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二氧化钛(钛白粉)
二氧化钛(钛白粉)0 r1 H" k( } n( K1 b7 T- R
0 ~! ?+ m7 x( `; p6 ]
JECFA关于二氧化钛(钛白粉)的结论
3 m4 \1 _. S' t9 N5 W5 p, L5 o/ Y6 n6 F: G: O0 u1 Y
摘要: 2006年JECFA关于二氧化钛的结论2 u7 Q0 z% ^; U8 H/ p
ADI值:不作限制。6 `* y8 l! r: q- Q( {
功能:着色剂& w {& l- G# P' u/ }: s
5 t+ v( s- L. g" iTITANIUM DIOXIDE
+ H* v$ l; g( E& EPrepared at the 67th JECFA (2006) and published in FAO JECFA5 q% x; L& j# `- Q; C1 j* x5 T" E2 @
Monographs 3 (2006), superseding specifications prepared at the 63rd; [( G2 h- Y4 L; m
JECFA (2004) and published in FNP 52 Add 12 (2004) and in the
0 c' w" t4 s3 z7 T' J! u- cCombined Compendium of Food Additive Specifications, FAO JECFA
! n: }- M+ q0 N5 [Monographs 1 (2005). An ADI “not limited” was established at the 13th
8 s7 s; g5 N5 I ]" @, AJECFA (1969).; _6 v( m1 K+ e. Y' i( A, O' ~2 C
SYNONYMS
3 ?3 R* g. [, T+ Q, I7 [Titania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171
6 o d% a3 [3 y& b9 EDEFINITION& H; N- d* B" O
Titanium dioxide is produced by either the sulfate or the chloride8 ~3 s1 k5 V( o* ^& D3 Y9 v
process. Processing conditions determine the form (anatase or rutile& W$ y$ @; ~6 I
structure) of the final product.
/ _( g0 Z3 [% ^4 _$ o" [In the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)
5 p6 J$ o1 t1 l4 {2 h& Bor ilmenite and titanium slag. After a series of purification steps, the' j$ u" @' v7 a. e) b9 s+ H
isolated titanium dioxide is finally washed with water, calcined, and
. i/ B: Z* `) y/ |% e1 E/ V' |micronized.* W* z2 g( Y% v7 ^3 j( G
In the chloride process, chlorine gas is reacted with a titaniumcontaining
& Y; E0 O; z- Z/ ?8 I0 tmineral under reducing conditions to form anhydrous
, M# T2 y3 I. X* H6 Stitanium tetrachloride, which is subsequently purified and converted to
0 R1 a9 U- W' [/ }' Ctitanium dioxide either by direct thermal oxidation or by reaction with
; W P) {( b/ K0 h" l X1 u3 Nsteam in the vapour phase. Alternatively, concentrated hydrochloric
* y4 e" O7 U8 X3 g# T# Aacid can be reacted with the titanium-containing mineral to form a
, a a! _0 ^2 J/ Tsolution of titanium tetrachloride, which is then further purified and! G5 f4 z9 K" W; m/ a# [
converted to titanium dioxide by hydrolysis. The titanium dioxide is
( G9 e; ]0 K5 {4 }filtered, washed, and calcined.
. j. u8 A4 g. K3 ^1 KCommercial titanium dioxide may be coated with small amounts of
! R) n6 ]6 V) A8 d7 w1 ialumina and/or silica to improve the technological properties of the( S; y- |1 I$ j6 V2 {$ Z" |6 ]
product.+ r- n: `: m8 ^' r1 d
C.A.S. number 13463-67-7# q9 n0 P& I0 M! v5 V) }) N. I7 P; E
Chemical formula TiO2
& i2 p* `) Z) a+ K+ X3 y- e RFormula weight: V2 w: z3 ^6 ?3 G
79.88; D* d; T4 q; d5 q, }6 m
Assay3 q$ o. A% D8 U
Not less than 99.0% on the dried basis (on an aluminium oxide and* `5 {6 J) v$ W0 K8 w
silicon dioxide-free basis): W+ c r! i! K- w- x6 F
DESCRIPTION
2 W6 z0 f5 D, W3 h' rWhite to slightly coloured powder
+ Q: V* n1 m6 g3 e. X; m# mFUNCTIONAL USES' C$ {: t+ Z" H
Colour% V# l# x7 i* R' h- s9 l
CHARACTERISTICS1 O! j& q& Z' A: z
IDENTIFICATION3 o1 @5 v7 x8 z, i' N
Solubility (Vol. 4)) [& s5 l" J/ B: V
Insoluble in water, hydrochloric acid, dilute sulfuric acid, and organic
) D9 h$ z4 G$ y7 J) Rsolvents. Dissolves slowly in hydrofluoric acid and hot concentrated
3 {3 ]! V5 y4 P' m) |* msulfuric acid.
