! M% D' B( I( [; T4 L4 [+ X ^ o ' b7 h6 c0 h3 R V% O6 b作者: 1123456789 时间: 2008-5-23 12:10 标题: 二氧化钛(钛白粉) 二氧化钛(钛白粉)" `, \9 }5 Z7 z1 b: I
+ [3 @% m3 t# \7 B1 a5 H
JECFA关于二氧化钛(钛白粉)的结论3 E, j& `5 O& j/ w5 t" @% ~
& I- d8 e P# h0 f m摘要: 2006年JECFA关于二氧化钛的结论" K. g) m% u/ `9 ^/ g
ADI值:不作限制。& D/ B8 p5 O9 P/ ]1 I% U* G+ d
功能:着色剂) P4 q: U% `9 ^9 a, G
' B7 s0 R6 l7 vTITANIUM DIOXIDE0 J: |' K2 B4 Q
Prepared at the 67th JECFA (2006) and published in FAO JECFA 5 i/ q+ s/ Z# {3 O$ C- {; D$ C: @Monographs 3 (2006), superseding specifications prepared at the 63rd% T ~( ]6 m g6 h3 S( G
JECFA (2004) and published in FNP 52 Add 12 (2004) and in the 5 C0 y0 b6 C4 T- L2 f- ]" s0 uCombined Compendium of Food Additive Specifications, FAO JECFA 1 c3 z$ s+ B& Z6 DMonographs 1 (2005). An ADI “not limited” was established at the 13th! A* i6 @' h0 f" J) {
JECFA (1969). 1 R; t! p7 o8 w3 B1 WSYNONYMS 5 i2 a. ?! l/ S% t6 yTitania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171 ' k: c) h( l/ f2 I7 EDEFINITION , _# ]3 E7 V( C+ H7 GTitanium dioxide is produced by either the sulfate or the chloride. X" x" c$ j- o5 u; ~
process. Processing conditions determine the form (anatase or rutile . m' s+ I' [. b6 y: x9 M. A0 Qstructure) of the final product.9 b3 j; @, a% a) d( D
In the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3) ' T& }0 b |2 Uor ilmenite and titanium slag. After a series of purification steps, the ; T4 _* P$ w& S7 T( d! }2 iisolated titanium dioxide is finally washed with water, calcined, and4 D) y, }, w6 j% Z% m. L+ \. ?
micronized. ' U) {; Q# u1 `In the chloride process, chlorine gas is reacted with a titaniumcontaining }( f$ F% A' n& k# Y7 Lmineral under reducing conditions to form anhydrous4 `4 Y+ U, b3 @
titanium tetrachloride, which is subsequently purified and converted to7 p: l. Y1 ~% A5 q: A
titanium dioxide either by direct thermal oxidation or by reaction with" A' `9 ?4 ~) ~' E2 G
steam in the vapour phase. Alternatively, concentrated hydrochloric) s+ \1 n/ `; b) q/ t- R
acid can be reacted with the titanium-containing mineral to form a / a9 x* L7 U% b8 a7 usolution of titanium tetrachloride, which is then further purified and" p( M) f2 E3 ^5 V: x* D" X
converted to titanium dioxide by hydrolysis. The titanium dioxide is8 b1 L, l- P/ D& j
filtered, washed, and calcined. ; G( `$ G! L5 _" i1 iCommercial titanium dioxide may be coated with small amounts of" L; f6 b* T F* Q+ B5 @* {
alumina and/or silica to improve the technological properties of the * S8 B4 A: {" J' z# tproduct.7 r( d* k2 v# {2 J$ r
C.A.S. number 13463-67-7 1 y( N/ p5 J* P$ U) i+ _Chemical formula TiO2 " ~- X1 \3 ~! d4 ]8 }. a1 WFormula weight ) p! m/ K0 k* H9 n0 v79.88 / v9 @9 z5 _* y p1 D3 }& JAssay 4 i. p4 q* a5 c5 Y9 WNot less than 99.0% on the dried basis (on an aluminium oxide and- K. D" E, q; j( V8 J
silicon dioxide-free basis) ( x4 m9 \0 _+ D3 s3 mDESCRIPTION; g3 q4 o# B$ j4 h
White to slightly coloured powder; L& {7 n n) }& v3 Q
FUNCTIONAL USES& r, K$ M/ g, ^) H
Colour - K9 x! v/ U4 @, Z' |1 D5 gCHARACTERISTICS' @! [' d9 i% b9 o6 i
IDENTIFICATION6 t% ?+ m$ m7 K: K ?7 l
Solubility (Vol. 4) 1 b7 v* u) z2 s f, U. B8 q& FInsoluble in water, hydrochloric acid, dilute sulfuric acid, and organic4 A3 G, X) ?, ]: [9 M
solvents. Dissolves slowly in hydrofluoric acid and hot concentrated 5 I N" i. s- x6 B/ C3 \sulfuric acid." }! f0 ~+ z4 ^6 X( c" l
Colour reaction . ^) W7 F V# eAdd 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of 9 S% f9 w; f( a+ f$ b$ ~ u" Bsulfuric acid appear, then cool. Cautiously dilute to about 100 ml with4 r, f' V! W3 c) A# N( Q
