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二氧化钛(钛白粉)
二氧化钛(钛白粉)+ X2 S/ ^, A- n! ?/ P; E6 o* y3 `
, ?. P3 w1 B/ H t5 l
JECFA关于二氧化钛(钛白粉)的结论
0 |% m9 e b" J% {" y- u0 Y( \1 M, F- `8 k' d9 B5 C
摘要: 2006年JECFA关于二氧化钛的结论5 b2 e) p' a9 I) o3 J( d
ADI值:不作限制。
( C. h! ~1 Z) ~7 A3 d. W! J/ w功能:着色剂- p+ }9 z' x L( H$ `. v
: [* {/ Y- H4 A5 f7 y7 ~5 [TITANIUM DIOXIDE0 I9 ]2 f6 ]& V5 e" V4 r5 E) S
Prepared at the 67th JECFA (2006) and published in FAO JECFA9 P) ~5 {4 k& d
Monographs 3 (2006), superseding specifications prepared at the 63rd
9 Y$ ~" n4 h2 z* IJECFA (2004) and published in FNP 52 Add 12 (2004) and in the
( b6 k5 U8 t5 g1 `Combined Compendium of Food Additive Specifications, FAO JECFA# W- A s- _+ ]" m" u# J) G2 l
Monographs 1 (2005). An ADI “not limited” was established at the 13th7 o* |! V# u, ~8 d* C$ t* T
JECFA (1969).; r: b6 R, G8 M2 I- I& R+ N
SYNONYMS" }' x4 O3 X+ @( Y7 Y1 Q
Titania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171
( b* h8 V, k# \ [4 EDEFINITION& t% N) H) p% c5 L- O
Titanium dioxide is produced by either the sulfate or the chloride7 K G' Y1 ~% y- l) i1 N
process. Processing conditions determine the form (anatase or rutile
0 ]+ j9 F& z* p8 ^" pstructure) of the final product.
' T/ r* D+ L# hIn the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)4 p# Q9 T4 r/ i9 F
or ilmenite and titanium slag. After a series of purification steps, the7 w% _& o$ @1 d$ ?
isolated titanium dioxide is finally washed with water, calcined, and
. k, F0 u: a5 ?micronized.
6 _8 n U: \$ X) m, N- h9 f' sIn the chloride process, chlorine gas is reacted with a titaniumcontaining
) v6 E( A! I! c. V& p1 g/ `. Imineral under reducing conditions to form anhydrous1 F1 t F: {' d* Q1 W) k
titanium tetrachloride, which is subsequently purified and converted to
8 Z) u' ]: U8 c: C4 Ftitanium dioxide either by direct thermal oxidation or by reaction with
. D. d& H3 E* N1 H5 Lsteam in the vapour phase. Alternatively, concentrated hydrochloric
- |: N( B) ] n* o/ I0 J, Vacid can be reacted with the titanium-containing mineral to form a
5 G5 Y* v+ R2 b8 I: vsolution of titanium tetrachloride, which is then further purified and0 }/ h7 J: F+ n( s" k1 S
converted to titanium dioxide by hydrolysis. The titanium dioxide is
* I& T5 w6 n: V/ b7 kfiltered, washed, and calcined.
