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二氧化钛(钛白粉)
二氧化钛(钛白粉)6 s& \. N( o2 Z. C* ?* A! P9 Z
: F4 X: F" p1 L5 ?9 ]) ?9 @JECFA关于二氧化钛(钛白粉)的结论; W1 d7 B, F" T1 Y: P6 X1 U/ X
. G* u7 c; }* B r6 E4 E/ C
摘要: 2006年JECFA关于二氧化钛的结论. r9 B3 ]% F- `% T6 O
ADI值:不作限制。- J8 }4 J3 |( W+ h. |/ d
功能:着色剂/ n! p" z7 V! \4 b) m
5 O$ K, b6 \) h- n6 A! f8 b8 ?TITANIUM DIOXIDE
) C5 U6 o0 w$ h# O: B% B) J) \Prepared at the 67th JECFA (2006) and published in FAO JECFA
6 e+ F8 v5 N D6 ^! ]( o) ~/ WMonographs 3 (2006), superseding specifications prepared at the 63rd; L2 [9 p, \+ J5 D, Q; G+ F* G1 g# ~
JECFA (2004) and published in FNP 52 Add 12 (2004) and in the
) X3 I1 {. A1 \7 Z% }Combined Compendium of Food Additive Specifications, FAO JECFA
T6 X9 `2 ?1 o' P5 C. ?Monographs 1 (2005). An ADI “not limited” was established at the 13th& I) m! Z4 n2 ?6 F9 M
JECFA (1969).
* x6 K9 ?5 i9 }6 [0 U. y( DSYNONYMS b2 D' j0 z: Q% m, Y: n. L3 D- ~
Titania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171- G. ^# n9 k% ]2 h
DEFINITION- c, h2 w# m% P, H6 h6 ?/ s9 f
Titanium dioxide is produced by either the sulfate or the chloride# S- _) z+ \8 D6 y' f% q
process. Processing conditions determine the form (anatase or rutile! A- z# g2 x2 x- {. x/ D# K
structure) of the final product.: P9 ?! a& J! F! N2 R
In the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)
! Y, P1 z% ?+ h- G [or ilmenite and titanium slag. After a series of purification steps, the N: L6 f+ s' ^; A6 K& n: Q% _
isolated titanium dioxide is finally washed with water, calcined, and
% n# S5 P2 p6 j+ fmicronized.- I2 E, x+ d5 M. Q* X2 W7 `: W6 I4 p
In the chloride process, chlorine gas is reacted with a titaniumcontaining
' m% t: b* r, `mineral under reducing conditions to form anhydrous& |# l8 g8 @$ [( w+ a* ~, D
titanium tetrachloride, which is subsequently purified and converted to, }/ n) G1 A* r$ _9 F% Q" ~6 g
titanium dioxide either by direct thermal oxidation or by reaction with" M( N; W; a- |/ Y9 d1 M& Q2 ?
steam in the vapour phase. Alternatively, concentrated hydrochloric
7 L1 e( e8 z, E3 c% m% c" J" T+ Bacid can be reacted with the titanium-containing mineral to form a8 f3 ?: V3 o& a8 c7 s8 N# ~
solution of titanium tetrachloride, which is then further purified and7 P0 i: B! {) m& X; }3 A
converted to titanium dioxide by hydrolysis. The titanium dioxide is7 g2 r! {" B4 U+ A
filtered, washed, and calcined.
; f P5 U% f5 W9 {Commercial titanium dioxide may be coated with small amounts of3 b2 q+ i7 }* \. l- Z
alumina and/or silica to improve the technological properties of the
! x4 d- ^0 o4 |product.
7 `2 h$ z5 Z. G4 {; ]2 w1 A. b) yC.A.S. number 13463-67-7" n: d) o# Q7 |' K9 @
Chemical formula TiO2
% V6 f( v% R" Y$ h \$ r' ~Formula weight
5 x9 Y9 s+ } E; V+ v0 f79.886 Z" K9 y3 V6 p4 ~: D8 K9 Q* U
Assay
: t$ ]* P; p& \. ^" T- KNot less than 99.0% on the dried basis (on an aluminium oxide and5 h$ }* w% k& ^/ e+ ?
silicon dioxide-free basis)
" m7 ~# ]7 [; d Q1 j" N a5 g- [DESCRIPTION
3 V8 }& M9 z( K. g, |White to slightly coloured powder
) A2 c3 |9 a2 G1 DFUNCTIONAL USES. o) o8 t+ Z$ W5 w
Colour
$ m& k. F0 i! Q+ `. JCHARACTERISTICS0 E: j! R' ~- h |
IDENTIFICATION7 S4 \: ~- V/ s
Solubility (Vol. 4)2 G: ?; \2 D0 n* u+ h
Insoluble in water, hydrochloric acid, dilute sulfuric acid, and organic& M1 P/ z. ^/ u8 I
solvents. Dissolves slowly in hydrofluoric acid and hot concentrated
3 b5 y( B8 V3 U+ }( G& _sulfuric acid.
