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The in luence o alkaline ac i a o on immobiliza ion o me als in alkali-
ac i a ed blas u nace slag
To ci e his a icle: E Bys ianska and J Koplik 2021 IOP Con . Se .: Ma e . Sci. Eng. 1039 012013
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The in luence o alkaline ac i a o on immobiliza ion
o me als in alkali-ac i a ed blas u nace slag
E Bys ianska1 and J Koplik1
1 B no Uni e si y o Technology, Facul y o Chemis y, Pu kyňo a 118, 612 00 B no,
Czech Republic
Email: emilia.bys ianska@ u .cz
Abs ac . In his wo k he in luence o alkaline ac i a o on immobiliza ion o lead and coppe
in alkali-ac i a ed blas u nace slag was in es iga ed. A o al o i e alkali ac i a o s we e used;
sodium wa e glass, po assium wa e glass, sodium hyd oxide, po assium hyd oxide and sodium
ca bona e. The leaching es acco ding o ČSN EN 12457؎4 was used o e alua e he le el
o immobiliza ion o hea y me als, he leached solu ions we e analyzed by ICP-OES. Fo a be e
unde s anding o immobiliza ion p ocess, he selec ed samples we e cha ac e ized by analy ical
me hods (SEM, XPS). I was ound ha he deg ee o immobiliza ion o Pb2+ and Cu2+ in AAS
was e y high ega dless o he ype o alkaline ac i a o used. The high deg ee
o immobiliza ion is caused by o ma ion o insoluble o poo ly soluble lead and coppe
compounds in an alkaline en i onmen while he insoluble compounds ha e been con i med by
SEM and XPS.
1. In oduc ion
Solidi ica ion/s abiliza ion (S/S) is one o he mos impo an echniques o ea ing was es con aining
hea y me al con aminan s. The pu pose o S/S echnology is physically as well as chemically ix hea y
me als (o pollu ed was e) in he solid ma ix o educe hei mobili y and he e o e minimize he h ea
o he en i onmen . This echnology is widely used o dispose o low-le el adioac i e was e, haza dous
and mixed was e. O dina y Po land cemen (OPC) has been he mos common solidi ica ion ma e ial
because o i s a ailabili y and low cos . Howe e , OPC binde s a e no e y e ec i e in s abilizing some
hea y me als [1–2].
The e iciency o he hea y me al immobiliza ion is s ongly ela ed o he mic os uc u e
o ha dened pas e and o al po osi y. Ha dened alkali-ac i a ed slag (AAS) binde s ha e less po osi y
han OPC binde . The e o e, he mi iga ion o solu ion in o he AAS binde is limi ed which esul s in
a lowe leachabili y o oxic was e. Excep o o al po osi y o binde s, pH alues o pas es play
an impo an ole in he p ocess o S/S and ype o C-A-S-H gel o ming in pas e oo. In a high alkaline
en i onmen , mos o he hea y me als p ecipi a e in o less soluble o insoluble compounds. Besides
low pe meabili y and alkaline po e solu ion, AAS binde s p esen o he impo an p ope ies including
high mechanical s eng h and high esis ance o acid o chlo ide a ack. Due o all hese physical and
chemical ad an ages, alkali-ac i a ed slag binde s a e conside ed o be mo e e ec i e o was e
immobiliza ion han OPC [3–5].
The abili y o alkali-ac i a ed slag o immobilize hea y me als o o he haza dous ma e ials in i s
s uc u e has been in es iga ed in a ious s udies [6–8]. The e iciency o hea y me al immobiliza ion
in alkali-ac i a ed slag binde s depends on many ac o s including na u e and concen a ion o alkaline
ac i a o used o ype o immobilized ma e ial and i s dosage. Hea y me als addi ion (Zn2+, Pb2+, Cd2+
a C 6+) up o 2% o slag weigh can be well s abilized in NaOH, Na2CO3, and sodium silica e-ac i a ed
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slag binde [9]. Solidi ica ion/s abiliza ion o Pb2+ and Cu2+ we e mos ly in es iga ed in ly ash-based
geopolyme s wi h high immobiliza ion e iciency [10–13].
