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二氧化钛(钛白粉)
二氧化钛(钛白粉)
1 ~) n' E% _4 u
# l. d5 G5 y1 P1 w; `8 Q( bJECFA关于二氧化钛(钛白粉)的结论5 r8 l5 V. K# f& v
N: t' |( k8 J' D$ L1 m+ U
摘要: 2006年JECFA关于二氧化钛的结论
; I& ^& R/ k6 x0 vADI值:不作限制。
5 t f+ D% O2 W$ \& X" L功能:着色剂0 `- T/ g, Z7 j$ y; l# w# i* i
, x1 M% V% J& l! k( J- q' q0 uTITANIUM DIOXIDE1 K, v# f* y) ?- R" \+ @- x
Prepared at the 67th JECFA (2006) and published in FAO JECFA( K0 d% o3 b; n2 H7 u
Monographs 3 (2006), superseding specifications prepared at the 63rd
- B; v) s/ y5 B4 E4 U* GJECFA (2004) and published in FNP 52 Add 12 (2004) and in the
8 m! B0 l7 n* W( O$ e LCombined Compendium of Food Additive Specifications, FAO JECFA* @$ s. v$ o5 r/ q+ S
Monographs 1 (2005). An ADI “not limited” was established at the 13th
( o: P. o& P* s7 @; }JECFA (1969).9 a' p7 b, `! p+ g9 Z
SYNONYMS3 L! k, }: X. t3 e! w4 s0 |- j
Titania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171
0 ` M5 H+ o3 x9 TDEFINITION6 Y k) `) e3 [0 q
Titanium dioxide is produced by either the sulfate or the chloride
$ {8 b% ?1 M$ ?7 H R! V* i5 pprocess. Processing conditions determine the form (anatase or rutile
4 A5 l5 m' `7 E/ I8 I+ y' R9 {structure) of the final product.
! W8 C( O9 }5 M! ?In the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)- q# k) A( Q$ Z$ S" h0 H
or ilmenite and titanium slag. After a series of purification steps, the. h% A4 k& P0 `+ y
isolated titanium dioxide is finally washed with water, calcined, and$ B6 P' ^4 {6 l+ b8 t( V
micronized.; p. s8 D+ V1 z% Z7 p" q5 t2 g+ _0 o
In the chloride process, chlorine gas is reacted with a titaniumcontaining. }. t; `& x1 V. M8 O$ P' P# `
mineral under reducing conditions to form anhydrous
9 B: v5 G6 q! q: A3 Stitanium tetrachloride, which is subsequently purified and converted to
+ C0 w& k& T# O! Y: dtitanium dioxide either by direct thermal oxidation or by reaction with( b) H3 r) p" k _1 |; J; _) E- P
steam in the vapour phase. Alternatively, concentrated hydrochloric% } @; V' V/ C8 k0 Y5 i
acid can be reacted with the titanium-containing mineral to form a
, R9 ^! |2 Y. f# @" t1 Wsolution of titanium tetrachloride, which is then further purified and1 L" \( e4 [9 b/ v8 s" k' }
converted to titanium dioxide by hydrolysis. The titanium dioxide is3 h# o7 V2 e: _. P3 A( _8 C# W+ ~
filtered, washed, and calcined. g3 _6 N# q. b/ _
Commercial titanium dioxide may be coated with small amounts of& c" Y2 k: A' T- [. q" T5 I
alumina and/or silica to improve the technological properties of the
0 ~* P) b/ c' o+ F0 W0 i+ Yproduct.