water and filter. To 5 ml of this clear filtrate, add a few drops of . |4 b8 U8 P# ~6 ghydrogen peroxide; an orange-red colour appears immediately. , A; x( q, x ?* |PURITY$ P/ b l/ _4 d9 [4 K* M
Loss on drying (Vol. 4) Not more than 0.5% (105°, 3 h) 8 i+ _/ \: x3 p$ r0 oLoss on ignition (Vol. 4)# Z7 i+ |" ^; Y! p* M
Not more than 1.0% (800o) on the dried basis* v$ Z5 g* D, [" D5 p
Aluminium oxide and/or! |2 i" K0 t& a( c( L9 h
silicon dioxide 4 e' d- s* }9 d1 p; t' bNot more than 2%, either singly or combined/ H( N. m9 L) I2 f& h8 W
See descriptions under TESTS 0 }7 ^1 n2 z9 F) F. J6 l+ r. {Acid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing , Q* |3 ?6 M. S3 I! F, }0 balumina or silica. " U& H/ e- i% W; J. H0 u/ ]Suspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and/ J. Z' w& w8 b! h9 ?' O' D
place on a steam bath for 30 min with occasional stirring. Filter. l1 ~- N; r( d0 A! E6 e5 `( {
through a Gooch crucible fitted with a glass fibre filter paper. Wash3 `# M# y- f& i6 S8 g) ~
with three 10-ml portions of 0.5 N hydrochloric acid, evaporate the: \3 z- l# V; |
combined filtrate and washings to dryness, and ignite at a dull red( J, z7 z* E* X/ l/ c+ c
heat to constant weight.! `6 s8 w- J, _4 v2 t% H4 t
Water-soluble matter 2 e7 a0 O `6 I$ s1 P7 T' K, s( {9 N(Vol. 4)% J/ Z& D* v* @# k8 x( q
Not more than 0.5% 5 c6 g4 L! f. |, p& M% D+ |* U8 @Proceed as directed under acid-soluble substances (above), using/ _2 \) J' e, }
water in place of 0.5 N hydrochloric acid. ' O- k0 x/ d* Q1 ]3 n" HImpurities soluble in 0.5 N+ o6 m4 ~8 s8 `
hydrochloric acid ! X* g( h' H5 j: c/ B+ o$ |2 O& XAntimony Not more than 2 mg/kg f7 J+ Z# g: O/ P
See description under TESTS 8 G1 \) h2 [- A( _+ }0 ?Arsenic Not more than 1 mg/kg# w+ L K2 E, L& Z
See description under TESTS4 ~& d7 W9 M8 O5 [' j, D& W$ K
Cadmium Not more than 1 mg/kg) [$ g' {+ i6 X$ q% }
See description under TESTS; L7 h9 o% d4 s9 E$ ?4 P! f1 l
Lead/ y/ e, o7 E& [/ `/ d2 M! g2 R+ o( \4 m/ \
Not more than 10 mg/kg 2 {+ M0 X0 K3 I# QSee description under TESTS . O, _+ G% d$ S7 |- G- Q- pMercury (Vol. 4) Not more than 1 mg/kg% X& _, `6 O" n i( |, @
Determine using the cold vapour atomic absorption technique. Select a& d& B# T- ~, q. n+ U: {0 z( E
sample size appropriate to the specified level ) Z( I5 Y9 U( ^TESTS " I# t* j3 c% ^: R* g1 OPURITY TESTS( O: m5 O! m- O, |! t
Impurities soluble in 0.5 N 9 a0 ?( k6 t0 e/ k7 S0 q+ _; S4 S4 whydrochloric acid7 e. o8 v1 k, Q0 k2 N& k
Antimony, arsenic,$ \4 _) _ P: E9 G0 W: o
cadmium and lead5 ]4 n8 P5 Q3 S! C. q! y
(Vol.4) ( O: e% }( H( [4 o% a$ UTransfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N 0 [( U; b9 G( B/ {# x' J D$ Hhydrochloric acid, cover with a watch glass, and heat to boiling on a 6 ^) `) O& N, \) m! K) ~hot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml 7 h c: A6 [2 dcentrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved- F4 S2 h1 F3 \1 ~% j9 B; x5 Y
material settles. Decant the supernatant extract through a Whatman # _2 j, ~: w2 {: F8 vNo. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml; ?& P. j& t f2 n2 A
volumetric flask and retaining as much as possible of the undissolved 9 t; w3 l$ k5 [material in the centrifuge bottle. Add 10 ml of hot water to the original' |' p1 Y, ]* e1 m5 Z
beaker, washing off the watch glass with the water, and pour the; |9 t3 E5 x c! B