& l# H- R3 r2 O4 j" BCommercial titanium dioxide may be coated with small amounts of1 T) W }* M4 Y Z, l
alumina and/or silica to improve the technological properties of the, W0 l. M0 H/ i; _7 z/ ^* v$ \0 q
product.- k2 R" y% t( I; J, {0 O. C
C.A.S. number 13463-67-7
7 b' b# ^# Z' W5 M9 F! GChemical formula TiO20 {) ]0 f% |9 a% k6 F
Formula weight
9 a3 f- N, t, l1 o8 H) b* U9 b79.88
- \, Z: O5 C* C# g$ B( h' F$ ZAssay& v/ D3 t7 ?3 l( l& [
Not less than 99.0% on the dried basis (on an aluminium oxide and3 O2 l: m2 u _, u2 K, J" K) Q
silicon dioxide-free basis)
/ |" ]9 z u$ f8 E: }4 P9 SDESCRIPTION
8 p: Z& {+ F/ H7 E! S, l1 QWhite to slightly coloured powder
) M$ w2 F8 t) C* j. ZFUNCTIONAL USES
* Q/ F# B1 Z" ~6 DColour: I. K6 S4 Q3 v! N/ P
CHARACTERISTICS
4 U1 }" Z) t1 e) j" F9 r# v) WIDENTIFICATION' g( t+ T' b. [8 F" F7 B# z2 W
Solubility (Vol. 4)
/ z, f/ {6 q2 W- `& K0 _( F0 FInsoluble in water, hydrochloric acid, dilute sulfuric acid, and organic
3 F' ?( ~: ?% [( o; h) T8 {solvents. Dissolves slowly in hydrofluoric acid and hot concentrated
8 c% _+ S0 F6 N: f3 u0 ysulfuric acid.% J/ z6 O+ i# Z: _* J
Colour reaction. X1 d0 d) e/ k3 H0 h
Add 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of
" ~# A4 L: o5 D8 p3 p; x( Z! asulfuric acid appear, then cool. Cautiously dilute to about 100 ml with6 W5 n& _" d G2 ^9 c
water and filter. To 5 ml of this clear filtrate, add a few drops of
. Q5 G& E6 o6 g% Z" e& thydrogen peroxide; an orange-red colour appears immediately. `- S6 b. `. y0 C2 U
PURITY& g( W5 s) d8 E% z: ^$ a+ Y! Q
Loss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)
/ n% Q* U! e0 t) n0 hLoss on ignition (Vol. 4)" H$ m Y# r% z& b6 d
Not more than 1.0% (800o) on the dried basis
1 |. h* ~/ F' C' z* r5 TAluminium oxide and/or4 H* E. ~$ d f3 z+ H- @
silicon dioxide
; Y3 V8 o0 {2 B' n* ^Not more than 2%, either singly or combined) j) g- n) n6 O3 S2 W
See descriptions under TESTS
?/ O V, F' ^1 `0 r! Z0 N$ yAcid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing: D+ F5 H8 r7 j# u
alumina or silica.7 E+ O- c' b, ?4 |1 o/ B- x
Suspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and
: b+ z' d9 g7 n4 [) Bplace on a steam bath for 30 min with occasional stirring. Filter7 _6 F' i( X7 ^
through a Gooch crucible fitted with a glass fibre filter paper. Wash1 d5 A0 ^; N6 N$ f* V
with three 10-ml portions of 0.5 N hydrochloric acid, evaporate the
: I- }4 i) G- ccombined filtrate and washings to dryness, and ignite at a dull red
+ @9 N0 W& s" Z S) |heat to constant weight.
$ d( u; t: m/ b6 r. ZWater-soluble matter- _8 K; ]% e% t3 U; h
(Vol. 4)
3 ]. ^ U* ~+ Q2 |6 JNot more than 0.5%
9 Q, {# q+ i* c! E* F8 pProceed as directed under acid-soluble substances (above), using
( T& c) X. n) I! s2 d9 bwater in place of 0.5 N hydrochloric acid.
; ]4 X+ C" o1 `: Z( QImpurities soluble in 0.5 N$ l2 U( {( M. v9 P) d. k+ Q
hydrochloric acid$ p* ?; N+ L- d& h
Antimony Not more than 2 mg/kg( }4 p; B7 c( `! p2 N: v
See description under TESTS. l; t6 D4 r6 y& e4 I; u) v1 k& y, K% v
Arsenic Not more than 1 mg/kg; Z2 v' z3 f4 W! d5 h
See description under TESTS' P+ Z7 b) Y4 O3 G6 j, W
Cadmium Not more than 1 mg/kg; b4 i4 W0 I. u N# p" ^! |, n
See description under TESTS' b# {0 X( g; {& R2 ]2 C( {: g
Lead! R- ?$ ]/ ~: ~$ U8 s/ J4 Q9 U, K
Not more than 10 mg/kg ?. _- H1 k* q
See description under TESTS
3 c) V4 P0 X' v" R5 t1 `# ^Mercury (Vol. 4) Not more than 1 mg/kg8 o8 U6 U% ?7 Q8 X0 z9 c% {2 ^
Determine using the cold vapour atomic absorption technique. Select a
0 Z0 t" f+ h) u( a' asample size appropriate to the specified level
; B& F2 L+ C0 T0 p: i! ?; yTESTS
% k& M$ n6 K6 r* ^% ?# J7 RPURITY TESTS
" E: C) S7 l4 N0 AImpurities soluble in 0.5 N, m- x) L9 w4 s- L% J2 I* _
hydrochloric acid2 M5 m! C" O. e# ?4 ]! B
Antimony, arsenic,
