TASK 4: Test program

The core part of most of research projects is the experimental stage, where various tests and/or
numerical simulations have to be developed in order to demonstrate your hypothesis. Therefore,
you are entitled to suggest a list of possible test to carry out, specifying:
-What do you want to measure and what for?
Modified concrete mix requires to have good mechanical properties, therefore standard resistance
tests will be performed to validate that the new mix satisfies or exceeds the mechanical properties
of a regular concrete. The properties to be controlled and studied are comprised of two stages. First
stage, the mechanical properties, then, if mechanical properties meet the requirements, the second
stage will evaluate the self-healing capabilities of the designed mixture.

STAGE 1: Resistance to compression, resistance to tension, workability, water penetration.

STAGE 2: corrosion levels, self-healing capacity

The addition of non-structural compounds as the superabsorbent polymer and the microorganism
clusters, as air voids or any possible compound added to the mixture are usually encountered to
have a detrimental effect on compressive strength of the material. Although tensile strength is not
the main characteristic of concrete, it is usually affected in a similar way as to the compressive
strength. Tensile strength will be evaluated by two different methods to better characterize the
material: Indirect tension test by applying a non-coaxial compressive force and flexural test (pure
bending).
One of the goals of this research is to develop a new self-healing concrete with 30 percent more
durability than current concrete mixes. To evaluate the performance and the maintenance spans
that the mix being studied requires. One of the main reasons of decreased durability of concrete
structures is related to the corrosion of the rebars. The proposed self-healing mixture is entitled to
provide some extra corrosion protection, then, corrosion tests will be also performed to determine
the degree or protection, if so.
Workability is a key factor to be also evaluated, so, slump tests have also been included in the
program, although they will be performed as part of the compressive strength test, results are to be
recorded and analysed for comparison against regular mix.
The concept applied for this development relies on the properties of certain microorganisms to
deposit calcium carbonates as by-products of their metabolic activities. In such fashion, that byproduct precipitates are expected to accumulate in the inside of concrete cavities, thus, giving the
structure the capacity to self-repair itself from the inside. In a similar way, the addition of a super
absorbent polymer matrix is proposed to be incorporated to the admixture to comply with a double
function. Fill the gaps of newly created cavities in a short term and to act as a containing media for
the bacterial clusters.
For this reason, measuring the self-healing capacity of the newly developed mixture is of high
relevance for this development. Dimensioning of controlled cracks and repairing rates must be
carefully recorded. Being this a novel application, no standard test has been developed yet. Using as

reference the work done by XXXX (insert reference from Delft M Jonkers). Also, evaluation of
sample structures under real environmental conditions should be evaluated.
This research does not consider the acquisition of any special testing equipment whatsoever, all
testing activities are commonly available and universities right now have the capabilities to perform
them at a reasonable cost. For that reason budget eligibility of the project, as specified on the call is
100% of the total of the research activities.

-Which tests do you think should be useful to measure the magnitudes you want to?
STAGE 1, General material characteristics:
Mechanical properties:
- EN 12390-3 Testing Hardened Concrete Part 3: Compressive Strength of Test Specimens.
- EN 12390-6 Testing Hardened Concrete Part 6: Tensile Splitting Strength of Test
Specimens.
- EN 12390-5 Testing Hardened Concrete Part 5: Flexural Strength of Test Specimens.
- BS EN 12350-2:2009 Testing fresh concrete. Slump-test.
Durability:

STAGE 2, Self-healing capabilities & durability:

-ASTM G109-7 Determining Effects of Chemical Admixtures on Corrosion of Embedded
Steel Reinforcement in Concrete Exposed to Chloride Environments
-Bacterial activation O2 test
-Strength regain tests:
- EN 12390-3 Testing Hardened Concrete Part 3: Compressive Strength of Test
Specimens.
- EN 12390-6 Testing Hardened Concrete Part 6: Tensile Splitting Strength of Test
Specimens.
- EN 12390-5 Testing Hardened Concrete Part 5: Flexural Strength of Test
Specimens.