! K' q7 u+ e6 u# D( x6 vColour reaction
# t" V/ g& P |6 }, b X5 sAdd 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of
# ~# k% ?6 C+ C) G- ~9 Q9 t: Usulfuric acid appear, then cool. Cautiously dilute to about 100 ml with
- L& `, t3 L' s/ ]9 b# c' xwater and filter. To 5 ml of this clear filtrate, add a few drops of
6 }7 S! k( D! q: ^hydrogen peroxide; an orange-red colour appears immediately." u+ ` L& R& P; T6 g3 E
PURITY; |. X- k" D( @% M! ]1 Q, j
Loss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)4 p; n# E3 k7 ]/ R7 y
Loss on ignition (Vol. 4)9 b: Q/ M+ c1 A4 f; N; d2 R' Q
Not more than 1.0% (800o) on the dried basis; {3 [+ ~" U9 X& _" R, v
Aluminium oxide and/or* {) E# T9 Q/ j/ k; A+ B
silicon dioxide
- a! o3 |: G3 L* E5 {$ BNot more than 2%, either singly or combined! O: K" J% ^1 z: K* Q
See descriptions under TESTS' d/ N; L% v* v# x8 c2 v
Acid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing' T# d, m+ h* Y- a1 ]& S/ M
alumina or silica.
3 |/ J9 A/ o. c# `3 [8 B# x3 D" v; k5 bSuspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and
) G) v3 _7 U( m- |2 Lplace on a steam bath for 30 min with occasional stirring. Filter
5 j, ^+ @8 @4 x; ~through a Gooch crucible fitted with a glass fibre filter paper. Wash
$ ]) \2 ~+ C! x) u) Q2 i* u$ Qwith three 10-ml portions of 0.5 N hydrochloric acid, evaporate the
1 l3 S1 ?; B6 S7 D# V9 Ucombined filtrate and washings to dryness, and ignite at a dull red9 F0 D- {# i6 b0 ^% R! D: `
heat to constant weight.
/ j8 a Y# v9 w/ uWater-soluble matter
3 g( J1 j' h% C# R6 U& G5 q; D0 W(Vol. 4). J# _/ ]9 K7 t( x
Not more than 0.5%( K% J1 n7 {1 e# S/ ]) x! r
Proceed as directed under acid-soluble substances (above), using8 x$ ]9 |4 ^" R1 P# T& H) C
water in place of 0.5 N hydrochloric acid.! a z( Y- O) _( ^/ |- r6 c
Impurities soluble in 0.5 N0 s& D/ T$ u |" O
hydrochloric acid; b/ W0 K- o# b8 \! S
Antimony Not more than 2 mg/kg
$ |* ^: o" x0 v7 @6 H9 m* A/ e/ M& q5 dSee description under TESTS
" w$ f' \. _+ fArsenic Not more than 1 mg/kg
1 Q |' Y) S+ U) uSee description under TESTS
7 _- j" H2 k4 @, LCadmium Not more than 1 mg/kg- \; ]7 y t. F% q
See description under TESTS/ N& w6 l) }" {$ C( u! R
Lead
' f5 H8 m8 w0 D( t6 u! fNot more than 10 mg/kg
% R3 Y0 ^7 S/ a8 ^. A5 S8 MSee description under TESTS
8 V8 X1 D% b8 j6 E6 NMercury (Vol. 4) Not more than 1 mg/kg
2 g! i- }' }3 w7 ]7 `Determine using the cold vapour atomic absorption technique. Select a# i' O# ]. n# |
sample size appropriate to the specified level
* H) o- e" J$ e$ [6 i$ K7 STESTS
9 K" `8 v' ~6 h; y9 B: PPURITY TESTS
" x! L1 m) p) w& o+ H8 pImpurities soluble in 0.5 N
: |) V8 Q# p5 P( ]hydrochloric acid `3 w$ ?+ M" F+ b8 m3 q2 z2 D
Antimony, arsenic,
2 ]' k* B) {7 q! p7 Vcadmium and lead( L8 p/ F$ g5 t0 V
(Vol.4)' x9 b7 P% m( B
Transfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N$ x# g8 u4 P4 P, f6 m' S s
hydrochloric acid, cover with a watch glass, and heat to boiling on a2 R9 L' l. h: ?$ t
hot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml7 _( a7 P) B( R) s- V
centrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved- \6 X5 {" S1 u# |9 D% R& @3 p
material settles. Decant the supernatant extract through a Whatman
