High Strength Concrete - Durability Investiga-

tions by Using the CDF-Test - First Results

Robert Krumbach1, Katrin Seyfarth2, Wolfgang Erfurt2, Karen Friedemann1

SUMMERY

Some unusual observations with respect to the durability of some high-strength

concretes (HSC) caused investigations on the influence of typical properties of
HSC’s like hydration behaviour and strength development, especially with regard
to the frost de-icing salt resistance (FDSR). The research project is a co-
operation with the F. A. – Finger-Institute of the Weimar-University. In this pa-
per first results are presented.

1 INTRODUCTION

Resulting from their high density, high-strength concretes differ from normal
strength concretes in a higher durability, e.g. a high frost de-icing resistance and a
high resistance to chemical substances. Some unusual observations on HSC’s
were made since the development and practical utilization of HSC which caused
objections regarding the durability. Tests on building members produced of HSC
showed, that a decrease of the compressive strength and a formation of mi-
crocracks can occur gradually. This happened primarily when concretes were
exposed to high temperatures during the hydration such as inside building mem-
bers. It was also observed that their resistance to freeze de-icing cycles can be
considerably lower than expected [1-4].
The guideline of the DAfStb (German Committee for Reinforced Concrete) [5]
reflects these problems: The utilization of concretes with a strength class higher
1
Dipl.-Ing., Institut für Massivbau und Baustofftechnologie, University of Leipzig
2
Dipl.-Ing., F. A.-Finger Institut für Baustoffkunde, Bauhaus-University of Weimar

57
LACER No. 3, 1998

than B 95 for exterior building members and the use of superplasticisers is lim-
ited.
Causes of the peculiarities of HSC’s and the risk of a possible microcrack forma-
tion mechanism are conceivable – e.g. the entering of moisture into building
components owing to capillary suction - which induce or intensify building dam-
age:
• Temporary temperatures up to 70 °C inside the structural component owing to
fast heat development during the hydration [6, 7]
• Stronger formation of monosulphate/AFm,
• At the same time entering of more water e.g. through cracks, makes the
chemical reaction Monosulphate/AFm → Ettringite/AFt possible (the
volume growing 2,3 times)
• Incomplete hydration connected with “inside drying-out” owing to extreme
low w-c ratios
• At the same time entering of more water, e.g. through microcracks makes
the swelling of the cement gel and the formation of new phases possible
being the reason for a considerable volume growing (e.g. C3A, C4AF,
C3AH6, Monosulphate/AFm → Ettringite/AFt).
• No capillary pores content, dense mortar matrix
• At the same time entering of more water e.g. through microcracks space
for expansion there is no for especially:
• De-icing water at freezing under hydrostatic pressure (volume growing
connected with blast effects)
• Development of new phases under imposed deformation (microcracks
into the concrete structure or flakings can occur)
A reduced durability of HSC’s cannot be excluded as mentioned above. Further-
more, unfavourable additional effects caused by high superplasticizer content (up
to 70 g/ml per kg cement) can occur depending on the moment of adding.
Our investigations shall clarify, whether and in which extent a reduced durability
must be expected, what is causing this and by which practical steps the risks can
be counteracted.

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 High Strength Concrete - Durability Investigations
by Using the CDF-Test - First Results

2 GENERAL ASPECTS

In our research project the influence of the typical properties the production of
HSC, like:
• extremely low w-c-ratio
• high content of superplasticizer at different times
• suffering high temperatures during the hydration
on the hydration process and on the strength development, especially on the
FDSR (CDF-test method), shall be investigated.
Additionally, the arrangement of the concrete structure as well as possible modi-
fications of the structure will be observed before and after different kinds of cur-
ing and after the CDF-test (ultrasonic). To get a wide spectrum of various
parameters influencing the concrete properties the concrete compositions indi-
cated in table 2 were selected. For comparison, the mixtures will be produced
with two cements with different sulphate resistance: CEM I 42,5 R and CEM I
42,5 HS (sulphate resistance, DIN 1164, tab. 1). The HS-cement showed after 28
days of hydration – that is before the frost de-icing salt test – slightly more AFm
phases than the ordinary Portland cement containing more C3A.
The concretes have w-c-ratios of 0,40 (no superplasticizer) and of 0,25 (5 M-% of
superplasticizer). The used superplasticizer (FM) is a mixture of melamine and
naphthalinsulphonic resin.
Depending on the concrete mixture microsilica (MS) was used (content: 0 and
10 M-%, tab. 2) in the form of a slurry with 50 M-% solid content.
As aggregates we use sand (0/2) from the river Main and gravel (2/8; 8/16) from
the river Rhine.

