First-Degree Reaction — the Transform of Sucros. Content Purposes and Demands Purposes and Demands...

35
First-Degree Reactio n—the Transform of S ucros

Transcript of First-Degree Reaction — the Transform of Sucros. Content Purposes and Demands Purposes and Demands...

Page 1: First-Degree Reaction — the Transform of Sucros. Content Purposes and Demands Purposes and Demands Principle Apparatus and Reagent Apparatus and Reagent.

First-Degree Reaction—the Transform of Sucros

Page 2: First-Degree Reaction — the Transform of Sucros. Content Purposes and Demands Purposes and Demands Principle Apparatus and Reagent Apparatus and Reagent.

Content

Purposes and Demands Principle Apparatus and Reagent Procedure Data Records and Processing Questions Attentions

Page 3: First-Degree Reaction — the Transform of Sucros. Content Purposes and Demands Purposes and Demands Principle Apparatus and Reagent Apparatus and Reagent.

Purposes and Demands

Measure the reaction rate constant and half-life of the transformation of sucrose.

Master the method of polarimetry to determine optical activity.

Page 4: First-Degree Reaction — the Transform of Sucros. Content Purposes and Demands Purposes and Demands Principle Apparatus and Reagent Apparatus and Reagent.

Principle

A reaction in which rate would increase in proportion to the concentration of reactant is defined to be the first-degree reaction. With the catalysis of H+ ion, the equation of transformation of sucrose is:

Page 5: First-Degree Reaction — the Transform of Sucros. Content Purposes and Demands Purposes and Demands Principle Apparatus and Reagent Apparatus and Reagent.
Page 6: First-Degree Reaction — the Transform of Sucros. Content Purposes and Demands Purposes and Demands Principle Apparatus and Reagent Apparatus and Reagent.

As the sucrose solution is very dilute, we can consider the concentration of water is invariable and rate is only due to the concentration (Cs) of sucrose. So this reaction is considered to be a first-degree reaction.

Page 7: First-Degree Reaction — the Transform of Sucros. Content Purposes and Demands Purposes and Demands Principle Apparatus and Reagent Apparatus and Reagent.

It can be expressed as the following formula:

(A)

V: reaction rate T: reaction time K: reaction constant C: concentration of sucrose (Time=t)

实验原理

Page 8: First-Degree Reaction — the Transform of Sucros. Content Purposes and Demands Purposes and Demands Principle Apparatus and Reagent Apparatus and Reagent.

The integral of formula A ln(C0/C)=-kt+B ( B )

The half-life of the reaction:

( C )

实验原理

Page 9: First-Degree Reaction — the Transform of Sucros. Content Purposes and Demands Purposes and Demands Principle Apparatus and Reagent Apparatus and Reagent.

optical activity

t=0 C0 0 0 α0 ( positive )

t C C0 - C C0 - C αt

t∞ 0 C0 C ( negative )

+66.6º +52.5º -91.9º

direction dextrogyrous dextrogyrous levorotatory

实验原理

Page 10: First-Degree Reaction — the Transform of Sucros. Content Purposes and Demands Purposes and Demands Principle Apparatus and Reagent Apparatus and Reagent.

Given by α = KBCB (D)

α : optical activity KB : proportion constant

CB : concentration of substance B

Page 11: First-Degree Reaction — the Transform of Sucros. Content Purposes and Demands Purposes and Demands Principle Apparatus and Reagent Apparatus and Reagent.

α0 = KS C0 (D1)

αt = KS C + (KD + KF )(C0 –C) (D2)

α∞ = (KD + KF )C0 (D3)

We can obtain

Page 12: First-Degree Reaction — the Transform of Sucros. Content Purposes and Demands Purposes and Demands Principle Apparatus and Reagent Apparatus and Reagent.

