1. Preparation of Chemical Compound in Laboratory Scale
SMK Negeri 13 Bandung

2. Objectives
After this session, the students are expected to be able to :
classify the apparatus of separation
Conduct the separation and isolation
Explain the steps of separation
arrange the planning of preparation of chemical compound according to the job sheet
- explain the objectives of every step
explain the function of reagents
conduct the test of physical and chemical properties of the chemical compound
- do the calculation in the determination of nickel
- arrange the report of the preparation of chemical compound

3. Separation Distillation - Simple distillation - Vacuum distillation
- Fractional distillation
- Steam distillation
Extraction
- Soxhlet
- separation funnel
Crystallization
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4. Simple distillation apparatus
1: Heat source 2: Still pot 3: Still head 4: Thermometer/Boiling
point temperature 5: Condenser 6: Cooling water in 7: Cooling water out 8: Distillate/receiving flask 9: Vacuum/gas inlet
10: Still receiver
11: Heat control
12: Stirrer speed control
13: Stirrer/heat plate
14: Heating (Oil/sand) bath
15: Stirrer bar/anti-bumping
granules
16: Cooling bath.
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5. Vacuum Distillation Apparatus
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6. Extraction Apparatus

7. Separation Funnel
Low density layer
High density layer
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8. Preparation of Cyclohexene
Weigh out 20 mL of cyclohexanol in to a round bottom flask of 200 mL
Add 2 mL of concentrated sulfuric acid and 2 or 3 boiling stones
Put a fractional colum and a reflux condenser on the top of the flask
Heat the flask in a heating mantle or oil bath. Set the temperature not more than 1300C in wise the distillation conduct at 950C

9. Procedure…..
Continue the distillation process until the residue produces white steam
Move the distillate in to a separation funnel and let the two layers separated
Remove the water layer
Wash the organic layer with 10 mL of water, then with 10 mL of 10% Na2CO3 and then with 10 mL of water

10. procedure
Pour the hydrocarbon layer through the top of the funnel in to a clean and dry Erlenmeyer flask
Add 3-4 gram of dry anhidrous CaCl2
shake for 2-3 minute. Let it for 15 minute with sporadic shaking
Pour the dried hydrocarbon in to a round flask of 50 mL and put some boiling stone

11. procedure Conduct the distillation at 80 – 900C
Collect the fractional part of C

12. Testing Reaction Prepare 3 test tube and fill each with
- 2 mL of % brom in CCl4
- 2 mL of 1% KMnO4
- 2 mL of concentrated H2SO4
Add to each test tube 1-2 drops of distillate
Watch the reaction and write

13. Physical Properties Test
Purpose
To identify the purity of product, it must be carried out the physical properties test and refer to handbook
Phase of matter
- Gas
- Liquid
- Solid

14. Physical Properties of Solid
Melting point
Crystal shape
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15. Physical Properties of Solid
Crystal Shape
NH4 Cl and NaCl

16. Melting Point Apparatus
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17. Melting Point Apparatus
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18. With your spatula, grind the sample into fine powder
Melting Point Determination
With your spatula, grind the sample into fine powder

19. Repeat this step, if necessary to obtain enough sample to see.
Poke the inverted capillary into the powder, trapping some sample in the open end.
Repeat this step, if necessary to obtain enough sample to see.

20. Pack the sample by bouncing it down your condenser several times.
. . .or you can hold the capillary with your thumb and forefinger, and RAP it sharply on the bench top; - but this could hurt!!

21. View the sample through the observation window and watch as it melts.
Insert the capillary into one of the 3 slots, and select a desired setting, -- say about 5.
View the sample through the observation window and watch as it melts.

22. It should melt something like THIS: only MUCH, MUCH SLOWER!!

23. Where it STARTS (when you see the first liquid run).
Record BOTH temperature readings (a melting point RANGE)
Where it STARTS (when you see the first liquid run).
Where it ENDS (when the last bit of solid becomes liquid).

24. Physical Properties of Liquid
Boiling Point
Freezing Point
Refractive index
Density

25. Refractometer /
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26. Densitometer
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27. Densitometer
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28. Picnometer Hole Cap Measuring flask http://2.bp.blogspot.com/
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29. Digital Handled Refractometer
Portable Refractometer
Digital Handled Refractometer
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30. Reading Refractometer
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31. Freezing Point Apparatus
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32. Freezing Point Apparatus
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33. Boiling Point Apparatus
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34. Apparatus for Physical Properties Determination
Density
- Picnometer
- Areometer
Boiling Point
- Distillation Apparatus
- Siwoloboff Apparatus
- BP meter
Melting Point
- Melting Block
- Thiele Apparatus

35. Apparatus for Physical Properties Determination
Refractive Index
- Refractometer
Freezing Point
- FP meter