Removal of Carbonates

Reagents
Sodium acetate (CH3COONa3H2O), 1 M adjusted to pH 5 with glacial
acetic acid
Sodium hd!o"ide (NaOH), 1 M
Equipment
25#$m% plastic ce&t!i'uge (ottles with lids
Sti!!i&g !ods
1##$m% g!aduated cli&de!
)ate! (ath set at *#+C
Ce&t!i'uge with head 'o! 25#$m% (ottles
Procedure
1, )eigh out a su'-cie&t amou&t o' sample to p!o.ide the desi!ed
amou&t (5/1# g) o' cla (02 1m), a&d t!a&s'e! it to a 5##$m%
ce&t!i'uge (ottle la(eled with the sample ide&ti-catio& &um(e!, 2he
sample should ma3e a lae! i& the (ottom o' the ce&t!i'uge (ottle that
is &o mo!e tha& 1,5 cm thic3,
2, 4dd 1## m% o' the pH 5 acetate solutio& to the ce&t!i'uge (ottle,
mi", a&d place i& the wate! (ath, Chec3 'o! e5e!.esce&ce to co&-!m
dest!uctio& o' ca!(o&ates, 4'te! the (u((li&g stops, place the (ottle i&
the ce&t!i'uge a&d ce&t!i'uge at a(out 15## !pm 'o! 5 mi&, 6t is
impo!ta&t to ma3e su!e that the ce&t!i'uge is (ala&ced, 7eca&t a&d
disca!d the clea! supe!&ata&t 8uid,
Caution: 6t is impo!ta&t that the sample &ot (e allowed to e.apo!ate
to d!&ess o& the wate! (ath du!i&g a& o' the p!et!eatme&t
p!ocedu!es utili9ed,
3, :epeat Step 2,
;, 4dd 3# m% o' distilled wate! to the ce&t!i'uge (ottle, mi", a&d adjust
to a pH o' < to 1# with 1 M NaOH, 2he pH ma (e chec3ed usi&g pH
i&dicato! pape!, =lace the (ottle i& the ce&t!i'uge a&d ce&t!i'uge at
a(out 15## !pm 'o! 5 mi&, 7eca&t a&d dis$ ca!d the clea! supe!&ata&t
8uid, 6' the suspe&sio& is &ot 8occulated, add a 'ew d!ops o' satu!ated
NaCl to the ce&t!i'uge (ottle, mi", a&d ce&t!i'uge 'o! 5 mi&, 7eca&t a&d
disca!d the clea! supe!&ata&t 8uid,
REMOVAL OF ORA!"C MA##ER
O&ce the solu(le salts, gpsum, a&d ca!(o&ates ha.e (ee& !emo.ed
'!om a sample, i' &ecessa!, the &e"t step is to !emo.e the o!ga&ic
matte!, 6' soil a&d sedime&t samples co&tai& o!ga&ic matte!, the a!e
tpicall t!eated to !emo.e it (e'o!e cla mi&e!alogical a&alses, 2he
p!ese&ce o' o!ga&ic matte! ma !esult i& agg!egatio& o' soil pa!ticles,
a&d its !emo.al is &ecessa! i' su(se>ue&t a&alses !e>ui!e sample
dispe!sio& (?u&9e a&d 7i"o&, 1<*@), O!ga&ic matte! ma also cause a&
