CEN EN 12457 Leaching Test: Comparison of Test Results Obtained by Part 1 and 2 With Test Results Obtained by Part 3

TR 539
Approved 2003-10
CEN EN 12457 leaching test:

Comparison of test results obtained by
part 1 and 2 with test results obtained
by part 3
1000000
2-stage batch
Eluate concentration (mg/l)
100000 Single batch
10000
1000
100
10
0 2 4 6 8 10 12 14
L/S (l/kg)
Dorthe Lærke Baun

Jesper Holm
Jette Bjerre Hansen
Margareta Wahlström
Published by Nordtest Phone: + 358 9 455 4600 Fax: + 358 9 455 4272
Tekniikantie 12 E-mail: nordtest@nordtest.org Internet: www.nordtest.org
FIN–02150 Espoo
Finland
NT TECHN REPORT 539
Approved 2003-10
Authors:
Dorthe Lærke Baun1 NORDTEST project number: 1587-02
Jesper Holm1 Institution:
Jette Bjerre Hansen1 1)
DHI Water and Environment, 2) VTT Processes
Margareta Wahlström2
Title (English): -
Title (Original): CEN EN 12457 leaching test: Comparison of test results obtained by part 1
and 2 with test results obtained by part 3
Abstract:
The report compares leaching results obtained by two one-step batch leaching tests (en 12457
part 1 and 2) with leaching results obtained by a two-steps batch-leaching test (EN 12457 part
3). The effect of the used contact time and the effect of using different number of leaching
steps were evaluated. The comparison made in the report was partly based on statistical
evaluations and partly based on the authors profound knowledge of leaching test and hereby
obtained data.
With respect to the contact time it was found that for two of the three test materials the contact
time had no major influence on the leached amount. For the third tested materials the contact
time significantly influenced the leaching of some elements. All in all it was concluded that a
contact time of 24 hours might be preferable in a one-stage leaching test both with respect to
fulfilling the equilibrium assumption and from a practical point of view.
With respect to different number of leaching steps (1 or 2 steps, respectively) it is concluded,
that the number of leaching steps had no major influence on the leached amount.
Nevertheless, when using a relatively high accumulated L/S-ratio as for instance 10 l/kg, it is
still recommended to use a two-stage leaching test, especially for materials which have not
been tested earlier.
Technical Group: Expert Group Environment and Natural Resources

ISSN: 0283-7234 Language: English Pages: 62
Class (UDC): 628.4.06 Key words: EN 12457, leacing tests, materials, statistical
evaluations, waste, analyse, methods
Distributed by: Publication code:
NORDTEST
Tekniikantie 12
FIN-02150 ESPOO Report Internet address:
Finland http://www.nordtest.org/register/techn/tlibrary/tec539.pdf
CONTENTS
PREFACE ...................................................................................................................................4
SUMMARY..................................................................................................................................5
1 INTRODUCTION ...........................................................................................................6
1.1 Background ...................................................................................................................6
1.2 Objective .......................................................................................................................6
2 THEORETICAL ASPECTS OF LEACHING ...................................................................7
3 EXPERIMENTAL WORK AND OBTAINED RESULTS ..................................................9

3.1 Experimental work .........................................................................................................9
3.1.1 Test materials................................................................................................................9
3.1.2 One-stage batch leaching test (EN 12457 part 1 and 2) ................................................9
3.1.3 Two-stage batch leaching test (EN 12457 part 3) ..........................................................9
3.1.4 Analytical parameters ..................................................................................................10
3.2 Results ........................................................................................................................10
3.2.1 Test material 1 (stabilised fly ash) ...............................................................................10
3.2.2 Test material 2 (aged bottom ash from a MSW-incinerator plant) ................................10
3.2.3 Test material 3 (wood and peat ash) ...........................................................................10
4 DESCRIPTION OF USED STATISTICAL TOOLS .......................................................14

4.1 Grubb’s test.................................................................................................................14
4.2 F-test ...........................................................................................................................15
4.3 Students T-test ............................................................................................................15
5 RESULTS AND DISCUSSIONS OF THE STATISTICAL ANALYSES .........................17

5.1 Grubb’s test.................................................................................................................17
5.2 Student’s T-test ...........................................................................................................18
5.2.1 Comparison of contact time .........................................................................................22
5.2.2 Comparison of one- and two-stage batch leaching test ...............................................23
6 CONCLUSIONS AND RECOMMENDATIONS ............................................................25
7 REFERENCES............................................................................................................26
APPENDICES
A Analytical reports from Analytica AB

B Dataset used for the student’s T-test
Nordtest Technical Report 539 3

PREFACE
This report is the result of the Nordtest Project No. 1587-02 “Comparison of leaching
test results from prEN 12457-1,2 with test results from prEN 12457-3” carried out
under the leadership of DHI, Denmark.
The objective of the project has been to compare leaching results obtained by two one-
step batch leaching tests (en 12457 part 1 and 2) with leaching results obtained by a
batch-leaching test including two steps (EN 12457 part 3).
The authors of the report have been Dorthe Lærke Baun, Jesper Holm, and Jette Bjerre
Hansen, DHI, Denmark and Margareta Wahlström, VTT, Finland.
4 Nordtest Technical Report 539

SUMMARY
This report compares leaching results obtained by two one-step batch leaching tests (en
12457 part 1 and 2) with leaching results obtained by a batch-leaching test including
two steps (EN 12457 part 3). Almost no comparisons exist of batch leaching test
including one and two steps, respectively, and this report is intended to support such
comparison. The comparison made in this report was partly based on statistical
evaluations and partly based on our profound knowledge to leaching test and hereby
obtained data.
On three different test materials (stabilised fly ash, aged bottom ash, and wood and peat
ash) five replicates of each of the batch leaching tests EN 12457 part 1-3 were
performed. The obtained results with five replicates of each sample showed good
reproducibility. Statistical outliers and stragglers were identified by the Grubb’s test and
from only 5 % of all the obtained dataset a value was excluded from further statistical
analyses.
The comparison of the leaching results was made by students T-test. By this test the
influence on the contact time and the number of leaching stage was tested.
The student’s T-test only showed statistical significant different leaching for few
elements when using different contact time (6 and 24 hours, respectively). However, it
was concluded that a contact time of 24 hours still might be preferable in a one-stage
leaching test both with respect to fulfilling the equilibrium assumption and from a
practical point of view.
When using different number of leaching steps (1 or 2 steps, respectively), the students
T-test showed significantly different leaching for few elements. For these elements the
leached amounts when using the two-stage test was generally higher than or equal to the
leached amount when using the one-stage test. However, the number of compounds for
which the leaching was considerably higher was modest, and it is concluded that the
number of leaching steps had no major influence on the leached amount. Nevertheless,
when using a relatively high accumulated L/S-ratio as for instance 10 l/kg, it is still
recommended to use a two-stage leaching test, especially for materials which have not
been tested earlier.

1 INTRODUCTION
1.1 Background
The Nordic countries have been strongly involved in the development and
standardisation of the batch leaching test CEN EN 12457 (CEN, 2002), especially part
3, which includes two leaching steps at liquid-to-solid ratios (L/S) of 0-2 l/kg and 2-10
l/kg, respectively. Part 3 is also a part of the Nordtest-method ENVIR 005 (Nordtest,
1998), which also contain CEN EN 12457 part 1, that includes only one leaching step at
L/S 2 l/kg. Furthermore, CEN EN 12457 part 3 is already incorporated in the legislation
of some of the Nordic countries. The participation of the Nordic countries in the CEN-
work concerning the batch leaching test have been partly financed by Nordtest through
a number of activities and projects in the period 1993-1995.
The batch leaching test EN 12457 consists of 4 parts:
1. EN 12457-1: Performed at L/S 2 l/kg on material < 4 mm (1 step)
3. EN 12457-3: Performed at L/S 2 l/kg and L/S 8 l/kg on material < 4 mm (2 step)
In CEN/TC 292 EN 12457 have been discussed extensively, especially the fact that the
standard contains 4 different parts. Many countries prefer a one-stage batch leaching
test (like part 1, 2, and 4), whereas the Nordic countries see the two-step method (part 3)
as the method that will give results closest to the results that can be expected at field
conditions. Today, almost no comparisons exist of batch leaching test including one and
two steps, respectively. Therefore, there is a pronounced need for data, which can
support such comparison.
1.2 Objective
The objectives of the project has been to compare leaching results obtained by two one-
step batch leaching tests (en 12457 part 1 and 2) with leaching results obtained by a
batch-leaching test including two steps (EN 12457 part 3). Five replicates of each
leaching test were produced.