实验原理

Combining Eqs. (D1), (D2) and (D3), we obtain Eqs.(E1)and .(E2):

C0=(α0–α∞){KS–(KD +KF )}–1 ( E1 )

C=(αt–α∞) {KS–(KD +KF )}–1 ( E2 )

Page 13: First-Degree Reaction — the Transform of Sucros. Content Purposes and Demands Purposes and Demands Principle Apparatus and Reagent Apparatus and Reagent.

实验原理

Adding Eq. (E2) to Eq.(B),we obtain another equation: :

Where αt stands for optical activity of an ongoing

reaction,α∞ stands for optical activity when reaction

terminates, K stands for reaction rate constant, T stands for time when reaction is ongoing and B is a constant.

Page 14: First-Degree Reaction — the Transform of Sucros. Content Purposes and Demands Purposes and Demands Principle Apparatus and Reagent Apparatus and Reagent.

实验原理

Draw a beeline of

against time, from which we can figure out the constant K that is negative to the slope.

Page 15: First-Degree Reaction — the Transform of Sucros. Content Purposes and Demands Purposes and Demands Principle Apparatus and Reagent Apparatus and Reagent.

Apparatus and Reagent

Polarimeter 1Super thermostatic trough 1Stopwatch 1Volumetric flask (50ml) 2Pipette (25ml) 1Spheric aspirator 1Y-pipe 1Washing bottle (250ml) 1Conical flask 2Sucrose (analytical pure) HCl solution ( c=2.0mol·dm-3 )

Page 16: First-Degree Reaction — the Transform of Sucros. Content Purposes and Demands Purposes and Demands Principle Apparatus and Reagent Apparatus and Reagent.

Procedure

1.Adjust temperature of the thermostatic bath at 30℃±0.1℃.

Page 17: First-Degree Reaction — the Transform of Sucros. Content Purposes and Demands Purposes and Demands Principle Apparatus and Reagent Apparatus and Reagent.

2. Preparation and thermostatic process Dissolve 10g of sucrose and make up the soluti

on in 50ml of volumetric flask. Shaking up, Pipette 25ml solution into a conical flask.

Page 18: First-Degree Reaction — the Transform of Sucros. Content Purposes and Demands Purposes and Demands Principle Apparatus and Reagent Apparatus and Reagent.

Pipette 25ml of HCl solution into another conical flask then take them into thermostatic trough.

Page 19: First-Degree Reaction — the Transform of Sucros. Content Purposes and Demands Purposes and Demands Principle Apparatus and Reagent Apparatus and Reagent.

3. Regulate the zero point 1) Electrify the polarimetry. After 2-3, regulate the focus to make the trisection visual field clear   

or

实验步骤

Page 20: First-Degree Reaction — the Transform of Sucros. Content Purposes and Demands Purposes and Demands Principle Apparatus and Reagent Apparatus and Reagent.

2) Filled the optical pile full of distilled water and set it into the polarimeter. Rotate the microscopy, when trisection visual field disappears, mark down the angle that is just the zero point.

Page 21: First-Degree Reaction — the Transform of Sucros. Content Purposes and Demands Purposes and Demands Principle Apparatus and Reagent Apparatus and Reagent.

Repeat this procedure three times. Subsequently, calculate the average value, then pour out water and get ready for next operation.

Page 22: First-Degree Reaction — the Transform of Sucros. Content Purposes and Demands Purposes and Demands Principle Apparatus and Reagent Apparatus and Reagent.

4. Determine optical activity of sucrose in transfer process.

1) Determination ofαt

After solution being kept temperature constant for 10min, add HCl solution into sucrose, meanwhile record the time with a stopwatch.

Page 23: First-Degree Reaction — the Transform of Sucros. Content Purposes and Demands Purposes and Demands Principle Apparatus and Reagent Apparatus and Reagent.

Wash the optical pile with mixture for 2-3 times, fill it with mixture, without any air bladder and leak, then put it into polarimeter again.

Page 24: First-Degree Reaction — the Transform of Sucros. Content Purposes and Demands Purposes and Demands Principle Apparatus and Reagent Apparatus and Reagent.