e"othe!mic !eactio& (etwee& 25# a&d 5##+C i& 724 studies,
4dditio&all, o!ga&ic matte! ma cause (ac3g!ou&d i&te!'e!e&ce a&d
p!e.e&t pa!allel o!ie&tatio& o' cla mi&e!als du!i&g p!epa!atio& o'
slides 'o! A:7 a&alsis (7ouglas a&d Biessi&ge!, 1<C1),
:emo.al o' o!ga&ic matte! '!om soils is ge&e!all accomplished usi&g
eithe! hd!oge& pe!o"ide (H2O2) o! sodium hpochlo!ite, 2hese two
methods a!e desc!i(ed i& the 'ollowi&g sectio&s, See Mi3utta et al,
(2##5) 'o! a comp!ehe&si.e !e.iew a&d histo! o' these methods,
$%drogen Pero&ide '$(O() Met*od
2he e5ecti.e use o' H2O2 'o! !emo.al o' o!ga&ic matte! !e>ui!es acidic
co&ditio&s, 2he!e'o!e, solu(le salts a&d ca!(o&ates that add al3ali&it
to the soil a!e !emo.ed (e'o!e !emo.al o' o!ga&ic matte!, 4!ti-cial
'o!matio& o' calcium o"alate is commo& whe& ca!$ (o&ates a!e p!ese&t
du!i&g H 2O2 o"idatio& o' o!ga&ic matte! (Ba!me! a&d Mitchell, 1<@3D
Mi3utta et al,, 2##5), 4 small amou&t o' glacial acetic acid ma (e
added to co&t!ol the o"idi9i&g e5ects o' ma&ga&ese o"ides, i' p!ese&t,
i& the sample (?u&9e a&d 7i"o&, 1<*@),Ma&ga&ese o"ides a!e .e!
st!o&g o"idi9i&g age&ts with o"idi9i&g pote&tials highe! tha& O2 (7i"o&
a&d )hite, 2##2),
Reagents
Hd!oge& pe!o"ide (H 2O2), 3#E
4cetic acid o! aceto&e, !eage&t g!ade
Sodium chlo!ide (NaCl), 1 M
Sodium chlo!ide (NaCl) satu!ated solutio&F Sha3e *# g o' !eage&t$g!ade
NaCl i& 2## m% o' wate!,
Equipment
25#$m% plastic ce&t!i'uge (ottles
Sti!!i&g !ods
Glt!aso&ic p!o(e o! .o!te" mi"e!
5$m% pipette (g!aduated)
)ate! (ath set at *#+C
Ce&t!i'uge with head 'o! 25#$m% (ottles
Procedure
1, 4dd app!o"imatel ;# m% o' wate! to the soil sample !emai&i&g i&
the ce&t!i'uge (ottle a'te! solu(le salts, gpsum, a&d ca!(o&ates ha.e
(ee& !emo.ed, Heat the (ottle to *#+C i& a wate! (ath o! o& a steam
ta(le,
2, 4dd app!o"imatel 2 m% o' H2O2 to the ce&t!i'uge (ottle, )he& the
o"idatio& o' o!ga&ic matte! (egi&s, as i&dicated ( '!othi&g, add a 'ew
d!ops o' acetic acid o! aceto&e a&d sti! co&sta&tl,
Caution: Se.e!e chemical (u!&s ca& !esult i' H2O2 comes i& co&tact
with the s3i&, 45ected a!eas should (e !i&sed tho!oughl with wate!