2 THEORETICAL ASPECTS OF LEACHING
When put into contact with a liquid, many solid materials to some extent will dissolve
and it is the degree of this dissolution in the contacting liquid that governs the relative
strength of the leachate that is produced (Chandler et al., 1997). There are a number of
factors including both physical and chemical aspects that can influence the rate at which
the solid materials dissolve.
The physical aspects influencing the leaching relate to the manner of contact between
the liquid and the solid material. A general assumption, that is related to the physical
aspects when performing batch leaching test is the local equilibrium assumption.
However, this assumption is closely related to the contact time and implies a sufficient
contact time. An L/S-ratio of 2 l/kg is used both in the batch leaching test EN 12457
part 1 and in the first step of the batch leaching test EN 12457 part 3. In the former a
contact time of 24 hours is used, whereas in the latter a contact time of 6 hours is used.
If the local equilibrium assumption is fulfilled when using both 6 and 24 hours as
contact time, the same leaching results are expected to be obtained and the applied
contact time is then of no importance.
Chemical aspects influencing the leaching relate to the fundamental processes

controlling the solubility of solids. These include:
− the influence of pH on controlling the solubility
− the influence of dissolved-phase complexing agents, that increase the dissolution
− the role of oxidation-reduction potential in increasing solubilisation
Chemical aspects can also include reprecipitation or sorption processes, whereby

dissolved constituents return to the solid phase.
The leaching of solubility-controlled elements might be dependent on the number of

leaching steps used during a batch-leaching test. In a single batch leaching test the L/S
describes the ratio between the volume of leachant added to a certain (dry) mass of solid
material. In a one-stage leaching test (like EN 12457 part 1 and 2) no removal of
leached substances will obviously take place during the test. In serial batch leaching
tests the L/S-ratio increases stepwise each time the leachant is renewed, and serial batch
leaching tests (like the two-stage test EN 12457 part 3) include removal of leached
substances after each stage. Serial batch leaching tests are expected to give results that
more resemble results obtained under field conditions than when using only one
leaching stage. Especially the risk of underestimating the leaching of solubility-
controlled elements is expected to be larger when using a one-step leaching test like EN
124547 part 2 than when using serial batch leaching test like EN 12457 part 3.
The difference between a one- and a two-stage batch-leaching test is illustrated in

Figure 2.1. The figure shows the results of a single batch leaching test performed at an
L/S-ratio of 10 l/kg and a 2-stage serial batch leaching test performed first at L/S = 2
l/kg and then at L/S = 8 l/kg, bringing the accumulated L/S to 10 l/kg as in the single
batch leaching test. The results are presented as eluate concentrations as a function of

the L/S-ratio. From Figure 2.1 it can be seen that the single batch leaching test
performed at L/S 10 l/kg provides only one average value whereas the two-stage test
gives averages for the L/S-ranges 0-2 l/kg and 2-10 l/kg.
1000000
2-stage batch
Eluate concentration (mg/l)
100000 Single batch
10000
1000
100
10
0 2 4 6 8 10 12 14
L/S (l/kg)
Figure 2-1 The results of a single batch leaching test performed at L/S 10 l/kg and
a serial batch leaching test performed at L/S 0-2 and 2-10 l/kg. Both
test were performed on MSWI fly ash, and the results show eluate
concentrations of chloride as a function of L/S. Note that the scale on
the ordinate axis is logarithmic.

3 EXPERIMENTAL WORK AND OBTAINED RESULTS
3.1 Experimental work
3.1.1 Test materials

For the conducted experiments three different solid test materials were used:
Test material 1: Stabilised fly ash from a municipal solid waste (MSW)
incinerator plant. The fly ash was stabilised with the VKI-
process (Hjelmar et al., 2001)
Test material 2: Aged bottom ash from a MSW-incinerator plant
Test material 3: Wood and peat ash (Wahlström et al 2001)
The batch leaching tests were performed in 5 replicates on all three solid test materials,
a total of 45 batch leaching tests.
The batch leaching tests on test material 1 and 2 were carried out at DHI, Hørsholm,
Denmark, whereas the batch leaching tests on test material 3 were carried out at VTT,
Espoo, Finland. The pH and the specific conductivity at 25 °C of the eluates were
determined at the laboratories, where the leaching tests were performed. All other
chemical analyses of the eluates were made at Analytica AB, Luleå, Sweden.
3.1.2 One-stage batch leaching test (EN 12457 part 1 and 2)

The batch leaching tests were performed with demineralised water on material with a
particle size < 4 mm and at an L/S-ratio of 2 l/kg (EN 12457 part 1) or 10 l/kg (EN
12457 part 2). In both the one-stage batch leaching tests the contact time between the
solid material and the leachant was 24 hours. After the leaching test the eluate was
filtrated through a 0.45 µm filter and analysed for a wide range of parameters (se
chapter 3.1.4).
3.1.3 Two-stage batch leaching test (EN 12457 part 3)

The batch leaching tests were performed with demineralised water on material with a
particle size < 4 mm and at an L/S-ratio of 2 l/kg followed by an L/S-ratio of 8 l/kg
which corresponded to an accumulated L/S-ratio of 10 l/kg (EN 12457 part 3). In the
first leaching step (L/S 2 l/kg) the contact time was 6 hours and in the second leaching
step (L/S 8 l/kg) the contact time was 18 hours corresponding to a total contact time
between the solid material and the leachant of 24 hours. After the leaching test the
eluates were filtrated through a 0.45 µm filter and analysed for a wide range of
parameters (se chapter 3.1.4).

3.1.4 Analytical parameters
For each test material 20 eluates were obtained. These in total 60 eluates were analysed
for a broad spectrum of parameter. All the eluates were analysed for pH, specific
conductivity (determined at 25 °C), Ca, K, Na, Ba, Cl, SO4, and TOC. The eluates
obtained from test material 1 and 2 were, furthermore, analysed for Mg, As, Cd, Cr, Cu,
Ni, Pb, and Zn. The eluates obtained from test material 3 were, furthermore, analysed
for Al and Mo.
3.2 Results
The results obtained when analysing the eluates are shown in Table 3-1 to Table 3-3.
The analytical reports from Analytica AB are shown in appendix A.
3.2.1 Test material 1 (stabilised fly ash)

The test material 1 was alkaline due to the high content of lime in the stabilised fly ash.
Generally the results of the leaching tests were in accordance with previous test results
on the same type of material showing very limited leaching of trace elements (Hjelmar
et al., 2001).
3.2.2 Test material 2 (aged bottom ash from a MSW-incinerator plant)

The pH of the test material 2 was almost neutral (pH 8-9) which was due to the ageing
and consequently carbonation of the bottom ash. The obtained leaching results were
generally in accordance with previous investigations of bottom ash from MSW-
incinerator plant.
3.2.3 Test material 3 (wood and peat ash)

The test material 3 was alkaline due to the high content of calcium oxide. The pH values
in the eluates from the second leaching step in the two step procedure (EN12457-3)
were lower than for the other collected eluates. This is probably due to the leaching of
Ca in the first leaching step, but probably also due to carbonation of the test sample
during the filtration process and sample handling.
The results from the leaching test were in accordance with previous test results obtained
at VTT. The test results for Al has also in previous studies shown significant variations
probably due to small concentrations and unstability of Al. The leached amounts of
TOC, SO4 and Cl were also low.
In the test interpretation special attention needs to be paid to Ca and Ba, which might
precipitate in the eluates before analysis.

11
Table 3-1 The accumulated leached amount during the performed leaching tests on test material 1 (stabilised fly ash). The unit of the
specific conductivity (25 °C) is mS/m, pH is without unit, and the unit of all other elements are in mg/kg TS.
Cl SO4 Ca K Mg Na As Ba Cd Cr Cu Ni Pb Zn DOC pH Spec.
cond.
L/S 2 l/kg, 24 hours (EN 12457 part 1)
Replicate 1 1700 4400 1456 754 < 1.8 1160 < 0.01 0.0902 < 0.001 0.748 < 0.002 < 0.001 0.0102 0.0160 9.80 10.3 618
Replicate 2 1740 4400 1480 770 < 1.8 1184 < 0.01 0.0878 < 0.001 0.758 < 0.002 < 0.001 0.00950 0.0139 8.00 10.4 624
Replicate 3 1680 4200 1482 752 < 1.8 1156 < 0.01 0.0870 < 0.001 0.762 < 0.002 < 0.001 0.00960 0.0130 6.80 10.4 617
Replicate 4 1860 4800 1480 748 < 1.8 1152 < 0.01 0.0900 < 0.001 0.772 < 0.002 < 0.001 0.00960 0.0130 5.80 10.4 615
Replicate 5 1700 4400 1476 752 < 1.8 1156 < 0.01 0.0892 < 0.001 0.754 < 0.002 < 0.001 0.00976 0.0125 7.00 10.4 615
Average 1736 4440 1475 755 < 1.8 1162 < 0.01 0.0888 < 0.001 0.759 < 0.002 < 0.001 0.00972 0.0136 7.48 10.4 618
Nordtest Technical Report 539

