S~~

P l l I \L . 3000. ~~-\1,
~
-
-
a.<i i fllJ..-
._~--a..e
1 a,q 5-
METALS (3000)
3030 C.
,
Treatment for Actd-Extractable Metais
', ; '"
~ ~ , r J
~ffJrtJ. , ' v .V
3030.0.,;: Digestion for Metais
, -, ~
Extractabl e .metl s are l i ghtl y adsorbed on parti cul ate mate-
ri al : Because somesampl e di gesti on may be unavoi dabl e use
ri gi dl y. control l ed condi ti ons .to obtai n meani ngful and repro-
duci bl e resul ts. Mai ntai n constant sampl e vol ume, aci d vol ume,
and contact ti me. !Express resul ts asextractabl e metal sand spec-
i fy extractorrrcondi ti ons. ' !'
At col l ecti on, aci di fy enti re sampl e wi th 5 mL cone HN03/L
sampl e: To prepare sampl e, mi xwel l , transfer 100mL to a-beaker
. i
To reduce i nterference by organi c matter and to convert metal
associ ated wi th parti cul ates to a form (usual l y-the fr~~]:netal ),
that can be determi ned by atomi c absorpti on spectrornetry or
i nducti vel y-coupl ed pl asma spectroscopy, use one of the di ges-
ti on techni ques presented bel ow. Use the l east ri gorous di gesti on
method requi red to provi de compl ete and consi stent, recovery
compati bl e wi th the anal yti cal method and the metal bengan-
al yzed.
Ni tri c aci dwi l l di gestmost sampl esadequatel y (Secti on 3030E).
Ni trate i san acceptabl e matri x for both fl arne and el ectrothermal
atomi c absorpti on. Some 'sampl es may requi re addi ti onfof per-
chl ori c, hydrochl ori c, or sul furi c aci d for compl ete' di gesti on.
These aci ds may i nterfere i n the anal ysi s of some metai s and al l
provi de a poorer 'matri x. for el ectrothermal 'anal ysi s. Confi rm
metal recoveryfor each di gesti on and anal yti cal procedure used.
Use Tabl e 3030:1 s' a gui de i n'determi ni ng .whi ch aci ds (i n:ad-
di ti on to HN03) to usefor compl ete di gesti n. As a general rul e,
HN03 al one i sl fadquate for cl ean sampl esor easi l y oxi di zed
materi ai s; HN03-HzS04.or HN0
3
-HCl di gesti on i s adequate for
readi l y oxi di zabl e organi crnatter; HN03~HC104ar HN0
3
-HC10
4
-
HF di gesti on i s'necessary for di ffi cul t-to-oxi di ze organi c matter
or mi nerai s. Dry ashi ng i shel pful i f l arge amounts of organi c
matter are present." F
Di l ute sampl es wi th Ag concentrati ons greater than 1 mg/L to
contai n l ess than 1 mg/L Ag for fl ame atomi c.absorpti on methods
and 25 f.Lg/L or l ess for el ectrothermal anal ysi s, To address prob-
l ems wi th si l ver hal i de sol ubi l i ty i n HN0
3
, di gest usi ngmethod
3030F.3b.
Report di gesti on techni que used.
Aci d di gesti on techni ques (Secti on 3030E-1) general l y yi el d
comparabl e preci si on and bi as for most sampl e typestht are
total l y di gested by the techni que. Because aci ds used i ndi gesti on
wi l l add metai s to the sampl es and bl anks, mi ni mi ze the vol ume
of aci ds used.