immediatel a'te! co&tact,
3, )he& the '!othi&g has su(sided, additio&al H2O2 should (e added to
the ce&t!i'uge (ottle i& app!o"imatel 1#$m% i&c!eme&ts, 2he solutio&
should (e sti!!ed co&sta&tl, a&d d!ops o' acetic acid o! aceto&e added
to co&t!ol '!othi&g,
;, :epeat Step 3 u&til a total o' 5# m% o' H2O2 has (ee& added,
!ote: 2he !ate at which the H2O2 is added depe&ds o& the .iole&ce o'
the '!othi&g that occu!s, Soils with high o!ga&ic matte! co&te&ts will
'!oth mo!e tha& those with low o!ga&ic matte! co&te&ts, Some soil ma
(e lost i' the solutio& o.e!8ows the (ottle du!i&g the !eactio& (etwee&
H 2O2 a&d o!ga&ic matte!, 6' M& o"ides a!e p!ese&t, the H 2O2 is
decomposed so that it is less e5ecti.e (o! i&e5ecti.e) at o"idi9i&g the
soil o!ga&ic matte!, Bi99i&g, !athe! tha& '!othi&g, !esults du!i&g the
e"othe!mic !eactio& o' M& o"ides, a&d H2O2 a&d ma cause the
suspe&sio& to o.e!8ow,
5, 2he o"idatio& o' o!ga&ic matte! is assumed to (e complete whe& a
total o' ap!o" 5# m% o' the 3#E H2O2 has (ee& added to the
ce&t!i'uge (ottle, a&d the '!othi&g !eactio& su(sides to mode!ate
(u((li&g, 2he (u((li&g is the !esult o' the the!mal decompositio& o'
H2O2, 2his will usuall ta3e se.e!al hou!s,
@, 4'te! H2O2 is decomposed a&d (u((li&g has su(sided, place the
(ottle i& the ce&t!i'uge a&d ce&t!i'uge at a(out 15## !pm 'o! 5 mi&, 6t
is impo!ta&t to ma3e su!e that the ce&t!i'uge is (ala&ced, 7eca&t a&d
disca!d the clea! supe!&ata&t 8uid, 6' the sample dispe!ses, add 2 o! ;
m% o' satu!ated NaCl solutio& a&d ce&t!i'uge agai&,
C, 4dd 1## m% o' 1 M NaCl solutio& to the ce&t!i'uge (ottle, dispe!se
the soil, a&d ce&t!i'uge at a(out 15## !pm 'o! 5 mi&, 7eca&t a&d
disca!d the clea! supe!&ata&t 8uid,
*, :epeat Step C,
<, 2he sample is &ow !ead 'o! !emo.al o' o"ides o! dispe!sio& a&d
pa!ticle$si9e '!actio&atio&,
REMOVAL OF "RO! O+",E-
2he p!ese&ce o' '!ee o"ides a&d hd!ous o"ides o' 4l, Be, M&, Si, a&d 2i
ma ma3e it di'-cult o! impossi(le to dispe!se soil samples (e'o!e
'!actio&atio& p!ocedu!es (ecause these compou&ds ma act as
ceme&ti&g age&ts, 2hese compou&ds ma e"ist i& c!stalli&e, poo!l
c!stalli&e (sho!t$!a&ge o!de!), a&dHo! &o&c!stalli&e (amo!phous)
'o!ms i& soils as a !esult o' pedoge&ic p!ocesses, 6& pa!ticula!, the
!emo.al o' '!ee i!o& o"ides e&ha&ces the pa!allel o!ie&tatio& o' lae!
silicate clas a&d allows 'o! the detectio& o' A$!a di5!actio& pea3s that
might othe!wise (e o(scu!ed (Meh!a a&d Iac3so&, 1<@#),
Most o' ou! e"isti&g i&'o!matio& o& 4l, Be, M&, Si, a&d 2i o"ides a&d
hd!o"ides i& soils has (ee& de!i.ed '!om selecti.e chemical
dissolutio& (SC7) a&alses, Selecti.e chemical dissolutio& a&alses
ma (e pe!'o!med eithe! o& the u&t!eated 02$mm soil '!actio& o! the
cla (02$1m) '!actio&, 7etailed i&'o!matio& co&ce!&i&g SC7 tech&i>ues
a&d thei! applica(ilit to 4l, Be, M&, Si, a&d 2i o"ides a&d hd!o"ides
a!e p!o.ided ( Sha&g a&d Jela9& (2##*, this .olume),
Reagents
Cit!ate (u5e! solutio&, comp!ised o' the 'ollowi&g two !eage&tsF
Sodium cit!ate, #,3 M Na3C@H5OC2H2O (** g %$1)
Sodium (ica!(o&ate, 1 M NaHCO 3 (*; g %$1)
=!emi" these !eage&ts at a !atio o' *F1 cit!ateH(ica!(o&ate solutio&s
(i,e,, ;# m% o' #,3 M sodium cit!ate to 5 m% o' 1 M sodium
(ica!(o&ate),
Sodium dithio&ite powde! (Na 2S2O;)
Sodium chlo!ide (NaCl) 1 M
Satu!ated NaCl solutio&
4ceto&e, !eage&t g!ade
Equipment
25#$m% plastic ce&t!i'uge (ottles
Sti!!i&g !ods
1##$m% g!aduated cli&de!