) Y- ?: F7 j6 X# w0 f. i7 PNo. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml# y, t! i& t& O# p
volumetric flask and retaining as much as possible of the undissolved) F; r9 R8 ~/ ]5 W
material in the centrifuge bottle. Add 10 ml of hot water to the original( j z; m) w% u
beaker, washing off the watch glass with the water, and pour the
+ t' g: g5 ?+ Q; J8 `# f* a& |9 { icontents into the centrifuge bottle. Form a slurry, using a glass stirring Z4 N6 H% ?; A: |3 {* `2 j
rod, and centrifuge. Decant through the same filter paper, and collect6 y3 {7 `5 C# [& e. D
the washings in the volumetric flask containing the initial extract.: F+ i7 d9 W/ n& H
Repeat the entire washing process two more times. Finally, wash the: v# N: h" t' l0 m* D) `% R3 H. n* ]
filter paper with 10 to 15 ml of hot water. Cool the contents of the flask
# v5 `3 X; d) ^; }; M I' n, bto room temperature, dilute to volume with water, and mix.
8 f/ ?: m0 ^* ~7 q9 u. rDetermine antimony, cadmium, and lead using an AAS/ICP-AES; {9 h {* X4 V6 `
technique appropriate to the specified level. Determine arsenic using the6 @$ S+ o2 X5 [2 b! n
ICP-AES/AAS-hydride technique. Alternatively, determine arsenic using6 e( V. [3 d$ A2 ^; i! W
Method II of the Arsenic Limit Test, taking 3 g of the sample rather than! P8 i1 Q7 |! g3 v/ j
1 g. The selection of sample size and method of sample preparation
' n: L; D! S( @/ h$ {: `may be based on the principles of the methods described in Volume 4.) D8 A6 A0 ?" N' u( M
Aluminium oxide Reagents and sample solutions) M- J" a* v3 m0 U( C9 n% p
0.01 N Zinc Sulfate
8 }1 ?& `9 x0 C1 _) a4 ^% eDissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to1 F/ c1 M4 K8 A4 P
make 1000 ml. Standardize the solution as follows: Dissolve 500 mg$ i5 ~& z" H6 x1 t
of high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of. z; b3 X# v7 y/ u% _5 t7 l
concentrated hydrochloric acid, heating gently to effect solution, then0 h) k2 r/ |- T, R
transfer the solution into a 1000-ml volumetric flask, dilute to volume
* B" G5 H9 ~/ d" ?( [. I0 Lwith water, and mix. Transfer a 10 ml aliquot of this solution into a 500
' r: J3 \2 h: R# p, [ml Erlenmeyer flask containing 90 ml of water and 3 ml of+ R0 M3 ?& T0 V1 Z
concentrated hydrochloric acid, add 1 drop of methyl orange TS and
# R f4 k7 S0 e+ ^) ~7 e25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,
. r+ n9 s0 M l2 Q. `' xdropwise, ammonia solution (1 in 5) until the colour is just completely
& v/ w8 ?0 a' E9 S9 h0 A8 T! rchanged from red to orange-yellow. Then, add:0 }( C! j1 U! q9 h H
(a): 10 ml of ammonium acetate buffer solution (77 g of! q; G, B5 k1 l' I
ammonium acetate plus 10 ml of glacial acetic acid, dilute to
$ q5 i- i' Y0 m, }" \6 Y6 e1000 ml with water) and( ~* q) W0 n( u% [( l+ f
(b): 10 ml of diammonium hydrogen phosphate solution (150 g
$ L! C6 d0 z3 E4 \of diammonium hydrogen phosphate in 700 ml of water,1 S a+ z' y$ j C
adjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,8 g6 I. s# h* O# Q
then dilute to 1000 ml with water).9 }/ Q$ ~0 f/ o4 _* {
Boil the solution for 5 min, cool it quickly to room temperature in a
, E5 I3 l1 P& a9 zstream of running water, add 3 drops of xylenol orange TS, and mix.