+ s( J6 ~3 s" V7 B) g+ P4 rcadmium and lead/ |2 C9 O2 }, I4 |5 f4 v. M5 R/ {
(Vol.4)- n2 v9 Q, v: r" A0 g# C
Transfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N
# a" ?0 N* I% c7 p" z% O1 _5 _hydrochloric acid, cover with a watch glass, and heat to boiling on a
; P9 c6 V- ^# x! s4 d( f! E# _hot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml! S% t+ m% J0 G# j. O' G9 f* J9 A
centrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved7 _+ o I/ h3 q3 I* r: s
material settles. Decant the supernatant extract through a Whatman
- k3 g) e2 l" T+ R- I. {) N7 a6 UNo. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml4 F' R$ y6 d( l& h. U l
volumetric flask and retaining as much as possible of the undissolved
% f c, o- `8 }) zmaterial in the centrifuge bottle. Add 10 ml of hot water to the original- ?7 O6 l4 q0 S% O$ r: R3 R
beaker, washing off the watch glass with the water, and pour the
9 o5 u; A2 c* \$ I- econtents into the centrifuge bottle. Form a slurry, using a glass stirring4 J- `' ]8 c: m1 R' [) z7 E
rod, and centrifuge. Decant through the same filter paper, and collect
4 g( V% O. _: R [the washings in the volumetric flask containing the initial extract.. E2 y/ l$ g- @6 C. e
Repeat the entire washing process two more times. Finally, wash the6 ]. I9 h% S; B0 V l, X3 g
filter paper with 10 to 15 ml of hot water. Cool the contents of the flask- @1 h: h% p1 q" f
to room temperature, dilute to volume with water, and mix.7 d( G% b& E2 h0 W" ^
Determine antimony, cadmium, and lead using an AAS/ICP-AES; @& j, }: Z' u& r# y
technique appropriate to the specified level. Determine arsenic using the$ X" i9 n& `8 R; q2 [
ICP-AES/AAS-hydride technique. Alternatively, determine arsenic using
& ?& l) r, U8 F2 mMethod II of the Arsenic Limit Test, taking 3 g of the sample rather than/ v) N1 a! y# x- |$ e0 L
1 g. The selection of sample size and method of sample preparation
0 ~) ]% O* V+ f; u {may be based on the principles of the methods described in Volume 4.
% U5 ]$ b4 i) a; Y$ r0 nAluminium oxide Reagents and sample solutions# w# |9 N5 k' G; h) Y
0.01 N Zinc Sulfate
% s. _& n! A2 g. L" O: i, F( p$ QDissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to
) q/ l8 b9 ]9 d2 e7 ]; A! _2 Gmake 1000 ml. Standardize the solution as follows: Dissolve 500 mg
5 W- t `4 t8 R8 Wof high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of
6 p+ `0 G- C1 @3 Lconcentrated hydrochloric acid, heating gently to effect solution, then. {% V' h# J. p: l" V
transfer the solution into a 1000-ml volumetric flask, dilute to volume3 _' x1 r" F6 e+ h0 `9 G. I6 {) G
with water, and mix. Transfer a 10 ml aliquot of this solution into a 500
! Q$ I. O9 t1 {- r; n& h) M3 ]3 Fml Erlenmeyer flask containing 90 ml of water and 3 ml of
; \- J' P! V2 ?concentrated hydrochloric acid, add 1 drop of methyl orange TS and
! q9 c( K5 T$ C/ y25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,
+ y5 j: u5 W; S& tdropwise, ammonia solution (1 in 5) until the colour is just completely
: k$ n* ?4 R5 S$ \0 ^4 S0 Schanged from red to orange-yellow. Then, add:
. W4 h" H/ O6 c8 q) X; ~1 O(a): 10 ml of ammonium acetate buffer solution (77 g of
$ Q& r% V8 }5 L5 f; X4 y- Cammonium acetate plus 10 ml of glacial acetic acid, dilute to
4 m1 ]* f5 i. v1000 ml with water) and
& L0 L4 o5 @$ m9 V0 [/ O0 ` E(b): 10 ml of diammonium hydrogen phosphate solution (150 g
: f8 _% d V! G& c4 uof diammonium hydrogen phosphate in 700 ml of water,
8 t* H. x4 N& q8 x7 Y# z( y, m/ Badjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,
/ ^1 j, Z+ N+ ~: C7 Rthen dilute to 1000 ml with water).
5 u6 @7 G* h2 o/ x/ W8 k CBoil the solution for 5 min, cool it quickly to room temperature in a" ~5 [/ |( F; o. K0 {
stream of running water, add 3 drops of xylenol orange TS, and mix.