contents into the centrifuge bottle. Form a slurry, using a glass stirring9 p7 D" H4 U+ n5 H( K% l
rod, and centrifuge. Decant through the same filter paper, and collect % t; w$ x7 y1 N: T [the washings in the volumetric flask containing the initial extract. 8 X/ E" U5 Z; b$ qRepeat the entire washing process two more times. Finally, wash the: i' l/ F, P4 n
filter paper with 10 to 15 ml of hot water. Cool the contents of the flask E0 i/ x% |0 }$ h3 C& Vto room temperature, dilute to volume with water, and mix. ( O1 r& k, F+ c" v, f n, w/ } W7 IDetermine antimony, cadmium, and lead using an AAS/ICP-AES # q0 Z, M8 X% t/ a6 \, Ttechnique appropriate to the specified level. Determine arsenic using the 3 D6 N. n# e7 Z" IICP-AES/AAS-hydride technique. Alternatively, determine arsenic using# t- z+ _$ _5 I9 [1 h- w
Method II of the Arsenic Limit Test, taking 3 g of the sample rather than: I7 ]: Y9 o! e+ C @# d* r1 @
1 g. The selection of sample size and method of sample preparation / d" N0 K/ B, @ o; I0 N# C/ m' [may be based on the principles of the methods described in Volume 4. 1 R+ q3 a6 n5 d6 hAluminium oxide Reagents and sample solutions : ~- ^1 b# Q+ R% O4 y0.01 N Zinc Sulfate- \$ ~! f) w6 n% V' T2 ] X) z
Dissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to0 x+ f3 D7 k! E! j7 V+ g
make 1000 ml. Standardize the solution as follows: Dissolve 500 mg ( p3 P9 e9 Y2 N! M1 Fof high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of % Q8 L& X2 G, a) c. u/ }$ r; }/ tconcentrated hydrochloric acid, heating gently to effect solution, then) ~8 ]' x+ l1 Z) m' W
transfer the solution into a 1000-ml volumetric flask, dilute to volume . B+ d: A! I- [4 a" iwith water, and mix. Transfer a 10 ml aliquot of this solution into a 500 ) o5 L* L1 F4 j. {' j3 J6 t6 _ml Erlenmeyer flask containing 90 ml of water and 3 ml of ' L4 j8 ~$ a8 J* g4 d- j ]$ y! Hconcentrated hydrochloric acid, add 1 drop of methyl orange TS and 8 R/ U6 J. r5 k* ~ h" q& W25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,3 t0 n ]# Q2 f* p$ D& O
dropwise, ammonia solution (1 in 5) until the colour is just completely + R! |7 @2 z. h: r7 Lchanged from red to orange-yellow. Then, add:! P0 Y7 X1 K# k2 F
(a): 10 ml of ammonium acetate buffer solution (77 g of5 f ~7 R2 g$ x
ammonium acetate plus 10 ml of glacial acetic acid, dilute to & I0 u& F O- Z+ m# R+ ?1000 ml with water) and9 _8 y. b3 Y4 m, a2 f& s
(b): 10 ml of diammonium hydrogen phosphate solution (150 g- {* @! ^( e0 M, Q8 |
of diammonium hydrogen phosphate in 700 ml of water,0 P' J8 p$ k, z1 t9 a2 E6 i
adjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid, " O- c( H3 R5 jthen dilute to 1000 ml with water).4 t4 Y6 A" {( m; a3 K
Boil the solution for 5 min, cool it quickly to room temperature in a ; J2 T1 I7 U/ w6 i9 _9 estream of running water, add 3 drops of xylenol orange TS, and mix./ o! y7 c5 k. Q# G2 j# I- Q
Using the zinc sulfate solution as titrant, titrate the solution to the first' g" s g; ^/ K. ~/ k
yellow-brown or pink end-point colour that persists for 5-10 sec. (Note: 0 F1 `2 L& K. LThis titration should be performed quickly near the end-point by% U1 J3 @1 |) I% Y
adding rapidly 0.2 ml increments of the titrant until the first colour ( w' A _* d9 s9 i4 H4 Y9 e# echange occurs; although the colour will fade in 5-10 sec, it is the true7 N5 G6 s% n; B6 \% s4 u
