Fly ash for concrete

the new EN 450

Backgrounds to the revision of

EN 450-1 and EN 450-2
EUROCOALASH 2010 COPENHAGEN

Background to the revision of EN 450

Introduction
Overview existing and revised requirements
Modification requirements EN 450-1
Modification requirements EN 450-2
Modification test methods EN 450-1

Introduction
In 1995, the first EU standard was published concerning this
item, namely the EN 450 Fly ash for concrete- Definition,
specifications and quality control.
This edition was followed up by a harmonized standard based
on mandate M 128 in 2005 (EN 450-1 andEN 450-2.
The scope of EN 450-1 clarifies that fly ash with percentages
of co-combustion material higher than those covered in EN
450-1 clause 4 or with other types of co-combustion material,
are outside the scope of EN 450-1.
In some countries the use fly ashes with a higher percentage
of co-combustion material was already common practice and
it was not accepted to see fly ashes from higher amounts of
co-combustion and other co-combustion materials excluded
from CE marking.

Introduction
It was agreed that ETAs could be granted for this
product according to article 8.2 of the Construction
Products Directive.
The mandate M 128 was updated with the clarification
that fly ash produced with other types than those
covered by EN 450-1 and fly ash produced with a
percentage of co-combustion material outside the limits
defined in EN 450, can be subject to ETAs, in order to
allow these products to be CE marked.
The experience gained with the fly-ashes conforming the
ETAs should be used for the next revision of EN 450-1.

Introduction
Due to the regular 5 year revision, WG 4 of CEN TC 104
incorporated the knowledge gained with the fly-ashes
conforming to these ETAs with EN450.
Other issues for the revision was a lack of clarity
regarding the conformity evaluation and some of the
other requirements.
This presentation gives insight into the background to
the modifications that have been taken up in the new EN
450-1 and of those requirements that have been deleted
from the current standard.

Members of CEN TC 104 WG4

Mr. H.A.W. Cornelissen

Mr. J.W. van den Berg
Mr. F.R. Koubowetz
Mr. B. Diricq
Mr. N. Bech
Mr. A. Hazime
Mr. W. Hintzen
Mr. W. Brameshuber
Mr. D. Heinz
Mr. F. Corazza
Mr. T. Szczygielski
Mr. D. Bochenczyk
Mr. Z. Giergiczny
Mr. J. Vale
Mr. S. Dietz
Mr. L.K.A. Sear
Mr. H. J. Feuerborn

Netherlands (convenor)
Netherlands (rapporteur)
Austria
Belgium
Denmark
France
Germany
Germany
Germany
Italy
Poland
Poland
Poland
Portugal
Switzerland
United Kingdom
ECOBA

Background to the revision of EN 450

Introduction
Overview existing and revised requirements
Modification requirements EN 450-1
Modification requirements EN 450-2
Modification test methods EN 450-1
Quality assurances

Overview existing and revised requirements

Phase

Property

unit

Existing

Revised

Workability

LOI

% m/m

5.0
2.0 7.0
4.0 9.0

5.0
7.0
9.0

Fineness fraction> 45 mu

% m/m

40 (N)
12 (S)

n.m.

Soluble phosphate (P2O5)

% m/m

0,01

n.m.

Total phosphate (P2O5)

% m/m

Initial setting

Min.

2C

n.m.

Sum SiO2 + Al2O3 + Fe2O3

% m/m

70

n.m.

Reactive SiO2

% m/m

25

Deleted

Activity index 28 days

91 days

75
85

n.m.

Alkali Silica Reaction

(ASR)

Na2O-equivalent

% m/m

5,0

n.m.

Reactive CaO

% m/m

10,0

n.m.

Soundness

SO3

% m/m

3,0

n.m.

Free CaO*

% m/m

2.5

1.5*

Soundness

mm

10

n.m.

Total MgO

% m/m

4,0

n.m.

Cl

% m/m

0,10

n.m.

Initial strength development

Strength development

*) if free lime is greater than 1.5 % by mass, than test for soundness

5.0

Changes of the requirements EN 450-1

In relation to the previous standard, the following
changes have been adapted:
The definition of fly ash has been modified (3.2 of the
EN 450).
The permitted amount and type of co-combustion
materials have been changed (4.2 of the EN 450).
The requirement for the lower limit of LOI for category
B and C fly ash has been deleted (5.2.2 of the EN
450).
The requirement for free lime (CaO) has been
changed (5.2.5 of the EN 450)
The requirement for reactive silicon dioxide has been
modified (5.2.7 of the previous EN 450)
The amount of total phosphate has been limited by a
new requirement (5.2.10 of the EN 450).