1 J- P+ I5 M0 G) I. d- M3 VUsing the zinc sulfate solution as titrant, titrate the solution to the first
! C; U" ^: Y4 ~# |0 b$ {yellow-brown or pink end-point colour that persists for 5-10 sec. (Note:
! r; k3 \$ E+ F% `This titration should be performed quickly near the end-point by
' E+ w: K' p1 Uadding rapidly 0.2 ml increments of the titrant until the first colour
5 [! M! V+ o9 l ]& M4 P3 [change occurs; although the colour will fade in 5-10 sec, it is the true
% a; E! C. ]7 ^6 I2 F! M4 g) Send-point. Failure to observe the first colour change will result in an
0 \2 E1 ^* Z! ^ ~6 X; ]incorrect titration. The fading end-point does not occur at the second7 _, X/ U, U1 p3 L. H
end-point.)
, I+ P( |) m3 L+ {' v$ A9 `- Z' OAdd 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a. }1 g2 H( G, W
stream of running water. Titrate this solution, using the zinc sulfate
5 V# {& |1 p$ X4 z+ Y3 u! {0 osolution as titrant, to the same fugitive yellow-brown or pink end-point
+ M# }; l5 f; Y; s5 Mas described above.! x# ~2 U) B7 b. X: a; `) V0 H
Calculate the titre T of zinc sulfate solution by the formula:/ `" X4 W( Y( @0 ~; t
T = 18.896 W / V" ~1 V& [! f# l, J
where9 w8 Y5 L/ I! z8 C
T is the mass (mg) of Al2O3 per ml of zinc sulfate solution) n' Q& T- k/ s( X2 Q) i/ P
W is the mass (g) of aluminium wire- N% O( X, x+ s4 Y$ s
V is the ml of the zinc sulfate solution consumed in the
; e- ~4 s. r- N& x6 E1 L |0 i& esecond titration. u6 \. A4 u2 b: f! I0 W
18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and8 h$ a& c) O5 n+ F8 X
R is the ratio of the formula weight of aluminium oxide to+ @& @( h3 B/ Z6 i
that of elemental aluminium.. k$ j; L2 Y" { M" H3 |% N: q
Sample Solution A" h: I& m* g8 S5 N- C7 V; e5 Z
Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica
$ W3 R5 l* h* Y0 [* G4 C* `) fglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
7 o# ?) \+ _# K0 n(Note: Do not use more sodium bisulfate than specified, as an excess
E5 d1 o! p; r- sconcentration of salt will interfere with the EDTA titration later on in the
8 i* h% F3 Q) p$ Hprocedure.) Begin heating the flask at low heat on a hot plate, and/ C1 l+ v: m$ H3 ?; u
then gradually raise the temperature until full heat is reached.$ j3 }) x8 u3 A+ i) C6 C
(Caution: perform this procedure in a well ventilated area. ) When
9 D9 {; J' p0 z3 r2 Z; l' ispattering has stopped and light fumes of SO3 appear, heat in the full
; D" u6 W+ w$ V7 q" J* Sflame of a Meeker burner, with the flask tilted so that the fusion of the
6 T- W# }: ^' isample and sodium bisulfate is concentrated at one end of the flask.
' E5 `$ \0 F. W3 y' ^5 X, oSwirl constantly until the melt is clear (except for silica content), but1 v( W$ W& f- _
guard against prolonged heating to avoid precipitation of titanium4 ?9 @$ U/ e0 |3 M' Y7 f+ q
dioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until/ T- t0 w; J- R. t) y9 ?0 j
the mass has dissolved and a clear solution results. Cool, and dilute to
# y) M8 R0 _7 O# R+ m" N5 p- r u120 ml with water. Introduce a magnetic stir bar into the flask.
$ y [; c: l8 `0 e6 ~! xSample Solution B# _* K x$ }- u7 D& X' E- o
Prepare 200 ml of an approximately 6.25 M solution of sodium
# V& Z' C V3 D. |% [; q' P9 I. ahydroxide. Add 65 ml of this solution to Sample Solution A, while
1 a0 S$ s& W( M0 I6 T: v/ @6 y1 ?stirring with the magnetic stirrer; pour the remaining 135 ml of the1 O: d0 z3 j5 D! R& |
alkali solution into a 500-ml volumetric flask./ g* f( X2 \, b7 @
Slowly, with constant stirring, add the sample mixture to the alkali
, G+ n3 m# M6 h6 K0 X" Osolution in the 500-ml volumetric flask; dilute to volume with water,
- j D& s( f% M( rand mix. (Note: If the procedure is delayed at this point for more than N% f' I6 n6 \/ B, ~ A' p
2 hours, store the contents of the volumetric flask in a polyethylene
Q/ J; ~2 |- d, gbottle.) Allow most of the precipitate to settle (or centrifuge for 5 min), u# j$ ^# G; E2 `" r
then filter the supernatant liquid through a very fine filter paper. Label. [1 D' C) w" Q- D) S9 R T
the filtrate Sample Solution B.- ~* S$ T# r; w1 `
Sample Solution C- M* y* s% `. V2 ?
Transfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer
" T1 K: W1 X) ^$ C: G U- P) vflask, add 1 drop of methyl orange TS, acidify with hydrochloric acid
; x7 y* K3 Q' j5 Z Jsolution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02
' ^" u( y7 o/ [, p/ a% `( gM disodium EDTA, and mix. [Note: If the approximate Al2O3 content is
/ E7 q1 f' H) j) aknown, calculate the optimum volume of EDTA solution to be added
7 `8 Y4 z7 J$ d5 d: }) k: S4 d# qby the formula: (4 x % Al2O3) + 5.]) |6 p2 [7 D7 r4 }" e! U& {, ]
Add, dropwise, ammonia solution (1 in 5) until the colour is just
' i# j1 o8 D/ D; Y" |completely changed from red to orange-yellow. Then add10 ml each
1 c' x7 D( m+ ?6 _of Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to% n: T l/ Z1 T: Z" w
room temperature in a stream of running water, add 3 drops of xylenol
, E0 [0 J% {6 n2 h" {orange TS, and mix. If the solution is purple, yellow-brown, or pink,) w; d o$ ?! U$ p x' p* K
bring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired+ P; R& P* L r+ v: g5 f& ~, u
pH, a pink colour indicates that not enough of the EDTA solution has
- w# G7 C: R+ zbeen added, in which case, discard the solution and repeat this7 U ?; G/ \3 B0 ~
procedure with another 100 ml of Sample Solution B, using 50 ml,
; r0 }% b( C$ T' Trather than 25 ml, of 0.02 M disodium EDTA.
" r, t* r) _ |+ I2 j' }' j0 _Procedure
) `2 e2 C( t: S9 u/ t3 V x* mUsing the standardized zinc sulfate solution as titrant, titrate Sample/ W. ]+ S1 @' j j( a
Solution C to the first yellow-brown or pink end-point that persists for
9 @4 ?7 p; t7 @7 p4 c5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first
' S2 { v' ?: rtitration should require more than 8 ml of titrant, but for more accurate
% m8 Y0 D9 ^# R) ^. z5 Y) Pwork a titration of 10-15 ml is desirable.! o! m" t6 A9 m6 T. [6 m
Add 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5
) }$ c3 Y9 ~3 `6 w3 b( Omin, and cool in a stream of running water. Titrate this solution, using5 a; U' p; x6 l5 W1 t3 t. G5 j
the standardized zinc sulfate solution as titrant, to the same fugitive& L ~9 L9 z5 e
yellow-brown or pink end-point as described above.# ]1 C: H; _4 {# N
Calculation:$ a8 M) f/ |; B7 h9 ^' m7 `6 U
Calculate the percentage of aluminium oxide (Al2O3) in the sample- X: @8 {3 X( ]
taken by the formula:
+ j5 I: f- m* J. ]- M% Al2O3 = 100 × (0.005VT)/S
7 h4 _+ \ ?% J: a, l8 gwhere8 x- O& t. C& A3 P" c
V is the number of ml of 0.01 N zinc sulfate consumed in
$ _1 |- D: [, P& V Ethe second titration,
4 H' h" b" {9 V5 ~9 r, Z4 eT is the titre of the zinc sulfate solution,
$ ?, S- }+ w8 L% dS is the mass (g) of the sample taken, and
h( h T6 T+ I5 K* X9 w0.005 = 500 ml / (1000mg/g × 100 ml).3 w, d$ G- Z& G/ R4 F
Silicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica: [$ ]% }2 e& Z; x# D7 R
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).; Z8 {' l- q% _8 x
Heat gently over a Meeker burner, while swirling the flask, until5 [1 o+ ]6 p4 Y4 G
decomposition and fusion are complete and the melt is clear, except* w1 f3 k+ b( x# H' @& T
for the silica content, and then cool. (Caution: Do not overheat the
6 q" F b0 S1 H- K# |( R8 ^contents of the flask at the beginning, and heat cautiously during4 I3 a1 Q# g( s5 g' c6 _, M' j3 m+ a
fusion to avoid spattering.)
