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二氧化钛(钛白粉)
二氧化钛(钛白粉)
/ P) S) r7 n4 e7 U0 o
" o8 C( q& Q7 G5 r6 c6 v) i iJECFA关于二氧化钛(钛白粉)的结论1 I3 u: Q4 T; ~ V/ N, f
, ?5 }. @& W/ S% U4 V' o+ o
摘要: 2006年JECFA关于二氧化钛的结论8 h6 ^5 S0 `- F
ADI值:不作限制。
- R# q0 s9 k5 M8 Q功能:着色剂! D8 [; ]' k7 v- n7 P2 J
# x6 x/ E- [' ^+ t0 M0 ITITANIUM DIOXIDE
% ^/ A% M1 K. d/ c. RPrepared at the 67th JECFA (2006) and published in FAO JECFA* O% v q& X9 J5 i
Monographs 3 (2006), superseding specifications prepared at the 63rd
3 r5 J. P3 ?) p" a- s& ^2 iJECFA (2004) and published in FNP 52 Add 12 (2004) and in the
4 ~5 `7 l! U4 m; u0 @0 k7 jCombined Compendium of Food Additive Specifications, FAO JECFA6 {7 t K0 S1 i3 F$ r8 I
Monographs 1 (2005). An ADI “not limited” was established at the 13th
; a; J3 E* H) |JECFA (1969).
* N+ P6 e' ~. h- w* o' jSYNONYMS! W O6 d/ k; @1 ]# h+ J6 d1 u5 C
Titania, CI Pigment white 6, CI (1975) No. 77891, INS No. 1715 M' s& Q/ L& W b- |
DEFINITION
0 m) I6 r7 F; R' t: t; H) eTitanium dioxide is produced by either the sulfate or the chloride# P- r, `3 N$ m1 ` y
process. Processing conditions determine the form (anatase or rutile
7 b5 A6 q, n$ m$ R% |/ y$ Qstructure) of the final product.
. `3 c6 { Z; o3 l, U. ?3 BIn the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3); n7 b# o8 k% |( @( p7 C/ w- O% R' h1 C
or ilmenite and titanium slag. After a series of purification steps, the7 l* i9 F- h3 A: W
isolated titanium dioxide is finally washed with water, calcined, and
9 ? i5 |' j1 k% G' r( smicronized.
1 g/ E' n4 L9 X, M/ xIn the chloride process, chlorine gas is reacted with a titaniumcontaining
# x P! `9 V I$ o# O/ C% f: \mineral under reducing conditions to form anhydrous
. |. l, X( M) L( ~' X8 E5 Ntitanium tetrachloride, which is subsequently purified and converted to
5 C# I/ c e3 A1 Qtitanium dioxide either by direct thermal oxidation or by reaction with
) |. I: I5 V* A+ _6 n6 U- D) d; `steam in the vapour phase. Alternatively, concentrated hydrochloric. z$ B* f% C0 |# w& p% h; G
acid can be reacted with the titanium-containing mineral to form a
5 `; _0 {* z0 z3 d) M8 Z5 C2 M* ysolution of titanium tetrachloride, which is then further purified and
4 N6 E) o2 G- x% lconverted to titanium dioxide by hydrolysis. The titanium dioxide is5 g3 i, |* [0 u4 X
filtered, washed, and calcined.0 }$ c( f- }8 [, f: k1 c# F
Commercial titanium dioxide may be coated with small amounts of
' p9 R e$ P( {! f, H* Jalumina and/or silica to improve the technological properties of the