. "TABL E 3030:1. . ACI DSUSED I NCONJUNCfI ON WI TH HN03 FOR
" . o.' '. SAMP L E P REP ARATI ON
MayBe
Hel pful for
Not Recommended
for "
'HCI - Sb, Ru, Sn
H2~O:C ",. '1,)Ti
HCI 04 Organi c materi ai s
H . r > ) , '.~'.'\',L ;-1.''''''', ''b" ",:.Si l i ceous materi ai s
Th,P b
Ag, P b, Ba
c '; ~';" ._, .. ,. I ' " ti"'
or fl ask, and add 5 mL 1 +1 hi gh-puri ty I :I CL Heat 15mi n on
a steam bath, .Fi l ter .through .a .membrane fi l ter and -careful l y
. transfer fi l trate to a tared vol umetri cfl ask. Adjust vol ume to
100rnL -wi th water , mi x, and anal yze.l f vol ume i s greater than
dOO mL , determi ne vol ume to nearest O.I -mL by wei ght, anal yze,
and correct fi nal concentrati on measurement by mul ti pl yi ng by
.the di l uti on, factor (fi nal vol ume -7- I OOk ': ~1 ;" '
-, ,
ffO: )-'f ~I~ :1 fO ., cy
t
3
. n'I'"
'---'
' , oo 1 )'I'\t
Because the aci d di gesti on techni ques (3030E and F) normal l y
arenot total di gesti ons, themi crowave di gesti onprocedure (3030K)
may be used as an al ternate to them. The mi crowave method i s
a cl osed-vessel procedure and thus i s expected to provi de i m-
proved preci si on when compared wi th hot-pl ate techni ques. The
mi Erowav~. di gesti on method ~. ecommended for the anal ysi s of
Ag, AI ; As, Ba Ca, Cd, C0, ,Cu,~, K, Mg, , Mo,
Na, N', P b, Sb, S I , an n.
Suggested samp e .vol umes are i ndi cated bel ow. I fthe rec-
ommended vol ume exceeds di gesti on vessel capaci ty, add sampl e
:as' evaporati on proceeds. For sampl es contai ni ng parti cul ates,
wi de-bore pi pets may be useful for. vol ume measurement and
transfer.
When sampl es are concentrated duri ng -di gesti on (e.g., >100
mL sampl eused) J determi ne metal recovery for each matri x di -
gested, to veri fy method val i di ty. Usi ng l arger sampl es 'wi l l re-
qui re addi ti onal aci d, whi ch al so woul d i ncrease the concentra-
ti on of -i mpuri ti es.
r-
Esti rnated Metal
Concentfati on "
mg/L ::= Wltl..
Sampl e V ol ume'
mL
<1
1-10
10-100
100-1000
1000
100
10
1
'For fl ame atomi c absorpti on spectrometry. For graphi te furnace or I CP ,
smal l er vol umes are appropri ate.
Report resul ts as fol l ows:
B
.- Metal concentrati on, rng/L = A x C
where; .
, 4 ., ;, co~centrati on of metal i n di gestedsol ~ti on, mg/L ,
B = fi nal vol ume of di gested sol uti on, mL , and
C = sampl e si ze, mL . . .
P repare sol i d sampl es ar l i qui d sl udges wi th hi gh sol i ds con-
tents on a wei ght basi s. Mi x sampl e and transfera sui tabl e amount
(typi cal l y 1 g of a sl udge wi th 15% total sol i ds) to a preweghed
di gesti on vessel . Rewei gh and cal cul a te wei ght of sampl e. P ro-
~~~~- - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - ~- - - - - - - - - - - - - - ~~=- - - - - - - - - ~~~=- ~~~~- ~- ~- - - - - - - - - - - - - - - ~
'REUMJI 'J,Af!Y ..l REATMENT (3030)/Di gesti on
ceed wi th one of the di gesti on techni ques presented Q~l i l w.. Re-...;
port resul ts on wer-or dry-wei ght basi sas fol l ows: ,',.. ,
..; , -, - -."- ':'..
Metal concentrati on, rng/kg (dry-wei ght baS;S) = A x 's ,x"~OOr,'
_. g sa~B~e~-'! D,
, .', '
. ,!
I ~~~~~r~~:.":(-:0- ( .:-,.;~; .: - i F:
. A = concentrati on of metal i n di gested sol uti on, mgI L ,
B = fi nal vol ume of di gested sol uti on, mL , and
D = total sol i ds, % (see Secti on 2540G) .
Al ways prepare aci d bl anks for each type of di gesti onper-
formed.Experi ence i ndi cates that a bl ank made wi th the same
aci ds and subjected to the same di gesti on procedure as the sam-
pI ecan correct for i mpuri ti es present i n aci ds, i n reagent water,
and on gl assware.