L/S 10 l/kg, 1 stage (EN 12457 part 2)
Replicate 1 1597 16966 6966 928 <9 1228 < 0.02 0.435 < 0.002 0.924 < 0.01 <0.005 0.0397 0.0788 17.0 10.2 317
Replicate 2 1597 16966 7066 925 <9 1218 < 0.02 0.438 < 0.002 0.907 < 0.01 < 0.005 0.0425 0.0700 16.0 10.4 319
Replicate 3 1590 16898 6888 923 <9 1223 < 0.02 0.432 < 0.002 0.941 < 0.01 < 0.005 0.0411 0.0779 18.9 10.4 317
Replicate 4 1597 16966 6966 926 <9 1228 < 0.02 0.435 < 0.002 0.921 < 0.01 < 0.005 0.0451 0.137 16.0 10.4 316
Replicate 5 1695 17946 7049 916 <9 1226 < 0.02 0.426 < 0.001 0.918 < 0.01 < 0.005 0.0408 0.0753 18.9 10.4 317
Average 1615 17148 6987 924 <9 1224 < 0.02 0.433 < 0.002 0.922 < 0.01 < 0.005 0.0418 0.0877 17.3 10.4 317
L/S 2 l/kg, 6 hours (EN 12457 part 3, stage 1)
Replicate 1 1740 4400 1482 748 < 1.8 1154 < 0.01 0.0896 < 0.001 0.742 < 0.002 < 0.001 0.00902 0.0218 8.00 10.2 610
Replicate 2 1680 4410 1571 754 < 1.9 1147 < 0.01 0.0930 < 0.001 0.729 < 0.002 < 0.001 0.0106 0.0150 6.72 10.4 593
Replicate 3 1739 4554 1513 758 < 1.9 1159 < 0.01 0.0911 < 0.001 0.722 < 0.002 < 0.001 0.0104 0.0139 5.59 10.5 598
Replicate 4 1720 4400 1460 746 < 1.8 1148 < 0.01 0.0854 < 0.001 0.708 < 0.002 < 0.001 0.00978 0.0152 6.00 10.4 607
Replicate 5 1742 4730 1578 763 < 1.9 1163 < 0.01 0.0957 < 0.001 0.746 < 0.002 < 0.001 0.0112 0.0151 7.31 10.4 584
Average 1724 4499 1521 754 < 1.9 1154 < 0.01 0.0910 < 0.001 0.729 < 0.002 < 0.001 0.0102 0.0162 6.72 10.4 598
L/S 2+8 l/kg, 2 stage (EN 12457 part 3)
Replicate 1 1756 17484 7043 989 <9 1286 < 0.02 0.433 < 0.002 1.03 < 0.01 < 0.005 0.0421 0.0931 18.5 10.2 284
Replicate 2 1713 17625 7080 982 <9 1268 < 0.02 0.439 < 0.002 0.991 < 0.01 < 0.005 0.0427 0.110 23.4 10.4 283
Replicate 3 1761 17701 7085 993 <9 1283 < 0.02 0.433 < 0.002 1.03 < 0.01 < 0.005 0.0429 0.0763 22.7 10.4 284
Replicate 4 1724 17526 6981 978 <9 1263 < 0.02 0.436 < 0.002 1.00 < 0.01 < 0.005 0.0438 0.0923 23.7 10.4 283
Replicate 5 1748 17848 7150 995 <9 1291 < 0.02 0.445 < 0.002 1.04 < 0.01 < 0.005 0.0440 0.0834 23.7 10.5 283
Average 1741 17637 7068 987 <9 1278 < 0.02 0.437 < 0.002 1.02 < 0.01 < 0.005 0.0431 0.0911 22.4 10.4 283
12
Table 3-2 The accumulated leached amount during the performed leaching tests on test material 2 (bottom ash). The unit of the
specific conductivity is (25 °C) mS/m, pH is without unit, and the unit of all other elements are in mg/kg TS.
Cl SO4 Ca K Mg Na As Ba Cd Cr Cu Ni Pb Zn DOC pH Spec.
cond.
Replicate 1 760 5000 1242 120.8 62.6 1396 < 0.005 0.0848 < 0.0002 0.00276 0.276 0.00830 0.00175 0.0222 24.0 8.40 517
Replicate 2 720 5000 1234 114.8 58.6 1334 < 0.005 0.0880 < 0.0004 0.00161 0.270 0.00810 0.00167 0.0174 22.0 8.49 497
Replicate 3 720 5000 1236 114.4 57.0 1306 < 0.004 0.0862 < 0.0002 0.00169 0.272 0.00746 0.00128 0.0156 22.0 8.22 492
Replicate 4 704 4824 1248 113.8 56.3 1282 < 0.004 0.0854 < 0.0002 0.00336 0.269 0.00704 0.00281 0.0182 24.1 8.55 485
Replicate 5 700 4800 1300 110.0 54.0 1300 < 0.004 0.0860 < 0.0001 0.00170 0.300 0.00770 0.00094 0.0130 22.0 8.55 489
Average 721 4925 1252 114.8 57.7 1324 < 0.004 0.0861 < 0.0002 0.00222 0.277 0.00772 0.00169 0.0173 22.8 8.44 496

Replicate 1 721 6814 2094 153.3 69.9 1393 < 0.001 0.424 < 0.0001 0.00759 0.424 0.0102 0.00215 0.0280 49.1 8.60 154
Replicate 2 709 6587 1946 145.7 65.7 1307 < 0.001 0.414 < 0.0001 0.00550 0.430 0.0145 0.00236 0.0276 34.9 8.70 152
Replicate 3 739 7193 2218 162.8 73.1 1479 < 0.001 0.442 < 0.0001 0.00958 0.462 0.0092 < 0.002 0.0240 42.0 8.80 160
Replicate 4 844 7845 2443 182.7 86.6 1718 0.00214 0.379 < 0.0001 0.00860 0.451 0.0136 0.00208 0.0225 41.7 8.70 179
Replicate 5 737 6972 2201 160.4 73.1 1464 0.00202 0.434 0.000132 0.0185 0.491 0.0318 0.0264 0.280 n.m. 8.80 159
Average 750 7082 2180 161.0 73.7 1472 < 0.0014 0.419 < 0.0001 0.00996 0.451 0.0159 0.00825 0.0764 41.9 8.72 161

Replicate 1 700 4600 1198 107.4 49.0 1268 < 0.005 0.0802 < 0.0001 0.00148 0.318 0.0100 0.00193 0.0228 28.0 8.36 477
Replicate 2 680 4600 1214 108.4 49.6 1286 < 0.005 0.0776 < 0.0001 0.00270 0.324 0.00848 0.00104 0.0142 28.0 8.50 481
Replicate 3 640 4400 1158 102.4 45.4 1188 < 0.004 0.0818 < 0.0002 0.00292 0.330 0.00944 0.0196 0.0620 26.0 8.54 461
Replicate 4 680 4600 1142 108.0 48.2 1258 < 0.004 0.0778 < 0.0001 0.00220 0.314 0.00870 0.000780 0.0132 26.0 8.56 473

Replicate 5 700 4600 1154 111.8 51.2 1318 < 0.004 0.0756 < 0.0001 0.00272 0.306 0.00914 0.000982 0.0120 26.0 8.54 487
Average 680 4560 1173 107.6 48.7 1264 < 0.004 0.0786 < 0.0001 0.00240 0.318 0.00916 0.00487 0.0248 26.8 8.50 476

Replicate 1 735 6957 2124 166.0 78.1 1491 < 0.01 0.442 < 0.0005 < 0.005 0.497 0.0148 0.00359 0.0412 48.7 8.43 80.0
Replicate 2 712 7223 2242 166.5 78.6 1504 < 0.01 0.436 < 0.0005 0.0105 0.512 < 0.01 0.00330 0.0339 45.5 8.75 84.0
Replicate 3 674 6926 2172 157.5 72.5 1389 < 0.01 0.436 < 0.0005 < 0.007 0.497 0.0135 < 0.002 0.0744 47.3 8.84 79.0
Replicate 4 713 7003 2122 165.3 76.2 1468 < 0.01 0.454 < 0.0005 0.00803 0.496 < 0.01 < 0.002 0.0236 42.3 8.86 80.0
Replicate 5 731 7460 2282 171.7 82.4 1543 < 0.01 0.436 < 0.0005 0.0116 0.494 0.0141 < 0.002 0.0337 84.7 8.86 86.0
Average 713 7114 2188 165.4 77.6 1479 < 0.01 0.441 < 0.0005 0.01003 0.499 0.0141 0.00344 0.0414 53.7 8.75 81.8
n.m.: not measured
13
Table 3-3 The accumulated leached amount during the performed leaching tests on test material 3 (VTT-reference material). The unit
of the specific conductivity (25°C) is mS/m, pH is without unit, and the unit of all other elements are in mg/kg TS.
Cl SO4 Al Ca K Na Ba Mo DOC pH Spec.cond.
Replicate 1 138 560 2.60 948 678 450 35.4 1.84 3.80 12.4 758
Replicate 2 182 40.0 2.62 940 658 442 34.4 1.74 3.20 12.4 758
Replicate 3 100 50.0 2.64 958 670 450 34.8 1.77 2.40 12.4 783
Replicate 4 98.0 50.0 2.24 906 654 444 34.8 1.66 1.08 12.5 785
Replicate 5 94.0 19.8 1.76 896 668 448 36.4 1.71 2.60 12.4 761
Average 122 144 2.37 930 666 447 35.2 1.75 2.62 12.4 769

Replicate 1 170 < 50 32.4 4680 676 455 74.8 4.36 <5 12.3 507
Replicate 2 132 < 51 29.0 4881 697 467 76.8 4.62 6.99 12.3 526
Replicate 3 160 < 50 30.7 4711 698 471 75.0 4.56 n.m. 12.3 516
Replicate 4 150 < 50 35.7 4440 690 465 74.3 4.45 9.40 12.3 497
Replicate 5 140 < 50 41.2 4280 657 444 71.2 4.47 11.0 12.3 481
Average 150 < 50 33.8 4598 684 460 74.4 4.49 9.13 12.3 505
Replicate 1 154 186 0.0680 1422 606 412 3.80 7.32 3.20 12.5 907
Replicate 2 158 108 0.113 1354 642 436 5.66 6.36 3.60 12.5 913
Replicate 3 144 260 0.0564 1484 634 428 3.00 8.88 2.60 12.5 942
Replicate 4 148 260 0.268 1548 616 418 2.82 8.54 1.54 12.5 921
Replicate 5 172 48.0 0.382 1362 590 410 10.4 4.24 1.94 12.5 916
Average 155 172.4 0.177 1434 618 421 5.14 7.07 2.58 12.5 920
Replicate 1 185 < 180 77.7 4170 654 444 63.9 7.72 <7 12.2 372
Replicate 2 176 < 120 66.0 4228 691 468 67.8 7.07 8.50 12.2 395
Replicate 3 170 < 240 59.9 4532 688 464 69.6 8.94 10.5 12.2 411
Replicate 4 192 < 250 70.8 4388 661 448 65.6 8.82 <5 12.2 379
Replicate 5 211 < 80 117 3713 640 443 58.2 6.00 8.17 12.2 327
Average 187 < 170 78.4 4206 667 453 65.0 7.71 9.05 12.2 377
n.m.: not measured
4 DESCRIPTION OF USED STATISTICAL TOOLS
The obtained data have been evaluated statistically by Grubb’s test, F-test, and student’s
T-test.
4.1 Grubb’s test

The results were checked for single data points amongst the five replicates that seemed
to differ significantly from the other replicates. As a first step, the analytical laboratory
was asked to double-check the results of the deviant analysis. However, no laboratory
errors were discovered. Subsequently, the data was analysed for outliers (data that
deviate so much from the comparable data in the same set of data that they are
considered irreconcilable with the other data). Outliers were identified using a statistical
method called Grubbs’ test (ISO 5725-2:1994) which is a numerical technique.
By the Grubbs’ test a potentially outlying observation can be identified as either a

straggler or a statistical outlier. Given a set of data Xi for i= 1,2,....p, arranged in
ascending order, then to determine whether the largest or smallest observation is an
outlier using the Grubbs’s statistic, G1 must be computed:
x − x1
G1 =
s
where G1 : the Grubb’s test statistic

x : the average value of the five (n) replicates
x1 : the potential outlying value
s : the standard deviation of the five (n) replicates
a) If the test statistic is less than or equal to its 5% critical value, the item tested is
accepted as correct.
b) If the test statistic is greater than its 5% critical value and less than or equal to its
1% critical value, the item tested is called a stranggler and is indicated by a single
asterisk.
c) If the test statistic is greater than its 1% critical value, the item is called a statistical
outlier and is indicated by a double asterisk.
Grubbs’ test was performed on the results to check if any data points should be
identified as strangglers or outliers. The 1 and 5 % critical value is tabulated in ISO
5725-2 (1994).
In the present study, it was determined that if the test statistic of potentially outlying
results was above the 5 % critical value, the result would be excluded from further
statistical analysis.

