Untangling complex syste.., p.47

Untangling Complex Systems, page 47

 

Untangling Complex Systems
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  FIGURE 8.16 Possible steady-state solutions for small (a), medium (b), and large (c) value of k .0

  228

  Untangling Complex Systems

  the formula of maximum a priori absolute error (knowing that the KBrO molecular weight

  3

  is MW = (167.01 ± 0.01) g/mol):

  ∆

  1

  [

  m

  m

  KBrO ]

  m

  ( MW )

  3

  =

  ∆

  ∆

  + −

  ∆ V

  0

  2

  2

  ( MW )( V )

  + − ( V)( MW)

  ( MW )( V )

  6

  = 6×10− + 2.1 10 5

  −

  2.63 10 4

  −

  .

  2 9 10 4

  ×

  +

  ×

  =

  × − mol/L

  The largest contribution to the total uncertainty on KBrO

  

  3 

   comes from

  0

  the determination of the volume. Finally, the value of the concentration is

  KBrO

  

  3 

   = (0.3503 ± 0.0003) mol/L. Similarly, we can estimate the uncertainties in the

  0

  concentration of the other stock solutions. After preparing the stock solutions, we mix spe-

  cific amounts of them to start the BZ reaction. In the first run of the experiment, the initial

  concentration of KBrO is:

  3

  [KBrO ]3 V ( .

  M)( mL)

  [KBrO

  0 1

  0 3503

  2

  ]3 =

  =

  0.08544 mol/L

  1

  Vfin

  (8 2. mL)

  =

  where:

  V

  stock solution that is taken and mixed with the other

  1 is the volume of the KBrO3

  reagents,

  V is the total volume of the reaction mixture.

  fin

  The uncertainty in KBrO

  

  3 

   is again estimated by the formula of maximum a priori abso-

  1

  lute error:

  V

  KBrO

  

  3 

  KBrO  V

  ∆ KBrO

  1

  0

  

  3

  

  

  

  V + −

  0 1 ∆

  3 

  ∆ KBrO

   =

  

  3 

  ∆

  V

  1

   +

  0

  1

  V

  2

  fin

  fin

  Vfin

  Vfin

  .

  −

  .

  (0 3503)(2)

  5

  0 3503

  =

  mol 

  7 3

  . 2 ×10 +

  0.016 + −

  0 070

  .

  =

  

  0 0015

  .

  2

  8.2

  (

  

  

  8.2)

   L 

  Therefore, the concentrations of KBrO in the three runs of the reaction are:

  3

  [KBrO ] ( .

  .

  )

  3

  = 0 0854 ± 0 0015 mol/L

  1

  [KBrO ] (0 064

  .

  0.

  )

  3

  =

  ± 001 mol/L

  2

  [KBrO ] ( .

  .

  )

  3

  = 0 0427 ± 0 0007 mol/L

  3

  Then, we calculate the logarithm of this quantities. The uncertainty in log KBrO

  

  3 

   is

  i

  determined by the maximum a priori absolute error’s formula:

  log e

  ∆(logKBrO

  10

  

  i ) =

  3 

  ∆ KBrO

  

  

  KBrO

  

  3 

  

  i

  3 

   i

  Figure 8.17 reports some spectra of the BZ reaction recorded in the absence (a) and the pres-

  ence (b) of the indicator ferroin. In (a), it is evident that the solution is uncolored when the

  chemical system is in its reduced state (i.e., when Ce+3 is the dominant form of the cerium

  ions), and it becomes slightly yellow when Ce+4 becomes the dominant form. In the presence

  of the redox indicator (see plot b), the solution is red when the coordination compound is in its

  reduced state (with iron in the Fe+2 state) because it absorbs all the visible wavelengths except

  those of the red region. When the solution is in its oxidized state, the complex ferriin (having

  the iron ion in its Fe+3 state) absorbs all the visible wavelengths except those of the blue region.

  The Emergence of Temporal Order in a Chemical Laboratory

  229

  1

  Ce+4

  A

  Ce+3

  0

  300

  400

  500

  600

  700

  800

  (a)

  λ (nm)

  2

  Fe+2

  A 1

  Fe+3

  0

  300

  400

  500

  600

  700

  800

  (b)

  λ (nm)

  FIGURE 8.17 Spectral evolution of the BZ reaction with the cerium ions as catalysts and in the absence

  (a) and the presence (b) of ferroin as the redox indicator.

  The profiles of the absorbance at 511 nm as a function of the time are plotted in

  Figure 8.18 for the three different concentrations of KBrO , labeled as 1 (in a), 2 (in b), and

  3

  3 (in c), respectively.

  The traces have been recorded for at least 30 minutes. From the kinetics, we determine

  the periods of the oscillations. Then, we calculate the log T. We will have as many log T

  as are the oscillations in each run. The best estimate will be the average, and its uncer-

  tainty will be the standard deviation of the mean. Finally, we plot log( T ) ∆

  ( )

  i ±

  log Ti versus

  log([KBrO ) ∆

  (

  ) and we determine the exponent n by fitting the data with

  3 ] i ±

  log [KBrO3] i ,

  the least-squares method, as shown in Figure 8.19.