I
3030 E., .Nitric Acid Digestion
1 . ppM~tus
.J
a. Hot plate.
b, Coni cal (erlenmeyer) flas ks , 125-mL , ar Gr iffin beakers,
150mL , aci d-washed and ri nsed wi th water.
c. Volumetr ic flas ks , 100-mL .
2. Reagents
j ', .H!
Ni tri c, aci d, HN03, cone,
3. Procedure
;a '''1 ., '' !". _ ..
Transfer a .measured vol ume of..wel l -mi xed, aci d-preserved
sampl e appropri ate for theexpected ;n~t!s concentrati ons t~a.
, .
'"
! -r
3030 F, .Nitrlc Acid-, Hydrochloric Acid Digestion
.'~,
1 : Apparatus
.i;.
. See 3030E.1. The fol l owi ng al so are. needed:
.z; 'Watch glasses. .., ;,
b. Steam bath. ..'
" ,
i.:
_ .' {
2. Re?g.ents ,
r ' f ~
. '.. - -.. - ..,-
il, Ni tri c ac'i d,.:HN.?:, cone; ,
. p: Hydrochlori c ,a~{d, ~;.~ 1 .'
3. Procedure
a. Total HN03/HCI: Transfer a measured vol ume of wel l -
mi xed, aci d-preserved sampl e appropri ate for the expected met-
aI s concentrati ons to a fl ask or beaker (see 3030D for sampl e
vol ume). Add 3mL cone HN03. P l ace fl ask ar beaker on a hot
pl ate and cauti ousl y evaporate to l ess than 5mL , maki ng certai n
that sampl e does not boi l and that no areaof the bottom of the.
contai ner i sal l owed to go dry. Cool and add 5mL cone HN0
3
.
."f
.' I'
fl askor beakei (see 303'OD'for'sam l e l ti me)'. dd 5ml , 'cone
HNO ;'ancla few boi l i ng '.hi ps, gl ass beads, or Hengargrari ul es .
Bri ng to a sl ow boi l and evaporate on a hot pl ate to the l owest
vol ume possi bl e (about 10to 20mL ) before preci pi tati on occurs.
Conti nue heati ng and addi ng conc HN03 asnecessary unti l di ges-
ti on i s compl ete as shown by a l i ght-col ored, cl ear sol uti on. Do
not l et sampl e dry duri ng di gesti on.
~.Wash dowi l fl ask ar beake~waI l s wi th water and then fi l ter i f
necessary (see Secti on 3030B). Transfer fi l trate to a 100-mL
vol umetri c fl ask wi th two 5-mL porti ons of water, addi ng these
ri nsi ngs to the vol umetri c fl ask. Cool , di l ute to mark, and mi x
thoroughl y. Take: porti ons of thi s sol uti on for requi red metal
determi nati ons.
, .,
.,
, I'
Cover contai ner wi th a watch gl ass and return to hot pl ate. I n-
crease ternperature of ht pl ate 'so that agentl e refl ux ~cti on
occurs, Conti nue heati ng, addi ng addi ti onal aci das necessary,
unti l di gesti on i s compl ete (general l y i ndi cated when the di ges-
tate i s l i ght i n col or or does not change i n appearance wi th
conti nued refl uxi ng). Evaporate to l ess than 5mL and coo!. Add
10rri L 1 +1 HCr and 15mL water per 100mL ari tci pated fi nal
vol ume. Heatfor ari addi ti onal 15mi n te>di ssol veny preci pi tate
or resi due: Cool , wash down beaker 'wal l s and watch gl asswi th
water ,-fi l ter to re'mov e i nsol ubl e 'materi al that 'coul d"cl og' the
nebul i zer ,'nd transfer fi l tra te'to a l UO-mL vol umetri c fl ask wi th
ri nsi ngs. Al ternati vel y centri fugeor l et settl e overni ght. Adjust
to vol ume and mi xthoroughl y -.
h. Recoverable HN0
3
/HCI:'-For thi s I essri gorous di gesti on
prcedure, transfer a measured vol ume of wel l -rni xed, aci d-pre-
served sampl e to a fl ask or beaker. Add 2mL 1 +1 HN03 and
10mL 1 +1 HeI and heat on a steam bath or hot pl ate .unti l
vol ume has been reduced to near 25mL , maki ng certai n sampl e
does not boi !. Cool and fi l ter to remove i nsol ubl e materi al ar
. al ternati vel y centri fuge -or I t settl ' vemi ght. Transfer sampl e
to vol umetri c fl ask, adjust vol ume to 100mL , and mi x.