Furthermore, elements for which at least 4 of the 5 replicates returned values below
detection limit were excluded from the statistical analysis.
The full data set can be seen in chapter 3, whereas the data set used for statistical
analyses (without the excluded values) is shown in appendix B.
4.2 F-test
An initial statistical analysis on the obtained leaching data was performed using the F-
test (Montgomery, 1991). By the F-test it is possible to determine whether two datasets
have significantly different variances.
S12
Fn1 −1, n2 −1 =
S 22
where Fn1 −1, n2 −1 : the F-test statistic

S12, S22: the two individual sample variances
The outcome of the F-test will result in one of the following results:
− the hypothesis that the two tested variances are equal is accepted on a 95 %
significance level
− the hypothesis that the two tested variances are equal is rejected on a 95 %
significance level
To determine whether to reject the mentioned hypothesis, the obtained F-test statistic
(Fn1-1, n2-1) are compared to the F-distribution with 4, 4 (n1-1, n2-1) degrees of freedom.
If the F-test statistic (Fn1-1, n2-1) is larger than the actual F-distribution on a 95 %
significant level the tested hypothesis is rejected, which imply that the two tested
variances differ.
If the two tested variances differ on a 95 % significant level, the subsequent T-test were
performed by assuming unequal variances, whereas if the two tested variances were
equal on a 95 % significant level, the subsequent T-test were performed by assuming
equal variances.
4.3 Students T-test

A statistical analysis on the obtained leaching data was performed using the student’s T-
test (Montgomery, 1991) on each test material separately.
When using the students T-test, two hypothesis were tested:
− do the results from the L/S = 2 l/kg test with a contact time of 24 hours differ from
the results from the L/S=2 l/kg test with a contact time of 6 hours ?

− do the results from the L/S = 10 l/kg two-stage test differ from the results from the
L/S=10 l/kg one-stage test ?
By the students T-test each of the two hypothesis were tested in a completely
randomised design. Two different test-designs were used depending on the result of the
F-test. If it could be assumed that variances were equal (σ12 = σ22 = σ2) the following
test design was used:
y1 − y 2
t0 =
1 1
Sp +
n1 n 2
where t0: the T-test statistic

y1 , y 2 : the sample means
n1, n2: the amount of replicates (here n1 = n2 = 5)
Sp2: an estimate of the common variance σ12 = σ22 = σ2
The common variance was computed from:
(n1 − 1) ⋅ S12 + (n2 − 1) ⋅ S 22

S =
2
p
n1 + n2 − 2
where S12, S22: the two individual sample variances
If it could not reasonably be assumed that the variances σ12 and σ22 were equal, then the
two-sample t-test had to be modified slightly. The test statistic becomes then:
y1 − y 2
t0 =
S12 S 22
+
n1 n 2
The outcome of the student’s T-test will result in one of the following results:
− the hypothesis that the two tested means are equal is accepted on a 95 %
significance level
− the hypothesis that the two tested means are equal is rejected on a 95 % significance
level
To determine whether to reject the mentioned hypothesis, the obtained T-test statistic
(t0) are compared to the t distribution with 8 (n1 + n2 – 2) degrees of freedom. If the T-
test statistic (t0) is larger than the actual t distribution on a 95 % significance level the
tested hypothesis is rejected, which imply that the two tested mean values differ.
The outcome of the T-test is shown in the chapter 5.2 and the dataset used for the
student’s T-test can be found in appendix B.

5 RESULTS AND DISCUSSIONS OF THE STATISTICAL
ANALYSES
5.1 Grubb’s test

In Table 5-1 the dataset for which Grubb’s test were performed and the obtained results
are shown.
Table 5-1 The reult of the Grubb’s test
Sample and element x1 x12 s3 G1 4 Result of

(mg/kg TS) (mg/kg TS) Grubb’s test
Test material 2, L/S 2 l/kg, 6 hours (EN 12457 part 3, stage 1)

Pb 0.00487 0.0196 0.0083 1.79 Outlier
Zn 0.0248 0.0620 0.021 1.75 Straggler
Test material 2, L/S 2+8 l/kg, 2 stage (EN 12457 part 3)

TOC 53.7 84.7 17 1.77 Outlier
Test material 2, L/S 10 l/kg, 1 stage (EN 12457 part 2)

Ni 0.0158 0.0318 0.0092 1.74 Straggler
Pb 0.00660 0.0264 0.011 1.78 Outlier
Zn 0.0764 0.280 0.11 1.79 Outlier
Test material 3, L/S 2 l/kg, 6 hours (EN 12457 part 3, stage 1)

SO4 (all replicates) 172 48 94 1.3 Accepted
Test material 3, L/S 2 l/kg 24 hours (EN 12457 part 1)

SO4 (all replicates) 144 560 230 1.79 Outlier
SO4 (without replicate 5) 40.0 19.8 14 1.42 Accepted
1
x : the average value of the five replicates
2
x1: the potential outlying value
3
s: the standard deviation of the five replicates
4
G1: the Grubb’s test statistic
Among the results obtained only nine potential outliers were identified (Table 5-1).
Performing Grubb’s test on these eight datasets resulted in five statistical outliers, two
statistical stragglers, and two accepted values. The five outliers and the two stragglers
were excluded from the student’s T-test.
The student’s T-test could potentially have been performed on 168 complete dataset
each consisting of five replicates. 29 of these dataset were excluded since at least four of
the five replicates for a specific element gave values below the detection limit. In the
remaining 139 complete dataset additional seven dataset or 5 % have one replicate
excluded due to the result of the Grubb’s test. This small number (5 %) shows that the
agreement between the five replicates of each leaching test generally was very good.

5.2 Student’s T-test
The results of the student’s T-test are given in Table 5-2 to 5-4. The dataset used for the
student’s T-test are given in appendix B. The three test materials were tested separately.
In case of a positive test outcome, which means that the two compared leaching tests
differ on a 95 % significance level, the difference in the mean values (in percentage) for
the replicates in the two leaching tests is shown. If the number is positive the 24 hour
leaching test at L/S 2 l/kg or the two-stage leaching test, respectively, have a
significantly larger average value than the 6 hours leaching test at L/S 2 l/kg or the one-
stage leaching test at L/S 10 l/kg. If the difference in the average values is negative the
opposite is the case. “Alike” indicates that there is no statistically significant difference
for the particular elements in the mean values of the two leaching tests that are
compared.

19
Table 5-2 The result of student’s T-test on test material 1 (stabilised fly ash).
Cl SO4 Ca K Na Ba Cr Pb Zn DOC pH Specific
mg/kg mg/kg mg/kg mg/kg mg/kg mg/kg mg/kg mg/kg mg/kg mg/kg cond.
(25°C)
mS/m
L/S 2 l/kg 24 hours (EN 12457 part 1)
Average 1740 4440 1470 755 1160 0.0888 0.759 0.00972 0.0137 7.48 10.4 618
Standard deviation 73 220 11 8.6 13 0.0014 0.0090 0.00026 0.0014 1.5 0.019 4.3
Relative standard deviation (%) 4.2 4.9 0.73 1.1 1.1 1.6 1.2 2.7 10 20 0,18 0,69

Average 1720 4500 1520 754 1150 0.0910 0.729 0.0102 0.0162 6.72 10.4 598
Standard deviation 26 15 53 7.0 7.1 0.0039 0.015 0.00083 0.0032 0.97 0.12 11
Relative standard deviation (%) 1.5 3.2 3.5 0.93 0.62 4.2 2.1 8.1 20 14 1,2 1,8
t0 0.74 0.63 0.091 0.78 0.29 0.28 0.0062 0.25 0.14 0.38 0.86 0.0047
Test result on a 95 %
1 alike alike alike alike alike alike 4.03 alike alike alike alike 3.23
significance level
Average 1740 17600 7070 987 1280 0.437 1.02 0.0431 0.0911 22.4 - -
Standard deviation 21 150 62 7.5 12 0.0049 0.022 0.00078 0.013 2.2 - -
Relative standard deviation (%) 1.2 0.82 0.88 0.76 0.94 1.1 2.1 1.8 14 9.9 - -
Average 1620 17100 6990 924 1220 0.433 0.922 0.0418 0.0877 17.3 - -
Standard deviation 45 450 72 4.6 4.3 0.0047 0.012 0.0021 0.028 1.5 - -
Relative standard deviation (%) 2.8 2.6 1.0 0.49 0.35 1.1 1.3 5.0 31 8.6 - -
-4 -7 -5 -5
t0 4.6·10 0.049 0.093 2.1·10 1.3·10 0.22 2.5·10 0.24 0.81 0.0029 - -
2 7.8 2.9 alike 6.9 4.4 alike 10 alike alike 29 - -
significance level
1
: Positive values indicate that the results of the 24 hour leaching test at L/S 2 l/kg are larger on a 95 % significant level than the results of the 6 hours leaching test at L/S 2 l/kg.
Negative values indicate the opposite case. The number shows the difference between the two mean values in percentage.
2
: Positive values indicate that the results of the two-stage leaching test at L/Stotal 10 l/kg are larger on a 95 % significant level than the results of the 1-stage leaching test at L/S
10 l/kg. Negative values indicate the opposite case. The number shows the difference between the two mean values in percentage.
20
Table 5-3 The result of student’s T-test on test material 2 (bottom ash).
Cl SO4 Ca K Mg Na Ba Cr Cu Ni Pb Zn DOC pH Specific
mg/kg mg/kg mg/kg mg/kg mg/kg mg/kg mg/kg mg/kg mg/kg mg/kg mg/kg mg/kg mg/kg cond.
(25°C)
mS/m
Average 721 4920 1250 115 57.7 1320 0.0861 0.00222 0.277 0.00772 0.00169 0.0173 22.8 8.44 496
Standard deviation 24 100 27 3.9 3.2 44 0.0012 0.00079 0.013 0.00050 0.00071 0.0037 1.1 0.14 13
Rel. stand. deviation (%) 3.3 2.1 2.2 3.4 5.6 3.4 1.4 36 4.6 6.5 42 20 4.9 1.6 2.5
Average 680 4560 1170 108 48.7 1260 0.0786 0.00240 0.318 0.00916 0.00118 0.0156 26.8 8.50 476
Standard deviation 24 89 31 3.4 2.1 48 0.0024 0.00058 0.0092 0.00061 0.00051 0.00492 1.1 0.081 9.8
Rel. stand. deviation (%) 3.6 2.0 2.6 3.1 4.3 3.8 3.1 24 2.9 6.7 43 32 4.1 0.96 2.1
t0 0.029 0.00033 0.0028 0.014 0.00079 0.074 0.00026 0.69 0.00041 0.0037 0.27 0.55 0.00048 0.44 0.022
1 6.0 8.0 6.7 6.7 19 alike 9.5 alike -13 -16 alike alike -15 alike 4.3
significance level

