1
Op imiza ion o wo me hods based on ul asound ene gy as
al e na i e o Eu opean s anda ds o soluble sal s ex ac ion
om building ma e ials
N. P ie o-Taboada*, O. Gómez-Lase na, I. Ma inez-A ka azo, M.A. Olazabal and J.M.
Mada iaga
Depa men o Analy ical Chemis y, Uni e si y o he Basque Coun y, (UPV/EHU), Ba io Sa iena s/n, 48940, Leioa, Spain.
Email*: nago e.p ie [email protected] Tel.: +34 94 601 82 94; Fax.: +34 94 601 35 00
Abs ac
The I alian ecommenda ion NORMAL 13/83, la e eplaced by he UNI 11087/2003 no m,
we e used as s anda d o soluble sal s ex ac ion om cons uc ion ma e ials. These
s anda ds a e based on long- ime s i ing (72 and 2 hou s, espec i ely) o he sample in
deionised wa e . In his wo k wo ul asound based me hods we e op imized in o de o
educe he ex ac ion ime while e iciency is imp o ed. The ins umen al a iables in ol ed
in he ex ac ion assis ed by ul asound ba h and ocused ul asounds we e op imized by
expe imen al design. As long as i was possible, he same non ins umen al pa ame e s alues
as hose o s anda d me hods we e used in o de o compa e he esul s ob ained on a mo a
sample showing a black c us by he s anda ds and he op imized me hods. The op imal
ex ac ion ime o he ul asounds ba h was ound o be o wo hou s. Al hough he ex ac ion
ime was equal o he s anda d UNI 11087/2003, he ob ained ex ac ion eco e y was
imp o ed up o 119%. The ocused ul asound sys em achie ed also be e eco e ies (up o
106%) depending on he analy e in one hou ea men ime. The epea abili ies o he
p oposed ul asound based me hods we e compa ables o hose o he s anda ds. The e o e,
he selec ion o one o he o he o he ul asound based me hods will depend on opics such
This is he accep ed manusc ip o he a icle ha appea ed in inal o m in Ul asonics Sonochemis y 19(6) : 1260-1265 (2012),
which has been published in inal o m a h ps://doi.o g/10.1016/j.ul sonch.2012.03.002. © 2012 Else ie unde CC BY-NC-ND
license (h p://c ea i ecommons.o g/licenses/by-nc-nd/4.0/)
2
as labo a o y acili ies o numbe o samples, and no in aspec s ela ed wi h hei quali y
pa ame e s.
1 INTRODUCTION
Soluble sal s a e conside ed de e io a ion compounds o med by eac ion among acid gases
p esen in pollu ed en i onmen s and di e en cons uc ion ma e ials. They can also
accumula e h ough in il a ion o wa e cha ged o sal s o hey can be pa o he o iginal
composi ion. In e e y way, hey a e one o he mos impo an de e io a ion ac o s o
cons uc ions ma e ials, especially in ca bona e based s ones such as limes one [1-5]. The
cha ac e iza ion o sal s in cons uc ion ma e ial is e y impo an because he damage hey
cause (c acking and ma e ial loss) depends on hei con en and na u e. Fo ins ance, sal s
ha ing se e al hyd a ion s a es wi h subs an ial molecula olume di e ences such as
mi abili e (Na2SO4·10H2O) and hena di e (Na2SO4) a e usually ound causing his e ec . The
ansi ion om one o ano he occu s a a wide ange o common empe a u e and ela i e
humidi ies wi h a densi y change om 1.49 o 2.7 g /cm3 [6-9]. Fu he mo e, such sal s a e
e en mo e damaging when o ming as sube lo escences because hey p oduce highe ma e ial
losses by he so called pla e damage o sal wea he ing [10, 11]. The e o e, he es ablishmen
o he soluble sal s con en could be essen ial when cons uc i e elemen s o buildings a e
going o be es o ed o he cons uc ion ma e ial is going o be eused [12].