* K, G8 s2 A: jColour reaction) b2 F1 a7 k5 a, u
Add 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of
% S- C4 R1 U+ K) u _/ |) o+ V) Zsulfuric acid appear, then cool. Cautiously dilute to about 100 ml with
8 e N* h+ }. y0 v" |1 w) wwater and filter. To 5 ml of this clear filtrate, add a few drops of
. G- z" E# E/ G- A bhydrogen peroxide; an orange-red colour appears immediately.% q3 B& ^( e3 t) F, H l/ y
PURITY. A2 L: X' g5 ~ \) L2 S c ]$ A
Loss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)
5 D9 U# [3 `" d" P; h4 W8 \2 {7 jLoss on ignition (Vol. 4)
; O7 E, f) Z" hNot more than 1.0% (800o) on the dried basis% u. e) c0 F9 m2 Z; L
Aluminium oxide and/or3 L9 C% h* Q9 V0 K6 E$ N
silicon dioxide' P$ U0 g U2 F* i
Not more than 2%, either singly or combined6 Y4 c5 q0 M7 a" \7 L
See descriptions under TESTS- o8 X. W( h! E z# N
Acid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing
2 S5 r. B2 O7 N/ palumina or silica.8 \. Z j- T* P* H4 T A
Suspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and% X0 r9 F4 B5 E! y" w
place on a steam bath for 30 min with occasional stirring. Filter
; m. b- c6 b; s( b# K0 ~through a Gooch crucible fitted with a glass fibre filter paper. Wash
3 ? x# F; d8 Rwith three 10-ml portions of 0.5 N hydrochloric acid, evaporate the
9 `9 P( X% P: N7 I* {6 F! O- t* ^combined filtrate and washings to dryness, and ignite at a dull red* h G) b% V1 _) I& j7 T% K
heat to constant weight.
7 w' @6 W% z, c4 JWater-soluble matter N0 n5 p M+ y" y/ b" _. E
(Vol. 4)+ }1 }0 W" R; V& B& R T6 {
Not more than 0.5%* }' K, Q& L/ z- ]: A$ q
Proceed as directed under acid-soluble substances (above), using5 {3 z. [# }( q) i, K5 T
water in place of 0.5 N hydrochloric acid.
7 z, w$ \& z: R& n& }" d b+ b' P( G: ^Impurities soluble in 0.5 N
. v# ~' `; x% A; t* G R0 i* n9 H* Shydrochloric acid
/ ?: W+ G- L+ w" t6 ^ ^2 dAntimony Not more than 2 mg/kg; p% T- |' H" q6 {3 [
See description under TESTS
4 ], L' e4 v* rArsenic Not more than 1 mg/kg' W8 Q' S. T/ h. c/ i
See description under TESTS8 z% t5 \: ]- C2 a# k0 H- s# a3 z" R
Cadmium Not more than 1 mg/kg1 ]; v% g! E1 ]+ R8 D! A
See description under TESTS, u- a' y0 S; q
Lead( ?+ J4 D B- S+ X3 ?( w
Not more than 10 mg/kg
* O. K! t0 R# e0 M/ qSee description under TESTS
5 S) C. y2 l, b* r- {& iMercury (Vol. 4) Not more than 1 mg/kg0 z& P7 V2 ]; L1 |. ]
Determine using the cold vapour atomic absorption technique. Select a
$ R$ N/ n+ T1 Q# jsample size appropriate to the specified level. u m! S4 S# e; j$ h4 D4 k7 |
TESTS
( V& X- H9 W I* g9 iPURITY TESTS
! d$ I+ U* N, G9 sImpurities soluble in 0.5 N
; S3 _7 u( R$ k2 ~& t6 d) thydrochloric acid
6 H. Q. N: O4 _+ [! f2 L L+ }Antimony, arsenic,
# j* E9 }& x5 ?8 ocadmium and lead3 x, z4 k1 L2 L: {
(Vol.4)
! ?0 A, L* W! k5 V, f4 uTransfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N, B) G# p9 J) M0 H
hydrochloric acid, cover with a watch glass, and heat to boiling on a
$ C- a- R4 _+ Q5 p) V9 |% l( P0 _hot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml+ J5 h, `* g) y4 z
centrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved0 t+ c/ [7 e5 ]/ |- l% m* Q