Average 713 7110 2190 165 77.6 1480 0.441 0.00602 0.499 0.0141 0.00344 0.0414 45.9 - -
Standard deviation 24 226 71.6 5.1 3.6 57 0.0079 0.0056 0.0072 0.00067 0.00020 0.020 2.8 - -
Rel. stand. deviation (%) 3.4 3.2 3.3 3.1 4.6 3.9 1.8 94 1.4 4.8 5.9 47 6.1 - -

Average 750 7080 2180 161 73.7 1470 0.419 0.00996 0.451 0.0119 0.00219 0.0255 41.9 - -
Standard deviation 54 480 180 14 7.8 150 0.024 0.0050 0.027 0.0026 0.00014 0.0027 5.8 - -
Rel. stand. deviation (%) 7.2 6.8 8.4 8.6 11 10 5.8 50 5.9 22 6.6 11 14 - -
t0 0.20 0.90 0.93 0.52 0.34 0.93 0.088 0.28 0.0051 0.21 0.0037 0.16 0.26 - -
alike alike alike alike alike alike alike alike 11 alike 57 alike alike - -
significance level2
1
: Positive values indicate that the results of the 24 hour leaching test at L/S 2 l/kg are larger on a 95 % significant level than the results of the 6 hours leaching test at L/S 2
l/kg. Negative values indicate the opposite case. The number shows the difference between the two mean values in percentage.
2
21
Table 5-4 The result of student’s T-test on test material 3 (VTT-reference material).
Cl SO4 Al Ca K Na Ba Mo DOC pH Specific cond.
mg/kg mg/kg mg/kg mg/kg mg/kg mg/kg mg/kg mg/kg mg/kg (25°C)
mS/m
Average 122 40.0 2.37 930 666 447 35.2 1.75 2.62 12.4 769
Standard deviation 38 14 0.38 27 9.8 3.7 0.79 0.068 1.0 0.015 14
Rel. stand. deviation (%) 31 36 16 2.9 1.5 0.83 2.2 3.9 39 0.12 1.8

Average 155 172 0.177 1430 618 421 5.14 7.07 2.58 12.5 920
Standard deviation 11 94 0.14 83 21 11 3.2 1.9 0.85 0.0058 13
Rel. stand. deviation (%) 7.0 54 80 5.6 3.4 2.6 61 26 33 0.05 1.5
-6 -6 -8 -6 -7
t0 0.099 0.028 1.9·10 1.2·10 0.0016 0.0010 3.2·10 0.00022 0.95 2.4·10 1.1·10
1 alike -77 1200 -35 7.8 6.2 580 -75 alike -0.69 -16
significance level
Average 187 b.d. 78.4 4210 667 453 65.0 7.71 9.05 - -
Standard deviation 16 - 23 310 22 12 4.4 1.2 1.2 - -
Rel. stand. deviation (%) 8.5 - 29 7.4 3.4 2.6 6.7 16 14 - -
Average 150 b.d. 33.8 4600 684 460 74.4 4.49 9.13 - -
Standard deviation 15 - 4.8 240 17 11 2.0 0.10 2.0 - -
Rel. stand. deviation (%) 10 - 14 5.2 2.5 2.4 2.7 2.2 22 - -
t0 0.0060 - 0.0027 0.055 0.22 0.37 0.0025 0.00040 0.95 - -
24 - 130 alike alike alike -13 72 alike - -
significance level2
1
: Positive values indicate that the results of the 24 hour leaching test at L/S 2 l/kg are larger on a 95 % significant level than the results of the 6 hours leaching test at L/S 2
l/kg. Negative values indicate the opposite case. The number shows the difference between the two mean values in percentage.
2
b.d.: The concentration of the element in the eluate of at least four of the five replicates was below the detection limit.
5.2.1 Comparison of contact time
The influence of the contact time on the obtained leaching results were evaluated by
student’s T-test. The results of a batch leaching at L/S 2 l/kg and a contact time of 24
hours (EN 12457 part 1) was compared with a batch leaching test at L/S 2 l/kg and a
contact time of 6 hours (EN 12457 part 3, stage 1).
Test material 1
For test material 1 (stabilised fly ash) the leached amounts of the analysed parameters
were generally independent of the used contact time. The specific conductivity at 25 °C
and the leached amount of Cr were statistically larger when using a contact time of 24
hours than when using a contact time of 6 hours. However, the differences were still
relatively small. Therefore, based on our general knowledge about leaching tests it can
for test material 1 generally be concluded that the leached amount were independent of
the used contact time.
Test material 2
For test material 2 (bottom ash) the two used contact times shows larger differences
than for test material 1. Only for pH, Na, Cr, Pb, and Zn no statistical significant
difference was found by the T-test. For the macro ions like Cl, SO4, Ca, K, and Mg the
largest amount was leached when using a contact time of 24 hours, whereas the largest
amount of the trace elements (Cu and Ni) and the DOC was leached when using a
contact time of 6 hours. The deviation in leached amounts when using different contact
times was though rather small for all parameters (4-19 %). Also the relative standard
deviation for the five replicates of each leaching test were very small (generally less
than 5 %) for all the parameters that showed statistically difference. This means that
even a small difference in the leached amount when comparing the two used contact
time will result in a statistically difference when using the T-test. Therefore, for test
material 2 it can be concluded that only smaller differences were observed when using
different contact time.
Test material 3
For test material 3 (wood and peat fly ash) the leached amounts of several analysed
parameters were dependent on the contact time. Only for DOC and Cl no statistically
difference was found by the T-test. For Al, K, Na, and Ba the largest amount was
leached when using a contact time of 24 hours, whereas the largest amount of SO4, Ca,
and Mo were leached when using a contact time of 6 hours. However, the deviations in
the leached amounts were relative small for Na and K. The variations in replicate
results, especially for Al, were more significant when the leached amounts were low.
For test material 3 the decrease in the leached amounts of Ca, Mo and SO4 was probably
due to precipitation maybe caused by formation of CaCO3 and CaSO4 and also due to
decrease in pH influencing the leachability of Mo. The influence of precipitation can
also be seen from the decrease in the specific conductivity at 25 °C.
The results from the batch test at L/S 2 l/kg can also be compared to column test results
obtained earlier at VTT for the test material 3. The present results obtained with the
contact time of 24 h indicated that the leached amount of Mo, Ba, and Ca were at the

same order of magnitude as obtained in the column test in which the eluates were
collected under air contact. On the other hand, column test performed with eluate
collection under nitrogen atmosphere gave lower results for Ba and higher results for
Mo.
Conclusions
Based on the obtained leaching results when using a contact time of 6 and 24 hours,
respectively, the contact time was not of major influence on the leached amount for test
material 1 and 2. For material 3 the contact time had a significant influence on the
leached amount of some of the analysed parameters (Ca, Al, Ba, Mo), and largest
amounts were leached when using a contact time of 24 hours. Since some differences,
thus, were observed a contact time of 24 hours might be preferable for two reasons.
Firstly, the precipitation rate of some minerals (e.g. CaSO4, CaCO3) might be slower
than the dissolution of the elements that form these minerals (e.g. Ca, CO3, SO4). This
means that the eluates might be supersaturated with the actual minerals after 6 hours
whereas a contact time of 24 hours might bring the solution in equilibrium and thereby
might give the minerals time to precipitate. Secondly, a contact time of 24 hours is
preferable from a practical point of view, since that allows the leaching test to be
launched at any time of a typical working day. Furthermore, the equilibrium of some
elements e.g. some of the trace elements are obtained rather slowly. This also speaks for
a contact time of 24 hours since that allows for a longer time of equilibrium and
therefore a higher probability of reaching equilibrium conditions for all parameters.
5.2.2 Comparison of one- and two-stage batch leaching test