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LACER No. 3, 1998

Table 1: Analysis of cements used

CEM I 42,5 R CEM 42,5 HS

Blaine fineness, cm²/g 3581 4449
Initial setting, start, min. 2:42 3:32
Required amount of water, M.-% 28,3 29,7
Compressive strength, N/mm²
(2d; 28d) 31,9; 59,0 31,4; 57,7
SiO2 20,5 19,5
Al2O3 5,3 4,0
Fe2O3 2,6 6,7
CaO 65,3 64,2
MgO 1,9 1,6
K2O 1,1 0,7
SO3 3,2 3,1

3 FIRST TEST RESULTS

3.1 Consistence and development of durability

The determination of the consistence of any concrete mixture is performed ac-

cording to DIN 1048.
Clear differences were found between the concrete series I (w/c = 0.40; no FM)
and series II (w/c = 0,25; 5 M-% FM added during mixing).
In spite of the extremely low w-c-ratio of the concretes of series II slumps be-
tween 43 cm and 55 cm are achieved by adding 5 M-% FM (II/III: 4,5 M-%;
II/IV: 4 M-%).
In contrast the concretes of series I were very sticky. The working quality was
unsatisfactory and the concrete had to be compacted on average for 2-3 min.. The
slumps achieved sizes below 35 cm.

60
 High Strength Concrete - Durability Investigations
by Using the CDF-Test - First Results

The consistencies of the concretes of series III (2 min. compacted, too) were also
unsatisfactory. The aim of these series was to test concretes with a w-c-ratio of
0,25 concerning their utilization as ready mixed concrete. We had planned to
investigate the hydration by delayed FM addition. It was the intention to add
3 M-% at the beginning of the mixing process and the second dose after 45 min.
(time of transport!). Between the beginning and 45 min the mixer should work
periodically (5 min.) 1 min. each.
However, the tests did not show the expected results because the consistencies of
the mixtures with only 3 M-% were so sticky, except for mixture III/I, that we
feared an early development of solidification. Therefore 4 M-% or 5 M-% FM
had to be added at the beginning of mixing, already. The slumps of the compara-
ble mixtures of series II, however, (see tab. 3) were not achieved also after 45
min. On the other hand the slumps of mixture III and IV from series III (10 M-%
silica) showed improved results.
The compressive strength tests according to DIN 1048 were carried out after 7 d,
28 d, 56 d and 182 d to estimate the strength development over a longer period.
The specimens were moist-cured in accordance with ENV206.
Table 2: Slumps and development of compressive strength

Series FM-addition Slumps Bulk density Compressive strength ßW.200 in

in % in cm in kg/m³ N/mm²
7d 28 d 56d 182d
I/I - 29 2,37 51 62 73
I/II - 29 2,39 54 69 73
I/III - 32 2,31 48 71 76
I/IV - 29 2,34 60 76 80 82
II/I 5 43 2,37 60 76 78 80
II/II 5 55 2,40 66 80 89 88
II/III 4,5 45 2,38 74 96 105 107
II/IV 4 51 2,36 70 95 97 98
III/I 3+2* 35 2,39 59 75 78 78
III/II 5+1* 29 2,39 71 84 83 87
III/III 4+1* 40 2,38 70 88 93
III/IV 4+1* 38 2,40 85 107 110
* after 45 min. added FM

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LACER No. 3, 1998

All concretes (tab. 2) met the 28 d-compressive strength-criterion of HSC of the

guideline of the DAfStb (ßw.200 > 55 N/mm², see tab. 2). It’s noticeable that the
tested compressive strengths of the concretes with HS-cement (concretes II and
IV) are higher than those of concretes with R-cement (concretes I and III; comp.
tab. 2, fig. 1).
As expected the concrete mixtures with 10 M-% silica (concretes III and IV of
series I – III) yielded higher compressive strengths than the concretes without
silica (concretes I and II of series I – III, tab. 2).
Mixtures with FM (w/c = 0,25) produce more favourable properties of green
concrete (slumps > 40 cm). The concretes can be compacted better and higher
compressive strengths are reached compared to concretes with w/c = 0,4 (without
FM, comp. tab. 2).
The bulk densities amount to 2,31 - 2,40 kg/cm³ (tab. 2).
Compressive strength ßw200 of series I, w/z = 0,4 without FM