  It results that log( T ) =cost + n log([KBrO

  (

  )

  3]) = (0.32 ± .

  0 05)+(− .

  1 61± 0.04)log [KBrO3]

  with a correlation coefficient r = 0 99972

  .

  . The lower the [KBrO ], the longer the period.

  3

  The exponent is roughly –(3/2). This result is consistent with a mechanism in which bro-

  mate plays a role in the rate-limiting steps.

  8.3. During the progress of the BZ reaction, changes in the concentrations of protons, bro-

  mate, malonic acid, and hypobromous acid are small because the amount of catalyst

  used is almost two orders of magnitude smaller. Therefore, assuming that [H+], [BrO−3],

  [CH

  and [HBrO] remain unchanged during the reaction, it is possible to write

  2 (COOH)2 ],

  the following system of three nonlinear differential equations:

  d  X

    = k [ H+ 2]  A Y k

  2

  2

  H+ X Y

  k 3 H+

  1

  A Z

  2 k 4 X

  dt

      − 

     +     −  

  d  Y

    = −

  +

  k

  2

  1[ H ] 

   A  Y  − k  +

  2  H   X   Y

  fk 5 O Z

  dt

    +

     

  d  Z

    = k 

  3 H +

  A Z

  k 5 O Z

  dt

  

     −   

  230

  Untangling Complex Systems

  1.5

  A

  600

  900

  1200

  1500

  1800

  (a)

  t (s)

  1.5

  A

  600

  900

  1200

  1500

  1800

  (b)

  t (s)

  1.5

  A

  600

  900

  1200

  1500

  1800

  (c)

  t (s)

  FIGURE 8.18 Trends of A recorded at 511 nm for the three distinct concentrations of KBrO : (1) 0.0854 M

  3

  in a; (2) 0.064 M in b; (3) 0.0427 M in c.

  2.6

  2.5

  2.4

  T) 2.3

  log( 2.2

  2.1

  2.0

  –1.40 –1.35 –1.30 –1.25 –1.20 –1.15 –1.10 –1.05

  log ([KBrO3])

  FIGURE 8.19 Linearization of the relation between log( T ) and log([KBrO )

  3 ] .

  The function file to integrate the system of differential equations in MATLAB should look

  like this:

  function dy = Oregonator(t, y)

  dy = zeros(3,1);

  options=odeset(‘RelTol’,10^-6,’AbsTol’,10^-10);

  k1 = 1.28;

  k2 = 800000;

  k3 = 8;

  The Emergence of Temporal Order in a Chemical Laboratory

  231

  k4 = 2000;

  k5 = 1;

  A = 0.12;

  O = 0.1;

  f = 0.6;

  dy(1)=k1*A*y(2)-k2*y(1)*y(2)+k3*A*y(1)-2*k4*y(1)*y(1);

  dy(2)=-k1*A*y(2)-k2*y(1)*y(2)+f*k5*O*y(3);

  dy(3)=k3*A*y(1)-k5*O*y(3);

  where

  k 1 is k

  + 2

  +

  +

  1[ H ] , k 2 is k 2[ H ], k 3 is k 3[ H ], y(1) is X, y(2) is Y, y(3) is Z. The script file should look like the following:

  [ ] =

  (‘

  , [0 1200], [0.0001 0.0001 0.002])

  t, y

  ode15s Oregonator’

  wherein [0 1200] is the time window, whereas [0.0001 0.0001 0.002] are the initial condi-

  tions for y(1), y(2), and y(3), respectively. The profiles of how the concentrations of X, Y

  and Z change over time (calculated in the case of A = 0.18) are shown in Figure 8.20. It is evident that when the concentration of the activator X is high, then the concentration of

  inhibitor Y is very low, and vice versa. This behavior is due to the coproduct autocontrol,

  which is the time needed to store Z that finally regenerates Y.

  The three-dimensional plot of Figure 8.21 shows that the chemical system approaches

  a limit cycle whatever is the initial condition. Moreover, if we look at the projection on the

  XY plane, we confirm that X and Y exclude reciprocally.

  To determine the average value of the period of the oscillations we use the Fourier

  transform of the trend of [ Z] versus time. An example of Fourier Transform is shown in

  Figure 8.22.

  The uncertainty on the frequency is given by the Half Width at Half Maximum of

  the peak with the largest amplitude (see Figure 8.22). The period is given by T = 1 ν .