The influence of the use of a single-step or a serial batch leaching test on the obtained
leaching results were compared by student’s T-test. The results of a one-stage batch
leaching test at L/S 10 l/kg and a contact time of 24 hours (EN 12457 part 2) was
compared with the results of a two-stage batch leaching test at L/S 0-2 l/kg and 2-10
l/kg and a contact time of 6 hours and 18 hours, respectively (EN 12457 part 3).
Test material 1
For test material 1 (stabilised fly ash) the result of the T-test to some degree showed
dependence between the number of leaching step and the accumulated leached amount.
Only for Ca, Ba, Pb, and Zn no statistical significant difference was found by the T-test.
For the other tested elements (Cl, SO4, K, Na, Cr, and DOC) the largest amounts were
leached when using the two-stage batch leaching test compared with the one-stage batch
leaching test. However, for all the parameters that shows statistically difference (except
DOC), both the deviation in the accumulated leached amounts when using different
number of leaching steps and the relative standard deviation for the five replicates of
each leaching test were rather small (less than 3 %). This means that even a small
difference in the leached amount when comparing the two used leaching tests (one or
two leaching steps) will result in a statistical significant difference when using the T-
test. Furthermore, some of the elements that showed statistical significant difference are
known to be solubility-controlled (e.g. SO4) whereas other are known to be availability-
controlled (e.g. Cl, K, Na). The identified statistical significant difference in
accumulated leached amounts, therefore, can probably not been proved to be related to
the leaching pattern for the specific elements. Summarised for test material 1 it can be

concluded that generally only smaller differences in the accumulated leached amounts
were observed when using one- or two-stage batch leaching tests, respectively.
Test material 2
For test material 2 (bottom ash) the leached amounts of the analysed parameters were
generally independent of the number of used leaching steps. Only the leached amounts
of Cu and Pb were statistically larger when using a two-stage batch leaching test than
when using a one-stage batch leaching test. For Pb the measured concentrations in the
eluates were close to or even below the detection limit. This indicates that the measured
values of Pb are encumbered with some uncertainties. For Cu the differences between
the accumulated leached amount in the two leaching tests were relatively small (11 %).
All in all for test material 2 it can generally be concluded that the accumulated leached
amount were independent of the use of one or two leaching stage.
Test material 3
For test material 3 (wood and peat fly ash) the leached amounts of several parameters
(Ca, K, Na and DOC) were independent of the number of used leaching steps. Only the
leached amounts of Al and Mo were statistically larger and for Ba statistically lower
when using a two-stage batch leaching test than when using a one-stage batch leaching
test. For Ba the difference between the accumulated leached amount in the two leaching
tests were relatively small (13 %). The one step leaching procedure gave slightly higher
results for Ba than the two step leaching procedure The leached amounts of SO4 cannot
be compared, because the obtained concentrations in the eluates were near the detection
limits.
Conclusions
Based on the obtained leaching results when using either a one- or a two-stage batch
leaching test, the number of leaching stage seems not to be of major influence on the
accumulated leached amount. However, since the obtained results indicated that the
largest accumulated amounts were leached when using the two-stage batch leaching
test, this might be preferable. This is also generally what is recommended, since the risk
of underestimating the leaching of solubility-controlled elements is expected to be
larger when using a one-stage leaching test than when using serial batch leaching tests.

6 CONCLUSIONS AND RECOMMENDATIONS
On three different test materials five replicates of each of the batch leaching tests EN
12457 part 1-3 were performed and the obtained results were compared.
The obtained results with five replicates of each sample showed good reproducability.
Statistical outliers and stragglers were identified by the Grubb’s test and from only 5 %
of all the obtained dataset a value was excluded from further statistical analyses.
The comparison of the leaching results was made by students T-test. By this test the
influence on the contact time and the number of leaching stage was tested.
For few elements the students T-test showed significantly different leaching when using
different contact time (6 and 24 hours, respectively). However, based on critical
evaluation of the obtained results combined with our general knowledge about leaching
test, it was concluded that the contact time for two of the test materials had no major
influence on the leached amount. For the third tested materials the contact time
influenced significantly the leaching of some elements. These differences were probably
due to the high content of calcium oxide and as a consequence the carbonation of
calcium that took place when the contact time was increased. However, a contact time
of 24 hours might still be preferable in a one-stage leaching test both with respect to
fulfilling the equilibrium assumption and from a practical point of view. The
equilibrium assumption will probably be better fulfilled both with respect to
precipitation and dissolution reactions when using a contact time of 24 hours, and the
practical point of view covers that a contact time of 24 hours allows the leaching test to
be launched at any time of a typical working day. A longer contact time (24 hours) is
especially recommended in cases where the amount leached is determined at a relatively
low L/S-ratio like L/S 2 l/kg.
As for the contact time, the students T-test for few elements showed significantly
different leaching when using different number of leaching steps (1 or 2 steps,
respectively). For the elements that showed significantly different leaching, the leached
amounts when using the two-stage test was generally higher than or equal to the leached
amount when using the one-stage test. However, the number of compounds for which
the leaching was considerably higher was modest, and it is concluded that the number of
leaching steps had no major influence on the leached amount. This conclusion is based
on critical evaluation of the obtained results combined with our general knowledge
about leaching test. Nevertheless, when using a relatively high accumulated L/S-ratio it
might still be recommended to use a two-stage leaching test since the obtained leaching
results indicated that the largest accumulated amounts were leached when using the
two-stage batch leaching test. Furthermore, the use of a two-stage batch leaching test
will minimise the risk of underestimating the leaching of solubility-controlled elements
compared with the use of a one-stage batch leaching test. The two-stage batch leaching
test is especially recommended for materials which have not been tested earlier.

7 REFERENCES
CEN (2002) CEN/TC292/WG2 EN 12457 Compliance test for leaching of granular
materials and sludges. Characterisation of waste. Leaching. European Committee
for Standardization.
Chandler, A.J., Eighmy, T.T., Hartlén, J., Hjelmar, O., Kosson, D.S., Sawell, S.E., van
der Sloot, H.A., and Vehlow, J. (1997) Municipal solid waste incinerator
residues. The international ash working group (IAWG). Elsevier Science BV,
Amsterdam, NL.
Hjelmar O., Birch H., Hansen J.B. (2001) The VKI process for treatment of APC
residues from MSW incineration: Process development and optimisation in pilot
scale. The Second ISWA seminar on Waste-to-Energy State of the Art and Latest
News. October 25-26, in Malmö, Sweden.
ISO (1994). ISO 5725-2:1994(E) Accuracy (trueness and precision) of measurement

methods and results. Part 2: Basic method for the determination of repeatability
and reproducibility of a standard measurement method.
Montgomery, D.C. (1991) Design and analysis of experiments. Third edition.John

Wiley & sons, New York, NY.
Nordtest (1998) NT ENVIR 005. Solid waste, granular inorganic material: Compliance
batch leaching test. Nordtest, Espoo, Finland.
Wahlström, M., Laine-Ylijoki, J., Pihlajaniemi, M., Production and use of laboratory
reference material when testing solid waste. (in Swedish) Espoo 2001, Nordtest
NT Techn Report 486, 41 p, NT Project 1492-00.

APPENDICES

APPENDIX A
Analytical reports from Analytica AB

Test material 1

Test material 2

Test material 3

APPENDIX B
Dataset used for student’s T-test

60
Table C-1 Dataset used for the student’s T-test on testmaterial 1 (stabilised fly ash)
mg/kg TS
Lab. test Soil type Rep. Cloride Sulfate Ca Na Cr Pb Zn K Ba TOC
DK L/S=2 one step C R64 1 1700 4400 1456 1160 0.748 0.01016 0.01596 754 0.0902 9.8
DK L/S=2 one step C R64 2 1740 4400 1480 1184 0.758 0.0095 0.01386 770 0.0878 8
DK L/S=2 one step C R64 3 1680 4200 1482 1156 0.762 0.0096 0.01296 752 0.087 6.8
DK L/S=2 one step C R64 4 1860 4800 1480 1152 0.772 0.0096 0.01298 748 0.09 5.8
DK L/S=2 one step C R64 5 1700 4400 1476 1156 0.754 0.00976 0.01248 752 0.0892 7
Average 1736.000 4440.000 1474.800 1161.600 0.759 0.010 0.014 755.200 0.089 7.480
Stdev 72.664 219.089 10.733 12.837 0.009 0.000 0.001 8.556 0.001 1.514
t-test C compared to A 0.738 0.630 0.091 0.291 0.006 0.251 0.138 0.778 0.281 0.375

DK L/S=10 one step D R64 1 1596.8 16966 6966.04 1227.54 0.924148 0.03972 0.078842 928.14 0.435128 16.966
DK L/S=10 one step D R64 2 1596.8 16966 7065.84 1217.56 0.907182 0.042515 0.06996 925.146 0.438122 15.968
DK L/S=10 one step D R64 3 1590.4 16898 6888.42 1222.62 0.941318 0.041052 0.07793 923.426 0.43239 18.886
DK L/S=10 one step D R64 4 1596.8 16966 6966.04 1227.54 0.921154 0.04511 0.136726 926.144 0.435128 15.968
DK L/S=10 one step D R64 5 1694.9 17946 7048.79 1226.31 0.918237 0.040777 0.075274 916.243 0.425719 18.943
Average 1615.140 17148.400 6987.026 1224.314 0.922 0.042 0.088 923.820 0.433 17.346
Stdev 44.673 446.843 71.816 4.280 0.012 0.002 0.028 4.566 0.005 1.489
t-test D to A+B 0.000 0.049 0.093 0.000 0.000 0.236 0.812 0.000 0.216 0.003

DK L/S=2 two step A R64 1 1740 4400 1482 1154 0.742 0.00902 0.0218 748 0.0896 8
DK L/S=2 two step A R64 2 1680 4410 1570.8 1146.6 0.7287 0.010647 0.015036 753.9 0.09303 6.72
DK L/S=2 two step A R64 3 1738.8 4554 1513.17 1159.2 0.72243 0.010412 0.013931 757.62 0.09108 5.589
DK L/S=2 two step A R64 4 1720 4400 1460 1148 0.708 0.00978 0.01518 746 0.0854 6
DK L/S=2 two step A R64 5 1741.5 4730 1578.1 1163.15 0.74605 0.011159 0.01505 763.25 0.095675 7.31
Average 1724.060 4498.800 1520.814 1154.190 0.729 0.010 0.016 753.754 0.091 6.724
Stdev 26.140 144.835 52.544 7.095 0.015 0.001 0.003 7.042 0.004 0.973