material settles. Decant the supernatant extract through a Whatman
7 d1 n% A6 M# i3 m7 w' ^No. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml
8 n/ Y/ A4 ]# U: cvolumetric flask and retaining as much as possible of the undissolved
/ M" b, A; ^; }material in the centrifuge bottle. Add 10 ml of hot water to the original6 q: H6 j& A; O5 z7 p' }
beaker, washing off the watch glass with the water, and pour the. a- b# |, {# o. P7 ?; V3 k
contents into the centrifuge bottle. Form a slurry, using a glass stirring
. d9 y6 `; y) E I5 ?rod, and centrifuge. Decant through the same filter paper, and collect
% `1 i7 K! b& {, F" z8 y6 Rthe washings in the volumetric flask containing the initial extract.3 P+ m, c3 h6 v- v# `# W
Repeat the entire washing process two more times. Finally, wash the- N% a' _* R" r6 r' M4 ^' i
filter paper with 10 to 15 ml of hot water. Cool the contents of the flask
& S' d: n$ g* v7 q. |3 C- a6 tto room temperature, dilute to volume with water, and mix.. t9 c# @. E5 u
Determine antimony, cadmium, and lead using an AAS/ICP-AES
: b' Q6 e" g9 b7 `: htechnique appropriate to the specified level. Determine arsenic using the
6 U `+ q3 A. ^7 @6 f) r- nICP-AES/AAS-hydride technique. Alternatively, determine arsenic using
, ` A( M4 L* p5 i6 _3 oMethod II of the Arsenic Limit Test, taking 3 g of the sample rather than
- _: }7 U8 n& r5 U' c; z1 g. The selection of sample size and method of sample preparation
8 m3 l0 l. A( R8 xmay be based on the principles of the methods described in Volume 4.# G* E, N* F/ w
Aluminium oxide Reagents and sample solutions& z1 o5 u/ V* p+ H
0.01 N Zinc Sulfate
+ Q" M& B6 k7 s, l' ?Dissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to
/ U/ A! I# G7 e) R1 @make 1000 ml. Standardize the solution as follows: Dissolve 500 mg. |! ]" H- s w; b- _# b( I2 P) r9 q: [
of high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of" B: z# }+ U; r. K# V. E
concentrated hydrochloric acid, heating gently to effect solution, then
! W4 p! h/ ]8 q3 r8 Ytransfer the solution into a 1000-ml volumetric flask, dilute to volume
3 s4 X- M5 \4 X4 a) F: O9 fwith water, and mix. Transfer a 10 ml aliquot of this solution into a 500
6 ]3 z! R4 z. P7 ~ml Erlenmeyer flask containing 90 ml of water and 3 ml of
! S/ |' y' U: `/ J' k+ B( x+ |' G; F2 Nconcentrated hydrochloric acid, add 1 drop of methyl orange TS and
8 p! @9 y9 X( X7 J25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,
. o. f6 x! E3 G; l' o, n0 \4 @dropwise, ammonia solution (1 in 5) until the colour is just completely+ y1 L8 x' L( l8 R( M3 _3 ?( H+ S
changed from red to orange-yellow. Then, add:
5 Q4 R7 u9 _! a(a): 10 ml of ammonium acetate buffer solution (77 g of
7 `5 c s( K4 d6 z: `ammonium acetate plus 10 ml of glacial acetic acid, dilute to
6 E( `! `7 S6 M9 c1000 ml with water) and- E+ O7 ^* Z) n" H
(b): 10 ml of diammonium hydrogen phosphate solution (150 g
C* ]$ Y( [( W7 qof diammonium hydrogen phosphate in 700 ml of water,$ \" j: r) v& @) _$ E7 H
adjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,
, S" s1 ~% ^' Othen dilute to 1000 ml with water).