Among cons uc ion ma e ials, mo a s ha e shown o be he mos suscep ible o su e om
he men ioned pa hologies due o hei po osi y ha acili a es he pene a ion o he sal s deep
in he ma e ial. Mo a s a e common cons uc ion ma e ial used in buildings no only as
3
binde s bu also wi h embellishing o deco a i e pu poses. The e o e, a good conse a ion
s a e o hese ma e ials is essen ial o p ese e he in eg i y o he building. Nowadays, hey
a e gene ally composed by conc e e, a id (usually sand o milled sands one), wa e and
addi i es in some cases. Howe e , in he ield o cul u al he i age he composi ion o mo a s
is limi ed o he aw ma e ials a ailable in he su oundings and hus, hey a e commonly
composed o calci e o gypsum ha cemen he a id g ains. Mo a s su e a as e deg ada ion
when beach sand is used as a id, due o i s high concen a ion o chlo ides ha a e e y
soluble [13, 14]. Fo all he men ioned, he de e mina ion o he soluble sal s con en is
especially impo an in mo a s.
In his sense, he mos common and haza dous soluble sal s ound in cons uc ion ma e ials,
since hey a ec o hei in eg i y, a e sulpha es, ni a es, chlo ides and
ca bona es/bica bona es [15]. Usually, he soluble sal s a e p esen in black c us s ha o en
appea co e ing acades p o ec ed om ain washing [16-18]. Al hough gypsum
(CaSO4·2H2O) and pa icula e ma e (soo , me als, o ganics,…) a e he p incipal componen s
o his kind o o ma ion, ni a es ha e been also ound a conside able concen a ion le els in
ecen s udies due o he inc ease o he impac o NOx gases [7, 19, 20].
Despi e i is well known ha sal s excess is comple ely ha m ul o he in eg i y o
cons uc ion ma e ials he e is no a global legisla ion conce ning he sa e y amoun s (in e ms
o ma e ial in eg i y) in building ma e ials. Only sulpha e and chlo ide concen a ions in
ma e ials and he wa e used wi h cons uc ion pu poses is con olled. Fo ins ance, acco ding
o he S uc u al Conc e e Ins uc ion EHE-08, app o ed by Royal Dec ee in 2008 in Spain
he concen a ion in he o iginal ma e ial should no exceed 0.8% w/w and 0.05% w/w o
sulpha e and chlo ide espec i ely.
4
The analyses ela ed wi h he soluble sal s con en in building a e ca ied ou by p o ocols
ecommended by di e en Eu opean s anda diza ion o ganiza ions used in di e en coun ies
as I aly, Ge many, B i ain, Sweden, Spain o F ance [21-27]. Besides, due o he impo ance
o he de e mina ion o o al soluble sal con en in such ma e ials, especially in he ield o
Cul u al He i age p o ec ion, a global Eu opean s anda d me hod ela ed o he
“De e mina ion o soluble sal s in na u al s ones and ela ed a i icial ma e ials used in
cul u al he i age” is cu en ly being de eloped [28]. One o he mos classical me hods is he
I alian NORMAL 13/83 p o ocol [29] which in ol es a 72 hou ea men . This no m was
la e eplaced by he UNI 11087/2003 [21]. Bo h me hods, as well as mos o he s anda ds,
a e based in he simply s i ing o he sample, bu he ad an age o he UNI 11087/2003 no m
o e he NORMAL 13/83 no m was ha ex ac ion ime is sho ened ill 2 hou s.
As al e na i e, new p ocedu es o moni o in si u soluble sal s con en in s one ma e ials a e
being de eloped [19, 30] and an ul asound ene gy based me hod applied o his ield can be
ound in bibliog aphy [7, 31]. Howe e , he eal possibili ies o his ins umen a ion o
imp o e he ac ual s anda d no ms ha e no been e alua ed in dep h. On he con a y, he use
o echniques based on ul asound ene gy has g own in he las yea s due o hei e ec i eness
and simplici y. Ul asound ene gy is used o many applica ions as al e na i e ex ac ion
me hod, o example, o mic owa e ex ac ion. The ul asound ba h (USB) is one o he mos
common ins umen s used nowadays o accele a ed ex ac ions due o i s simplici y and
e ec i eness. On he o he hand, ocused ul asound (FUS) sys ems ha apply he ul asound
ene gy h ough a ip imme sed di ec ly in he sample, a e becoming mo e and mo e popula
because, among o he s, o i s highe epea abili y [32]. Despi e FUS has been used wi h good
5
esul s in o he ields he use o his echnique has no been desc ibed o he ex ac ion o
soluble sal s up o now.
The aim o he p esen s udy was o op imize he ex ac ion o soluble sal s om mo a s
assis ed by ul asound ba h (USB) and ocused ul asound sys ems (FUS) and subsequen ly,
o compa e he e iciency o ul asound assis ed ex ac ion me hods wi h he cu en ly used
s anda ds.