. r
"
METALS (3000)
3030 G. Nitric Acid-Sulfurc Acid Digestio~
1 . Apparatus
, 'See'3030E.l . 'i '
', ,i .
si i ; ".-
'j
i "
2. Beaqents.
a. Ni tri c aci d, HN03, cone.
b. Sulfuri c aci d, H2S04, cone.
3. Procedure
,:I '~;;tnsfyra>i pe~sur~I .v.0~up~ of:-V ,e,l I ~mi xed?, a,c,i d-pres,er~e,q,
sampl appropri ate forthe expected metal s concentrati ons.toa
. 1.1':" ;!' I I I . :'1 ';-'
L , I
1-':-1 /.. .., .
"
fl ask or beaker (see 3030D for sampl e vol ume). Add 5mL cone
HN03 and a few boi l i ng ehi ps, gl ass beads, or Hengar granul es.
Bri ng tosl ow boi l on hot pi a te,and evaporateto 15to 20mL .
Add 5,mL cone HN0
3
and 10mL cone H2S04. Evaporate on a
hot pl ate unti l dense whi te fumes of S03just appear. I f sol uti on
does not c\ear, add 10mL cone HN03 and repeat evaporati on
to fumes of S03' Heat to remove al i HN03 before eonti nui ng
treatment. Al i HN0
3
wi l l be removed when the sol uti on i s c\ear
and no browni sh fumes are evi dent. Do not l et sampl e dry duri ng
di gesti on.
Cool and di l ute to about 50mL wi th water. Heat to al most
boi l i ng to di ssol ve sl owl y sol ubl esal ts. Fi l ter i f neeessary, then
compl ete proeedure as di reeted i n Seeti on 3030E.3.J:>egi nni ng
wi th, "Transfer fi l trate ... " ,
t "1 .
c. r.f
, i '1 ( I
3Q3({H., .NitriqAcid-Perchloric Acid Digestion
1 . Apparatus
See 3030E.1. The fol l owi ngare al so, needed: ,
a. Safety shi eld.
b. Safety goggles.
c. Watch glasses.
2. Reagents
a. Ni tri c aci d, HN03, cone.
b. Perchlori c aci d, HCI 04 ." , , _ "
c. Ammoni um acetate soluti dh: Di ssol ve 500'g NH4C2H302 i n
1 :> i , ~.... ' i '. '
600mL water,
<,
',o
3. Procedure (
1 .' i, \' _.';: ~'.. f, !r
CAUT}O N: H eated mi xtures of/i Cl.04 and orgq,,!i cmattermay
explode vi olently. Avoi d thi s. hazard bytaki ng .th.e[ollowing. pr e-
cauti ons: (a) do not add HCL04 to. a hot soluti on contai ni ng or-
gani c matter; (b) always pretreat samples contai ni ngorgani c mat-
ter wi th HN03 before addi ng f!CI04; {c)avoi q repeated fuming
wi th HCIO4 i n ordi nary hoods (For routi ne operati ons, use a.water
pump attached to a glass fume eradi cator. Stti i nless steelf~ne
hoods wi th adequate water washdown faci li ti es are avai lable corn-
. .
.'
merci ally and are acceptable for use wi th HCL04.); and (d) never
let samples bei ng di gested wi tn HCl04 evaporateto dryness.
Transfer a measured vol ume of wel l -rni xed, aci d-preserved
sampl e appropri ate fortheexpected metai s eoneentrati ons to a
fl ask ar beaker (see 3030D for sarnpl e vol ume); Add 5mL cone
HN03 and a few boi l i ng ehi ps, gl ass beads, or Hengar granul es,
and evaporate on a hot pl ate to 15to 20mL . Add 10mL eaeh
of cone HN03 and HCI 04 , eool i ng fl ask or beaker between ad-
" di ti ons. Evaporate gentl y on ~hot pl ate unti l dense whi te fumes
of HCI 04 just appear. I f sol uti on i s not c\ear, eover eontai ner
wi th a watch gl ass and keep sol uti on just boi l i ng unti l i t c\ears.