% D7 Q% X# U5 z9 @% `3 K/ [C.A.S. number 13463-67-7
9 P, s# D5 e; E( y5 BChemical formula TiO2
$ Z2 k, U3 \* v( G* y( UFormula weight
5 w! T9 l& \. s; t79.88) g3 W5 @* @; p; z% |" G8 S% w3 E3 N
Assay' K9 s2 H5 W8 `/ N; {0 W% w. J
Not less than 99.0% on the dried basis (on an aluminium oxide and
) \( k: E: g& t9 usilicon dioxide-free basis)
$ G i# O6 K% [$ t. WDESCRIPTION
- g) G* F1 |0 B8 ~) WWhite to slightly coloured powder
: T/ {( g, M% g' h* A0 W- LFUNCTIONAL USES2 \8 D, J$ H0 a. \3 }6 s, K) d
Colour
; }2 f0 X/ d8 j+ rCHARACTERISTICS
* |" \' `/ ?& a# o# S! oIDENTIFICATION1 q- {+ A3 W) ~! l& \ k
Solubility (Vol. 4)# u" g2 ~) {1 p0 k
Insoluble in water, hydrochloric acid, dilute sulfuric acid, and organic
. @: U+ I% N* D) @9 P2 A \solvents. Dissolves slowly in hydrofluoric acid and hot concentrated
/ x9 D- O: I8 r+ j& usulfuric acid.
/ M9 D; D% u; V7 m$ K. S6 VColour reaction9 a3 n! {/ Z7 A* O
Add 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of
2 Q5 `1 |: m6 s ysulfuric acid appear, then cool. Cautiously dilute to about 100 ml with7 f, L& C7 S& L1 N
water and filter. To 5 ml of this clear filtrate, add a few drops of; P/ M& H6 K+ ]" Q, ~; N7 t" L
hydrogen peroxide; an orange-red colour appears immediately.
/ {$ n* k+ V8 zPURITY! q5 N4 S# L# Z; {# o
Loss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)/ c; L1 w' P8 y0 m
Loss on ignition (Vol. 4)
% G9 s, m" B+ q, M- |# JNot more than 1.0% (800o) on the dried basis
& j. i0 ? e: z: h4 G8 I4 x D _Aluminium oxide and/or2 }# h: k0 q' P s: X
silicon dioxide
H/ P9 g. l, ?4 s/ H3 \! yNot more than 2%, either singly or combined: x/ z1 p( w1 H r! ]& o: Y( L
See descriptions under TESTS' |. m* d# D: e/ `* H |& V
Acid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing5 a& g( r+ ]- n
alumina or silica.9 x8 u; @! d5 {) q5 u1 D) f* V
Suspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and- r: \% i U4 u2 \6 r2 w1 a
place on a steam bath for 30 min with occasional stirring. Filter# K) ~' @/ L: e1 Q
through a Gooch crucible fitted with a glass fibre filter paper. Wash
8 d" f5 |: P! f8 |: b, |with three 10-ml portions of 0.5 N hydrochloric acid, evaporate the+ M8 e. S# b/ O; r
combined filtrate and washings to dryness, and ignite at a dull red: H) U$ u" Y3 O# e
heat to constant weight.
* L1 F. e7 ^8 v t( UWater-soluble matter( H( l" ?2 m' d
(Vol. 4); ^+ ^& A; n. q! @; b- P
Not more than 0.5%
, L' a, c$ c/ v3 m5 `* G& p7 OProceed as directed under acid-soluble substances (above), using0 A. O5 V4 o$ D3 k
water in place of 0.5 N hydrochloric acid.$ e; W" a/ Z6 o, W
Impurities soluble in 0.5 N; @; M! ?. p- @9 _1 d+ k
hydrochloric acid
+ y6 C. D2 Z4 l9 u: L' i) N- K TAntimony Not more than 2 mg/kg
4 G% Z7 t$ N( b; O0 i. lSee description under TESTS% L) E( C3 J* Z' P2 K; L
Arsenic Not more than 1 mg/kg( Y2 x( K" w) R+ _' C/ D
See description under TESTS# s6 A! N0 l$ X# X, Q
Cadmium Not more than 1 mg/kg) ]0 K7 v$ z b) F$ n, H
See description under TESTS
! y6 w0 P }; U* K5 `4 KLead
. m; P4 r4 `1 C9 f1 o) wNot more than 10 mg/kg i* S' X( b& S+ i+ e% C+ C, `
See description under TESTS3 Z2 c5 q$ ~, a4 G2 |
Mercury (Vol. 4) Not more than 1 mg/kg
! {# E3 o" _, J0 q* fDetermine using the cold vapour atomic absorption technique. Select a4 A4 U0 G! C! {( E9 ]4 ?