Background to the revision of EN 450

Introduction
Overview existing and revised requirements
Modification requirements EN 450-1
Modification requirements EN 450-2
Modification test methods EN 450-1
Quality assurances

Definition of fly ash

Text EN 450-1 +A1:2007
Fine powder of mainly spherical, glassy particles,
derived from burning of pulverised coal, with or without
co-combustion materials, which has pozzolanic
properties and consists essentially of SiO2 and Al2O3.
The content of reactive SiO2, as defined and described
in EN 197-1 being at least 25% by mass.

Text EN 450-1 new

Fine powder of mainly spherical, glassy particles,
derived from burning of pulverised coal, with or without
co-combustion materials, which has pozzolanic
properties and consists essentially of SiO2 and Al2O3.

Definition of fly ash

Background
The requirement of reactive SiO2 has been deleted in
the definition of the revised EN 450, but is exist as
requirement (5.2.7 of the revised EN 450-1).
Fly ash derived from burning of pulverized coal and cocombustion materials is only possible in dedicated
boilers where combustion takes place in a cloud, with
combustion temperatures of 1300-1500 C.

Definition of fly ash

Background
Ashes from other boilers like grate-fired and fluidized
bed boilers do not meet the definition.
The definition guarantees that combustion takes place at
high temperature, which is high enough to facilitate glass
formation in the fly ash.
Municipal and industrial waste incineration ashes do not
conform to the definition.

Definition of fly ash

Background
Coal contains mineral matter that will form the glass
phase during combustion. Also part of the secondary
fuels contain mineral matter that contribute to glass
formation.
The presence of the glass phase is further assured by
the requirement for the minimum total amount of SiO2 +
Al2O3 +Fe2O3 (as main fraction of potential glass forming
matter).
On performance level, the requirement for the activity
index after 28 and 91 days provide enough assurance
for a sufficient pozzolanic behaviour of the fly ash.

Co-combustion materials
Text EN 450-1 +A1:2007
FIy ash from co-combustion as defined in 3.2 is obtained
from pulverised coal fired simultaneously with cocombustion materials as listed in Table 2. The minimum
percentage, by dry mass, of coal (Kc) shall not be less
than 80 % and the maximum proportion of fly ash
derived from co-combustion materials (M) shall not be
greater than 10 % when calculated from the Formula (1).

Co-combustion materials
Table 1 Types of co-combustion materials
1 Vegetable material like wood chips, straw, olive shells and other vegetable
fibres

2 Green wood and cultivated biomass

3 Animal meal
4 Municipal sewage sludge
5 Paper sludge
6 Petroleum coke
7 Virtually ash free liquid and gaseous fuels

Co-combustion materials
Text EN 450-1 new
Fly ash from co-combustion as defined in 3.2 is obtained
from pulverised coal fired simultaneously with or without
co-combustion materials as listed in Table 1. The
minimum percentage, by dry mass, of coal (Kc) shall be
not less than 60% or 50% if the co-combustion material
is only green wood. The maximum proportion of ash
derived from co-combustion materials (M) shall not be
greater than 30% by dry mass when calculated from the
equation (1).
Provided that the biomass used for co-combustion is
green wood i.e. not recycled wood, the maximum
percentage of co-combustion material can be increased
to 50 % by mass.

Co-combustion materials
Table 1 Types of co-combustion materials
1 Solid Bio Fuels complying with CEN/TS 14588 including animal husbandry
residues

2 Animal meal (meat and bone meal)

3 Municipal sewage sludge
4 Paper sludge
5 Petroleum coke
6 Virtually ash free liquid and gaseous fuels
Materials not included in the list should be subject for ETA

Co-combustion materials
Background
The classification of secondary fuels has been changed in
the revised EN 450. Class 1 and 2 secondary fuels have
been merged as these are from the same origin.
The minimum proportion of coal has been decreased from
80% m/m to 60% m/m (50% m/m for green wood).
Further, the maximum proportion of ash derived from
secondary fuels has been increased from 10 % m/m to
30% m/m.
Since 2005, ETAs are being used for testing the technical
and environmental suitability of fly ash, exceeding the cocombustion limits of the EN 450, for use as addition in
concrete.
Before ETAs were available, Dutch fly ashes from cocombustion were tested according to CURRecommendations (since 1999).