I f necessary, add 10mL coneHN03 to compl ete di gesti on. Cool ,
di l ute to about 50mL wi th-water, and. boi l to expel any ehl ori ne
or oxi des of ni trogen. Fi l ter, then compl ete proeedure asdi rected
i n 3030E.3 begi nni ng wi th, "Transfer fi l trate .. .."
I f l ead i s to be determi ned i n the presenee of hi gh amounts
of sul fate (e.g., determi nati on of P b i n power pl ant fl y ash sam-
pi es), di ssol ve P bS04 preei pi tate as fol l ows: Add ,50mL am-
moni um aeetate sol uti on to fl ask or beaker i n whi eh di gesti on
was earri ed out and heat to i nei pi ent bol i ng. Rotate contai ner
oeeasi onal l y to wet al i i nteri or surfaces and'di ssol ve any depos-
i ted resi due. Reeonneet fi l ter and sl owl y draw sol uti on through
i t. Transfer fi l trate to a 100-mL vol umetri e fl ask, cool , di l ute to
mark, mi x thoroughl y, and set asi de for determi nati on of l ead.
3030 L Nitric Acld-Perchlorc Acid-Hydrofluoric Acid Digestion
1 . Apparatus
a. Hot plate.
b. .TFE beakers, 250-mL , aei d-washed and ri nsed wi th water.
c. Volumetri c flas ks , 100-mL , pol ypropyl ene or other sui tabl e
pl asti e.
2. Reagents
a. Ni tri c aci d, HN03, cone and 1 +1.
b. Perchlori c aci d, HCI '04'
c. Hydrofluori c aci d, HF, 48 to 51%.
riELlMINARY TREATMENT (3030)/Microwav e-Assisted Digestion
3. Procedure
CAUTIO N: See precauti ons for usi ng H CIO 4 i n 3030H ; handle
HF wi th extreme care and provi de adequate venti lati on, .especi ally
for the heated soluti on. A voi d all contact wi th exposed ski n. -Pro-
vi de medi cal attenti on for HF burns. s , ',' 1-. i ."
Transfer a measured vol ume~f wel l -mi xed, aci d-preserved
sampl e appropri ate for the expected metai s concentrati ons i nto
3-7
a 250-mL Tl -E'beaker (see 3030D for sampl e vol ume). 'Add a:
few boi l i ng chi ps and bri ng to a sl ow boi !. Evapoate 'on'a hof
pl ate to 15to 20mL . Add 12ml .rconc HN0
3
ari d evaporate to
near dryness, Repeat HN03. addi ti on and evaporati on. L eI 50-
l uti on cool , add 20 mL HCI 04 and L 'rnl , HF, and boi I unti l
sol uti on i scl ear and whi te fumes ofHCI 04 have appared. -Cool ,'
add about 50mL water, fi l i er, and proceed asdi rected i n3030E.3
begi nni ng wi th, "Transfer fi l trate .. '."
',', J
3030J. Dry As hi hg
The procedure appeari ng i n previ ous edi ti ons of Standqrd
Methods has been del eted from thi s edi ton. ",' " -e
/ ~
3030 K. Mlcrowav e-Asslsted Di ges ti on (PROPOSED)
1 . Apparatus
a. Mi crowave uni t wi thprogrammabl e power '(mi ni mum 545.
W) to wi thi n 10W of requi red power, havi ng cbrrd~i on-'
resi stant; wel l -venti l ated cavi ty and havi ng al i el ectroni cs .p'ro~.
tected agai nst corrosi on for safe operati on. Use a uni thavl ng a
rotati ng turntabl e wi th a mi ni mum speed of 3 rpm to i ~st~e'
homogeneous di stri buti on of mi crowave radi ati ori . Onl y l bor~-
tory-grade mi crowave equi pment and ci osed di gesti on contaners'
wi th pressure rel i ef that are speci fi cal l y desi gned for hot 'aci d
may be used.' " . , '::'.<: d
b.: Vessels constructed of perfl uoroal koxy (P FArtefl n~,:* '
capabl e of wi thstandi ng pressures of at l east 760 '70kP a (110'1
10psi ) , and capabl e of contrl l ed pressure rel i ef ai the rnan- I
ufacturer's maxi mum pressure rati ng.