2 MATERIAL AND METHODS
2.1 Samples
A ende ing mo a showing a black c us was used in he p esen s udy. The sample belonged
o a building loca ed in a highly indus ialized neighbou hood o Bilbao which has su e ed
se e al loods in he pas due o he closeness o he Ne bion-Ibaizabal Ri e . The samples
wi h black c us ha e a high soluble sal s concen a ion due o he capaci y o black c us o
ap con aminan s [18, 19]. The e o e, he ende ing mo a o he building was conside ed an
app op ia e sample o e alua e he soluble sal s ex ac ion me hods. This ac was con i med
by means o Raman spec oscopy measu emen s. An InnoRam BW&Tek handheld Raman
spec ome e was also used in o de o iden i y he o iginal composi ion o he mo a and he
deg ada ion compounds. The equipmen is composed o a 785nm lase and a Pel ie cooled
CCD de ec o . The signal is ansmi ed by an op ic ibe connec ed o a p obe, which o e s
he possibili y o pe o m mic oscopic analysis by using di e en op ical lens (4x, 20x and
50x) in a ange o 3000-100 cm-1 (non changeable) wi h a spec al esolu ion o 3.5 cm-1.
Acco ding o he spec a ob ained on he mo a , i was mainly composed o calci e, i on
oxides and aluminosilica es as shown in igu e 1. The sui abili y o his echnique has been
6
widely demons a ed o cha ac e iza ion o o iginal composi ion and soluble sal s in p e ious
wo ks [18, 19, 33]. Wi h ega d o he soluble sal s, sulpha es (mainly gypsum, CaSO4·2H2O)
and ni a es we e he mayo sal s ha we e iden i ied by Raman (see Figu e 1) bu also
chlo ides we e ound by means o ion ch oma og aphy ollowing a p ocedu e desc ibed
elsewhe e [34], wi h a o al soluble sal con en o app oxima ely 8% w/w.
In o de o ob ain a homogeneous sample, he mo a was g inded i s ly in a ball mill
Pul e ise e om F i sch and hen wi h an aga e mo a . A e , he sample was d ied a 60ºC
o 24 hou s. This ea men allows o achie e sample wi hou humidi y and a homogeneous
pa icle size. The sample was kep in a desicca o ill he ex ac ion ea men .
2.2. Ins umen s
2.2.1 Ul asound based sys ems
An Ul asons-H ba h om P-Selec a wi h a wo king equency o 40 kHz (1000 W) was used
o op imize he ex ac ion by he ul asound ba h. The conduc i i y was moni o ed wi h a
C ison CM/35 po able conduc i i y me e om C ison Ins umen s o de ine he op imal
ex ac ion ime as ecommended in he NORMAL 13/83 me hod [29, 35].
The ocused ul asound (FUS) sys em used o he op imiza ion was an HD 2070 Sonopuls
Ul asonic Homogenize om Bandelin equipped wi h a GM 2070 gene a o (maximum 70W,
20 kHz), an UW 2070 ul asonic con e e a SH 70G ho n and a MS 73 i anium p obe
(3mm). In his case he i anium p obe was chosen because i allows powe se ing ill 100%
ins ead o 30% o he glass p obe. Acco ding o he echnical equi emen s he maximum
ex ac ion olume is 50 ml in o de o assu e a co ec ul asound ene gy ansmission.
7
Finally, in o de o accomplish he ex ac ion acco ding o Eu opean no ms he s i ing o he
samples was ca ied ou by a P-Selec a Asinc o s i e (30W).
2.2.2. Quan i a i e analysis by Ion Ch oma og aphy
Wi h he aim o compa ing he esul s ob ained by s anda d me hods and p oposed ul asound
based me hods, he ex ac ed sal s we e quan i ied by a Dionex ICS 2500 ionic
ch oma og aph wi h an ED50 supp essed conduc i i y de ec o . An IonPac AS23 (4×250 mm)
column and IonPac AG23 (4×50 mm) p ecolumn om Ve ex we e used o he sepa a ion o
anions ( luo ide, chlo ide, sulpha e and ni a e). The quan i ica ion o ca ions (sodium,
po assium and calcium) was conduc ed by using an IonPac CS12A (4×250 mm) column and
IonPac CG-12A (4×50 mm) p ecolumn om Ve ex. The ch oma og aphic condi ions used in
anion quan i ica ion we e 5 mM Na2CO3/0.8 mM NaHCO3, 25 mA and 1 ml/min as mobile
phase, supp ession cu en and low, espec i ely. In he case o ca ions 20 mM CH4SO3 as
mobile phase, 59 mA o supp ession cu en and 1 ml/min low we e used. P io o he
analysis he samples we e il e ed wi h a 0.45 µm nylon sy inge il e s and b ough o a inal
olume.