end-point. Failure to observe the first colour change will result in an ' N4 R$ k$ @# n3 ]0 `. y. U6 ~8 uincorrect titration. The fading end-point does not occur at the second / }5 r% @+ g+ y) x7 k& `0 k& iend-point.) 8 Y& S2 W h CAdd 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a& [3 L4 N3 X8 \: j$ @& \ U1 U
stream of running water. Titrate this solution, using the zinc sulfate ( [* J) J- G) K, k4 Wsolution as titrant, to the same fugitive yellow-brown or pink end-point ( }, C! o, b* p$ N9 ~! U2 sas described above.% ^, G$ d6 s* H1 U$ H
Calculate the titre T of zinc sulfate solution by the formula:! V2 ?+ }& S" d3 C" G6 Q' B
T = 18.896 W / V+ Q1 I; R% z0 E2 p
where- R* X: D: J) z5 a( K
T is the mass (mg) of Al2O3 per ml of zinc sulfate solution8 ~( B9 R2 g, n( r
W is the mass (g) of aluminium wire : h% t0 ^5 ], `* }& fV is the ml of the zinc sulfate solution consumed in the% v' `( R; f/ v9 i0 _) I! V
second titration# S9 b7 R, J2 @3 E
18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and+ [# N. P# H3 }) O
R is the ratio of the formula weight of aluminium oxide to& B! n! \7 ~3 I3 L
that of elemental aluminium., @( B: {) }3 c) r) I! F' |1 Q
Sample Solution A( f; `0 ]4 h0 z
Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica0 v8 c5 t4 Y2 B$ L X
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O). ( a. T# |% i; C$ v2 Z/ g' Z( A% p(Note: Do not use more sodium bisulfate than specified, as an excess - J' H( J+ C$ w/ @1 W. Rconcentration of salt will interfere with the EDTA titration later on in the ( F2 B6 o$ K$ yprocedure.) Begin heating the flask at low heat on a hot plate, and # o" }0 _! Q1 r# d2 s/ P% Qthen gradually raise the temperature until full heat is reached.1 }6 o6 s6 ]$ M& `
(Caution: perform this procedure in a well ventilated area. ) When9 w: B, {# [, J- C: h# }
spattering has stopped and light fumes of SO3 appear, heat in the full# o2 J- H( x& {$ K
flame of a Meeker burner, with the flask tilted so that the fusion of the 9 Z/ k |9 ?1 M. j6 Q, }sample and sodium bisulfate is concentrated at one end of the flask. y5 d. a q) c9 ^- p
Swirl constantly until the melt is clear (except for silica content), but, v1 L1 B: ~5 a
guard against prolonged heating to avoid precipitation of titanium " j1 Z/ i: P: J( a6 Ndioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until 1 R* l* t6 \4 _1 Cthe mass has dissolved and a clear solution results. Cool, and dilute to7 R4 h L1 L% n3 d/ s7 s9 l
120 ml with water. Introduce a magnetic stir bar into the flask. ; D8 e% C# N9 P+ NSample Solution B 8 w" b9 ]5 N$ Y5 pPrepare 200 ml of an approximately 6.25 M solution of sodium$ |( m( J$ ^1 g& s! H. j* {
hydroxide. Add 65 ml of this solution to Sample Solution A, while* A3 W5 ^; V" F: {# v. O
stirring with the magnetic stirrer; pour the remaining 135 ml of the - _+ p0 m) ^$ g/ K) E# Ealkali solution into a 500-ml volumetric flask.4 @* u- ~1 p& `; F, Q
Slowly, with constant stirring, add the sample mixture to the alkali + A' n% Y- O" H# {solution in the 500-ml volumetric flask; dilute to volume with water, 4 d$ S8 e S2 P8 E. f9 Gand mix. (Note: If the procedure is delayed at this point for more than( g2 E# }& x: Y% J+ ]
2 hours, store the contents of the volumetric flask in a polyethylene 2 |, b# v6 y7 Z/ x f/ m4 Abottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),+ W& ^, e* s" p- n
then filter the supernatant liquid through a very fine filter paper. Label & Y( T. }" V$ `0 H6 Zthe filtrate Sample Solution B., l8 j# w8 K9 |- [: B. ~0 ^
Sample Solution C# ~' a' K: p( \
Transfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer4 r% [/ t x* e" b' Y3 ?