sample size appropriate to the specified level
" [& s6 T9 H! w8 Q- Y" _5 TTESTS, ?! M' U$ J6 Z- T1 b+ a3 y( ^- t( Q$ U
PURITY TESTS V0 S& J, V) J9 T4 W. ~+ Z
Impurities soluble in 0.5 N, N2 H3 @& i7 d+ T5 U
hydrochloric acid
* U4 Y5 \) ~3 n6 d1 ~3 J8 GAntimony, arsenic,0 h1 Y: X, D. e+ d- Q" s/ J
cadmium and lead5 b8 d/ `5 f+ g$ U- r
(Vol.4)
% M1 p1 q9 c: T4 E: [Transfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N
5 V, Y& j$ r* F6 d |+ n: Ahydrochloric acid, cover with a watch glass, and heat to boiling on a. s2 \* Z- [/ E. `0 R1 j
hot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml' c8 p9 A( c8 J. v6 d
centrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved# N$ U, S+ b: R" U; t9 q% H
material settles. Decant the supernatant extract through a Whatman5 r' y: R. \; g' {* y
No. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml0 Z, r+ \- V- X0 P* W
volumetric flask and retaining as much as possible of the undissolved
# b/ x: h1 t1 |; `5 N9 d( N: }# gmaterial in the centrifuge bottle. Add 10 ml of hot water to the original t& v* ]/ b6 X
beaker, washing off the watch glass with the water, and pour the6 m; @; J/ u) [) m- ~6 A( [
contents into the centrifuge bottle. Form a slurry, using a glass stirring
7 b G! d) S% t( brod, and centrifuge. Decant through the same filter paper, and collect
, S! [4 G! C, U1 R: W) uthe washings in the volumetric flask containing the initial extract.
* _8 S. T+ ^# Z/ [. h( yRepeat the entire washing process two more times. Finally, wash the
" F; Z! `# t2 _5 a& W' |3 afilter paper with 10 to 15 ml of hot water. Cool the contents of the flask
( ?/ |* J4 o% r) tto room temperature, dilute to volume with water, and mix.
* ]& e: [2 K5 ADetermine antimony, cadmium, and lead using an AAS/ICP-AES* J# z0 q& J! j8 }6 ^
technique appropriate to the specified level. Determine arsenic using the9 d: y1 d& V, Z- ~ C: l0 b1 Q
ICP-AES/AAS-hydride technique. Alternatively, determine arsenic using& I0 `: q* N0 D; Z* h
Method II of the Arsenic Limit Test, taking 3 g of the sample rather than
) G& U# V7 A& n# U6 U$ F q1 g. The selection of sample size and method of sample preparation
! {0 `1 ?5 r( h+ I1 Bmay be based on the principles of the methods described in Volume 4.. q5 u, y+ u W6 `
Aluminium oxide Reagents and sample solutions# j2 T2 G- x' Z- L4 h3 ^9 E$ Q
0.01 N Zinc Sulfate
* P( R) }* \, r1 I- TDissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to+ P( |5 a7 n4 \
make 1000 ml. Standardize the solution as follows: Dissolve 500 mg
/ \$ m( ], W" F2 rof high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of& {0 n6 |3 p# R1 O" r0 y& W3 |
concentrated hydrochloric acid, heating gently to effect solution, then
$ ^( W- Y0 ?! O1 `. ?transfer the solution into a 1000-ml volumetric flask, dilute to volume# i' @1 f0 f$ ~/ \
with water, and mix. Transfer a 10 ml aliquot of this solution into a 500
0 \/ }6 M& G; a$ x' F7 A9 r- m5 Xml Erlenmeyer flask containing 90 ml of water and 3 ml of! D: t# i# v* e
concentrated hydrochloric acid, add 1 drop of methyl orange TS and
% A+ | C% a0 V# @25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,