DK L/S=10 two step A+B R64 1 1756.345 17483.765 7043.066 1285.761 1.029164 0.04213 0.093111 988.6257 0.433467 18.49105
DK L/S=10 two step A+B R64 2 1713.304 17624.579 7080.145 1267.756 0.991228 0.042692 0.110347 981.5029 0.439398 23.35465
DK L/S=10 two step A+B R64 3 1760.871 17701.081 7084.939 1283.062 1.030124 0.042922 0.076304 993.4367 0.432967 22.7435
DK L/S=10 two step A+B R64 4 1723.997 17526.196 6980.884 1263.052 0.999565 0.043812 0.092266 977.9568 0.436195 23.73625
DK L/S=10 two step A+B R64 5 1748.442 17847.536 7149.831 1290.974 1.040994 0.04399 0.083433 995.3694 0.444821 23.73749
Average 1740.592 17636.632 7067.773 1278.121 1.018 0.043 0.091 987.378 0.437 22.413
Stdev 20.863 145.210 61.930 12.068 0.022 0.001 0.013 7.507 0.005 2.230
Test
5 % significance level
D with A+B (one step or two step) 7.77 2.85 same 4.39 10.39 same same 6.88 same 29.21
C with A (contact time) same same same same 4.03 same same same same same
Table C-2 Dataset used for the student’s T-test on testmaterial 2 (bottom ash)
61
mg/kg TS
Lab. test Soiltype Cloride Sulfate Ca K Mg Na Ba Cr Cu Ni Pb Zn TOC
DK L/S=2 one step C R65 1 760 5000 1242 120.8 62.6 1396 0.0848 0.00276 0.276 0.0083 0.001748 0.0222 24
DK L/S=2 one step C R65 2 720 5000 1234 114.8 58.6 1334 0.088 0.001614 0.27 0.0081 0.001672 0.01744 22
DK L/S=2 one step C R65 3 720 5000 1236 114.4 57 1306 0.0862 0.001686 0.272 0.00746 0.001282 0.01556 22
DK L/S=2 one step C R65 4 703.5 4824 1248.21 113.766 56.28 1282.38 0.08543 0.003357 0.26934 0.007035 0.002814 0.018211 24.12
DK L/S=2 one step C R65 5 700 4800 1300 110 54 1300 0.086 0.0017 0.3 0.0077 0.00094 0.013 22
Average 720.7 4924.8 1252.042 114.753 57.696 1323.676 0.08609 0.002223 0.277468 0.007719 0.001691 0.017282 22.824
Stdev 23.82121 103.32086 27.37862 3.88131 3.2022 44.48511 0.0012 0.000792 0.012861 0.000504 0.000706 0.003405 1.129106
t-test C compared to A 0.028647 0.0003348 0.002762 0.01444 0.00079 0.074279 0.00026 0.691533 0.000411 0.003653 0.268952 0.55306 0.000481
Lab. test Soiltype Rep. Cloride Sulfate Ca K Mg Na Ba Cr Cu Ni Pb Zn TOC
DK L/S=10 one step D R65 1 721.44 6813.6 2094.18 153.306 69.9396 1392.78 0.42385 0.007585 0.423846 0.01022 0.002154 0.027956 49.098
DK L/S=10 one step D R65 2 708.58 6586.8 1946.1 145.708 65.6684 1307.38 0.41417 0.005499 0.430138 0.014471 0.002355 0.027645 34.93

DK L/S=10 one step D R65 3 739.26 7192.8 2217.78 162.837 73.1268 1478.52 0.44156 0.00958 0.461538 0.009171 b.d. 0.023976 41.958
DK L/S=10 one step D R65 4 844.05 7844.7 2442.78 182.712 86.5896 1717.89 0.37933 0.008599 0.450822 0.013604 0.002075 0.022541 41.706
DK L/S=10 one step D R65 5 737.04 6972 2201.16 160.356 73.1064 1464.12 0.43426 0.018526 0.491028 outlier outlier outlier n.m
Average 750.074 7081.98 2180.4 160.984 73.6862 1472.138 0.41863 0.009958 0.451474 0.011867 0.002195 0.025529 41.923
Stdev 53.99068 480.45539 182.3471 13.8586 7.83372 153.2498 0.0243 0.005023 0.026855 0.002568 0.000144 0.00269 5.785931
t-test D to A+B 0.199884 0.8962663 0.930034 0.52442 0.34417 0.928047 0.08781 0.982949 0.005115 0.20507 0.003728 0.156005 0.257152
Lab. test Soiltype Rep. Cloride Sulfate Ca K Mg Na Ba Cr Cu Ni Pb Zn TOC
DK L/S=2 two step A R65 1 700 4600 1198 107.4 49 1268 0.0802 0.00148 0.318 0.01002 0.00193 0.0228 28
DK L/S=2 two step A R65 2 680 4600 1214 108.4 49.6 1286 0.0776 0.0027 0.324 0.00848 0.001044 0.01424 28
DK L/S=2 two step A R65 3 640 4400 1158 102.4 45.4 1188 0.0818 0.00292 0.33 0.00944 outlier outlier 26
DK L/S=2 two step A R65 4 680 4600 1142 108 48.2 1258 0.0778 0.0022 0.314 0.0087 0.00078 0.01324 26
DK L/S=2 two step A R65 5 700 4600 1154 111.8 51.2 1318 0.0756 0.00272 0.306 0.00914 0.000982 0.01196 26
Average 680 4560 1173.2 107.6 48.68 1263.6 0.0786 0.002404 0.3184 0.009156 0.001184 0.01556 26.8
Stdev 24.4949 89.442719 31.03546 3.37343 2.13822 48.02916 0.00242 0.000581 0.009209 0.000611 0.00051 0.004916 1.095445
test
Lab. L/S=10 two step Soiltype Rep. Cloride Sulfate Ca K Mg Na Ba Cr Cu Ni Pb Zn TOC
DK L/S=10 two step A+B R65 1 735.3782 6957.3863 2123.662 165.967 78.0789 1490.547 0.44167 b.d. 0.496651 0.014822 0.003587 0.041199 48.68749
DK L/S=10 two step A+B R65 2 712.0926 7223.1205 2241.676 166.468 78.647 1504.163 0.43646 0.0105 0.511517 b.d. 0.003301 0.033924 45.507
DK L/S=10 two step A+B R65 3 673.704 6926.1065 2172.189 157.484 72.5021 1388.847 0.43557 b.d. 0.497134 0.013476 b.d. 0.074422 47.31596
DK L/S=10 two step A+B R65 4 712.9839 7002.6969 2121.986 165.265 76.2256 1468.312 0.45429 0.008028 0.495548 b.d. b.d. 0.023587 42.2564
DK L/S=10 (totrin) A+B R65 5 731.1459 7460.3582 2282.175 171.712 82.3575 1542.907 0.43624 0.011552 0.493723 0.014089 b.d. 0.033703 outlier
Average 713.0609 7113.9337 2188.338 165.379 77.5622 1478.955 0.44084 0.010027 0.498915 0.014129 0.003444 0.041367 45.94171
Stdev 24.36716 225.88241 71.58303 5.09872 3.59965 57.21109 0.0079 0.001809 0.007166 0.000674 0.000202 0.019512 2.780789
Test
D with A+B (one step or two step) same same same same same same same same 10.51 same 56.92 same same
C with A (contact time) 5.99 8.00 6.72 6.65 18.52 same 9.52 same -12.86 -15.69 same same -14.84
62
Table C-3 Dataset used for the student’s T-test on testmaterial 3 (wood and peat ash)
mg/kg TS
Lab. test Soiltype Al Ca K Na Ba Mo Cl So4 TOC
FIN L/S=2 one C refmat-VTT 1 2.601132 948.4128 678.2952 450.1959 35.41541 1.842802 138.0601 outlier 3.801655
FIN L/S=2 one C refmat-VTT 2 2.620153 940.0548 658.0383 442.0258 34.402 1.744102 182.0106 40.00233 3.200187
Average 2.373315 929.8102 665.7521 446.9016 35.16807 1.745201 122.4264 39.95527 2.616685
Stdev 0.378245 27.09952 9.746681 3.699143 0.78596 0.067647 37.74617 14.23476 1.018939
t-test C compared to A 1.95E-06 1.17E-06 0.001643 0.00102 3.19E-08 0.000219 0.09895 0.028006 0.947177

FIN L/S=10 oneD refmat-VTT 1 32.39963 4679.947 675.9923 454.9948 74.79915 4.35995 169.9981 b.d. b.d
FIN L/S=10 oneD refmat-VTT 2 28.95998 4880.668 696.6596 466.8025 76.75407 4.617395 131.6363 b.d. 6.986848
FIN L/S=10 oneD refmat-VTT 3 30.7054 4710.828 698.1227 471.0828 75.01319 4.560802 160.0281 b.d. n.m.
Average 33.79311 4598.298 683.5564 460.377 74.41344 4.49164 150.3328 #DIV/0! 9.128998
Stdev 4.83078 237.3748 17.22598 10.88646 2.019632 0.100177 15.30599 #DIV/0! 2.02037
t-test D to A+B 0.002692 0.054876 0.223169 0.367112 0.002452 0.000401 0.006001 #DIV/0! 0.954024

FIN L/S=2 two sA refmat-VTT 1 0.068002 1422.051 606.0217 412.0147 3.800136 7.320262 154.0055 186.0067 3.200115
Average 0.177483 1434.025 617.6107 420.8072 5.140066 7.068134 155.2026 172.4036 2.576043
Stdev 0.142151 82.51279 20.99307 11.00625 3.158561 1.871734 10.82497 93.75117 0.853872