# u* x0 \+ q7 y5 ?+ }6 eproduct.
3 x' U5 |$ G o: SC.A.S. number 13463-67-7
- |, x7 L& i* w" KChemical formula TiO29 n( ^1 h8 [1 t3 y( ?/ |
Formula weight% y$ i5 c2 C1 _5 E, U
79.88, u. a8 J1 n5 W+ K' z# i1 t9 d7 `
Assay
. d; Y G7 \$ I& J* O$ @Not less than 99.0% on the dried basis (on an aluminium oxide and
! i/ i. r! K1 b5 q0 ?7 isilicon dioxide-free basis); `# b" g% W; e, l( C& B
DESCRIPTION3 r6 K- ?! @5 p; b9 j( Z v5 a+ x4 f
White to slightly coloured powder# M9 G) ^( C9 x5 j5 v
FUNCTIONAL USES0 U- e3 L0 @2 L
Colour; A6 ^$ l3 U2 p, j, [
CHARACTERISTICS
B7 s$ ]; N+ l$ N: ZIDENTIFICATION3 p/ |! X! N$ ~: [& t
Solubility (Vol. 4)
/ h2 i% M; n2 O+ L' kInsoluble in water, hydrochloric acid, dilute sulfuric acid, and organic
1 l' ?* D) {% X4 csolvents. Dissolves slowly in hydrofluoric acid and hot concentrated+ i5 ^2 y# F( m2 j! j' b
sulfuric acid." X1 i( D/ t3 Q! e/ R9 L: i8 x
Colour reaction5 k8 U& E! [) ^
Add 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of
1 z! C0 v2 W; _ n3 C$ h: psulfuric acid appear, then cool. Cautiously dilute to about 100 ml with
, z5 c# w2 {! Q$ [+ Z5 ]water and filter. To 5 ml of this clear filtrate, add a few drops of
4 M9 ?' ^1 |7 G* P, Xhydrogen peroxide; an orange-red colour appears immediately.
8 O1 B2 U2 \1 WPURITY
+ N U4 i6 |$ r) B8 m% tLoss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)5 z& t5 X6 v4 R; S% J( d7 ?
Loss on ignition (Vol. 4)
# V# u- k4 s9 u8 fNot more than 1.0% (800o) on the dried basis6 |9 w, p0 M7 Q1 ]5 w- ^ j
Aluminium oxide and/or# a( ~$ c" h. A
silicon dioxide6 `- i# P. z- e! {/ y
Not more than 2%, either singly or combined [& y0 h, { q& a4 [7 U
See descriptions under TESTS
6 S/ E3 B8 d0 YAcid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing
0 X& M2 Z ?2 U! ^* Oalumina or silica.: a& y$ t5 A% {; a9 g
Suspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and
4 f: r0 J! y$ v, Z& p4 gplace on a steam bath for 30 min with occasional stirring. Filter" L3 u, M5 R J4 P6 V! T
through a Gooch crucible fitted with a glass fibre filter paper. Wash0 ]! \8 I% G- F% s$ b9 Q" a$ k
with three 10-ml portions of 0.5 N hydrochloric acid, evaporate the
/ ~2 U0 x2 P! R4 y/ X: F) C: z Tcombined filtrate and washings to dryness, and ignite at a dull red
7 j9 N; F# l# {7 x' N: E5 y, lheat to constant weight.7 R6 ^/ O" a2 r! @: \, U5 g6 R2 d
Water-soluble matter2 `% O; f" |) e# k0 v) z
(Vol. 4)
% r/ F+ D, }% ?# q, d( v" j( yNot more than 0.5%
3 d, K, b& o4 b0 W, HProceed as directed under acid-soluble substances (above), using( D1 O) q t% A5 k7 j* f, d