Glt!aso&ic p!o(e o! .o!te" mi"e!
)ate! (ath set at *#+C
Ce&t!i'uge with head 'o! 25#$m% (ottles
4&altical (ala&ce
Procedure
!ote: 2his p!ocedu!e p!oduces a st!o&g K!otte& eggL smell with
i!!itati&g 'umes a&d
should (e co&ducted u&de! a .e&tilated 'ume hood,
1, Ce&t!i'uge a&d disca!d the clea! supe!&ata&t '!om the p!e.ious
t!eatme&t 'o! !emo.al o' o!ga&ic matte! o! solu(le salts,
2, 4dd 2# to 3# m% o' satu!ated NaCl solutio& a&d 3## m% o' distilled
wate! to the ce&t!i'uge (ottle, mi", a&d dispe!se the sample, =lace the
(ottle i& the ce&t!i'uge a&d ce&t!i'uge at a(out 15## !pm 'o! 5 mi&, 6t
is impo!ta&t to ma3e su!e that the ce&t!i'uge is (ala&ced, 7eca&t a&d
disca!d the clea! supe!&ata&t 8uid,
3, 4dd 2## M5 m% o' cit!ate (u5e! solutio& a&d heat the (ottle to C5 to
*#+C i& a wate! (ath,
;, )he& the sample !eaches C5 to *#+C, add app!o"imatel 2 g o' Na
2S2O; to the (ottle, Sti! co&ti&uousl 'o! 1 mi&, a&d the& occasio&all
'o! 5 mi&,
5, 4dd a seco&d 2$g po!tio& o' Na2S2O; to the (ottle a&d sti! as
desc!i(ed a(o.e,
@, 4dd a ;$g po!tio& o' Na2S2O; a&d sti! as desc!i(ed a(o.e,
C, 4'te! 1# to 15 mi&, !emo.e the (ottle '!om the wate! (ath a&d cool,
=lace the (ottle i& the ce&t!i'uge a&d ce&t!i'uge at a(out 15## !pm 'o!
5 mi&, 7eca&t a&d disca!d the clea! supe!&ata&t 8uid,
*, 4dd 2# m% o' satu!ated NaCl solutio&, 2# m% o' aceto&e, mi", a&d
dispe!se the sample, =lace the (ottle i& the ce&t!i'uge a&d ce&t!i'uge
at a(out 15## !pm 'o! 5 mi&, 7eca&t a&d disca!d the clea! supe!&ata&t
8uid,
<, 4dd 2## m% o' 1 M NaCl solutio& to the (ottle, mi", a&d dispe!se the
sample, =lace the (ottle i& the ce&t!i'uge a&d ce&t!i'uge at a(out 15##
!pm 'o! 5 mi&, 7eca&t a&d disca!d the clea! supe!&ata&t 8uid,
1#, :epeat Step <,
-eparation of Cla% '.( /m)
2he 'ollowi&g p!ocedu!e is (ased o& the use o' a 25#$m% ce&t!i'uge
(ottle, &o mo!e tha& 1,5 cm o' sedime&t, a&d < cm to the top o' the
suspe&sio& i& the (ottle, 4s stated a(o.e, the a&alst &eeds to chec3
the e>uipme&t (ei&g utili9ed 'o! '!actio&atio& pu!poses a&d adjust the
e>uatio& 'o! calculati&g ce&t!i'ugi&g times as app!op!iate,
1, Ma3e a ma!3 o& the ce&t!i'uge (ottle at < a&d 3 cm '!om the (ottom
o' the (ottle, 2he sedime&t i& the (ottle should (e app!o"imatel 1,5
cm i& thic3&ess,
2, 4dd deio&i9ed wate! up to the <$cm ma!3 o& the (ottle,
3, Mi" tho!oughl a&d the& ce&t!i'uge at 5## !pm 'o! @ mi&,
;, Sipho& the 02$1m '!actio& i& suspe&sio& '!om 3 cm a(o.e the
(ottom o' the (ottle i&to a 1###$ o! 2###$m% (ea3e!, 6' the sample is
dispe!sed, the suspe&sio& should (e cloud o! tu!(id, 6' the sample is
&ot dispe!sed, as i&dicated ( a clea! suspe&sio&, the clea!