Co-combustion materials
Experience gained with ETAs
The test results showed that in nearly all cases, the
chemical requirements of the ETA were met.
This can be explained by the fact that the co-combustion
amount was adjusted to the chemical requirements or to
operational conditions (fuel feed, slagging, corrosion
etc.).
The results showed also that the XRD analyses of fly
ash did not provide extra information for quality control.
In all cases no other minerals were identified than listed
in the ETA. Therefore this criterion was not taken over in
the revised EN 450.

Co-combustion materials
A direct relation between the requirement and the influence of co-combustion
is noted with VV; an indirect relation with V.
phase

Requirement EN 450-1

Main influence co-combustion

Ca

workability

Mg

LOI
Water requirement
fineness fraction > 45 m

initial strength
development

strength
development
Alkali Silica
Reaction

Soluble P2O5

VV

total P2O5

VV

initial setting

VV

sum SiO2 + Al2O3 + Fe2O3

activity index
VV

Na2O equivalent
reactive CaO

VV

SO3
soundness/
durability

free CaO

VV

Soundness

total MgO
Cl-

VV

Co-combustion materials
Experience gained with ETAs
For a selection of fly ashes, concrete specimens were
produced to check if the proposed test methodology is
adequate.
The performance of concrete did not show significant
influence of co-combustion.
The results are described in several reports and
presentations.
The performance of fly ash obtained from different cocombustion materials could be explained by the
mineralogical composition of the fly ash and that this
could be related to the origin of the co-combustion
material.
It was shown that depending on the origin of the fuel
high co-combustion percentages are possible.

Loss on ignition (LOI)

EN 450-1 +A1:2007
Property

unit

Requirement

LOI

% m/m

5.0
2.0 7.0
4.0 9.0

Property

unit

Requirement

LOI

% m/m

5.0
7.0
9.0

EN 450-1 new

Loss on ignition (LOI)

With the introduction of the revised EN 450-1:2005 three
categories of LOI were introduced, each covering a
range of 5 % by mass but only category A with a lower
limit of zero. The statistical assessment has to be
evaluated by variables. The system used is designed for
normally distributed data sets and acceptability constant
together with producer and consumers risk. The system
was established by D.B. Owen in 1962, but for one sided
evaluations only.

Loss on ignition (LOI)

The consumer risk of 5 % is the right
tail of the curve, the producer risk of
10 % is under the curve between UL
and UK-kA*s. For LOI category A no
result can exceed the single result
limit of 7% LOI.

LOI Distribution
0,45

LOI(mean)UL-kA*s

0,4
0,35

10% PR

0,3
0,25

Upper limit

0,2

Prob.

5% CR

0,15
0,1

Single result limit

0,05

The area under the normal curve at the zero point is negligible for
category A fly ash as its not possible to have an LOI value <0%. But for
category B or category C fly ash the lower limits of 2 or 4 % by mass
cause compliance problems and reduce the possible mean LOI
between category A and B.
By this category B fly ash can only be produced in a very small and non
practical production window.
Based on the well proven systems of assessment by variables the
lower limits need to be deleted as the evaluation is valid for one-sided
systems only.
0

0,00

2,00

4,00

6,00

8,00

LOI

10,00

12,00

14,00

Free calcium oxide

Text EN 450-1 +A1:2007
The content of free calcium oxide shall be determined by
the method described in EN 451-1 and shall not be
greater than 2,5 % by mass. If the content of free
calcium oxide is greater than 1,0 % by mass, then the fly
ash shall be tested for conformity to the requirements for
soundness in 5.3.3.
Text EN 450-1: new
The content of free calcium oxide shall be determined by
the method described in EN 451-1. If the content of free
calcium oxide is greater than 1,5 % by mass, then the fly
ash shall be tested for conformity to the requirements for
soundness in 5.3.3.

Free calcium oxide

Background
The minimum free lime content above which soundness
has to be tested has been increased from 1% m/m to
1,5% m/m. Further, the maximum amount of free lime of
2,5 m/m has been deleted.
A statistical analysis of data show that up to 1.5% m/m
free CaO, soundness is established. Above this content
the soundness values may increase, but still hardly any
fly ash exceeds the limit of 10 mm.
Based on these data it is concluded that only above 1.5
% m/m free lime, soundness has to be proven.
The criterion of soundness together with the criterion of
reactive CaO provides enough insurance that further
limitation of the amount of free CaO is superfluous.