water in place of 0.5 N hydrochloric acid.9 C) I+ S; h0 y4 c2 K3 |2 U
Impurities soluble in 0.5 N! B) N. [- e3 a* l
hydrochloric acid$ @6 `1 M. z+ E% V8 ^
Antimony Not more than 2 mg/kg
' H, \9 S9 I: N1 r6 qSee description under TESTS! B Z5 p7 N' q& J3 Q
Arsenic Not more than 1 mg/kg: W6 M/ r( Z- \; ]5 o
See description under TESTS6 i3 ]7 H$ c% P4 E4 h/ `
Cadmium Not more than 1 mg/kg
" i0 D2 r3 z" ?: I' c" k- `See description under TESTS
) i" g; z s0 b) E* WLead
* A/ K1 r: Z/ I1 d: j8 L4 bNot more than 10 mg/kg
/ D" ?+ d$ A- }" ~: PSee description under TESTS
) K+ ]# i- U2 b- W" gMercury (Vol. 4) Not more than 1 mg/kg. u6 H; n- H! _, m
Determine using the cold vapour atomic absorption technique. Select a
( `) l1 v0 r; c. j0 {sample size appropriate to the specified level
5 B. y5 Q( \0 u; m) l/ H, o9 u+ g9 KTESTS8 D4 v; n5 r/ B; q; l. ?
PURITY TESTS
# G& Y1 q! F* x+ i/ BImpurities soluble in 0.5 N- }; m. X& G8 w
hydrochloric acid
# K+ m, N- d+ Q. w/ YAntimony, arsenic,1 H) N+ _' }8 N e ^
cadmium and lead
6 R2 _9 r/ Q: [(Vol.4)
6 l, o8 R( P/ t* F: b( V3 i& mTransfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N
' h' y! Z* [5 ?6 [4 K S& Uhydrochloric acid, cover with a watch glass, and heat to boiling on a: B( ]4 a F' q
hot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml
( b' r# O+ b4 l0 M5 r- M3 ]centrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved7 x) O* I( v9 u7 Q
material settles. Decant the supernatant extract through a Whatman& K* M% S( g) N0 x, J- w7 W
No. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml
8 }) w+ @7 [% t& Jvolumetric flask and retaining as much as possible of the undissolved
* E: q7 p1 J" J2 Imaterial in the centrifuge bottle. Add 10 ml of hot water to the original
! L7 v. a% B9 d: T' @& s8 T. nbeaker, washing off the watch glass with the water, and pour the
" k7 n7 p3 ~9 Q2 ~- f$ S8 C( I+ Tcontents into the centrifuge bottle. Form a slurry, using a glass stirring
0 S5 O4 i" q- C* A0 l. g/ Z! urod, and centrifuge. Decant through the same filter paper, and collect6 W$ I# l7 R* L* `- @8 j
the washings in the volumetric flask containing the initial extract.* P" M* f: F- d1 y0 b! C
Repeat the entire washing process two more times. Finally, wash the6 u0 K2 j# `2 q+ Z3 E! c. `" F T! C- a
filter paper with 10 to 15 ml of hot water. Cool the contents of the flask9 b2 M. Z+ }: t1 E( N
to room temperature, dilute to volume with water, and mix.) f+ E/ x; g7 m; s8 i, ?
Determine antimony, cadmium, and lead using an AAS/ICP-AES
' z) z4 ?( { l+ A$ r) Y' r, }: ]technique appropriate to the specified level. Determine arsenic using the7 p! F, ]/ g7 ?
ICP-AES/AAS-hydride technique. Alternatively, determine arsenic using
' e! q0 `8 P% ^; J% M2 kMethod II of the Arsenic Limit Test, taking 3 g of the sample rather than+ t6 m. w; F0 o+ P; G
1 g. The selection of sample size and method of sample preparation
1 |5 P* U! O v2 @6 p! Tmay be based on the principles of the methods described in Volume 4.$ |' b; R- \- _3 V$ h
Aluminium oxide Reagents and sample solutions
v/ u, o3 C2 s: R" i! D0.01 N Zinc Sulfate$ p: D7 n5 v) C
Dissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to7 T! y; N, c6 s9 n; |6 m; _
make 1000 ml. Standardize the solution as follows: Dissolve 500 mg
2 ~ {2 N" _. a/ T; |of high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of# o* j' a& Z# }7 k! ]/ _
concentrated hydrochloric acid, heating gently to effect solution, then
$ f$ j) u4 j# s+ r+ x, n# ntransfer the solution into a 1000-ml volumetric flask, dilute to volume7 Z$ c+ q' Y) q$ a0 Z
with water, and mix. Transfer a 10 ml aliquot of this solution into a 5008 I3 X$ p* s; N. C
ml Erlenmeyer flask containing 90 ml of water and 3 ml of% w$ J p. }4 f8 ]: v4 @+ g
concentrated hydrochloric acid, add 1 drop of methyl orange TS and9 I6 [+ k7 T1 R7 a; u
25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,& b- M8 X2 ^4 v2 G; c; X6 Z
dropwise, ammonia solution (1 in 5) until the colour is just completely
. d: i4 ]4 ]. l1 U# E" Ichanged from red to orange-yellow. Then, add:8 C/ A v( X; \, `7 k
(a): 10 ml of ammonium acetate buffer solution (77 g of( X2 y+ _/ F. H' s& R4 X! @" L9 ?1 j
ammonium acetate plus 10 ml of glacial acetic acid, dilute to& k6 W6 I7 U/ ]. k
1000 ml with water) and
& u" Y. `# x( e/ R# |8 P1 n& _(b): 10 ml of diammonium hydrogen phosphate solution (150 g# E, T( |# l* e8 ^ u+ \7 M8 G
of diammonium hydrogen phosphate in 700 ml of water,7 _9 j- n& M* U7 @" b. O4 S
adjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,
9 |. a# V4 A rthen dilute to 1000 ml with water).