Aci d wash al i di gesti on vessel s and ri nse wi th reagent water.
For new P FA Tefl on@;* vessel s or when changi ng betweenhi gh- '
and l ow-concentrati on sampl es, cl ean by l eachi ng wi th hot hy-
drochl ori c aci d (1:1) for a mi ni mum of 2 h and then wi th hot
ni tri c aci d (1:1) for a mi ni mum of 2 h; ri nse wi th-reagent water
and dry i n a cl ean envi ronment. Use thi s procedure whenver
the previ ous use of di gesti on vessel s i s unknownor cross-con-
tami nati on from vessel s i s suspected.
c. Plasti c contai ner wi th cover, I -L , preferabl y made of P FA
Tefl on@. * L I ) ~
d. Bottles, pol yethyl ene, 125-mL , wi th caps.
e. Thermometer, accurate to 0.1e.
f. Balance, l arge-capaci ty (1500g), accurate to 0.1 g.
g. Fi ltrati on or centri fuge equi pment (opti onal ).
2. Reagents
a. Reagent water: .See Secti on 1080.
b. Ni tri c aci d, HN0
3
, cone, sub-boi l i ng di sti l l ed. Non-sub-
boi l i ng aci ds can be used i f they are shown not to contri bute '
bl anks.
Or equi val ent.
3. Calibration of Microwav e Unit
For cavi ty-type mi crowave equi pment, eval uate absol ute power
(watts) by measuri ng the temperature ri sei n 1 kgwater exposed
to mi crowave radi ati on for a fi xed ti me. Wi th thi smeasurement,
the rel ati onshi p between avai l abl e power '(W) 'andthe parti al
power setti ng (%) of the uni t can be esti mated, and ri y absol ute
power i n watts may be transferred fromone uni t to another. T\1e
cal i brati on format requi red dependson 'type of el ectroni c system
used by manufacturer to provi de parti al mi crowave power. Few
uni ts have an accurate and preci se l i near rel ati onshi p between
percent power setti ngs and absorbed power. Where l i near ci rcui ts
have been used, determi ne'cal i brati o~" curve by a three-poi nt
cal i brati on method; otherwi se, usethe mul ti pl e-poi nt cal i brati on
method. '..' ,
a. Three-poi nt cali brati on ;ne!hod: Measur,e pow~r at 1.00~.
and 50% power usi ng the procedure descri bed i ri ~3c and cal -
cul ate power setti ng correspondi ng to requi red power i i rwJt~'.
as speci fi ed i n the procedure from the two-poi nt l i ne. Masure'
absorbed power at the cal cul ated parti al power setti ng. I f the
measured absorbed power does not correspond to the eal cul ated-
powerwi thi n 10W, usethe mul ti pl e-poi ';l t cal i brati on method,
~ 3b. Use thi spoi ri t prodi cl l y to veri fyi nfegri ty'fa:\i b'rati 9,n.