STAGE 3, Real life application:

-Visual inspection of external surfaces
-Non destructive

-For each type of magnitude (or response), which are the possible influencing variables (input
variables)? For initial stages and clearer evaluation purposes, it was decided that concrete mix
chosen has been will keep cement and water ratios constant for all mixtures, so only coarse and fine
aggregates will be modified when adding the bacterial clusters and the super-absorbent polymer.
It is expected that all mechanical properties be affected by the substitution of the aggregates for the
bacteria-embedded SAP. But for stage 2, only the samples where the self-healing agents be added
shall show some level of improvement on the regained strength properties, while control mix
samples without them are expected to keep the same level of resistance after the cracking and retest.
STAGE 1
Compressive strength

% Bacterial content, % SAP, %Fine agg., %Corse agg

Tensile strength

% Bacterial content, % SAP, %Fine agg., %Corse agg

Flexural strength

% Bacterial content, % SAP, %Fine agg., %Corse agg

Workability

% Bacterial content, % SAP, %Fine agg., %Corse agg

Permeability

% Bacterial content, % SAP,

STAGE 2
Bacterial activation

% Bacterial content, % SAP

Self-healing capacity

% Bacterial content, % SAP

Regained compressive strength

% Bacterial content, % SAP

Regained tensile strength

% Bacterial content, % SAP

Regained flexural strength

% Bacterial content, % SAP

Regained permeability

% Bacterial content, % SAP

MAGNITUDES:
-How many replicas do you suggest to do in each type of test?
The initial proposal for the quantity of samples suggested by the standards used is 3, instead 9
samples will be used for statistical significance.
STAGE 1

No. of Replicas

Compressive strength

Tensile strength

Flexural strength

Workability

Permeability

STAGE 2
Corrosion potential

Self-healing capacity

Regained compressive strength

Regained tensile strength

Regained flexural strength

Regained permeability

-How many tests are needed to perform for each response? Perform a DOE, in order to determine the total number of
tests.

DESIGN OF EXPERIMENTS
STAGE 1, Mixture design.
To determine the total sample quantity and sampling matrix is necessary to know all the different
combinations of components that will be used. With help of Minitab v.17 software a mixture design
was prepared for all the tests taking into account the following assumptions:
a) The proposed mixture has a concrete to water ratio of 2:1, this same proportion is maintained for
all the mixtures.
b) Aggregate mix will be composed of 1:1 fine aggregate (sand) to coarse aggregates (gravel for all
the samples.
c) The control mix is composed in the following way:

CONTROL MIXTURE
Component

% by weight

CEMENT

20

WATER

10

GRAVEL (Coarse Agg.)

35

SAND (Fine Agg)

35

d) Self-Healing Mixture
The additives, here considered as the bacterial clusters and the super-absorbent polymer and each will vary
from 1 to 3% of the total mixture weight. That will be compensated by removing the same amount from the
aggregate mix. I. E. for a mixture containing 1% of bacterial clusters and 2% of SAP, the aggregate mixture will
be 67%.
SELF-HEALING MIXTURE Example
1% Bact., 3% SAP
Component

% by weight

CEMENT

20

WATER

10

GRAVEL (Coarse Agg.)

33.5

SAND (Fine Agg)

33.5

BACTERIAL CLUSTERS

S. A. POLYMER

The results obtained with the mixture design from Minitab v.17 yielded nine (9) different combinations as
shown below (values represent % by weight of overall mixture weight).
For the detailed process of the mixture design model, please refer to the next section Calculations-DOE.

MIX No.

BACTERIA

SAP

AGGREGATES
(mix 50/50)

TOTAL

1
2
3
4
5
6
7
8
9

3
3
1
2
2
1
2
3
1

3
1
3
2
3
2
1
2
1

64
66
66
66
65
67
67
65
68

70
70
70
70
70
70
70
70
70

INSERT TEST MATRIX AND SAMPLE NUMBER, MENTION THAT THE MIXTURE DESIGN IS
APPLICABLE TO ALL THE TESTS AND THEY ALL HAVE THE SAME NUMBER OF SAMPLES,
THERES A LINK NEEDED BETWEEN ALL TESTS AND THE DOE. SPECIFY THE RESPONSES.

CALCULATIONS, DOE Mixture design based on Minitab v.17

Based on the same assumptions of section Stage 1 Mixture Design the following steps were
followed for the creation of the model.
A Mixture Design was selected for the purposes of the task, linear and quadratic models were
explored, also mixture optimization was performed to better match the needs of the project.

First run was generated using extreme vertices design so the possibility to choose the limits for the
components of the mix. Three (3) components were used to generate the mixture, with linear
elements and single replicas and not randomized runs as shown in the images below.

Generation of the model

Further exploration was performed (listed below) in a second run of mixtures after analysing the
sample distribution of the mixture for the linear elements and finding the mixture distribution too
close to each other. As the mix behaviour is unknown at this point, more scattered design will help to
better identify the relation of the different proportions of the elements in the mixture with the
outputs. Later, if certain behaviour can be determined, then a new set of narrower mixes can be
generated to further characterize the new concrete mix properly.

Generating a quadratic model...