2.3. Op imiza ion o he ul asound assis ed ex ac ion
Ul asound ba h and ocused ul asound condi ions we e op imized o ca y ou sal s
ex ac ion. Fou eplica es o he ex ac ion we e ca ied ou a he op imum alues and he
esul s we e assessed by compa ison wi h hose ob ained wi h s anda ds (NORMAL 13/83
and UNI 11087/2003). Sample weigh and wa e olume we e kep cons an in he
op imiza ion: 100 mg o sample and 100 ml o deionised wa e . Tha is, only ins umen al
a iables we e s udied.
8
2.3.1. Ul asound ba h op imiza ion
The unique ins umen al a iable o op imize in he ul asound ba h was he ex ac ion ime.
The op imal ex ac ion ime was es ablished a he maximum cons an (conduc i i y/sample
weigh ) acco ding o he con inuous measu emen s pe o med on each o he ou eplica es.
2.3.2. Focused ul asound op imiza ion
The a iables o op imize we e powe se ing (P, 0–100%) which allows con olling
ampli ude o he deli e ed ul asound, cycles (c, 1-9) and ex ac ion ime ( ). Cycles a e an
ins umen al a iable ha indica es a pulsed mode; o ins ance, cy = 4 means a 0.4 s ac i e
pe iod ollowed by a 0.6 s passi e pe iod [32]. Acco ding o ins umen al equi emen s, and
in o de o a oid ecommended limi alues, he ex ac an olume was se a 45 ml. These
ins umen al equi emen s a om being nega i e, could in ol e o ob ain concen a ions
abo e de ec ion limi s in some cases, since he inal olume is educed.
A ull ac o ial design was ca ied ou in o de o de e mine he signi ican a iables om he
ini ial hypo hesis. Powe (10-90%), cycles (1-9) and ex ac ion ime (5-100 min) we e s udied
h ough quan i ica ion by ionic ch oma og aphy. The h ee a iables we e checked ill he
maximum ixable alue excep o he powe , o which 90% was se as maximum alue in
o de o p ese e he ip om damage. The high le el o ime was de e mined by he
maximum wo king ime o he ins umen . The signi icance o he ci ed a iables was
analysed by a ull ac o ial design accomplished by he UnSc amble 9.2 so wa e [36].
A e , a cen al composi e design (CCD) was ca ied ou o de e mine he op imal condi ions
wi h he signi ican a iables. NLREG 6.3 p og am [37] was also used o de e mine he
esponse equa ions o each o he analy es.
9
2.4. Compa ison o op imized ul asound me hods wi h s anda ds
The I alian NORMAL 13/83 o 1983 and i s ac ualiza ion so called UNI 11087/2003 we e
used o ex ac he soluble sal s om he mo a in o de o compa e hei ex ac ion
capabili ies as well as o assess he sui abili y o he op imized me hods. Bo h s anda d
me hods consis on s i ing o 100mg o he sample in 100ml o deionised wa e . The
di e ence be ween hem is ha ex ac ion ime was educed om 72 hou s o 2 hou s in he
UNI 11087/2003 me hod. The non ins umen al pa ame e s we e kep cons an as a as i was
possible in he op imiza ion o he ul asound based me hods. Fou eplica es o he samples
we e pe o med by each o he me hods o accomplish he compa ison s ep.
3 RESULTS AND DISCUSSION
3.1 Op imiza ion o he ul asound assis ed ex ac ion
3.1.1. Ul asound ba h op imiza ion
The ex ac ion o he sal s by he ul asound ba h was op imized by moni o ing he
conduc i i y a di e en ex ac ion imes. Besides, he empe a u e a di e en posi ions o he
ba h was moni o ed as well. Tempe a u e showed di e en ends in he ba h depending o he
posi ion o he bake , which could a ec o he epea abili y o he analysis and he e o e o
he elec ion o he op imal ime. The empe a u e inc eased om oom empe a u e o 51ºC
wi h di e ences up o 4ºC depending on he posi ion o he bake in he ba h. Figu e 2 shows
ha maximum conduc i i y alue was achie ed app oxima ely a 100 minu es o some
samples. Howe e , 120 minu es was chosen as ex ac ion ime in o de o ensu e cons an
conduc i i y alues. The mos ele a ed empe a u es obse ed in he di e en posi ions in he
ba h seemed no o be ela ed wi h maximum conduc i i y alues achie ed in he ex ac ion.