flask, add 1 drop of methyl orange TS, acidify with hydrochloric acid . _ I2 E( z# x) \4 Osolution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02 / f( e$ @5 a% a+ L5 w0 QM disodium EDTA, and mix. [Note: If the approximate Al2O3 content is 1 q; c' ] q, m; w+ @/ v$ iknown, calculate the optimum volume of EDTA solution to be added( G0 D2 b5 `& N
by the formula: (4 x % Al2O3) + 5.]) c8 O$ }, m0 O5 [8 Q
Add, dropwise, ammonia solution (1 in 5) until the colour is just ! n# l1 Y* R, Q" a! h6 u5 x% B8 h3 ycompletely changed from red to orange-yellow. Then add10 ml each" q9 [$ B, b( t' \3 P0 E T
of Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to6 F" P% |& O) k
room temperature in a stream of running water, add 3 drops of xylenol , A, j1 ~7 k9 N/ worange TS, and mix. If the solution is purple, yellow-brown, or pink,; W3 w6 }- P, `" x" h: y1 I
bring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired " V5 u* l! R8 V6 c: ypH, a pink colour indicates that not enough of the EDTA solution has $ \2 @( ?, r! D9 bbeen added, in which case, discard the solution and repeat this" i5 X$ m/ ~( s6 L& X
procedure with another 100 ml of Sample Solution B, using 50 ml, $ f3 Y3 m: \- L( u [& o( h* yrather than 25 ml, of 0.02 M disodium EDTA.+ V% [9 h3 I$ {( @5 u
Procedure( n0 B- \) I T" P3 R
Using the standardized zinc sulfate solution as titrant, titrate Sample* G, Q2 O3 a8 s( V
Solution C to the first yellow-brown or pink end-point that persists for ) v+ G2 D# _: v4 T8 a1 A% K5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first& ]5 B6 C7 z. S s) k) d4 C, }
titration should require more than 8 ml of titrant, but for more accurate, R/ _/ c5 F( m1 R
work a titration of 10-15 ml is desirable. " t# H8 [8 k. ~8 @Add 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5 8 Q1 d. D0 l9 @9 }- `( o9 `min, and cool in a stream of running water. Titrate this solution, using , }$ l# g0 X+ \$ {; othe standardized zinc sulfate solution as titrant, to the same fugitive; E' C% N2 A1 T. r, `) p: G) f
yellow-brown or pink end-point as described above.9 _ x5 d( p4 `" g$ R$ Z! n$ b: U
Calculation: 9 E. o# ?0 t4 V8 b& |Calculate the percentage of aluminium oxide (Al2O3) in the sample 5 A5 _; T! L: R$ T; qtaken by the formula:& e! z! K d% s* V0 }
% Al2O3 = 100 × (0.005VT)/S ( {5 ~" d" n$ [3 lwhere" j; G5 e$ A1 c. S9 |2 ~" S; }% M: T2 H
V is the number of ml of 0.01 N zinc sulfate consumed in' X% W! G' Q5 \' C5 i
the second titration,# z: Q4 A( d0 x, Q" R
T is the titre of the zinc sulfate solution, ; \: r% h0 t! h9 {0 S1 v3 S) e% ~S is the mass (g) of the sample taken, and6 ~) {- U5 l6 E2 C% x8 o" P: K
0.005 = 500 ml / (1000mg/g × 100 ml). : c/ K: l# a) u! X4 t$ TSilicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica3 `: h8 U/ g$ @7 M% O$ S
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).- |3 a2 V% J' ~. d+ i* w$ E
Heat gently over a Meeker burner, while swirling the flask, until , b( `, j$ p& c2 {% M5 j4 |decomposition and fusion are complete and the melt is clear, except $ _4 K) |: F; @7 M2 Rfor the silica content, and then cool. (Caution: Do not overheat the , ]3 g) I6 z& d5 Y$ Mcontents of the flask at the beginning, and heat cautiously during, N! q3 l* \* ?