Soundness / Free CaO

10
9

min
max
mean
s
n

soundness [mm]

CaOfree
0,05
4,1
1,28
0,49
734

soundness
0,00
9,5
1,86
1,10
734

6
5
4
3
2
1
0
0,0

0,5

1,0

1,5

2,0

2,5

CaOfree [% by mass]

3,0

3,5

4,0

4,5

Reactive silicon dioxide

Text EN 450-1 +A1:2007
The amount of reactive silicon must be analyzed in
accordance with EN 197-1:2000 and must not be less
than 25% m/m. Only fly ash from the combustion of
pulverized coal shall be deemed to satisfy this
requirement.
Text EN 450-1:new
In the initial type test for fly ash from co-combustion (4.2)
the amount of reactive silicon must be analyzed in
accordance with EN 197-1 and must not be less than
25% m/m. Fly ash obtained from combustion of
pulverised coal only shall be deemed to satisfy this
requirement.

Phosphate
Text EN 450-1 +A1:2007
The content of soluble phosphate (P2O5) shall be determined in
accordance with EN 196-2 and shall not be greater than 100 mg/kg.
Fly ash obtained from combustion of pulverised coal only shall be
deemed to satisfy this requirement.

Text EN 450-1: new

The content of total phosphate (P2O5) shall be determined in
accordance with EN 196-2 and shall not be greater than 5.0 % by
mass. Fly ash obtained from combustion of pulverised coal only
shall be deemed to satisfy this requirement.
In the initial type test for fly ash from co-combustion (4.2) the content
of soluble phosphate (P2O5) shall be determined in accordance with
the method descried in Annex C and shall not be greater than 100
mg/kg.

Phosphate
Background
The requirement for phosphate has been extended with a
requirement for total phosphate (maximum content of 5% m/m).
Phosphate a compound that is normally present in fly ash from
100% coal in low concentrations; normally below 1% m/m.
Co-combustion of specific co-combustion materials will cause an
increase of the phosphate content, like animal meal, municipal
sewage sludge and solid bio fuels like cacao residues and wheat
husks.
The research data concerning the performance of concrete with
phosphate enriched fly ash is up to about 5% m/m P2O5, originating
from different co-combustion materials.
The assessment involved workability, strength development, freezethaw resistance and chloride permeability.
There were no specific effects identified of phosphate on concrete
performance. Therefore, it is stated that fly ash may contain up to
5.0 % m/m P2O5.

Phosphate
Relation between the content of total phosphate and soluble phosphate
100

min
mean
max
s
n

90
80

soluble P2 O5 in [mg/kg]

total
0,1
0,6
4,3
0,69
209

70

water
soluble
n= 212
0,2
2,7
97
16,3
209

60
50
40
30
20
10
0
0

0,5

1,5

2,5

total P2O5 in [% by mass]

3,5

4,5

Background to the revision of EN 450

Introduction
Overview existing and revised requirements
Generation of fly ash
Modification requirements EN 450-1
Modification requirements EN 450-2
Modification test methods EN 450-1

Modification requirements EN 450-2

In relation to the previous standard, the following
editorial changes have been adapted:
The definition of the management representative has
been modified (4.1.3.2 of the EN 450-2).
A link for the detailed methodology for calculation of
the acceptability constant kA in table 3 of EN 450-1
has been changed (8.2.1 of the EN 450-1).
A requirement for the evaluation of the accuracy of
the autocontrol testing have been adapted (A.3.4 of
Annex of EN 450-2)

Management representative acc.

Text EN 450-2:2005
If the producer is a person authorized by the production plant (see
3.1.15), suitable relations between the producer and the production
plant shall be established and documented in order to ensure that
the requirements of this document are met.

Text EN 450-2:new
The producer shall appoint a management representative who,
irrespective of other responsibilities, shall have defined authority and
responsibility for ensuring that the requirements of this part of this
European standards for the evaluation of conformity are
implemented and maintained.
If the producer is a person authorized by the production plant (see
3.1.15), suitable relations between the producer and the production
plant shall be established and documented in order to ensure that
the requirements of this document are met.

Management representative acc.

Background:
The basic of EN 450-2 was DIN 18990 for conformity evaluation.