The result with the quadratic element type yielded 13 points. The run was later optimized to nine
points to provide the same amount of samples that the linear model but slightly more adapted to the
needs of the scope, that is broader difference between the mixture composition.
Mixture design chosen:

Quadratic design (13 points) vs Quadratic design (9 points)

Runs completed:
-Linear elements, 3 components.
-Quadratic elements, 3 components.
-Quadratic elements, 3 components (Optimization).
-Quadratic elements, 3 components, (Optimization) 3 replicas, minimum.
-Quadratic elements, 3 components, (Optimization) 9 replicas, selected = 81 samples /
magnitude.

Linear model (3 samples / mix, 9 points)

Extreme Vertices Design SINGLE RUN CALCULATION (3 samples per mixture)
Components:
Process variables:

3
0

Design points:
Design degree:

9
1

Mixture total: 70.00000

Number of Boundaries for Each Dimension
Point Type
Dimension
Number

1
0
4

2
1
4

0
2
1

Number of Design Points for Each Type

Point Type
Distinct
Replicates
Total number

1
4
1
4

2
0
0
0

3
0
0
0

0
1
1
1

-1
4
1
4

Bounds of Mixture Components

Comp
A
B
C

Amount
Lower
Upper
1.0000
3.0000
1.0000
3.0000
64.0000 68.0000

Proportion
Lower
Upper
0.014286 0.042857
0.014286 0.042857
0.914286 0.971429

Design Table
Run
1
2
3
4
5
6
7
8
9

Type
1
1
1
1
0
-1
-1
-1
-1

A
1.0000
3.0000
1.0000
3.0000
2.0000
1.5000
2.5000
1.5000
2.5000

B
1.0000
1.0000
3.0000
3.0000
2.0000
1.5000
1.5000
2.5000
2.5000

C
68.0000
66.0000
66.0000
64.0000
66.0000
67.0000
66.0000
66.0000
65.0000

Pseudocomponent
Lower
Upper
0.000000 0.500000
0.000000 0.500000
0.000000 1.000000

Quadratic design (3 samples / mix, 13 points)

Extreme Vertices Design
Components:
Process variables:

3
0

Design points:
Design degree:

13
2

Mixture total: 70.00000

Number of Boundaries for Each Dimension
Point Type
Dimension
Number

1
0
4

2
1
4

0
2
1

Number of Design Points for Each Type

Point Type
Distinct
Replicates
Total number

1
4
1
4

2
4
1
4

3
0
0
0

0
1
1
1

-1
4
1
4

Bounds of Mixture Components

Comp
A
B
C

Amount
Lower
Upper
1.0000
3.0000
1.0000
3.0000
64.0000 68.0000

Proportion
Lower
Upper
0.014286 0.042857
0.014286 0.042857
0.914286 0.971429

Pseudocomponent
Lower
Upper
0.000000 0.500000
0.000000 0.500000
0.000000 1.000000

Linear Constraints of Mixture Components

Constraint
1

Lower
64.000000

A
1.000000

B
1.000000

C
1.000000

*** indicates inconsistent or unnecessary constraint.

* NOTE * Flagged constraints are ignored.
Design Table
Run
1
2
3
4
5
6
7
8
9
10
11
12
13

Type
1
1
1
1
2
2
2
2
0
-1
-1
-1
-1

A
1.0000
3.0000
1.0000
3.0000
1.0000
2.0000
3.0000
2.0000
2.0000
1.5000
2.5000
1.5000
2.5000

B
1.0000
1.0000
3.0000
3.0000
2.0000
1.0000
2.0000
3.0000
2.0000
1.5000
1.5000
2.5000
2.5000

C
68.0000
66.0000
66.0000
64.0000
67.0000
67.0000
65.0000
65.0000
66.0000
67.0000
66.0000
66.0000
65.0000

Upper
70.000000

***

Quadratic design OPTIMIZED (3 samples / mix, 9 points)

Optimal Design: BACTERIA, SAP, AGGREGATES (50/50)
Mixture design selected according to D-optimality
(parameters calculated for component proportions)
Number of candidate design points: 13
Number of design points in optimal design: 9
Model terms: A, B, C, AB, AC, BC
Initial design generated by Sequential method
Initial design improved by Exchange method
Number of design points exchanged is 1
Optimal Design
Row number of selected design points: 4, 2, 3, 9, 8, 5, 6, 7, 1
Condition number:
D-optimality (determinant of XTX):
A-optimality (trace of inv(XTX)):
G-optimality (avg leverage/max leverage):
V-optimality (average leverage):
Maximum leverage:
Data Matrix
Run
4
2
3
9
8
5
6
7
1