The aim o his wo k is o compa e he abili y o AAS binde s ac i a ed by di e en ypes o alkaline
ac i a o s o immobilize Pb and Cu in hei s uc u e. In he p esen wo k, we ha e also ied o de e mine
i he hea y me als a e s abilized by chemical con e ing in o hei less soluble o insoluble o ms.
2. Expe imen al p ocedu e
2.1. Ma e ials
2.1.1. G ound g anula ed blas u nace slag. G ound g anula ed blas u nace slag (GGBFS) was
ob ained om Ko ouč Š ambe k, L d. ha ing a Blaine speci ic su ace a ea o 400 m2∙kg−1. The GBFS
was mos ly amo phous bu i also con ained c ys alline phases such as åke mani e, calci e, me wini e,
and qua z (measu ed by X- ay powde di ac ion). The chemical composi ion o GGBFS measu ed by
he X- ay luo escence echnique used o alkali ac i a ion is gi en in able 1.
Table 1. Chemical composi ion o g ound g anula ed blas u nace slag.
GGBFS Ko ouč Š ambe k [w . %]
CaO
SiO2
MgO
Al2O3
SO3
TiO2
K2O
MnO
Na2O
Fe2O3
41.1
34.7
10.5
9.1
1.4
1.0
0.9
0.6
0.4
0.3
2.1.2. Alkaline ac i a o s. Fo his wo k i e alkaline ac i a o s we e used: Liquid sodium wa e glass
(S-WG) – Silica e modulus Ms = 1.96; Liquid po assium wa e glass (P-WG) – Silica e modulus
Ms = 1.67; Sodium hyd oxide (SH); Po assium hyd oxide (PH) and Sodium ca bona e (SC). Sodium
and po assium hyd oxide we e used as 50% solu ion. Sodium ca bona e was dissol ed in wa e and
cooled o ambien empe a u e be o e alkali ac i a ion. The Na2O/K2O dosage o he alkaline ac i a o
was kep he same.
2.1.3. Hea y me als. The hea y me al-con aining compounds Pb(NO3)2 p.a. and Cu(NO3)2.3H2O p.a.
ha e been used in sample p epa a ion. The amoun s o hea y me als (Pb2+, Cu2+) adding o he hyd a ing
samples we e on le el 1% o slag weigh .
2.2. Tes s and me hods
2.2.1. Sample p epa a ion. The pas es we e p epa ed a he wa e o binde a io equal o 0.38 (w/b was
kep he same o each ac i a o used). The concen a ion o alkaline ac i a o in he slag binde was 6%
o Na2O/K2O o he slag con en o each ac i a o used. The alkaline ac i a o s we e ully dissol ed in
wa e and a e ha mixed wi h slag. The pas es we e mixed in a s anda d labo a o y mixe o 180 s,
cas in o moulds (20 × 20 × 100 mm) and ib a ed o 30 s o emo e la ge ai bubbles. All he samples
we e ma u ed in he moulds o he i s 24 h a 20 C and 100% ela i e humidi y. A e ha samples
we e open-ai cu ed a ambien condi ions.
2.2.2. Mechanical p ope ies es ing. Specimens wi h dimensions 20 × 20 × 100 mm we e used o
comp essi e s eng h de e mina ion using he Des es 4310 Compac A (Be on Sys em, L d.).
The comp essi e s eng h o he alkali-ac i a ed slag was measu ed a e 1, 7, and 28 days on h ee
samples.
2.2.3. Leaching es . The leaching es s we e pe o med using an adap a ion o s anda d ČSN EN
12457–4:2002. A e 28 days o cu ing, specimens o dimensions 20 × 20 × 100 mm we e placed in o
he PET bo le wi h dis illed wa e a a liquid/solid a io 10:1 and o a ed a 10 pm o 24 h.