, u2 C. D; w: u+ ^ J+ T$ x uBoil the solution for 5 min, cool it quickly to room temperature in a
, i. x9 d: y1 ?7 }9 c5 Rstream of running water, add 3 drops of xylenol orange TS, and mix., @* t. v: n9 B) s# N7 }4 L
Using the zinc sulfate solution as titrant, titrate the solution to the first% P# ?' S2 X$ _6 c
yellow-brown or pink end-point colour that persists for 5-10 sec. (Note:+ @0 I0 i% E* p4 E# u
This titration should be performed quickly near the end-point by7 j! X! G; O- s
adding rapidly 0.2 ml increments of the titrant until the first colour
* X; x& s. e7 L2 H; _6 }change occurs; although the colour will fade in 5-10 sec, it is the true
3 h* G9 }. v, o! t, L# }9 Pend-point. Failure to observe the first colour change will result in an. x, ^. p$ s6 C- G; E
incorrect titration. The fading end-point does not occur at the second: r2 ]) P# t$ m
end-point.)
6 V6 M. _- u3 G* kAdd 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a% b, O: L+ V7 U+ g6 U
stream of running water. Titrate this solution, using the zinc sulfate# D; R5 m P/ j, x$ t
solution as titrant, to the same fugitive yellow-brown or pink end-point* a' A# j( t1 J
as described above.
- Q7 c6 h6 l8 w- `7 w( v* f7 \Calculate the titre T of zinc sulfate solution by the formula:/ V4 h4 c& w# V0 G
T = 18.896 W / V/ \3 B! V8 e: z
where
4 w" w' f4 `, @3 V. {T is the mass (mg) of Al2O3 per ml of zinc sulfate solution% G1 j. z/ u i/ B+ c6 @
W is the mass (g) of aluminium wire
3 P- X$ C6 B _V is the ml of the zinc sulfate solution consumed in the
E h2 [. b$ \7 |! f/ Wsecond titration* i" A, z4 e/ q" |) B/ ~0 f x8 i
18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and+ g# }( _( r) k9 K
R is the ratio of the formula weight of aluminium oxide to- R' P' A4 i9 g
that of elemental aluminium.
! z. o0 E8 r* X" Y% ~Sample Solution A
% F8 ^! k' s' nAccurately weigh 1 g of the sample and transfer to a 250-ml high-silica
& A8 i) ^0 F7 l/ d& Gglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
6 j; l7 N( h" q5 A# d8 |, r6 }(Note: Do not use more sodium bisulfate than specified, as an excess
* }. x0 \7 t! X- u6 U* T5 }concentration of salt will interfere with the EDTA titration later on in the- _& h d* J" I1 F: }: ]
procedure.) Begin heating the flask at low heat on a hot plate, and. s, ?! G4 h2 q' ^
then gradually raise the temperature until full heat is reached.
/ }, v& a3 ]; j4 D/ M( T& b' Z(Caution: perform this procedure in a well ventilated area. ) When- \& h) h" d3 S9 P/ \' r
spattering has stopped and light fumes of SO3 appear, heat in the full
6 \& S+ S/ s4 b1 mflame of a Meeker burner, with the flask tilted so that the fusion of the
( k6 _( q# \7 E% h% c2 m( z1 dsample and sodium bisulfate is concentrated at one end of the flask.
: D0 B/ i/ S" Q8 _) b: b2 N' QSwirl constantly until the melt is clear (except for silica content), but; c5 h9 ?6 y9 `7 {+ u, @; ?- \/ N
guard against prolonged heating to avoid precipitation of titanium6 R7 B5 @2 h6 I* q3 s8 o
dioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until
% t+ w" g8 c9 G; x4 n% _the mass has dissolved and a clear solution results. Cool, and dilute to
( m$ \& A+ D7 m7 W4 p. W120 ml with water. Introduce a magnetic stir bar into the flask., L! P8 J6 x- U% ^: _4 x
Sample Solution B, [" A- M; a. N, }. o3 s
Prepare 200 ml of an approximately 6.25 M solution of sodium. O& T* f: ]7 }, [
hydroxide. Add 65 ml of this solution to Sample Solution A, while J i2 _- h0 u- X f
stirring with the magnetic stirrer; pour the remaining 135 ml of the0 r. Y' h- i" g# J
alkali solution into a 500-ml volumetric flask.