90
CEM I 42.5 HS, 10 M-% silica
85
[N/mm²]

CEM I 42.5 R, 10 M-% silica

80

75
w200

CEMI 42.5 HS
CEM I 42.5 R
Compressive strength ß

70

65

60

55

50

45

40
0 7 28 182
Concrete age [d]

Fig. 1: Compressive strengths ßw.200 of series I – w/c = 0,4; without FM

62
 Table 3: Survey of concretes and the different kinds of curing and test methods

Series of concrete/ Cement Water- Content of Content of Curing Test methods

concrete cement silicaslurry FM
ratio in % in %
CDF, 28/56* cycles; ultra-
I I CEM I 42,5 R 0,4 0 0 DIN 1048 sonic
48 h 60°C,.till 7th d water
immersion CDF, 28 cycles; ultrasonic
CDF, 28/56* cycles; ultra-
II 0,4 0 0 DIN 1048 sonic
CEM I 42,5 HS 48 h 60°C, till 7th d water
CDF, 28 cycles; ultrasonic

High Strength Concrete - Durability Investigations

immersion
CDF, 28/56* cycles; ultra-
III CEM I 42,5 R 0,4 10 0 DIN 1048 sonic
63

48 h 60°C, till 7th d water

immersion CDF, 28 cycles*; ultrasonic
CDF, 28/56* cycles; ultra-

by Using the CDF-Test - First Results

IV CEM I 42,5 HS 0,4 10 0 DIN 1048 sonic
48 h 60°C, till 7th d water
immersion CDF, 28 cycles*; ultrasonic
CDF, 28/56* cycles; ultra-
II I CEM I 42,5 R 0,25 0 5, immedi- DIN 1048 sonic
ately
60°C und 80°C, no curing* CDF, 28 cycles*; ultrasonic
CDF, 28/56* cycles; ultra-
II CEM I 42,5 HS 0,25 0 5, immedi- DIN 1048 sonic
ately
60°C und 80°C, no curing* CDF, 28 cycles*; ultrasonic
 LACER No. 3, 1998
Series of concrete/ Cement Water- Content of Content of Curing Test methods
concrete mix cement- silicaslurry FM
ratio in % in %
CDF, 28/56* cycles; ultra-
II III CEM I 42,5 R 0,25 10 5, immediately DIN 1048 sonic
60°C und 80°C, no cur- CDF, 28 cycles*; ultrasonic
ing*
CDF, 28/56* cycles; ultra-
IV CEM I 42,5 HS 0,25 10 5, immediately DIN 1048 sonic
60°C und 80°C, no cur- CDF, 28 cycles*; ultrasonic
ing*
CDF, 28/56* cycles; ultra-
64

III I CEM I 42,5 R O,25 0 5, dosed (3+2) DIN 1048 sonic

60°C, no curing* CDF, 28 cycles*; ultrasonic
CDF, 28/56* cycles; ultra-
II CEM I 42,5 HS O,25 0 6, dosed (5+1) DIN 1048 sonic
60°C, no curing* CDF, 28 cycles*; ultrasonic
CDF, 28/56* cycles; ultra-
III CEM I 42,5 R O,25 10 5, dosed (4+1) DIN 1048 sonic
60°C, no curing* CDF, 28 cycles*; ultrasonic
CDF, 28/56* cycles; ultra-
IV CEM I 42,5 HS O,25 10 5, dosed (4+1) DIN 1048 sonic
60°C, no curing* CDF, 28 cycles*; ultrasonic
* planned curing and test methods
 High Strength Concrete - Durability Investigations
by Using the CDF-Test - First Results

Compressive strength ßw200; w/c=0.25; 5 M-% FM (series II)

120
CEM I 42.5 R
110
Compressive stregth ßw200 [N/mm²]

CEMI 42.5 HS
100

90
CEM I 42.5 R, 10 M-% silica
80

CEM I 42.5 HS, 10 M-% silica

70

60

50

40
0 7 28 56 182
Concrete age [d]

Fig. 2: Compressive strengths ßw.200 of series II, w/c = 0,25%; 5 M-% FM

Compressive strength ß w200 of series III, w/c=0.25;