Rotate the microscopy, mark down the angle(Xt) as soon as trisection visual field disappear. In the first hour, take an angle per 5min, then per 10min after one hour until a negative value appears.

Page 25: First-Degree Reaction — the Transform of Sucros. Content Purposes and Demands Purposes and Demands Principle Apparatus and Reagent Apparatus and Reagent.

2) Determination ofα∞

Heat the mixture remained in a water bath at 50-60℃. After half an hour, cooled it till room temperature. Then take it into thermostatic trough staying for 10 min. Repeat the complete procedure and determine X∞.

Page 26: First-Degree Reaction — the Transform of Sucros. Content Purposes and Demands Purposes and Demands Principle Apparatus and Reagent Apparatus and Reagent.

Data Records and Processing

Room temperature: Concentration of sucrose solutionConcentration of HCl solution:Xt: X∞:αt = Xt - X0 α∞ = X∞ - X0

Page 27: First-Degree Reaction — the Transform of Sucros. Content Purposes and Demands Purposes and Demands Principle Apparatus and Reagent Apparatus and Reagent.

t/min 5 10 15 20 25 30 35 40 45

Xt/℃                  αt /(°)                  

(αt-α∞)/(°)                  ln{(αt-α∞)/(°)}                  

t/min                  Xt/℃                  αt/(°)                  

(αt-α∞)/(°)                  ln{(αt-α∞)/(°)}                  

Page 28: First-Degree Reaction — the Transform of Sucros. Content Purposes and Demands Purposes and Demands Principle Apparatus and Reagent Apparatus and Reagent.

实验数据记录和处理

Draw a graph of against time. Take two points A and B on the beeline to calculate the slope by the formula as following:

Half-life :

Page 29: First-Degree Reaction — the Transform of Sucros. Content Purposes and Demands Purposes and Demands Principle Apparatus and Reagent Apparatus and Reagent.

Questions

Why sucrose should be confected freshly at the time you start the experiment?

Page 30: First-Degree Reaction — the Transform of Sucros. Content Purposes and Demands Purposes and Demands Principle Apparatus and Reagent Apparatus and Reagent.

Attentions

1. Optical pipe must be filled full of liquid without any air bladder.

2. Rotate the cover moderately. If it is too tight, the knob will be damaged, and the glass patch pressed may produce the fault optical activity.

Page 31: First-Degree Reaction — the Transform of Sucros. Content Purposes and Demands Purposes and Demands Principle Apparatus and Reagent Apparatus and Reagent.

3. For the mixture is rather acid and corrosive, the apparatus must be washed cleanly and wiped dry after the expriment is finished.

Page 32: First-Degree Reaction — the Transform of Sucros. Content Purposes and Demands Purposes and Demands Principle Apparatus and Reagent Apparatus and Reagent.

Outline for using the polarimeter

1. Switch on the electrical source(220V) and turn on the Na-light. As the lamp-house is stable, regulate focus of the ocular until trisection visual field is clear, just like the following pictures.

or

Page 33: First-Degree Reaction — the Transform of Sucros. Content Purposes and Demands Purposes and Demands Principle Apparatus and Reagent Apparatus and Reagent.

2. Regulate the zero point. Fill the optical pipe full of distilled water. When rotate the microscopy, mark down the point on which trisection visual field disappears.

Page 34: First-Degree Reaction — the Transform of Sucros. Content Purposes and Demands Purposes and Demands Principle Apparatus and Reagent Apparatus and Reagent.

Reading on the dial after “0”.

6

0

A

0

X0 =+ 1.6° 、

B 20

0X0 =﹣ 2.8°

(177.2°﹣180°)

Page 35: First-Degree Reaction — the Transform of Sucros. Content Purposes and Demands Purposes and Demands Principle Apparatus and Reagent Apparatus and Reagent.

3. Repeat the same procedure and determine the optical activity of sample.

Finally, the apparatus should be cleaned and put away trimly.