3 W1 V9 I5 u' [Slowly, with constant stirring, add the sample mixture to the alkali+ o1 l3 {6 [( X- q
solution in the 500-ml volumetric flask; dilute to volume with water,
9 H1 W) ^+ G& O: d2 I5 Uand mix. (Note: If the procedure is delayed at this point for more than
! d8 `# g8 M4 i$ N2 hours, store the contents of the volumetric flask in a polyethylene T: b/ _ u/ x( i- r; v# G# k
bottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),; o, J/ A: ]) U# |
then filter the supernatant liquid through a very fine filter paper. Label4 ]6 J9 b7 u/ u$ E" w1 A0 g; S
the filtrate Sample Solution B.
4 W5 v& o8 P- d/ M, J/ {Sample Solution C- g2 s1 H e6 B
Transfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer
1 q6 E: c, ?1 D# }$ [; t& h% Gflask, add 1 drop of methyl orange TS, acidify with hydrochloric acid7 K$ T K9 ~' {5 F+ [
solution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.028 y7 g* L, K2 ^) t+ ^8 b
M disodium EDTA, and mix. [Note: If the approximate Al2O3 content is
. M2 V0 t7 N0 {, P: s$ W$ Wknown, calculate the optimum volume of EDTA solution to be added( b' ]- Q" [6 _
by the formula: (4 x % Al2O3) + 5.]* P t# x" y' G7 o
Add, dropwise, ammonia solution (1 in 5) until the colour is just
( v G% ?7 v4 e4 v$ A; fcompletely changed from red to orange-yellow. Then add10 ml each! U+ u2 W4 d, K1 Q0 I! K7 B; X
of Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to5 I" V8 H' y1 }" L2 R+ k
room temperature in a stream of running water, add 3 drops of xylenol
4 W$ H: ]% T1 Y4 qorange TS, and mix. If the solution is purple, yellow-brown, or pink,
" n/ n+ U. P- Z6 ubring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired' [$ v3 x' o* V0 w- F8 r. |+ T
pH, a pink colour indicates that not enough of the EDTA solution has+ s7 A8 r$ R' L* J/ n" u' a
been added, in which case, discard the solution and repeat this
' B* X7 C& j% K8 xprocedure with another 100 ml of Sample Solution B, using 50 ml,
! F% A w" U& v8 @( srather than 25 ml, of 0.02 M disodium EDTA.
$ O, u7 L5 M; K, @' G$ D! y# |) tProcedure
' B4 m, B, ]/ y3 A* m4 xUsing the standardized zinc sulfate solution as titrant, titrate Sample
, q+ U" z% ?( wSolution C to the first yellow-brown or pink end-point that persists for
4 j, i* I, e0 f6 O B5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first) x- i H9 C0 I: l& C
titration should require more than 8 ml of titrant, but for more accurate4 ]8 D z8 Z; G _/ _. D/ R7 z3 `
work a titration of 10-15 ml is desirable.! A! w: p j' i- T( E" ^2 ]
Add 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5
& ^$ x, ^+ ~5 M) L9 }* J9 Cmin, and cool in a stream of running water. Titrate this solution, using- F1 [* s, x. u/ T* G
the standardized zinc sulfate solution as titrant, to the same fugitive
7 O' S4 i1 D9 z' Zyellow-brown or pink end-point as described above.+ }9 N4 B+ o% m( O
Calculation:9 }1 B! o9 a7 `+ P, X, O0 k, H3 z
Calculate the percentage of aluminium oxide (Al2O3) in the sample8 N( B: T7 t6 P' g6 R& W5 E, I% L
taken by the formula:2 }# |8 B( I; Q+ S
% Al2O3 = 100 × (0.005VT)/S
0 m7 P: D2 T f2 c# gwhere8 ]$ v( M7 B. A( P" R( a
V is the number of ml of 0.01 N zinc sulfate consumed in1 L. E$ @) _, R$ H" R) l! V5 K! s
the second titration,
* U, o0 i, Y! t7 q1 Z0 yT is the titre of the zinc sulfate solution,* }* P( q) \/ D, D# {) R
S is the mass (g) of the sample taken, and
( |; |. Q, U7 K# |, D0.005 = 500 ml / (1000mg/g × 100 ml).0 V3 l+ V3 H9 h4 ^& M4 Q5 B! J
Silicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica
# b& [; Y% e# dglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O). P |" h! d1 R/ g9 C$ D4 T
Heat gently over a Meeker burner, while swirling the flask, until- a7 A7 K8 ?: R, w8 Q# n. N
decomposition and fusion are complete and the melt is clear, except
: l! w& B, `; D% Y& rfor the silica content, and then cool. (Caution: Do not overheat the
0 S9 V# I' `9 {contents of the flask at the beginning, and heat cautiously during0 }0 k+ Q- [, n! e" D3 y
fusion to avoid spattering.)