. `" f7 H. v' b/ \Using the zinc sulfate solution as titrant, titrate the solution to the first
6 } M0 |$ t) u ^yellow-brown or pink end-point colour that persists for 5-10 sec. (Note:
, ?4 ?2 p) O) ~1 d2 ?5 pThis titration should be performed quickly near the end-point by6 w3 ]( z2 G! j! U& K, i
adding rapidly 0.2 ml increments of the titrant until the first colour
' S* l' u9 X5 P2 c* ]& s) ychange occurs; although the colour will fade in 5-10 sec, it is the true
- Z9 W+ W/ r+ f, X6 oend-point. Failure to observe the first colour change will result in an6 S, | P6 g( i. H* D0 I& R f- E
incorrect titration. The fading end-point does not occur at the second
# Z5 q6 Q( I6 B4 U Cend-point.)8 E# J5 z. u5 x; h# n
Add 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a
w2 j* G/ d) T' q1 l& qstream of running water. Titrate this solution, using the zinc sulfate; y1 k" v5 u4 k4 B3 C
solution as titrant, to the same fugitive yellow-brown or pink end-point
# X. N* k+ j5 O# u1 P% ]as described above.
1 f: x- X% u' U2 gCalculate the titre T of zinc sulfate solution by the formula:+ `. }6 E0 O3 A
T = 18.896 W / V# p' x' [4 A9 S$ Q/ K
where7 w% R# z* W. x5 q
T is the mass (mg) of Al2O3 per ml of zinc sulfate solution
7 v j Z. R2 y# g) GW is the mass (g) of aluminium wire
4 J8 j7 x! |7 a, b6 ^* EV is the ml of the zinc sulfate solution consumed in the* y% Q- V7 l+ i+ Z) f) Q7 t# y
second titration
* S, \1 N1 Q) D18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and& n6 x% a! L$ p7 k' K# u
R is the ratio of the formula weight of aluminium oxide to
c+ y: q8 R/ D: F9 Ythat of elemental aluminium.* [8 o! D5 ?$ G8 q' v4 w/ Z& r: H
Sample Solution A
8 M, r' z* ^1 }5 y$ [9 B: [/ YAccurately weigh 1 g of the sample and transfer to a 250-ml high-silica
3 w t- G! @7 I# P" nglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).' W4 R. e2 T, _1 d* |" f- e
(Note: Do not use more sodium bisulfate than specified, as an excess) n3 U$ W; B& b
concentration of salt will interfere with the EDTA titration later on in the1 ?! E1 @) ]6 {% N
procedure.) Begin heating the flask at low heat on a hot plate, and
6 ^$ x/ s v# g6 U' othen gradually raise the temperature until full heat is reached.# {' P6 F: b! v( I2 G
(Caution: perform this procedure in a well ventilated area. ) When
) W. Z2 B" p3 z7 A( x5 Vspattering has stopped and light fumes of SO3 appear, heat in the full
/ K* o# C* J4 w9 i" r* k! zflame of a Meeker burner, with the flask tilted so that the fusion of the
: }# o# b. S( Y- H: x9 Usample and sodium bisulfate is concentrated at one end of the flask.
$ @6 X( j5 f- ?2 CSwirl constantly until the melt is clear (except for silica content), but
) G" A. U1 B3 ]7 \6 F) a5 dguard against prolonged heating to avoid precipitation of titanium
4 w u3 v# `) f3 s5 h- j# Gdioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until
3 b. ]) b- ?. O+ U: D1 qthe mass has dissolved and a clear solution results. Cool, and dilute to, Q) |! P% k5 }( x5 S0 X+ }& l
120 ml with water. Introduce a magnetic stir bar into the flask.! O$ h+ f- G3 u; a
Sample Solution B
: z9 I( g6 h- G) _Prepare 200 ml of an approximately 6.25 M solution of sodium( i# J& i) F6 Q
hydroxide. Add 65 ml of this solution to Sample Solution A, while
: v" o" l" ], ^7 o2 I: t1 bstirring with the magnetic stirrer; pour the remaining 135 ml of the
1 L) K. g0 f6 t6 s0 T# I' @alkali solution into a 500-ml volumetric flask.! {1 _- u+ F" z6 K" G
Slowly, with constant stirring, add the sample mixture to the alkali
1 q7 @+ N! o- U3 Y" Isolution in the 500-ml volumetric flask; dilute to volume with water,5 x5 Q5 P" O8 y
and mix. (Note: If the procedure is delayed at this point for more than, | v# s7 B$ W# b2 z/ i0 a3 j
2 hours, store the contents of the volumetric flask in a polyethylene
, k+ D# a3 a% @2 f5 l3 Hbottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),
# u+ `# z9 z9 ~! V( `2 J- cthen filter the supernatant liquid through a very fine filter paper. Label W+ ~3 j2 M/ N- A; D
the filtrate Sample Solution B.