b. Multi ple-poi nt cali brati on method: Foi each mi cro\v'ave'ni !;'
measure the 'fol l owi ng power setti ngs: 100, 99/98;-9;7-;~95, '90;\
80, 70, 60, 50, and 40% usi ng the procedure descri bedi n-fSc.i
These data are cl ustred about the customary worki ngtpower
ranges, Nonl i nari ty commonl y sencountered t th.upper end
of the cal i brati on curve. I f theunt'setecrroni cs 'are'knownto
nave nonl l near devi ati ons i n any regi on 'o: pr0por'ti ohal power
control , make a 'set of measuremeri ts that brcketthe pwr-to
beused. The fi nal cal i brati on poi nt shoul d b t the'parti al power
setti ng that wi l l beusedi n the test.'Check thi s setti ng p~ri odi cal l y
to eval uate the i ntegri ty of the cal i brati on.: I f a si gni fi cari t change
( 10W)i s detected, re-eval uate enti re' cal i brati on.": ",
c. Equi l i brate a l arge vol ume of water to'room ternperature
(232C). Wei gh 1 kgreagent water' ~1000g 1 g) or measure
(1000 mL 1 mL ) i nto a pl asti c, ri ot gl ass, contai ner, and
measure the tempei ature to 0.1e. Condi ti on mi crowave uni t
by heati ng a gl ass beaker wi th 500to 1000mL tap water at ful l
~"""""""""""""""- - - q
t\- ~ di7 'm1i ot (~ ~ Jl-) . ?~ L
B - ~ +h.Ct ao: ~ O-ME~ (30~;
G-~k~,
facturer of the mi crowave equi pment.'The change i n power,
ti me, and temperature profi l e i s not di rectl y proporti onal ta the
change i nthe number of sampl es; thus, di fferent power programs
wi l l be requi red for di fferent numbersofvessel s contai ni ng the '
appropri ate amount of sampl e and aci d. L
Wei gh enti re di gesti on vessel assembl ta 0.1 gbefore use and
reca~ Accuratel y transfer 45 mL of wel l -shakj; sarnpl e
i .!U9.the~esti an vesse!. P i pe ' mL orc HN0
3
'i nt each vesse~
I nsure that pressure-cap rel i ef di sks are i nserted accordi ng ta
manufacturer's di recti ons, Ti ghten cap ta manufacturer's ~ec-
i fi cati ons, Wei gh each capped vessel ta the nearest 0.1 g.
P l ace appropri ate number of vessel s evenl y di stri buted m the
carousel . Treat sampl e bl anks, known addi ti ons, and dupl i cates
i n the same manner as sampl es. When fewer sampl es than the
appropri ate numbr are di gested, fi l l remi ni ng vessel s wi th 45
mL reagent water and 5 mL cone HN03 ta 'abtai n ful l compl e-
ment of vessel s for the parti cul ar program bei ng used.
P l ace carousel i n uni t and seat i t careful l y on turntabl e. P ro-
gram mi crowave uni t ta heat sampl es ta 160 4C i n 10mi n
and then, for the second stage, ta permi t a sl ow ri se ta 165ta
170C for 10mi no Start rni crowave generator, maki ng sure that
turntabl e i s turni ng and that exhaust fan i s on. .
At cornpl eti on of the mi crowave program, l et vessel s cool for
at l east 5mi n i n the uni t before removal , Sampl es then may be
cool ed furth~~ ai i tsi d~ the uni t by removi ng the cara usei and
l etti ng th'em-caal on a bench ar i n a water bath. Whe'n cool ed
ta room 'temperature, wei gh (ta 0.1 g) each vessel and record
wei gh~@. . " ,,'
I f the net wei ght of sampl e pl us aci d decreased by more than ,
10%, di scard sampl e, ' r
.Cornpl ete sampl e preparati on bycareful l y uncappi ng andvent-
i ng each vessel i n a' fume haad. Transfer ta aci d-cl eaned non-
contami nati ng pl asti c bottl es. I f the di gested sampl e contai ns
parti cul ates, thenei ther centri fuge at 2000ta 3000rpm for 10
mi n and fi l ter, ar Jet settl e overni ght.
power for ~. mi n ,-;,,i th.tpe, exhaust, fan .on.. L oosel y cover pl asti c
contai ner ta reduce heat.l oss, and pl acei n normal sampl e path
(at a~t~r edge~f'r~t~ti ng't~~i ~~l e,); ci rcul are conti nuousl y through
the mi crowaye fi el d lar, gg s ,,!tdesi red pawe.r setti ng \."i th,ex-
haust fana~ asi twi l l beduri ng,p.armal operati on, Remove pl asti c
contai ner and sti r water vgorousl y. Use a magneti c sti rrng bar
i nserted i mmdi atel y after mcrowave..i rradi ati on; record rnaxi -
mum temperature Wi thl thefi rstJ s ta ;: 0.1 -c. ~~e. a new
sampl e for each addi ti onal measurement. I f the water i sreused,
return both water and beaker ta 23 2e. Make three meas-
urements at each power setti ng. When any part of the hi gh-
vol tage ci rcui t, power source, or control cornponents i nthe uni t
have been servi ced ar repl aced, recheck cal i brati on pwer. I f
power output has changed by more than 10W, re-eval uate
enti re cal i brati on.