In addi ion, e-adso p ion phenomena we e also occasionally obse ed as can be seen in
Figu e 2 (se ie A).
16
[13] A. Sil a, T. C uz, M. Pai a, A. Candeias, P. Ad iano, N. Schia on, J. Mi ão, En i on.
Ea h Sci. 63 (2011) 1641-1650.
[14] E.A.L. Cos a, V.P. Campos, L.C.P. da Sil a Filho, H.A. G e en, J. En i on. Manage. 90
(2009) 1060-1068.
[15] H. B ocken, T.G. Nijland, Cons . Build. Ma e . 18 (2004) 315-323.
[16] P. Ma a elaki-Kalai zaki, Anal. Chim. Ac a 532 (2005) 187-198.
[17] C. Sabbioni, G. Zappia, N. Ghedini, G. Gobbi, O. Fa oni, A mos. En i on. 32 (1998)
215-223.
[18] N. P ie o-Taboada, M. Magu egui, I. Ma inez-A ka azo, M. Olazabal, G. A ana, J.
Mada iaga, Anal. Bioanal. Chem. 399 (2010) 2949-2959.
[19] I. Ma ínez-A ka azo, M. Angulo, L. Ba olomé, N. E xeba ia, M.A. Olazabal, J.M.
Mada iaga, Anal. Chim. Ac a 584 (2007) 350-359.
[20] S.W. Massey, Sci. To al En i on. 227 (1999) 109-121.
[21] UNI 11087:2003. Beni cul u ali - Ma e iali lapidei na u ali ed a i iciali. De e minazione
del con enu o di sali solubili, En e Nazionale I aliano di Uni icazione (UNI), (2003).
[22] WTA 4-5-99: E alua ion o mason y, WTA-Me kblä e , (1999).
[23] BS EN 772-5:2001 Me hods o es o mason y uni s. De e mina ion o he ac i e
soluble sal s con en o clay mason y uni s, The B i ish S anda ds Ins i u ion (BSI), (2002).
[24] SIS EN 1015-17/A1:2004 Me hods o es o mo a o mason y - Pa 17:
De e mina ion o wa e -soluble chlo ide con en o esh mo a s, Swedish S anda ds Ins i u e
(SIS), (2004).
[25] DIN 5110: Tes ing o ce amic aw ma e ials and ma e ials; de e mina ion o soluble sal s
(pe cola ion me hod), Deu sches Ins i u Fu No mung E.V. (Ge man Na ional S anda d),
(1957).
[26] UNE EN 1744-5:2006 Tes s o chemical p ope ies o agg ega es - Pa 5:
De e mina ion o acid soluble chlo ide sal s, Asociación Española de No malización y
Ce i icación (AENOR), (2007).
[27] NF EN 1744-5: Tes s o chemical p ope ies o agg ega es - Pa 5 : de e mina ion o
acid soluble chlo ide sal s, Associa ion F ançaise de No malisa ion (AFNOR), (2007).
[28] Eu opean Commi ee o S anda diza ion (CEN) h p://www.cen.eu .
[29] Raccomandazioni No mal 13/83: Dosaggio dei Sali solubili (No mal 13/83
ecommenda ion: De e mina ion o To al Amoun o Soluble Sal s, Consiglio Nazionale delle
Rice che and Is i u o Cen ale del Res au o (CNR-ICR), (1983).
17
[30] C. T opea, M.P. Samma ino, G. Visco, Cu . Anal. Chem. 6 (2010) 94-99.
[31] A.C. Iñigo, R. Alonso, S. Vicen e-Ta e a, Ul ason. Sonochem. 8 (2001) 127-130.
[32] S. Fdez-O iz de Vallejuelo, A. Ba ena, G. A ana, A. de Diego, J.M. Mada iaga, Talan a
80 (2009) 434-439.
[33] M. Pé ez-Alonso, K. Cas o, I. Ma ínez-A ka azo, M. Angulo, M.A. Olazabal, J.M.
Mada iaga, Anal. Bioanal. Chem. 379 (2004) 42-50.
[34] E. Pin o Gue a, Rissanamen o di mu a e umide e deg ada e, second ed., Da io
Flacco io, I alia, 2011.
