sio2 SILICATE

Method: AmmoltturuMolyeonre SpEcrRopHoroMETRtc

ro:r.ie Version: 1

o
L Apparatus

5 a. Spectrophotomefer,
for use at 815 nm, having1 cm lightpath.
E
o Reagerr(s

o 4 Storeall reagentsin plasticcontainers.

o
L
b. Sulphuicacid,H2SO4,
1N.
c. Hydrochloricacid, HCl, 1 + 1

r d Ammoniummolybdatereagent:Dissolve10 g (NHa)6Mo7O2a.4H2O in distilledwater,with

stiningand gentlewarming,and diluteto 100 mL. Filterif necessary_
and 8 with silicafree NH4OHor NaOHand storein potyethylene
AdjustpH between7
botfleto stabitise.
I

IE e. Oxalicacidsolufibn:Dissolve7.5 g H2C2O4.H2O
in distilledwaterand diluteto 100 mL.

II
o f Stocksilicaso/utloniDissolve313.0mg sodiumhexafluorosilicate,
water;1 ml = 0.1mg SiOr.
distilled
Na2SiF6,
in 1000mL

g. Silicastandardworkingsolution:Ditute100mL stocksolutionto 1000m1;1mL=10pg

{i
si02.

I h. Reducingagenf.'Dissolve 500 mg 1-amino-2-naphthol-4-sulphonic acidand 1 g Na2SO3

in 50 mL distilledwater,with gentlewarmingif necessary;add this to a solutionof 30 g
IE NaHSogin 150 mL distilledwater.Filterintoa plasticbotfle.Discardwhenthe solution
g becomes-dark. Prolongreagentlife by storinga refrigerator
awayfromlight.

Procedure

a To 50 mL sample,containingbetween20 and 1OOpg silica,add in rapidsuccession1.0

E mL (1 + 1) HCIand 2 mL ammoniummolybdatereagent.Mix thoroughlyand let standfor 5
L to 10 min.Add 2.0 mL oxalicacid solutionand mix.Measuringtimefromthe momentof

IE addingoxalicacid,waitat least2 minbutnot morethan15 min,add2 mL reducingagent

and mixthoroughly.
E ,. Readabsorbanceat 815 nm after5 min,adjustingthe instrumentto zeroabsorbance

c usingdistilledwaterblank.
c. Dilute2.0, 4.0, 6.0, 8.0 and 10.0mL silicaworkingstandardsolutionto 50 mL volumes
and proceedas in a and b aboveto preparea calibrationcurve.
IE
fl Calculation

o Readsilicacontentof samplefromthe calibrationcurve.

LaboratoryManual lD: 1.38Version:'l Page'.112