( E# _ S; {5 e" F0 `To the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat
4 n1 }: e: ?! d, Xcarefully and slowly until the melt is dissolved. Cool, and carefully add# M1 e- R! t& y+ x) w% d W
150 ml of water by pouring very small portions down the sides of the5 O2 X( l* T$ U8 o9 r
flask, with frequent swirling to avoid over-heating and spattering. Allow
" d5 B* ]: w1 u. X3 |- G! Xthe contents of the flask to cool, and filter through fine ashless filter
" F9 M2 @' ]4 Y/ [/ epaper, using a 60 degree gravity funnel. Rinse out all the silica from, A, T# M y; }+ C
the flask onto the filter paper with sulfuric acid solution (1 in 10).
' k4 N5 _- M0 O; e* I6 I( nTransfer the filter paper and its contents into a platinum crucible, dry in
# T0 g/ Z S2 [ E- Yan oven at 1200, and heat the partly covered crucible over a Bunsen. [9 L9 X$ E: [, \/ ^% S0 n
burner. To prevent flaming of the filter paper, first heat the cover from2 K9 ^- q, Y' o0 b& K
above, and then the crucible from below., q& y1 z! [( _( [- J
When the filter paper is consumed, transfer the crucible to a muffle
% O) G2 ]# j, F! \+ yfurnace and ignite at 1000o for 30 min. Cool in a desiccator, and
- B& O: B+ `4 O3 O% S2 A+ fweigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated \# { y, ?4 H3 R0 H6 j) G7 H6 ]
hydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first; B: v5 _: m8 ~1 O1 a
on a low-heat hot plate (to remove the HF) and then over a Bunsen6 g0 u# ~* C: S/ D7 z; |3 V
burner (to remove the H2SO4). Take precautions to avoid spattering,! l7 q: C! M- e8 g: n
especially after removal of the HF. Ignite at 1000o for 10 min, cool in a+ V% p$ |5 a, M7 U0 \9 {% Y& @/ O
desiccator, and weigh again. Record the difference between the two
: ]2 Z( q4 R( x' `$ [) l8 \: Tweights as the content of SiO2 in the sample.0 j, {2 d; b& p6 d5 \7 E' v
METHOD OF ASSAY( w2 A: |7 U; E3 d5 {! O$ `
Accurately weigh about 150 mg of the sample, previously dried at 105o1 ]: s9 F! ~! Z d
for 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water
, t5 H/ X+ u3 y9 I5 h" `and shake until a homogeneous, milky suspension is obtained. Add 30
! S9 `: W: n! `4 [/ Nml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially @8 D; W( ^3 M2 W8 d
heat gently, then heat strongly until a clear solution is obtained. Cool,# V2 H% ~( Z6 W% C
then cautiously dilute with 120 ml of water and 40 ml of hydrochloric6 O$ q3 ~6 _+ w4 g
acid, and stir. Add 3 g of aluminium metal, and immediately insert a3 z' K1 t+ T! |' B/ U" A3 v- P9 |
rubber stopper fitted with a U-shaped glass tube while immersing the! ]0 r$ O4 e( S3 ?
other end of the U-tube into a saturated solution of sodium/ v/ e9 b. X, U
bicarbonate contained in a 500-ml wide-mouth bottle, and generate9 T4 o5 C! P4 t
hydrogen. Allow to stand for a few minutes after the aluminium metal# ?: x& Y8 S! `- k% Z0 U
has dissolved completely to produce a transparent purple solution.( G/ M d) O! ~& G& J
Cool to below 50o in running water, and remove the rubber stopper4 ~% e/ O% p' @5 J# Q# N. d
carrying the U-tube. Add 3 ml of a saturated potassium thiocyanate
" S$ \; e& f Y/ Z% S8 esolution as an indicator, and immediately titrate with 0.2 N ferric0 p: z# W* V) Y
ammonium sulfate until a faint brown colour that persists for 30
@- t: ?/ Q* u/ }1 t% B8 ~3 Nseconds is obtained. Perform a blank determination and make any1 \* R* \1 B: I! |" ~3 o" b
necessary correction. Each ml of 0.2 N ferric ammonium sulfate is
2 K U Q- l/ Z" B( }- [) iequivalent to 7.990 mg of TiO2.( F: f/ I1 v5 ^7 J- d) r) @
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