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The leacha es we e analysed on ICP-OES spec oscope (Induc i ely coupled plasma op ical emission
spec ome y).
2.2.4. Cha ac e iza ion o ma e ials, hyd a ion p oduc s and mic os uc u e analysis. The GGBFS was
cha ac e ized by XRD and XRF me hods. XRD measu emen was pe o med using a PANanaly ical
Empy ean X- ay di ac ome e . The ube ol age and cu en we e 40 kV and 30 mA, espec i ely.
The ube anode was CuKα1 (1.54 Å). The sample was s ep-scanned om 5° o 90° 2θ using e ical
high- esolu ion goniome e wi h a s ep size o 0.01313 2θ. Times pe s ep we e 96 s.
The chemical composi ion o GGBFS was de e mined wi h he Xenem ics EX-6600 XRF
spec ome e . Measu emen o GGBS powde was pe o med in acuum using accele a ed ol age
30 kV.
Hyd a ion p oduc s and mic os uc u e in es iga ions o AAS wi h and wi hou hea y me als
addi ion we e ca ied ou by SEM and XPS (X- ay pho oelec on spec oscopy). These in es iga ions
we e pe o med on samples a e 28 days o cu ing.
The SEM analysis was pe o med on ZEISS EVO LS 10 wi h he ene gy dispe si e X- ay
spec oscopy (EDS) de ec o . Accele a ed ol age was se o 15 kV and he wo king dis ance was
12 mm. All samples we e spu e ed by gold o ob ain good su ace conduc i i y.
The XPS analyses we e conduc ed wi h K a os Axis Ul a DLD spec ome e using a monoch oma ic
Al Kα (hν = 1486.7 eV) X- ay sou ce ope a ing a 150 W (10 mA, 15 kV). The high- esolu ion spec a
we e measu ed wi h a s ep size o 0.1 eV and 20 eV pass ene gy. The ins umen base p essu e was
2 × 10-8 Pa.
3. Resul s and discussion
3.1. Comp essi e s eng h
As can be seen om da a ob ained ( able 2) he ype o he alkaline ac i a o used s ongly in luenced
he comp essi e s eng h o AAS pas es. Wi hou hea y me als addi ion he highes 28-day comp essi e
s eng hs we e ob ained om AAS samples ac i a ed by sodium and po assium wa e glass. E ec
o ca ions (Na+,K+) om silica e ac i a o s canno be desc ibed because o di e en silica e modulus
o wa e glass ac i a o s used. Howe e , in sodium and po assium hyd oxide ac i a ion wi h same
dosage, KOH-ac i a ed samples o med dense mic os uc u e [14]. Sodium ca bona e-ac i a ed slag
pas es equi ed a p olonged se ing ime so hey we e kep in moulds o 3 days. The longe ha dening
p ocess is ela ed o he slow de elopmen o he alkalini y equi ed o ini ializing slag dissolu ion.
Al hough, a e 28 days o cu ing, he sodium ca bona e-ac i a ed samples gained ela i ely high
comp essi e s eng hs (56.9 MPa) [15].
The in luence o 1% Pb2+ addi ion on he comp essi e s eng h o alkali-ac i a ed slag is no e y
signi ican . In wa e glass-ac i a ed samples he measu ed 1-, 7- and 28-day comp essi e s eng hs we e
e y compa able o he e e ence samples. Samples wi h Pb2+ addi ion ac i a ed by sodium o po assium
hyd oxide exhibi ed s eng h loss up o 30% a e 28 days o cu ing. The addi ion o 1% Cu2+ in luenced
he comp essi e s eng h mo e signi ican ly ega dless o alkaline ac i a o used. Sodium ca bona e-
ac i a ed samples we e mos a ec ed by Cu2+ addi ion and he 28-day comp essi e s eng hs eached
only hal he s eng h compa ed o he e e ence samples.
The na u e o alkaline ac i a o plays an impo an ole in comp essi e s eng h de elopmen .