, z2 Z8 _: ]; `# ]6 m6 o) c) s; T0 DSample Solution C* W2 Y1 @$ W( V( B% [, w3 X7 R
Transfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer/ I, Y! {, p ]% w
flask, add 1 drop of methyl orange TS, acidify with hydrochloric acid
) w2 _, p$ c% H [7 rsolution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02
4 f) _, l6 S+ C- YM disodium EDTA, and mix. [Note: If the approximate Al2O3 content is
0 z( w# U: M& d6 f' X. b5 pknown, calculate the optimum volume of EDTA solution to be added3 ]# {7 @& o8 p/ H1 W2 h7 y. p; h
by the formula: (4 x % Al2O3) + 5.]
- F% `6 q9 B. ~* b1 Z# R8 ?$ tAdd, dropwise, ammonia solution (1 in 5) until the colour is just$ W8 _3 U1 ^: q6 y
completely changed from red to orange-yellow. Then add10 ml each0 h7 F/ Q+ }( ^# A5 W
of Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to G1 n& [& c1 N: V2 x3 P
room temperature in a stream of running water, add 3 drops of xylenol7 m6 o- ?) ^% G1 \
orange TS, and mix. If the solution is purple, yellow-brown, or pink,4 O( b, F$ J2 C& L. B1 O c6 A
bring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired& D# _+ |2 J) k) F/ K& B0 Z- L- V
pH, a pink colour indicates that not enough of the EDTA solution has
# m8 a, b/ u& f0 [8 k. ubeen added, in which case, discard the solution and repeat this3 V: l+ ^$ m2 e/ n
procedure with another 100 ml of Sample Solution B, using 50 ml,. J' W$ ^$ }, }! M9 a% U O
rather than 25 ml, of 0.02 M disodium EDTA.
/ ?+ ?/ r7 [8 ~( PProcedure
9 {2 S O% b, P* ?6 [/ {Using the standardized zinc sulfate solution as titrant, titrate Sample/ t) o2 o% V6 Y9 g Q- k3 K
Solution C to the first yellow-brown or pink end-point that persists for0 _) x; w9 Y" S3 H1 a# l
5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first
# E- }' N6 i/ Z5 E7 m8 k( |titration should require more than 8 ml of titrant, but for more accurate
4 g) M+ |4 t' o' e8 Ework a titration of 10-15 ml is desirable.
- g& v, m0 a: r. sAdd 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5
: i9 c3 D# Z' C) [( l5 Wmin, and cool in a stream of running water. Titrate this solution, using ^; V* I5 T3 ?5 D& p
the standardized zinc sulfate solution as titrant, to the same fugitive
y' m1 O" N# ^! Y% Gyellow-brown or pink end-point as described above.
! D- S0 ]$ q* q' @9 ` s0 hCalculation:
! L- A' B/ G" l! W% ?( o# VCalculate the percentage of aluminium oxide (Al2O3) in the sample
+ U; [. G' Y# ^) O7 dtaken by the formula:
4 G: Y+ {! l Z/ F& j* w% Al2O3 = 100 × (0.005VT)/S' m n# V: g5 T+ p2 s5 j, L( Y: R7 m% I
where
: A! n3 w. f, i, b4 g! yV is the number of ml of 0.01 N zinc sulfate consumed in
/ l% X( d+ t1 f _" kthe second titration,; S1 Q( k& X+ r+ h5 M& B
T is the titre of the zinc sulfate solution,
9 W) T4 z1 }% I( c- k# L1 iS is the mass (g) of the sample taken, and) v/ \8 w" |4 L+ j
0.005 = 500 ml / (1000mg/g × 100 ml).