Compute absorbed power by the fol l owi ng rel ati onshi p:
r / '
p = (K) (Cp) (m) (H)
t
where:
P = apparent power absorbed by sampl e, W;
K = conversi on factor for thermochemi cal cal ori es sect ' to watts .
(4.184),
Cp = heat capaci ty, thermal capaci ty, orspeci fi c heat (cal g-::'\ C-l )
,', of water,
m = mass, ef. water sampl e, g, :: ", .., ;:l, ' -s r . '
IlT = fi nal temperature mi nus i ni ti al temper')tl ,l re, C, and
t = ti me, s; , ;,
For the experi mental condi tons ?f.J:~O:s .~d 1, k& di sti l l ed
water (Cp at 25C = 0.9997), the cal i bpti a.~<:9uati an si mpl i fi es
ta: ',' '
t J~
.i ,i
__ , l.;
, ' ,_o f, ". <"L:;! . 1':!;1:.. ,
Stabl e l i ne vol tage i s necessary for accurate and repro.d';l Ri bl e
cal i brati on and operati on, I t shau\q b~,wi ~~i f1,t~e,.\l l <~I ?-ul act~l fer's '
speci fi cati on , Duri ng measurement and .operati on .i t must not
vary by more than 2 V . A cnsJ!!~po;,v suppl y, may be
necessa,r~i f l i ne vol tage .i s unst,abl e.' J' ', < ;',
4 . Procedure
AUTI ON: Thi s method 4des igned jor";'i ~row9ve'di gesti on of
waters only. It i s not i ntended for the di gesti on pf.~oli l~"jn whi ch
hi gh concentrati ons of organi c compounds.may result i n . high.
pr es s ur es and possi bly uns afe condi ti ons.r '~,,', J.. ; e"~;
. The.fol l owi ng procedurei s based an h~ati ng,~ci cl \fi ~.d,"samp,l ~s!
i n two stages where the fi rst stage i s to reach 1.60.(~OC i n 10
mi nand the second stage i sta permi t a sl owXi seto V i 5,t.o110C,
duri ng the second 10mi no f:. veri fi ed program al meets thi s
ternperature-ti me .profi l e i s 545 W f()r)O'mi n fol l owed by A4 4
W for i l P mi n usi ng fi ve si ngl e-wal l I ,>FATefl ont di gesti on,
vessel s., The usabl e number of vessel s i s deterrni ned by vessel
desi gn ~d power output. I f more vessel s are used i n a hi gh~r~,
wattage uni t, vri fyti me-temperature profi l e to conform to. the
gi ven i t.wo~stage.profi l e.j-Thi s may be done by l aboratory per-
sonnel i f i >l ,l i .t,abl et~st, equi pment i s avai l abl e.. a,r by the manu-
.:. '.
"
t Or ,equi val ent.
"
,--i
5. Calculations
. Di luti on correcti on: Mul ti pl y resul ts by 50/45 ar 1.11 to
account for the di l uti on caused by the addi ti on of 5 mL aci d to
45.mL sampl e.
b. Di scardi ng of sample: To determi ne i f the net wei ght of
sampl e pl us aci d decreased by more than 10% duri ng the di ges-
ti on process, use the fol l owi ng cal cul ati on:
[(B - A) - (C - A) ] x 100> 10%
(B - A)
6. Quality Control
P referabl y i ncl ude a qual i ty-control sampl e i n each l oaded
carouse!. P repare sampl es i nbatches i ncl udi ngpreparati on bl anks,
sampl e dupl i cates, and pre-di gesti on known addi ti ons. Deter-
mi ne si ze of batch and frequency of qual i ty-control sampl es by
method of anal ysi s andI aboratory practi ce. The power of the
mi crowave uni t and batch si zemay prevent i ncl udi ng one or more
of the qual i ty-control sampl es i n each carouseI . Da not graup
qual i ty-control sampl es together but di stri bute them throughout
the vari ous carousel s ta gi ve the best moni torng of di gesti on.