5 M-% FM, splite
120
CEM I 42.5 HS, 10 M-% silica
110

100 CEM I 42.5 R, 10 M-% silica

CEM I 42.5 HS
90

80
CEM I 42.5 R
70

60

50

40
0 7 28 56 182

Concrete age [d]

Fig. 3: Compressive strengths ßw.200 of series III, w/z = 0,25; 5 M-% FM delayed

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LACER No. 3, 1998

3.2 The frost de-icing salt resistance of the investigated high strength
concrete

Our investigations base on different questions. On the one hand the influence of
the concrete composition (w/c = 0,4 or 0,25; FM contents = 0 or 5 M-%; silica
contents = 0 or 10 M-%, comp. tab. 2) on the FDSR shall be analysed. On the
other hand the influence of the cement composition itself shall be investigated.
The CDF-Test according to SETZER [8] was carried out on specimens
150x150x75 mm3. All specimens of series I – III were exposed to 28 freeze de-
icing cycles, one cycle takes in any case 12 h.
The first FDSR investigations (tab. 2) produced the expected results. HSC with
w/c ≤ 0,4 shows a high or very high FDSR. The very dense structure of these
concretes prevents the increase of mass by capillary suction of the 3 %-NaCl-
solution. The amount of the increasing mass was always below 0,35 M-% (tab. 4;
compared with normal concrete: 0,8 – 1,5 M-%). Especially the concretes with
w/c = 0,25 have a very small mass increase: 0,07 ≤ ∆m ≤ 0,12 M-% (tab. 4).
The results correspond to the CDF–tests: the rates of scaling of concretes with
w/c = 0,4 (28 cycles: 188 – 603 g/m²) are higher than the rates of scaling with
w/c = 0,25 (28 cycles: 51 – 104 g/m²).
As expected silica containing specimens (concretes III and IV) have lower rates
of scaling than specimens without silica (concrete I and II, tab. 4, fig. 4-6). This
points to a denser paste matrix by the “filling effect” caused by silica [9].
An influence of the cement quality on the results can be recognised on concretes
of series I (w/c = 0,4, tab. 4, fig. 4). Concretes produced with CEM I 42,5 HS
yield significant higher rates of scaling (compare 28 cycles, tab. 4) than those
with CEM I 42,5 R. This tendency was also observed in earlier investigations
[10]. Furthermore, the two cement qualities lead to a different formation of the
concrete structure. This connection has to be considered, too.
Compared with that, the concretes of series II and III (w/c = 0,25) have smaller
differences between the rates of scaling with respect to R- and HS-cements. Here,
these small differences correspond with the results of pore radii distribution
(PRV) of the mortar matrix, because the concretes produced with R- and HS-
cements show a nearly identical PRV.
It is known, that CEM I 42,5 R , with w/c ≥ 0,4, shows a higher content of capil-
lary pores and a lower content of gel pores as well as microairpores than the HS-

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 High Strength Concrete - Durability Investigations
by Using the CDF-Test - First Results

cement [10]. Concerning this an improved FDSR of HS-cement should be ex-

pected. However, the opposite tendency could be observed. Consequently, a valid
physical correlation between CDF-Test result and PRV cannot be derived [11].
The causes for that are based on occurring chemical reactions, probably.
Table 4: Frost de-icing salt resistance

Concrete Mass growth by Rates of scaling (CDF-test) in g/m²

capillary suction Number of cycles:
in %
4 8 14 28
I/I 0,32 31,6 93,2 260,4 603,1
I/II 0,33 35,3 133,5 348,1 921,1
I/III 0,30 - 75,3 105,3 188,1
I/IV 0,21 - 106,4 198,3 347,3
II/I 0,07 20,2 38,1 66,2 96,9
II/II 0,12 16,8 30,2 53,3 104,4
II/III 0,07 8,9 17 31,1 56,8
II/IV 0,07 6,2 9,3 42,2 84,0
III/I 0,09 8,2 25,6 65,8 98,2
III/II 0,08 6,5 7,8 37,3 79,5
III/III 0,08 10,8 12,1 26,7 51,1
III/IV 0,08 - 16,1 26,7 56,0

The measured rates of scaling (after 28 cycles) of all series meet the acceptance
criterion of 1500 g/m².

