample.

2. Using both the Toluene concentrations for the unknown sample. Calculate the Average concentration of Toluene using the table below

 

Toluene Concentration

mg L-1

Method 1

4.8553

Method 2

 

Average concentration

 

 

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