. j/ R8 @+ P7 Ndropwise, ammonia solution (1 in 5) until the colour is just completely
5 L8 y8 S2 k5 i& {changed from red to orange-yellow. Then, add:
4 j; p, c1 |6 |$ o$ R' f(a): 10 ml of ammonium acetate buffer solution (77 g of
, r1 O/ b( f; `* j6 S2 Iammonium acetate plus 10 ml of glacial acetic acid, dilute to
/ C5 H- A9 P- v* D4 D8 x1000 ml with water) and
( E" Y4 S9 G* s4 K(b): 10 ml of diammonium hydrogen phosphate solution (150 g
+ {! L0 c7 o, I3 }/ `) o0 o$ C7 wof diammonium hydrogen phosphate in 700 ml of water,
/ L, e/ `2 i# W. Jadjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,
- Q+ J6 X) F7 s! h2 Jthen dilute to 1000 ml with water).
- v, W7 t5 F3 Z* s7 F6 BBoil the solution for 5 min, cool it quickly to room temperature in a( N [* S( S4 Y8 o. b, p5 u# }* n2 z
stream of running water, add 3 drops of xylenol orange TS, and mix.
! s6 K7 U, i; cUsing the zinc sulfate solution as titrant, titrate the solution to the first$ p; T3 T6 U; A& M8 F ~
yellow-brown or pink end-point colour that persists for 5-10 sec. (Note:
' G& v0 D2 F+ S" C$ K* dThis titration should be performed quickly near the end-point by
' Y: g/ @ A( ^0 m, v7 wadding rapidly 0.2 ml increments of the titrant until the first colour3 m3 P' h5 t3 P: [& J# @& B
change occurs; although the colour will fade in 5-10 sec, it is the true
" p6 x. z6 ]2 M7 {6 Aend-point. Failure to observe the first colour change will result in an# ?6 T) \( X% z: j% c
incorrect titration. The fading end-point does not occur at the second! `' R2 w' \; U. i
end-point.)
" F$ Y, T0 v+ Z4 A! L2 J3 l1 \/ BAdd 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a- @' Y' }3 O7 N' B) N
stream of running water. Titrate this solution, using the zinc sulfate
" B+ I% ~( m( a. |1 T, ^9 P4 D4 F jsolution as titrant, to the same fugitive yellow-brown or pink end-point
% b# C# M( p5 g% V( Y0 ~# \as described above.
% Q7 A* r! c7 L! o5 f. ~/ n, E1 rCalculate the titre T of zinc sulfate solution by the formula:/ e4 u# [1 @: w- C
T = 18.896 W / V
: M2 W. O; t+ W, o/ s9 H) N0 _* Fwhere
. A& a H% N( V7 f1 f+ _* H6 VT is the mass (mg) of Al2O3 per ml of zinc sulfate solution
" t6 L% N) O3 Q. z) c( [- }W is the mass (g) of aluminium wire) b6 p& z% z; N- A# s
V is the ml of the zinc sulfate solution consumed in the
' G9 q& M% C; r) `& asecond titration) E# j8 {& |: `
18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and
( r2 }* u7 {2 L) r. ?2 E# }, YR is the ratio of the formula weight of aluminium oxide to
+ ~ W4 t6 ]& Y/ w- x4 uthat of elemental aluminium.: W2 P" o7 j- i. ?1 I7 @, O
Sample Solution A
- S) S: K8 k# D! {/ u" oAccurately weigh 1 g of the sample and transfer to a 250-ml high-silica' b5 s: W2 G P, Y
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
2 n' d+ s" i9 }5 V$ f! b. z(Note: Do not use more sodium bisulfate than specified, as an excess
1 V3 s0 h; r' U# v1 |8 Y; ~- Gconcentration of salt will interfere with the EDTA titration later on in the
( c7 T. ]# E5 D- J; Vprocedure.) Begin heating the flask at low heat on a hot plate, and' t7 q- G. }: J4 d0 u9 [* p
then gradually raise the temperature until full heat is reached.