1 e e$ D" x5 K$ u& L; ZBoil the solution for 5 min, cool it quickly to room temperature in a
, y* n. s% I4 ~9 E' I" ystream of running water, add 3 drops of xylenol orange TS, and mix.5 d$ z: S; V( G) v. Z
Using the zinc sulfate solution as titrant, titrate the solution to the first
* h/ I/ x& N/ L# r$ ]yellow-brown or pink end-point colour that persists for 5-10 sec. (Note:/ g' ~- H0 j2 [% M; Q5 P. K
This titration should be performed quickly near the end-point by; `: N& n5 l4 G6 B! V- p
adding rapidly 0.2 ml increments of the titrant until the first colour7 b+ O& a, y9 q/ m9 U2 G# o
change occurs; although the colour will fade in 5-10 sec, it is the true; B z8 K* F. m6 X* }* |1 W( N, d
end-point. Failure to observe the first colour change will result in an
2 C" o, Z( p! T- q1 Hincorrect titration. The fading end-point does not occur at the second' B" B5 e5 B9 l9 p% G0 B
end-point.)
$ B- n: _; u- h- N2 h% s% WAdd 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a& Z1 @+ l4 B' W0 y! W( x
stream of running water. Titrate this solution, using the zinc sulfate) e$ M+ F ~: }- d- b
solution as titrant, to the same fugitive yellow-brown or pink end-point4 b& u$ X5 G9 T; z" z$ e5 ~' J
as described above.
( y) C6 `9 z$ t: qCalculate the titre T of zinc sulfate solution by the formula:
8 J/ {+ o B+ jT = 18.896 W / V! |4 h- c5 e- R
where0 K/ O/ [! y5 |3 i& y; j
T is the mass (mg) of Al2O3 per ml of zinc sulfate solution
( J& ]% W( |; rW is the mass (g) of aluminium wire1 D8 i) x! g1 I7 ~" J0 H
V is the ml of the zinc sulfate solution consumed in the# U8 X$ y- J1 m! N& h5 U+ B4 X
second titration+ l3 H. m* x3 T' p5 \6 s
18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and
/ g) j9 n& o/ K% G0 z9 {; jR is the ratio of the formula weight of aluminium oxide to
5 N. P/ c H* O& c5 c9 Jthat of elemental aluminium.
6 C" w" p- k( @" p6 u$ c$ C" [Sample Solution A
4 O z! w" o/ EAccurately weigh 1 g of the sample and transfer to a 250-ml high-silica
1 M$ z. {# _3 \+ \' Nglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).5 r; K3 U5 j0 x$ \3 r
(Note: Do not use more sodium bisulfate than specified, as an excess! C, H6 P$ x7 Z7 q
concentration of salt will interfere with the EDTA titration later on in the _) [+ `" L) {
procedure.) Begin heating the flask at low heat on a hot plate, and2 a) o0 U; f2 Z( v L! n! B/ v
then gradually raise the temperature until full heat is reached.6 D- K3 Q# a7 [' {
(Caution: perform this procedure in a well ventilated area. ) When. W |0 J# H& C$ ^( y1 l
spattering has stopped and light fumes of SO3 appear, heat in the full
9 u, c' e& ~5 \& Y* @flame of a Meeker burner, with the flask tilted so that the fusion of the! [1 @/ `" t! s, R
sample and sodium bisulfate is concentrated at one end of the flask.
1 }" \% g; k/ k* K' `, WSwirl constantly until the melt is clear (except for silica content), but" B/ Y9 R" z, r0 L
guard against prolonged heating to avoid precipitation of titanium4 }5 O* ^) s7 Q& U' \
dioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until
0 u- r' C+ }/ X9 ]the mass has dissolved and a clear solution results. Cool, and dilute to
. h4 P% W' C1 z; u0 ~+ c# i/ u120 ml with water. Introduce a magnetic stir bar into the flask.+ ^# [& p8 a' \ E+ k* Q
Sample Solution B
2 h7 h6 q# T x' L& D6 c/ q) ]; \' a' DPrepare 200 ml of an approximately 6.25 M solution of sodium3 Y' {/ {( s7 S8 s: J
hydroxide. Add 65 ml of this solution to Sample Solution A, while5 H+ A/ l' @4 C: A! S
stirring with the magnetic stirrer; pour the remaining 135 ml of the$ f& ~+ i6 n& M/ P! d" |( h( t# \
alkali solution into a 500-ml volumetric flask.9 ]+ d9 R9 [1 h$ ]2 q# }6 K# ^, E
Slowly, with constant stirring, add the sample mixture to the alkali
4 x. L8 u& B+ j. t9 dsolution in the 500-ml volumetric flask; dilute to volume with water,; s' K" G+ p" {- d: t' }* }! l9 O
and mix. (Note: If the procedure is delayed at this point for more than
. Y; K n' `- Y$ [" B2 hours, store the contents of the volumetric flask in a polyethylene
7 ^! ~: r7 B! z ]bottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),6 o$ l) Q5 `1 y3 y3 w# ]
then filter the supernatant liquid through a very fine filter paper. Label. Y& W3 u6 ]8 @9 d( y# r( G1 R
the filtrate Sample Solution B.