A
3.000
3.000
1.000
2.000
2.000
1.000
2.000
3.000
1.000

B
3.000
1.000
3.000
2.000
3.000
2.000
1.000
2.000
1.000

C
64.000
66.000
66.000
66.000
65.000
67.000
67.000
65.000
68.000

83215526
0.0000000
75408530
0.827586
0.666667
0.805556

Quadratic design OPTIMIZED (9 samples / mix, 81 points vs 117 non optimized)

Optimal Design: BACTERIA, SAP, AGGREGATES (50/50)
Mixture design selected according to D-optimality
(parameters calculated for component proportions)
Number of candidate design points: 117
Number of design points in optimal design: 81
Model terms: A, B, C, AB, AC, BC
Initial design generated by Sequential method
Initial design improved by Exchange method
Number of design points exchanged is 1
Optimal Design
Row number of selected design points: 1,
4, 1, 3,
6,
8, 9, 1,
2,
4, 5, 6,
7,
8, 1, 2,
3,
Condition number:
D-optimality (determinant of XTX):
A-optimality (trace of inv(XTX)):
G-optimality (avg leverage/max leverage):
V-optimality (average leverage):
Maximum leverage:
Data Matrix
Run
1
4
2
3
9
8
6
7
1
2
3
4
9
5
2
4
1
3
6
7
8
1
2
3
4
9
5

A
1.000
3.000
3.000
1.000
2.000
2.000
2.000
3.000
1.000
3.000
1.000
3.000
2.000
1.000
3.000
3.000
1.000
1.000
2.000
3.000
2.000
1.000
3.000
1.000
3.000
2.000
1.000

B
1.000
3.000
1.000
3.000
2.000
3.000
1.000
2.000
1.000
1.000
3.000
3.000
2.000
2.000
1.000
3.000
1.000
3.000
1.000
2.000
3.000
1.000
1.000
3.000
3.000
2.000
2.000

C
68.000
64.000
66.000
66.000
66.000
65.000
67.000
65.000
68.000
66.000
66.000
64.000
66.000
67.000
66.000
64.000
68.000
66.000
67.000
65.000
65.000
68.000
66.000
66.000
64.000
66.000
67.000

4, 2, 3, 9, 8, 6, 7, 1, 2, 3, 4, 9, 5, 2,
7, 8, 1, 2, 3, 4, 9, 5, 6, 4, 2, 3, 1, 7,
3, 4, 5, 6, 7, 8, 1, 2, 3, 4, 9, 1, 2, 3,
8, 1, 2, 3, 4, 9, 1, 2, 3, 4, 9, 5, 6, 7,
4, 9, 1, 2, 3, 4, 5, 6
120211066
0.0000000
9292199
0.958025
0.0740741
0.0773196

6
4
2
3
1
7
8
9
1
2
3
4
5
6
7
8
1
2
3
4
9
1
2
3
4
5
6
7
8
1
2
3
4
9
1
2
3
4
9
5
6
7
8
1
2
3
4
9
1
2
3
4
5
6

2.000
3.000
3.000
1.000
1.000
3.000
2.000
2.000
1.000
3.000
1.000
3.000
1.000
2.000
3.000
2.000
1.000
3.000
1.000
3.000
2.000
1.000
3.000
1.000
3.000
1.000
2.000
3.000
2.000
1.000
3.000
1.000
3.000
2.000
1.000
3.000
1.000
3.000
2.000
1.000
2.000
3.000
2.000
1.000
3.000
1.000
3.000
2.000
1.000
3.000
1.000
3.000
1.000
2.000

1.000
3.000
1.000
3.000
1.000
2.000
3.000
2.000
1.000
1.000
3.000
3.000
2.000
1.000
2.000
3.000
1.000
1.000
3.000
3.000
2.000
1.000
1.000
3.000
3.000
2.000
1.000
2.000
3.000
1.000
1.000
3.000
3.000
2.000
1.000
1.000
3.000
3.000
2.000
2.000
1.000
2.000
3.000
1.000
1.000
3.000
3.000
2.000
1.000
1.000
3.000
3.000
2.000
1.000

67.000
64.000
66.000
66.000
68.000
65.000
65.000
66.000
68.000
66.000
66.000
64.000
67.000
67.000
65.000
65.000
68.000
66.000
66.000
64.000
66.000
68.000
66.000
66.000
64.000
67.000
67.000
65.000
65.000
68.000
66.000
66.000
64.000
66.000
68.000
66.000
66.000
64.000
66.000
67.000
67.000
65.000
65.000
68.000
66.000
66.000
64.000
66.000
68.000
66.000
66.000
64.000
67.000
67.000