9 r3 N7 E9 @6 {8 C8 X(Caution: perform this procedure in a well ventilated area. ) When
4 R' \/ R7 k4 A" P" Vspattering has stopped and light fumes of SO3 appear, heat in the full
8 _, r* K; k1 _ rflame of a Meeker burner, with the flask tilted so that the fusion of the
" d' ^" B, E7 H' I" ~- F6 hsample and sodium bisulfate is concentrated at one end of the flask.# B. r4 O; v$ J
Swirl constantly until the melt is clear (except for silica content), but
; Q! b' o/ d4 _ x! c! Bguard against prolonged heating to avoid precipitation of titanium
6 J8 a8 @+ k$ H5 `, {8 odioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until
5 G( U+ R+ h: P* Q* Wthe mass has dissolved and a clear solution results. Cool, and dilute to
4 T2 y: d$ m0 l2 E* e6 l120 ml with water. Introduce a magnetic stir bar into the flask.3 b+ E* Q) M ]) S4 R. i$ a
Sample Solution B0 T4 V2 _0 \2 H; V3 F! Q
Prepare 200 ml of an approximately 6.25 M solution of sodium+ V6 ?* r$ Y5 |
hydroxide. Add 65 ml of this solution to Sample Solution A, while* ~$ w4 K9 g8 a; m
stirring with the magnetic stirrer; pour the remaining 135 ml of the
- k/ @+ p. |$ R. g! \& k! ~/ jalkali solution into a 500-ml volumetric flask.
& E z- S: a, G& OSlowly, with constant stirring, add the sample mixture to the alkali
! M% I6 G' z: h( esolution in the 500-ml volumetric flask; dilute to volume with water,
4 v. c* }1 H1 p% l% E |and mix. (Note: If the procedure is delayed at this point for more than& C! Q o6 P3 F: D) B5 }6 x _
2 hours, store the contents of the volumetric flask in a polyethylene! d3 J% I/ }( n7 o1 X
bottle.) Allow most of the precipitate to settle (or centrifuge for 5 min), _, b! u( z! F+ ~% w
then filter the supernatant liquid through a very fine filter paper. Label
y) m9 M5 L) v; Z! Cthe filtrate Sample Solution B.! V- F" y4 e8 a+ I+ x
Sample Solution C
, l' U6 {( p* m! TTransfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer) Z ~, \' }' {- B( _2 y
flask, add 1 drop of methyl orange TS, acidify with hydrochloric acid0 Z0 i5 \4 r/ v
solution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02- ]( C- b# |1 I4 v5 t+ V
M disodium EDTA, and mix. [Note: If the approximate Al2O3 content is" m2 I9 L3 e+ K6 V) X- M6 v9 x3 [
known, calculate the optimum volume of EDTA solution to be added9 r2 n# ]5 d" N j! s! J
by the formula: (4 x % Al2O3) + 5.]0 x6 d0 M' r$ |3 y
Add, dropwise, ammonia solution (1 in 5) until the colour is just) I$ h0 ^9 ^1 S z
completely changed from red to orange-yellow. Then add10 ml each" i+ [: I; ?. s% G n1 l
of Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to) u: m7 }+ @2 a4 }
room temperature in a stream of running water, add 3 drops of xylenol) u0 `0 o+ w" G0 S5 v1 N
orange TS, and mix. If the solution is purple, yellow-brown, or pink,( d* B2 K% z3 }$ g" y0 a3 r& J
bring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired: K O* C6 G; v3 G9 t3 x& B2 X8 E, p
pH, a pink colour indicates that not enough of the EDTA solution has8 Q" R/ F9 t, q0 d- U# t& {& t
been added, in which case, discard the solution and repeat this, H- w+ ]$ j, v8 g: d K( n
procedure with another 100 ml of Sample Solution B, using 50 ml,1 y% r! h& x& U1 u$ c
rather than 25 ml, of 0.02 M disodium EDTA.