0 \" c# b) B; |8 P4 z( q# VSample Solution C6 s; h8 H: e& Z( i3 Z5 P: x' V
Transfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer
' _2 _ \" X( O0 Q2 Gflask, add 1 drop of methyl orange TS, acidify with hydrochloric acid6 n, t- x" m# ?8 L, R" c, A
solution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02
. g$ g, V7 D$ s6 E/ B( qM disodium EDTA, and mix. [Note: If the approximate Al2O3 content is; T& L: @9 A7 t
known, calculate the optimum volume of EDTA solution to be added$ J1 j5 D* O3 r
by the formula: (4 x % Al2O3) + 5.]
1 c$ Q2 c w% R+ u: g6 ~ ~' ZAdd, dropwise, ammonia solution (1 in 5) until the colour is just J* G& i8 I3 Y& C0 c
completely changed from red to orange-yellow. Then add10 ml each' z) x3 o3 G/ @" o0 y
of Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to+ X0 U) x( P7 N" {4 z4 c9 c
room temperature in a stream of running water, add 3 drops of xylenol4 U, M( g U) J4 `5 L
orange TS, and mix. If the solution is purple, yellow-brown, or pink,! P# ~7 A7 j% j
bring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired8 B8 ~( n+ O; ~
pH, a pink colour indicates that not enough of the EDTA solution has
& Y* Z3 `% q; u1 C- O- V( Ibeen added, in which case, discard the solution and repeat this
9 {1 ^7 i- m% [- [3 S; Oprocedure with another 100 ml of Sample Solution B, using 50 ml,2 ^( [0 @' a' i/ @) S$ |! H, B
rather than 25 ml, of 0.02 M disodium EDTA.2 A8 V4 Q8 y0 c0 q% O9 J
Procedure; Y8 \) i& Q8 Q
Using the standardized zinc sulfate solution as titrant, titrate Sample
4 P. g& ]( [ L& ~- N! K/ zSolution C to the first yellow-brown or pink end-point that persists for
' q9 F4 ~# J3 U5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first
4 i% O9 m6 y+ {% ntitration should require more than 8 ml of titrant, but for more accurate" M9 B, h4 J! r/ K* `
work a titration of 10-15 ml is desirable.& u6 c; d7 Z, s5 K d
Add 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5- A- y( r N l7 ]: ~0 o8 [2 T
min, and cool in a stream of running water. Titrate this solution, using
0 }/ D, ?, ^+ P4 A3 ~the standardized zinc sulfate solution as titrant, to the same fugitive
0 I* W5 p( T7 c& K8 Nyellow-brown or pink end-point as described above.
, i$ v( d# D9 J6 ~$ P. TCalculation:5 d0 h- e" ~/ l: ^4 t6 W
Calculate the percentage of aluminium oxide (Al2O3) in the sample4 J# M/ Z; ^6 F
taken by the formula:
" O' Y& d* }1 e% Al2O3 = 100 × (0.005VT)/S1 A) {: B( |- X
where7 z" F- y9 \$ k1 G2 [6 |
V is the number of ml of 0.01 N zinc sulfate consumed in& G" k) b4 P* Z$ n" ~4 _
the second titration,
. e- p9 }* t! Z" q7 uT is the titre of the zinc sulfate solution,
! ^! f' |& d2 K$ wS is the mass (g) of the sample taken, and
$ ]2 c3 U; S5 N3 _8 o* a, v* V" g' c2 x0.005 = 500 ml / (1000mg/g × 100 ml).
" K$ ^( K* [8 f/ x: p# q8 d* ]Silicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica) j( P" [, ~: L/ f( G
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
2 j- p- \% h' U* v/ E1 {Heat gently over a Meeker burner, while swirling the flask, until
& m6 B/ _; q: Z( x" N, mdecomposition and fusion are complete and the melt is clear, except4 x1 _5 ?8 c/ q1 L1 t; d
for the silica content, and then cool. (Caution: Do not overheat the
8 J9 t2 H4 X) r3 i# Y& ~+ b3 a. e$ Scontents of the flask at the beginning, and heat cautiously during* ?$ r( U; W6 L" S' A" x5 w
fusion to avoid spattering.)