The highes comp essi e s eng hs we e ob ained by sodium and po assium wa e glass and he lowes
comp essi e s eng h we e measu ed on he samples ac i a ed by sodium o po assium hyd oxide.
Simila esul s we e ound in o he s udies [9, 16].
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Table 2. Comp essi e s eng h o AAS samples wi h di e en alkali ac i a o used.
Comp essi e s eng h [MPa]
Sample
1 day
7 days
28 days
Na-WG
19.4
69.2
102.1
Na-WG (1% Pb)
18.6
68.0
94.9
Na-WG (1% Cu)
11.2
39.6
77.5
NH
10.4
22.0
37.4
NH (1% Pb)
4.6
16.3
24.6
NH (1% Cu)
4.3
9.3
22.6
K-WG
20.6*
50.6
76.5
K-WG (1% Pb)
20.1*
44.9
78.1
K-WG (1% Cu)
10.5*
17.0
59.4
KH
10.2
30.2
44.3
KH (1% Pb)
5.2
19.1
36.3
KH (1% Cu)
4.4
12.7
31.5
NC
-
51.1
56.9
NC (1% Pb)
-
13.1
45.8
NC (1% Cu)
-
10.1
28.4
*samples measu ed a e 3 days o cu ing
3.2. Leaching es s
Leaching es s we e pe o med based on he ČSN EN 12457–4:2002. Th ee specimens om each sample
we e subjec ed o a leaching es in dis illed wa e o 24 hou s. Resul s om hea y me al leaching a e
gi en in able 3 and able 4. The esul s showed ha he immobiliza ion e iciency o bo h hea y me als
(Cu and Pb) is e y high. The highes Pb elease occu ed in sodium wa e glass-ac i a ed samples which
could be a esul o mic oc acks obse ed in hese samples. The leaching a e o Pb2+ co esponds
o he indings ob ained by Deja e al who epo ed ha amoun s o Pb2+ ions leached om wa e glass-
ac i a ed mo a s a e highe han om Na2CO3-ac i a ed mo a s [9].
Samples wi h Cu2+ addi ion also showed a low concen a ion o hea y me al in leacha es. F om
he da a ob ained he bes coppe and lead s abiliza ion is achie ed by po assium wa e glass-ac i a ed
slag binde . I should be no ed ha concen a ions o bo h hea y me als in all samples a e low and all
ypes o alkaline ac i a o s p o ide sa e hea y me als immobiliza ion. High immobiliza ion e iciency
o Pb2+ and Cu2+ in alkali-ac i a ed GGBFS was p esen ed in he wo k o Gie giczny e al [12].
Table 3. Concen a ion o Pb2+ in leacha e.
sample
Na-WG (1 % Pb)
NH (1 % Pb)
K-WG (1 % Pb)
KH (1 % Pb)
NC (1 % Pb)
c(Pb2+)
[mg/l]
3.070 ±1.146
0.870 ±0.345
0.413 ±0.039
2.797 ±0.050
1.240 ±0.388
Table 4. Concen a ion o Cu2+ in leacha e.
sample
Na-WG (1 % Cu)
NH (1 % Cu)
K-WG (1 % Cu)
KH (1 % Cu)
NC (1 % Cu)
c(Cu2+)
[mg/l]
0.950 ±0.138
0.930 ±0.043
0.443 ±0.072
0.980 ±0.024
0.470 ±0.076
3.3. Mic os uc u e o pas es
The mic os uc u e o ha dened alkali-ac i a ed pas es wi h hea y me als addi ion was in es iga ed by
SEM analysis. All he AAS samples ( ega dless o alkaline ac i a o used) had a e y dense s uc u e
wi h C-(A)-S-H gel as he main componen . The signi ican di e ences be ween he samples doped wi h
hea y me als and e e ence samples we e no obse ed. The samples wi h sodium wa e glass ac i a ion
showed highe amoun s o mic oc acks han any o he samples ( igu e 1). Hea y me al compounds (lead
and coppe ) we e a he cumula ed in some egions han dispe sed h ough he s uc u e.