  The uncertainty of the period is calculated by using the formula of the propagation of the

  “a priori maximum absolute error”:

  ∆ T = − 1 ∆ν

  2

  ν

  [ Z]

  [ X]

  [ Y]

  0.002

  [ X] and [

  0.0002 Y

  [ Z] (M)

  ] (M)

  0.001

  0.000

  0.0000

  550

  600

  650

  700

  Time (s)

  FIGURE 8.20 Trends of [ Z], [ X] and [ Y] over time, when [ A] = 0.18 M.

  232

  Untangling Complex Systems

  0.0025

  0.0020

  0.0015

  [ Z]

  0.0010

  0.0000

  0.0005

  0.0001

  0.0000

  [ Y ]

  0.0000

  0.0001

  0.0002

  0.0002

  0.0003

  [ X]

  FIGURE 8.21 Three-dimensional phase space of the Oregonator model.

  0.0010

  0.0008

  0.0006

  Width at half maximum

  0.0004

  Amplitude

  0.0002

  0.00000.00

  0.02

  0.04

  0.06

  0.08

  0.10

  v (Hz)

  FIGURE 8.22 Fourier transform of the time series [ Z] versus time when [ A] = 0.18 M.

  The numerical integration of the system of three differential equations and the determi-

  nation of the period of the oscillations after the calculation of the Fourier Transform are

  repeated for all the conditions proposed in the text of this exercise. Finally, to establish the

  exponential term n of the relation T

  n

  ∝

  −

  [BrO3 ] , it is convenient to build a log-log plot, like

  that shown in Figure 8.23. The straight line determined by the least-squares method has a

  slope n = −(0 6

  . ± 0. )

  1 .

  8.4. The function file to integrate the system of three differential equations in MATLAB should

  look like that presented in exercise 8.3. The values of the kinetic constants at the three tem-

  peratures proposed in the text of the exercise are reported in Table 8.8.

  They have been calculated through the Arrhenius equation ( k T

  ( Eact R( T 0 T

  − i

  ( ) (

  ))

  0 ))

  i

  k T

  = e

  .

  The script file to solve this exercise should look like the following one:

  [t y]=ode15s(‘Oregonator’,[0 1200], [0.0001 0.0001 0.002]);

  The Emergence of Temporal Order in a Chemical Laboratory

  233

  2.05

  2.00

  1.95

  T) 1.90

  log( 1.85

  1.80

  1.75

  –1.1

  –1.0

  –0.9

  –0.8

  –0.7

  log([KBrO3])

  FIGURE 8.23 Linearization of the relation between log( T) and log([KBrO ]).

  3

  TABLE 8.8

  Values of the Kinetic Constants for the Elementary Steps Appearing in the Oregonator

  Model

  T (K)

  k1 (mol−3dm9s−1)

  k2 (mol−2dm6s−1)

  k3 (mol−2dm6s−1)

  k4 (mol−1dm3s−1)

  k5 (mol−1dm3s−1)

  293.15

  2

  1,000,000

  10

  2000

  1

  303.15

  4.16

  1,402,878

  22.5

  4758

  2.58

  313.15

  8.24

  1,925,972

  48.2

  10709

  6.27

  wherein [0 1200] is the time window, whereas [0.0001 0.0001 0.002] are the initial condi-

  tions for y(1), y(2), and y(3), respectively. Feel free to change slightly the initial conditions.

  The calculated average values of the periods are 79 s (at 293.15 K), 30 s (at 303.15 K),

  and 13 s (at 313.15 K). If we plot ln(1/∆ T) versus 1/ T and we determine the fitting straight

  line with the least-squares method, we obtain a slope of (−8300 ± 130), which corresponds

  to E

  (69000 1000)J mol (69 )

  act =

  ±

  =

  ±1 kJ / mol.

  8.5. The concentrations of the reactants in the proposed five experiments are listed in Table 8.9

  (such values have been inspired by the demonstration on chemiluminescence by Prypsztejn

  et al. [2005]).

  TABLE 8.9

  Concentrations of the Reagents for the Orbán Reaction in Five Distinct Experiments

  C(H2O2) M

  V(KSCN) M

  V(Luminol) M

  V(NaOH) M

  V(CuSO4) M

  Exp. 1

  0.2

  0.03

  7.4·10−4

  0.02

  2.4·10−4

  Exp. 2

  0.2

  0.03

  1.48·10−3

  0.04

  1.2·10−4

  Exp. 3

  0.2

  0.06

  7.4·10−4

  0.02

  1.2·10−4

  Exp. 4

  0.2

  0.03

  7.4·10−4

  0.04

  1.2·10−4

  Exp. 5

  0.64

  0.03

  7.4·10−4

  0.02

  2.4·10−4

  234

  Untangling Complex Systems

  Exp. 1

  3.0 × 108

  0.0

  0

  1000

  2000

  3000

  9.0 × 108

  Exp. 2

  6.0 × 108

  3.0 × 108

  0.0

  0

  1000

  2000

  3000

  1.2 × 109

  Exp. 3

  9.0 × 108

  6.0 × 108

  intensity 3.0 × 108

  ed

  0.0 0

  500

 

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