supe!&ata&t ca& (e pou!ed o5 a&d disca!ded, 6' the sample 'ails to
dispe!se, add o&e d!op o' satu!ated NaCl solutio&, !emi" the sample,
a&d ce&t!i'uge, Ca!e should (e ta3e& to e&su!e that &o po!tio& o' the
sedime&t i& the (ottom o' the (ottle, o! (elow the 3$cm ma!3, is
sipho&ed o5 o! disca!ded du!i&g this p!ocedu!e,
5, :epeat Steps 2 th!ough ; se.e!al times u&til the suspe&sio& is clea!
o! o&l slightl cloud 'ollowi&g ce&t!i'ugatio&, 6& ou! e"pe!ie&ce, eight
!epetitio&s a!e ge&e!all ade>uate to e5ecti.el sepa!ate the 02$1m
'!actio&, N"cessi.e !epetitio&s ma p!oduce cla mecha&icall,
@, 2he suspe&sio& i& the (ea3e! &ow co&tai&s the Na$satu!ated cla ( 0
2$1m) '!actio& '!om ou! sample,
Flocculation of t*e Cla%
2he cla '!actio& is suspe&ded i& a !athe! la!ge .olume o' wate!
'ollowi&g '!actio&atio&, 2he wate! co&te&t should (e !educed 'o!
sto!age a&d su(se>ue&t a&alses, Blocculatio&(chemicall i&duced
agg!egatio&) o' cla i& suspe&sio& g!eatl i&c!eases the !ate o' pa!ticle
settli&g, a&d p!oduces a clea! supe!&ata&t that ca& (e sipho&ed o5 to
achie.e the .olume !eductio&, 2he!e a!e se.e!al p!ocedu!es to
8occulate cla i& suspe&sio&, 2he (est p!ocedu!e depe&ds somewhat
o& the cha!acte!istics o' the sample, 2he easiest method is to add
satu!ated NaCl to the suspe&sio&, sti!, co.e!, a&d allow to settle 'o!
se.e!al hou!s, 2he i&c!ease i& io&ic st!e&gth with the additio& o' the
satu!ated NaCl !educes dou(le lae! thic3&ess, allowi&g pa!ticles to
app!oach closel e&ough so that 'o!ces o' att!actio& ca& i&duce
8occulatio&, Howe.e!, some samples do &ot !eadil 8occulate with
NaCl, 4&othe! method is to adjust the pH close to the 9e!o poi&t o' &et
cha!ge 'o! the majo! mi&e!al compo&e&ts a&ticipated i& the sample,
Bo! e"ample, adjusti&g the pH to a(out ;,# is sometimes e5ecti.e i&
i&duci&g 8occulatio& 'o! cla '!om acidic soils domi&ated ( 3aoli&ite,
2he pH should (e adjusted (ac3 to a !a&ge suita(le 'o! sta(le sto!age
o&ce 8occulatio& has (ee& achie.ed to p!e.e&t mi&e!alogical a&d
othe! sample cha&ges caused ( the acid used 'o! 8occulatio&,