The p ecipi a ed lead compound can be seen in igu e2 and hollow compound con aining coppe is

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shown in igu e 3. F om EDS analysis aken in a eas wi h high hea y me al concen a ion ( able 5, able
6) can be seen ha lead and coppe a e p ima y cumula ed wi h oxygen.
Table 5. EDS analysis o he a ea wi h high Pb concen a ion om igu e 2.
Elemen
O
Na
Mg
Al
Si
Ca
Pb
A om. %
41.21
3.29
0.37
0.33
7.35
1.13
15.73
Table 6. EDS analysis o he hollow pa icle con aining coppe om igu e 3.
Elemen
O
Na
Si
Cl
Ca
Cu
A om. %
61.89
9.54
0.72
5.31
1.22
20.34
Figu e 1. Sodium wa e glass AAS binde doped wi h Pb2+.
Figu e 2. Sodium ca bona e AAS binde doped wi h Pb2+.
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Figu e 3. Sodium hyd oxide AAS binde doped wi h Cu2+.
3.4. XPS analysis
The XPS spec a o Pb o sample Na-WG (1% Pb) is showed in igu e 4. The binding ene gies o Pb
4 7/2 and Pb 4 5/2 a e 138.6 eV and 143.3 eV. These alues a e ypical o Pb(OH)2. The highly soluble
p ima y phase Pb(NO3)2 dissol es du ing sample p epa a ion and Pb2+ ions in an alkaline solu ion
p ecipi a e in o an insoluble hyd oxide.
Figu e 4. XPS spec a o Pb in sample ac i a ed by sodium wa e glass.
In XPS spec a ( igu e 5) o a sample con aining coppe and ac i a ed by 50% solu ion o sodium
hyd oxide (1% Cu) a e shown wo di e en chemical s a es. The i s , Cu 2p3/2 componen wi h binding
ene gy 935.35 eV wi h s ong shake-up sa elli es belongs o Cu(OH)2. Shake-up sa elli es occu when
an ou going elec on in e ac s wi h a alence elec on and exci es i (shakes i up) o a highe ene gy
le el. As a consequence, he ene gy co e elec on is educed and a sa elli e s uc u e appea s a ew eV
below (KE scale) he co e le el posi ion. The second peak, Cu 2p3/2 wi h binding ene gy 933.50 eV,
ep esen s he bond be ween Cu and O. Tha can be in e p e ed as he o ma ion o coppe oxide o
130132134136138140142144146148150
in ensi y [a.u]
binding ene gy [eV]
Pb 4 7/2
Pb(OH)2
Pb 4 5/2
Pb(OH)2
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he o ma ion o he bond wi h he ma ix. Bo h coppe compounds (CuO and Cu(OH)2) a e insoluble
in dis illed wa e [17, 18].
Figu e 5. XPS spec a o Cu in sample ac i a ed by sodium hyd oxide.
4. Conclusion
The in luence o alkaline ac i a o ype on hea y me als (Pb and Cu) immobiliza ion was in es iga ed.
Fi e alkaline ac i a o s we e used: sodium wa e glass, po assium wa e glass, sodium hyd oxide,
po assium hyd oxide and sodium ca bona e. F om he esul s ob ained by leaching es s (ČSN EN
12457–4:2002) can be seen ha he immobiliza ion e iciency o hea y me als (Pb2+ and Cu2+) is e y
high o all ypes o alkaline ac i a o used. Sligh ly highe concen a ions o hea y me als in leacha es
we e obse ed when he samples we e ac i a ed by sodium wa e glass. I was p obably caused by
p esence o mic oc acks which allowed leaching ou hea y me als om samples. F om SEM obse a ion
can be seen ha bo h hea y me als – lead and coppe , we e a he cumula ed in some a eas han dispe se
h ough he whole s uc u e. Finally, XPS analysis con i med ha Pb and Cu o med insoluble sal s in
alkali-ac i a ed slag binde s.
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shake-up sa elli es
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