( Z/ R; @# K0 s6 m0 Q8 LTo the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat
: e$ h. o% w( [carefully and slowly until the melt is dissolved. Cool, and carefully add
" b {- h6 Z! l! F" I( v" K9 @: |' T# n150 ml of water by pouring very small portions down the sides of the
4 u7 o+ b$ D7 @* Uflask, with frequent swirling to avoid over-heating and spattering. Allow
# Z! K: S( p" p' bthe contents of the flask to cool, and filter through fine ashless filter% J, H$ S7 l5 m2 P. r8 W! K
paper, using a 60 degree gravity funnel. Rinse out all the silica from
/ A, v! Q9 z5 I. G0 ^, I* ]+ ithe flask onto the filter paper with sulfuric acid solution (1 in 10).
. o W# E( ?' a+ A" l' wTransfer the filter paper and its contents into a platinum crucible, dry in" L( c# R4 ?5 o$ n$ \# `
an oven at 1200, and heat the partly covered crucible over a Bunsen& S" l: p2 E: I: L8 s) T- H
burner. To prevent flaming of the filter paper, first heat the cover from
0 L& r+ T; r/ Tabove, and then the crucible from below./ ?; m4 f6 U3 g9 G6 l, l( {) A4 U
When the filter paper is consumed, transfer the crucible to a muffle9 V, Q! |/ _- b" ?9 G' g
furnace and ignite at 1000o for 30 min. Cool in a desiccator, and
% }0 a' i9 A' ]2 Z9 d! Nweigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated& F4 ?- _+ X7 A% f! Q$ f
hydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first
1 z; A7 s8 d1 ^3 gon a low-heat hot plate (to remove the HF) and then over a Bunsen
/ k9 t8 H( V n! E- D# Pburner (to remove the H2SO4). Take precautions to avoid spattering,
3 [$ Y! |1 ?" c2 y9 u+ tespecially after removal of the HF. Ignite at 1000o for 10 min, cool in a5 g# E+ H( l" q6 y
desiccator, and weigh again. Record the difference between the two( n' J. a* n J5 O0 @, t. d& l
weights as the content of SiO2 in the sample.
c2 ~0 q! a/ s+ U6 JMETHOD OF ASSAY) w, d$ @& z$ d" Z' k' O- H& X
Accurately weigh about 150 mg of the sample, previously dried at 105o3 {# d5 C/ ~" U9 i# v0 f
for 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water+ c+ B+ b f4 ]
and shake until a homogeneous, milky suspension is obtained. Add 30' W% w0 W: u) t, p2 @4 `: j+ `4 d
ml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially) c+ x( s5 S3 g
heat gently, then heat strongly until a clear solution is obtained. Cool,
) A# N/ [+ N) Z/ j1 y% ]then cautiously dilute with 120 ml of water and 40 ml of hydrochloric9 o: @. j- [0 H% [7 h
acid, and stir. Add 3 g of aluminium metal, and immediately insert a
$ a* X6 k1 Y+ ^: N7 n' Lrubber stopper fitted with a U-shaped glass tube while immersing the! m! w" ]! d) {7 R% v1 x2 o
other end of the U-tube into a saturated solution of sodium9 V$ A) j. D' U% I. ?
bicarbonate contained in a 500-ml wide-mouth bottle, and generate, F3 K; V+ M3 D
hydrogen. Allow to stand for a few minutes after the aluminium metal
% g: j. Y3 O! ^3 u4 zhas dissolved completely to produce a transparent purple solution.
9 j8 p2 B1 r$ r. N4 R0 X, vCool to below 50o in running water, and remove the rubber stopper
" r+ u% ~% Z/ `- c Acarrying the U-tube. Add 3 ml of a saturated potassium thiocyanate9 E& m( Y: B' l7 y N/ f1 H
solution as an indicator, and immediately titrate with 0.2 N ferric0 _7 H7 w* E7 \$ h. O
ammonium sulfate until a faint brown colour that persists for 30
" N( \7 Q. S$ ^- mseconds is obtained. Perform a blank determination and make any- X* g8 V7 h2 C: F: V: u
necessary correction. Each ml of 0.2 N ferric ammonium sulfate is0 [9 T, l7 O. @+ J8 C9 v- P' n
equivalent to 7.990 mg of TiO2.
1 G; Q; m) Y' c: n% H j |
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