; I' F/ Q7 F* q6 }2 _8 ~To the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat
/ F9 J" ^: q3 Ycarefully and slowly until the melt is dissolved. Cool, and carefully add
% M0 `9 Y' U7 O# V& n150 ml of water by pouring very small portions down the sides of the" e; t1 {: R) i) Z, M9 E
flask, with frequent swirling to avoid over-heating and spattering. Allow
) K9 U. q t% Qthe contents of the flask to cool, and filter through fine ashless filter
/ K+ _/ \ \* F8 Bpaper, using a 60 degree gravity funnel. Rinse out all the silica from
% @. e6 P+ ~ |* ]# i5 D$ Bthe flask onto the filter paper with sulfuric acid solution (1 in 10).
# Y' K+ |$ n# e# \% QTransfer the filter paper and its contents into a platinum crucible, dry in
0 x4 }6 k/ [8 U7 w f7 \an oven at 1200, and heat the partly covered crucible over a Bunsen
2 W+ I& g: K2 Uburner. To prevent flaming of the filter paper, first heat the cover from
* f3 Y# I$ b! y; W- V4 qabove, and then the crucible from below.
+ v$ \; Q- e$ B4 C7 A- w! WWhen the filter paper is consumed, transfer the crucible to a muffle/ _( n( `/ n1 u2 a1 l. H
furnace and ignite at 1000o for 30 min. Cool in a desiccator, and
$ \% z6 t* Z! q, Z& a& Oweigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated) ~8 ^) f& i% R) g' y- W* g
hydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first
# Z" t7 m, [0 R8 X6 ?) s! [on a low-heat hot plate (to remove the HF) and then over a Bunsen
2 U/ R1 a2 `, f0 C& ?5 w b! Y2 g6 aburner (to remove the H2SO4). Take precautions to avoid spattering,
1 E! t! t6 E( u- c: {especially after removal of the HF. Ignite at 1000o for 10 min, cool in a6 ~6 I* ~; V& M+ m. ~6 T
desiccator, and weigh again. Record the difference between the two! i5 z: D+ g- q. e! V3 d
weights as the content of SiO2 in the sample.% M6 U# W6 F6 D+ F, ^7 o
METHOD OF ASSAY9 z0 L( |, D7 Q+ t; _7 t
Accurately weigh about 150 mg of the sample, previously dried at 105o/ B: m2 V! H0 g P7 U" m P
for 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water
2 h: h% {9 V3 |3 K0 T# Pand shake until a homogeneous, milky suspension is obtained. Add 30
* ]! t) D3 c9 b w T, r! uml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially
- x5 v) S% m* F- uheat gently, then heat strongly until a clear solution is obtained. Cool,
o4 I4 Q' f* U/ S* pthen cautiously dilute with 120 ml of water and 40 ml of hydrochloric
. o b; G5 f) Z/ Eacid, and stir. Add 3 g of aluminium metal, and immediately insert a+ V2 }9 [2 _: c/ c/ y2 I p
rubber stopper fitted with a U-shaped glass tube while immersing the; t7 S" {1 t$ E" r, r) ?* T
other end of the U-tube into a saturated solution of sodium2 F- ^ N6 R! V. J* a
bicarbonate contained in a 500-ml wide-mouth bottle, and generate% _9 R% L9 B9 C2 }
hydrogen. Allow to stand for a few minutes after the aluminium metal8 g1 C! h9 [& |
has dissolved completely to produce a transparent purple solution.
5 n' b6 H3 i3 R: DCool to below 50o in running water, and remove the rubber stopper8 ]7 m$ ?; m; S0 A8 h( z' Z
carrying the U-tube. Add 3 ml of a saturated potassium thiocyanate3 E1 J6 ~+ u, i% l; W4 J- S
solution as an indicator, and immediately titrate with 0.2 N ferric. R4 b1 X! }6 J0 N1 l8 S. ?
ammonium sulfate until a faint brown colour that persists for 302 Z& n- F& m: @* f& N
seconds is obtained. Perform a blank determination and make any
/ n& {8 j0 T y, r$ onecessary correction. Each ml of 0.2 N ferric ammonium sulfate is
' _- z9 @% k. ?+ e9 B! H/ Xequivalent to 7.990 mg of TiO2.- ?' q7 }- S1 T2 r! `1 w
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