[35] H. S ahn, Non-des uc i e ield es s in s one conse a ion, Riksan ik a ieämbe e ,
S ockholm, 2006.
[36] Camo P ocess, 9.2 (2005).
[37] P.H. She od, (1992-2005).
[38] A.F. Whi e, S.L. B an ley, Chem. Geol. 202 (2003) 479-506.
18
Table 1.- Ex ac ion alues o he I alian s anda d NORMAL 13/83 and he UNI 11087/2003
exp essed in mg/kg, as well as he eco e y o he analy es o he UNI 11087/2003 s anda d in
compa ison o p eceding no m.
Table 2.- Resul s in mg/kg ob ained by ion ch oma og aphy o he expe imen s o he CCD
designed o he FUS me hod op imiza ion.
Table 3.- Summa y o he pa ame e alues ixed o he p oposed ul asound me hodologies
and s anda ds used in he p esen wo k.
19
Figu e 1.- Raman spec a o he black c us ed mo a used in his wo k. a) calci e, gypsum
some ni a es and silica es , b) sulpha es and i on oxides c) calci e and shoo , d) gypsum
Figu e 2.- Resul s ob ained o some o he posi ion (se ies) in he ul asound ba h du ing
moni o ing o he co ec ed conduc i i y (conduc i i y/sample weigh ) a di e en ex ac ion
imes.
Figu e 3.- Rep esen a ion o he concen a ion in mg/kg ob ained wi h he di e en p o ocols:
1 NORMAL 13/83, 2 UNI 11087/2003, 3 USB and 4 FUS
Figu e 4.- Summa y o he s eps o be ollowed o accomplish he ex ac ion me hods
op imized in his wo k.
1
Table 1.- Ex ac ion alues o he I alian s anda d NORMAL 13/83 and he UNI 11087/2003 exp essed in mg/kg, as well as he eco e y o he
analy es o he UNI 11087/2003 s anda d in compa ison o p eceding no m.
CHLORIDE
NITRATE
SULPHATE
SODIUM
POTASIUM
CALCIUM
NORMAL 13/83
2284
1945
38386
2043
988
31865
S anda d de ia ion
36
102
333
341
68
5535
RSD
2%
5%
1%
17%
7%
17%
UNI 11087/2003
2071
1723
36955
959
770
27200
S anda d de ia ion
15
38
246
50
13
801
RSD
1%
2%
1%
5%
2%
3%
Reco e y
91%
89%
96%
47%
78%
100%
1
Table 2.- Resul s in mg/kg ob ained o he expe imen s o he CCD designed o he FUS me hod op imiza ion.
Time (min)
Powe
Cycles
Chlo ide
Ni a e
Sulpha e
Sodium
Po assium
Calcium
*L:A-a
4.98
50
5
1637
1255
37699
678
491
23391
*H:A-a
99.98
50
5
1997
1603
38834
826
637
23238
*L:B-a
52.5
10
5
2173
1480
38526
1296
310
24502
*H:B-a
52.5
90
5
1954
1569
38635
807
663
23314
*L:C-a
52.5
50
1
2176
1467
38311
1317
291
21602
*H:C-a
52.5
50
9
2322
1597
39546
1421
426
24087
Cube001a
22.8
25
3
2044
1436
38803
1292
291
22643
Cube002a
82.2
25
3
2164
1536
38650
1251
276
23935
Cube003a
22.8
75
3
1798
1474
39073
751
530
22096
Cube004a
82.2
75
3
2282
1609
39308
1310
353
24046
Cube005a
22.8
25
8
1939
1501
40034
792
589
24266
Cube006a
82.2
25
8
2312
1576
39603
1406
388
22463
Cube007a
22.8
75
8
1952
1531
39676
807
637
23216
Cube008a
82.2
75
8
2103
1672
39209
880
736
23620
Cen -a
52.5
50
5
2070
1652
40472
852
680
24105
Cen -b
52.5
50
5
1991
1579
39228
827
658
23461
Cen -c
52.5
50
5
1942
1572
39007
814
644
23096
1
Table 3.- Summa y o he pa ame e alues ixed o he p oposed ul asound me hodologies and s anda ds used in he p esen wo k.
STANDARDS
CURRENT WORK
NORMAL 13/83
UNI 11087/2003
USB
FUS
Weigh (g )
0.1
0.1
0.1
0.1
Volume (ml)
100
100
100
45
Time (h)
72
2
2
1
Me hod
Agi a ion
Agi a ion
Ul asound ba h
Focused ul asound