FIN L/S=10 twoA refmat-VTT 1 77.71743 4170.289 654.2918 443.9066 63.86737 7.719328 184.571 b.d. b.d.
FIN L/S=10 twoA refmat-VTT 2 65.9785 4228.389 691.4268 468.4314 67.83876 7.067839 176.4028 b.d. 8.500908
FIN L/S=10 twoA refmat-VTT 4 70.79423 4387.539 660.8219 448.0229 65.6314 8.815428 191.9211 b.d. b.d.
Average 78.35313 4206.264 666.8819 453.4789 65.02834 7.707719 186.7843 #DIV/0! 9.045085
Stdev 22.77997 309.7341 22.37026 11.91061 4.383783 1.233828 15.80377 #DIV/0! 1.23717
Test
D with A+B (one step or two step) 131.8613 same same same -12.6121 71.60145 24.24722 #DIV/0! same
C with A (contact time) 1237.209 -35.16083 7.794781 6.201031 584.1949 -75.30889 same -76.82458 same
TECHNICAL REPORTS ENVIRONMENT
Notice: Only technical reports with a bold number on the left leaf of the page can be ordered free of charge from the
Nordtest secretariat. Others have to be ordered from the publishing organisation or institute. Information for ordering
those reports can be obtained from Nordtest secretariat and Nordtest Web-site.
463 Johnsen, T., Pretlove, B. & Jensen, S.B., The state-of-the-art on research in solid waste and Life Cycle
Assessment (LCA) in the Nordic countries. Espoo 2000. Nordtest, NT Techn Report 463. 25 p. NT Project No.
1491-00.
464 Hjelmar, O., Broholm, K., Larsson, L.B. & Wahlström, M. Development of tests for characterising the leaching
of organic compounds from contaminated soils and waste products. Espoo 2000. Nordtest, NT Techn Report
464. 28 p. NT Project No. 1394-97
465 Endresen, Ø., G.Estensen, A.S. & Nesgård, B.S., Indicator parameters for polluted leachate water from
landfills. Høvik 2000. Det Norske Veritas AS, Report 2000-3082. 60 p. (in Norwegian) NT Project No. 1397-98.
466 Lehmann, N.K.J., Hansen, J.B., Wahlström, M., Fällman, A.-M. & Hjelmar, O., Influence of critical test
conditions on results of ph-dependent leaching tests. Espoo 2000. Nordtest, NT Techn Report 466. 88 p.
NT Project No. 1448-99.
468 Dybdahl, H.P, Oreld, F., Lund, H., Nylund, K., Hartonen, K., Bøwadt, S. & Sporring, S., Alternative Extraction
Procedures for the Analysis of Contaminants from Environmental Matrices. Espoo 2001. Nordtest, NT Techn
Report 468. 13 p. NT Project No. 1419-99.
469 Cedheim, L., Fagerli, A.K., Halonen, I., Möller, S. & Tapper, M., Determination of total PCA in extract from tyres
– Framework for Nordic environmental labelling. Espoo 2001. Nordtest, NT Techn Report 469. 26 p. NT Project
No. 1476-00.
473 Bjerre-Hansen, J., Engelund-Holm, P., Aagård-Hansen, E. & Hjelmar, O., Use of lysimeters for characterisation
of leaching from soil and mainly inorganic waste materials. Espoo 2001. Nordtest, NT Techn Report 473. 53 p.
486 Wahlström, M., Laine-Ylijoki, J. & Pihlajaniemi, M., Production and use of laboratory reference material when
testing solid waste. Espoo 2001. Nordtest, NT Techn Report 486. 43 p. (in Swedish) NT Project No. 1492-00.
517 Bjarnadóttir, H.J., Friðriksson, G.B., Johnsen, T. & Sletsen, H., Guidelines for the use of LCA in the waste
management sector. 96 p. (+3 appendices). Appendix –1: Icelandic comparative case study – landfill, biocell,
compost. 58 p. Appendix – 2: Icelandic descriptive case study – landfill without gas collection. 21p. Appendix –
3: Summary of Norwegian case studies. 13 p. Espoo 2003. Nordtest, NT Techn Report 517.
518 Haarstad, K., Borch, H. & Linderoth, M., Biotest and guideline for investigations of biochemical disorder based
upon characterisation of pollutants in landfill leachates. Espoo 2003. Nordtest, NT Techn Report 518. 36 p.
519 Lehmann, N.K.J., Lærke Jensen, D., Asmussen, O.W., Hjelmar, O. & Wahlström, M., Automatic column leaching
testing with NT ENVIR 002 - Evaluation. Espoo 2003. Nordtest, NT Techn Report 519. 34 p. (in Danish)
520 Hjelmar, O., Bjarnadóttir, H.J. & Halldórsson, B., Acceptance criteria for landfilling of waste under Nordic
conditions. Espoo 2003. Nordtest, NT Techn Report 520. 76 p . NT Project No. 1538-01.
539 Lærke-Baun, D., Holm, J., Bjerre-Hansen, J. & Wahlström, M., CEN EN 12457 leaching test: Comparison of
test results obtained by part 1 and 2 with test results obtained by part 3. Espoo 2004. Nordtest, NT Techn
Report 539. 62 p . NT Project No. 1587-02.
NORDTEST
TECHNICAL REPORT 539
Nordtest, founded in 1973, is an institution under the Nordic Council of

Ministers and acts as a joint Nordic body in the field of conformity
assessment. The emphasis is on the development of Nordic test methods
and on Nordic co-operation concerning conformity assessment. The main
task is to take part in the development of international pre-normative
activity. Nordtest is yearly funding projects in its field of activity.
Nordtest endeavours to
• promote viable industrial development and industrial competitive-
ness, remove technical barriers to trade and promote the concept
“Approved Once Accepted Everywhere” in the conformity assess-
ment area
• work for health, safety, environment in methods and standards
• promote Nordic interests in an international context and Nordic par-
ticipation in European co-operation
• finance joint research in conformity assessment and the develop-
ment and implementation of test methods
• promote the use of the results of its work in the development of
techniques and products, for technology transfer, in setting up stand-
ards and rules and in the implementation of these
• co-ordinate and promote Nordic co-operation in conformity assess-
ment
• contribute to the Nordic knowledge market in the field of conform-
ity assessment and to further development of competence among
people working in the field
12

CEN EN 12457 Leaching Test: Comparison of Test Results Obtained by Part 1 and 2 With Test Results Obtained by Part 3

Uploaded by

Document Information

Original Description:

Original Title

Copyright

Available Formats

Share this document

Share or Embed Document

Sharing Options

Did you find this document useful?

Is this content inappropriate?

Copyright:

Available Formats

CEN EN 12457 Leaching Test: Comparison of Test Results Obtained by Part 1 and 2 With Test Results Obtained by Part 3

Uploaded by

Copyright:

Available Formats

TR 539

CEN EN 12457 leaching test:

100000 Single batch

Dorthe Lærke Baun

Technical Group: Expert Group Environment and Natural Resources

2 THEORETICAL ASPECTS OF LEACHING ...................................................................7

3 EXPERIMENTAL WORK AND OBTAINED RESULTS ..................................................9

4 DESCRIPTION OF USED STATISTICAL TOOLS .......................................................14

5 RESULTS AND DISCUSSIONS OF THE STATISTICAL ANALYSES .........................17

6 CONCLUSIONS AND RECOMMENDATIONS ............................................................25

A Analytical reports from Analytica AB

Nordtest Technical Report 539 3

4 Nordtest Technical Report 539

Nordtest Technical Report 539 5

The batch leaching test EN 12457 consists of 4 parts:

1. EN 12457-1: Performed at L/S 2 l/kg on material < 4 mm (1 step)

2. EN 12457-2: Performed at L/S 10 l/kg on material < 4 mm (1 step)

4. EN 12457-4: Performed at L/S 10 l/kg on material < 10 mm (1 step)

6 Nordtest Technical Report 539

Chemical aspects influencing the leaching relate to the fundamental processes

− the influence of pH on controlling the solubility

− the influence of dissolved-phase complexing agents, that increase the dissolution

− the role of oxidation-reduction potential in increasing solubilisation

Chemical aspects can also include reprecipitation or sorption processes, whereby

The leaching of solubility-controlled elements might be dependent on the number of

The difference between a one- and a two-stage batch-leaching test is illustrated in

Nordtest Technical Report 539 7

100000 Single batch

8 Nordtest Technical Report 539

3.1 Experimental work

3.1.1 Test materials

Test material 2: Aged bottom ash from a MSW-incinerator plant

Test material 3: Wood and peat ash (Wahlström et al 2001)

3.1.2 One-stage batch leaching test (EN 12457 part 1 and 2)

3.1.3 Two-stage batch leaching test (EN 12457 part 3)

Nordtest Technical Report 539 9

3.2.1 Test material 1 (stabilised fly ash)

3.2.2 Test material 2 (aged bottom ash from a MSW-incinerator plant)

3.2.3 Test material 3 (wood and peat ash)

10 Nordtest Technical Report 539

Nordtest Technical Report 539

L/S 10 l/kg, 1 stage (EN 12457 part 2)

L/S 2 l/kg, 6 hours (EN 12457 part 3, stage 1)

Nordtest Technical Report 539

L/S 2+8 l/kg, 2 stage (EN 12457 part 3)

Nordtest Technical Report 539

4.1 Grubb’s test

By the Grubbs’ test a potentially outlying observation can be identified as either a

where G1 : the Grubb’s test statistic

14 Nordtest Technical Report 539

where Fn1 −1, n2 −1 : the F-test statistic

4.3 Students T-test

When using the students T-test, two hypothesis were tested:

Nordtest Technical Report 539 15

where t0: the T-test statistic

The common variance was computed from:

(n1 − 1) ⋅ S12 + (n2 − 1) ⋅ S 22

where S12, S22: the two individual sample variances

16 Nordtest Technical Report 539

5.1 Grubb’s test

Table 5-1 The reult of the Grubb’s test

Sample and element x1 x12 s3 G1 4 Result of