As the producer of a fly ash is not necessarily the operator of the

power plant but can also be a marketer as being holder of the
certificate there are two types of management representatives.
The sentence in EN 450-2:2005 reflects the situation that the
producer of the fly ash, i.e. holder of the certificate, is not the
operator of a power plant.
A sentence for the situation that a power producer is the producer
was missing but is absolutely necessary for understanding. Sector
group 02 in its guidance document reflected that situation.
By this problems within the introduction of EN 450 could be abused.
To correct the clause in EN 450-2 the original text from DIN 18990
were placed again.

Statistical evaluation for assessment

procedure by variables
Comparison EN450-1:2005 kA values vs Natrella Approximation

It was agreed that values

for the margins could be
computer using the Natrella
approximation, allowing
compliance monitoring
spreadsheets to be created
and removing the rather
stepped function seen
in the table within EN 450
In conclusion the decisions taken have removed the
main problems associated with statistical compliance for
LOI within EN 450-1. However, it is recommended that
the basis of compliance both within EN 197-1 and
EN 450-1 should be reviewed again in any post 2010
revisions.
1.9

1.8

EN450-1:2005

Value kA

Calculation (Natrella)

1.7

1.6

1.5

1.4

50

100

150

200

Number of results in analysis

250

300

350

400

Evaluation procedure for accuracy of

autocontrol testing
Annex A of EN 450-2 describes the procedures to be
used to evaluate the representativeness and the
accuracy of the fineness test results. The evaluation
shall preferably be made in connection with the routine
yearly inspection by the inspection body. Two
procedures are described:
A.3.3 Evaluation of whether set A and set B belong
to the same population (sampling error check)
A.3.4 Comparison between set B and set C in order
to check the accuracy of the autocontrol testing
(testing error check)
The procedures described in A.3.4. need revision.

Evaluation procedure for accuracy of

autocontrol testing
Text EN 450-2:2005
Set B and set C shall be compared on the basis of the
requirements on the reproducibility specified in EN 451-2.
Text EN 450-2:new
Two conditions should be satisfied:
a) SD 4.5 % by mass
b) [MB MC] 6 %

Background:
In EN 451-2 no requirements on the reproducibility are specified.
By this, the accuracy of autocontrol testing can not be evaluated.
Based on historical data criteria were developed and placed in
A.3.4. of Annex A. .

Background to the revision of EN 450

Introduction
Overview existing and revised requirements
Generation of fly ash
Modification requirements EN 450-1
Modification requirements EN 450-2
Modification test methods EN 450-1

Test methods - Chemical composition

The content of silicon dioxide (SiO2), magnesium
oxide (MgO), aluminium oxide (Al2O3), and iron oxide
(Fe2O3) shall be determined in accordance with EN
196-2, modified as indicated in 5.2.1.
Background:
The new standard EN 196-2 allows using other
methods than the classical chemical methods, namely
X-ray fluorescence analysis (XRF-EN196-2.2). By this,
the use of XRF to determine the oxides by XRF need
no longer to be classified as alternative method with
the proof of equivalent results but can be used directly
as reference method.

Test methods - fineness wet/dry

Text EN 450-1:new, clause 5.3.1
The fineness of fly ash shall be expressed as the mass
proportion in percent of the ash retained when sieved
on a 0,045 mm mesh sieve. The sieving can be
determined in accordance with EN 451-2 or by airjet
sieving according EN 933-10 and shall fall within the
limits of the categories specified below:

Category N: The fineness shall not exceed 40 % by mass, and

it shall not vary by more than 10 percentage points from the
declared value.
Category S: The fineness shall not exceed 12 % by mass. The
10 percentage points fineness.
Note: In case of dispute the wet sieving method shall be used as
reference method.

Evaluation
Due to the regular 5 year revision, WG 4 of CEN TC 104
incorporated the knowledge gained with the fly-ashes
conforming to the ETAs with EN450. All requirements
were subject to critical review. Other issues for the
revision was a lack of clarity regarding the conformity
evaluation. Proposed changes are documented in a
respective background report. This report gives more
detailed insight in the modifications that have taken up in
the new EN 450-1 and EN 450-2.
The revised European standards EN 450-1 and EN 4502 is sent by CEN for a 5 month period of Enquiry and
after the Formal Vote is to be expected to be published
in 2011.

Thank you for your attention

Questions?