fusion to avoid spattering.)5 ^9 a L, \0 |: p
To the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat # _. g) C Z$ P" ?carefully and slowly until the melt is dissolved. Cool, and carefully add% w: E; N7 E5 D4 k
150 ml of water by pouring very small portions down the sides of the w$ o0 X8 c7 w5 _( Z9 o
flask, with frequent swirling to avoid over-heating and spattering. Allow0 [4 U3 O% L8 a( e7 Y* T
the contents of the flask to cool, and filter through fine ashless filter ) [3 R( Q' _$ a4 b* I& r4 H! lpaper, using a 60 degree gravity funnel. Rinse out all the silica from ; I8 N- R2 B& Z& F$ a8 Y/ Cthe flask onto the filter paper with sulfuric acid solution (1 in 10).0 y6 s7 |- q5 `+ q
Transfer the filter paper and its contents into a platinum crucible, dry in Z4 x# `6 k2 `. q. Ian oven at 1200, and heat the partly covered crucible over a Bunsen ! c/ F' F; ^* b1 B, [2 i qburner. To prevent flaming of the filter paper, first heat the cover from% S0 L1 [8 L( D: S5 n+ J
above, and then the crucible from below.! R( H: }, e: c( R& C, v4 @
When the filter paper is consumed, transfer the crucible to a muffle: L" Q4 e, g+ e/ j. m6 s
furnace and ignite at 1000o for 30 min. Cool in a desiccator, and9 Z" K' g* R: H, N
weigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated, D8 a" _$ M: Y* L, [6 i+ n1 p
hydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first4 c8 F- v; d/ k" z4 z+ r
on a low-heat hot plate (to remove the HF) and then over a Bunsen5 ?$ C; B Q$ f7 M: h& W' ]
burner (to remove the H2SO4). Take precautions to avoid spattering, + k0 [" V( i' t8 q# I; yespecially after removal of the HF. Ignite at 1000o for 10 min, cool in a. t3 L/ |1 b8 s4 o7 B+ C! `+ _9 y- O' d4 Q
desiccator, and weigh again. Record the difference between the two 3 e! q4 V( l- U8 G( w7 U8 Jweights as the content of SiO2 in the sample. ! x+ ]6 J2 @3 z# fMETHOD OF ASSAY, X& o! D" n* p( r8 J
Accurately weigh about 150 mg of the sample, previously dried at 105o : R1 b) w- |! Jfor 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water. l- |: ?1 j `
and shake until a homogeneous, milky suspension is obtained. Add 30 3 R, ^( T V% u! d# c0 nml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially 0 I7 W! {* a* J$ P1 X+ ?+ o: c& Vheat gently, then heat strongly until a clear solution is obtained. Cool, " R i/ p/ ~3 J' ?) @then cautiously dilute with 120 ml of water and 40 ml of hydrochloric5 S5 o% d X; N2 H) d7 z
acid, and stir. Add 3 g of aluminium metal, and immediately insert a # `3 @. G+ {" }# srubber stopper fitted with a U-shaped glass tube while immersing the( ^3 D3 N0 T8 S
other end of the U-tube into a saturated solution of sodium " b7 ?* J* k: L% Lbicarbonate contained in a 500-ml wide-mouth bottle, and generate' e1 l) x, O% i3 a# h( i
hydrogen. Allow to stand for a few minutes after the aluminium metal + \: G1 e% I+ Y Z) r; J7 E9 \+ shas dissolved completely to produce a transparent purple solution.2 l7 I9 n7 L$ x
Cool to below 50o in running water, and remove the rubber stopper2 v- h: e6 B- s" j/ Q3 J T0 n& z: f
carrying the U-tube. Add 3 ml of a saturated potassium thiocyanate/ C. Y/ @5 t: x3 J
solution as an indicator, and immediately titrate with 0.2 N ferric . M O% ?* I5 C8 Y/ }6 Cammonium sulfate until a faint brown colour that persists for 30 4 D& s4 x9 ~# Q* l3 u8 bseconds is obtained. Perform a blank determination and make any7 U* X7 {& R5 {; ~/ x2 y0 @
necessary correction. Each ml of 0.2 N ferric ammonium sulfate is 5 n; x. o8 A- f/ \equivalent to 7.990 mg of TiO2.. Q( ]1 L# u. g# C0 K