8 n; l) e) }; K( @0 zSilicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica
' L& n* a6 h0 i/ rglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
" X. l1 l. p& ^" bHeat gently over a Meeker burner, while swirling the flask, until
9 |' c8 F: w% l, ^- tdecomposition and fusion are complete and the melt is clear, except
4 E d. L' G2 _for the silica content, and then cool. (Caution: Do not overheat the
2 z! z* M8 b% C' U3 E. }contents of the flask at the beginning, and heat cautiously during
, B1 U; M/ g% ^. M ^6 Afusion to avoid spattering.)$ H9 e( t/ s; \9 Y( y1 s$ |0 ]
To the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat& v7 o+ x8 B: T8 ?; \/ B: c
carefully and slowly until the melt is dissolved. Cool, and carefully add
: i Q( z$ W! c2 l# e150 ml of water by pouring very small portions down the sides of the1 _5 r* x( F- B7 K; X
flask, with frequent swirling to avoid over-heating and spattering. Allow
" I/ Y& o) Y! g: w7 Bthe contents of the flask to cool, and filter through fine ashless filter8 v N$ ~6 F) Q$ D# M, M( v+ c
paper, using a 60 degree gravity funnel. Rinse out all the silica from
: p) P; `1 _- x3 k4 ]9 E0 p; Hthe flask onto the filter paper with sulfuric acid solution (1 in 10).% j. @# n+ l5 ]' A$ S5 J" `. m; w: |
Transfer the filter paper and its contents into a platinum crucible, dry in
; i/ G. a2 h# X5 s, Kan oven at 1200, and heat the partly covered crucible over a Bunsen- M) K' Y9 E: j! g6 n* b' h
burner. To prevent flaming of the filter paper, first heat the cover from
& e0 r" ^9 N \( p7 w! Q9 s/ N9 Rabove, and then the crucible from below.
. q" f' } X0 j/ w; ?" }, Z2 mWhen the filter paper is consumed, transfer the crucible to a muffle
# i* @( ]) b3 K4 u$ z; [furnace and ignite at 1000o for 30 min. Cool in a desiccator, and: E# i: k. A: W! Z0 [$ e
weigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated
* x' @1 Q1 P( |4 P$ [/ t. }/ Xhydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first
. E! q( I& Y. f0 Qon a low-heat hot plate (to remove the HF) and then over a Bunsen6 k6 B5 z+ W0 }2 J G4 Z0 Q
burner (to remove the H2SO4). Take precautions to avoid spattering,
& M+ E- U# @1 ]# B; e1 V' Qespecially after removal of the HF. Ignite at 1000o for 10 min, cool in a
. f9 m, e' c/ g% v# Hdesiccator, and weigh again. Record the difference between the two8 Z3 ]4 a9 i1 o
weights as the content of SiO2 in the sample.) c: n: I7 q3 I3 S
METHOD OF ASSAY9 m; K2 {, R% C& x
Accurately weigh about 150 mg of the sample, previously dried at 105o
3 n7 Q+ x9 |6 b1 j) X( C( R. Kfor 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water4 B0 c3 A4 O7 F0 d3 ?8 \* c
and shake until a homogeneous, milky suspension is obtained. Add 30% ]" j Z5 d9 C2 T8 h) Y, R# I
ml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially) k$ ?2 x8 q6 U/ o$ K# o1 w
heat gently, then heat strongly until a clear solution is obtained. Cool,
6 w1 H9 t3 R) m0 ^) ?" R) wthen cautiously dilute with 120 ml of water and 40 ml of hydrochloric( m0 ]9 @) A9 T' c6 W, A* F
acid, and stir. Add 3 g of aluminium metal, and immediately insert a, d$ S! r9 U: R: U1 w) [
rubber stopper fitted with a U-shaped glass tube while immersing the
/ h! H8 o( J7 _& yother end of the U-tube into a saturated solution of sodium7 v8 i' f/ t( c; ]/ G- t. C4 q
bicarbonate contained in a 500-ml wide-mouth bottle, and generate
) D- ]% J* B* p3 N' chydrogen. Allow to stand for a few minutes after the aluminium metal; v, U/ E0 ^2 P6 B8 [
has dissolved completely to produce a transparent purple solution.( `9 F! T- ~+ q7 W% q
Cool to below 50o in running water, and remove the rubber stopper5 V! {* \" G# y6 J/ i
carrying the U-tube. Add 3 ml of a saturated potassium thiocyanate) k* S6 m. ]4 O4 ]" ~
solution as an indicator, and immediately titrate with 0.2 N ferric, G! X) p, K1 v/ g
ammonium sulfate until a faint brown colour that persists for 30+ U" L7 W8 O; W7 d
seconds is obtained. Perform a blank determination and make any& X) a6 ?: U( I0 p+ C, d* h9 v$ ^
necessary correction. Each ml of 0.2 N ferric ammonium sulfate is9 D/ t- _- e( A2 X, b# P
equivalent to 7.990 mg of TiO2.
3 f7 @+ a) Y7 J$ d! p |
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