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LACER No. 3, 1998

Frost de-icind salt resistence (CDF-test)

w/c = 0.4; without FM (Series I )

1000

900
CEMI 42.5 HS
800

700
CEM I 42.5 R
600

500

400
CEM I 42.5 HS, 10 M-% silica
300

200

100
CEM I 42.5 R, 10 M-% silica
0
0 8 14 28
Number of freezing and thawing cycles

Fig. 4: Frost de-icing salt resistance of series I

Frost de-icing salt resistance (CDF-test) w/c = 0.25; 5 M-% FM

(Series II)
120

CEMI 42.5 HS
100

80
Scaling [g/m²]

CEM I 42.5 R
60 CEM I 42.5 HS, 10 M-% silica

40

CEM I 42.5 R, 10 M-% silica

20

0
0 4 8 14 28
Number of freezing and thawing cycles

Fig. 5: Frost de-icing salt resistance of series II

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 High Strength Concrete - Durability Investigations
by Using the CDF-Test - First Results

Frost de-icing salt resistance (CDF-test) w/c = 0,25; FM split (series III)

100

CEM I 42.5 R
80

CEMI 42.5 HS

60

CEM I 42.5 R, 10 M-% silica

40

CEM I 42.5 HS, 10 M-% silica

20

0
0 4 8 14 28
Num ber of freezing and thawing cycles

Fig. 6: Frost de-icing resistance of series III

3.3 Results of ultrasonic investigations

All specimens (150x150x75 mm3) of the series I – III (tab. 2) were tested by
ultrasonic before and after the CDF-Test. The aim of these investigations was to
get an information about possible damage inside the concretes structure or modi-
fications underneath the concrete surface.
To guarantee the required sensitivity high frequency testing heads (eigenfre-
quency in any case 250 kHz) were used. By a broad band receiver the sound
signal is detected. Afterwards, the detected vibration signal is digitalized and
evaluated by a transient recorder. The sound signal is generated by an ultrasonic
generator of the company GEOTRON-ELEKTRONIC. The specimens are cou-
pled to the sound converters in a special measuring device. Thus, an adjustment
of a reproducible coupling pressure is possible. Clay was used for coupling. The
position of the sound converter during the measuring is shown in figure 7.

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LACER No. 3, 1998

Ultrasonic generator

Transmitter

B
Scaled
surface Specimen A A
B

Receiver

Transient recorder

Fig. 7: Position of the sound converter during the measuring

The sound converters are coupled to the specimens as shown in figure 7 (both
positions A – A and B – B). So, exact localisation of occurring damage near the
surface or inside the concrete structure is possible.
Figure 8 shows the differences between the measured sound velocities before and
after the CDF-test. At the series I (w/c = 0,4) the sound velocities are lower than
the sound velocities of specimens of the series II and III (w/c = 0,25).
The measured sound velocities after the 28 freeze de-icing-cycles are slightly
higher than the sound velocities before the CDF-test, except concretes I/II and
II/I. This fact may be caused by the crystallization of NaCl during the drying of
the specimens after the CDF-test.
The obtained differences of sound velocities of ≤ 50 m/s can be neglected due to
low water penetration.
Consistent damage of the material structure could not be observed.

70
 High Strength Concrete - Durability Investigations
by Using the CDF-Test - First Results

5100

5000

4900
Sound velocity [m/s]

4800

4700

4600

4500

4400
I/II I/III I/IV II/I II/II II/III II/IV III/I III/II III/III III/IV

bevore CDF-test after CDF-test

Fig. 8: Sound velocities before and after CDF-test

4 FURTHER INVESTIGATIONS

Up to now, we have also made observations indicating different behaviour of the

investigated HSC’s under extreme conditions. Especially if the specimens were
exposed to higher temperatures in the first two days during the curing higher rates
of scaling could be obtained. The further investigations shall simulate the devel-
opment of the hydration heat of 60 °C and 80 °C. It is also planned, to increase
the number of the freeze de-icing – cycles up to 56 (tab. 2).
For the evaluation of the hydration process extensive analytical investigations by
XRD, REM/ESMA or ESEM, DTA/DTG/TG shall be carried out.

REFERENCES

[1] Guse, U.; Hilsdorf, H.: Zum Frost- und Frost- Tausalz- Widerstand
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LACER No. 3, 1998

[2] Penttala, V.: Effects of delayed dosage of superplasticizer on high per-

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[3] Larsen, E., Lauridsen, J.; Eriksen, K.; Hansen, O.; Molgaard, T.: Betons
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[7] Dilger, H. W.; Wang, C.: Effects of W/C, Superplasticizers and Silika
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