0 d# j0 q* K( e0 X/ w+ bProcedure
4 ^1 Q. T3 b# O# O, D9 N- @Using the standardized zinc sulfate solution as titrant, titrate Sample8 v. L1 o7 n' W
Solution C to the first yellow-brown or pink end-point that persists for) A2 o; x) e) U! c- r+ k
5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first* c; A5 J- U6 L
titration should require more than 8 ml of titrant, but for more accurate# q! P! f9 ?: f/ g9 U2 g
work a titration of 10-15 ml is desirable.# W' C. Q2 `+ F3 e
Add 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5
- `! l# B9 \% I! y6 d, S0 Smin, and cool in a stream of running water. Titrate this solution, using8 r3 |2 C8 V2 M
the standardized zinc sulfate solution as titrant, to the same fugitive, ]6 L3 J' [! w
yellow-brown or pink end-point as described above.- p1 T! G8 A9 t1 v
Calculation:
, i: G2 w! T& V% h6 _Calculate the percentage of aluminium oxide (Al2O3) in the sample
. w2 n. W* V; h; `% m( [# l+ n7 ^+ G Gtaken by the formula:% N4 D ^9 h9 s6 w: g4 H
% Al2O3 = 100 × (0.005VT)/S0 N8 z2 |7 x9 A0 w. r$ E. ?
where* f7 _. l8 H8 T- j, }( {
V is the number of ml of 0.01 N zinc sulfate consumed in0 D6 o5 S- Z0 Q2 I4 L
the second titration,' z6 U, n1 k# N1 i4 i/ p7 n8 S
T is the titre of the zinc sulfate solution,
8 y: z, C; W: yS is the mass (g) of the sample taken, and
4 w+ n8 L& F, v# W% ] X6 w1 v0.005 = 500 ml / (1000mg/g × 100 ml).$ y( S' L5 G# y6 a# `
Silicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica
* ]0 x5 M5 e, x* N, H6 C# Iglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).4 w' }6 T& ?6 J5 A
Heat gently over a Meeker burner, while swirling the flask, until
: r1 g* s- j2 o! F6 ~decomposition and fusion are complete and the melt is clear, except
- `2 l p- I3 o& c$ gfor the silica content, and then cool. (Caution: Do not overheat the( Q U7 C3 i! U) Q1 l4 @
contents of the flask at the beginning, and heat cautiously during3 q8 `, t5 e8 ^7 l' \0 V
fusion to avoid spattering.)3 P1 v( C! \1 @
To the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat
: F5 A+ o3 @' W* v: ]3 p6 a. B+ Tcarefully and slowly until the melt is dissolved. Cool, and carefully add
- r8 r3 e3 D9 s: A150 ml of water by pouring very small portions down the sides of the
- b" S% @" j0 L+ hflask, with frequent swirling to avoid over-heating and spattering. Allow
$ N. B1 R2 }, z, v* Zthe contents of the flask to cool, and filter through fine ashless filter
# D$ T- D$ E7 ~) {4 Upaper, using a 60 degree gravity funnel. Rinse out all the silica from
/ W; \( h5 N4 c* \the flask onto the filter paper with sulfuric acid solution (1 in 10).# Q* ]5 ]6 P/ {, |' Z$ r z
Transfer the filter paper and its contents into a platinum crucible, dry in
0 c9 h4 m7 \7 f# h8 Aan oven at 1200, and heat the partly covered crucible over a Bunsen8 H3 d' ^. t' J9 B- v* d9 D
burner. To prevent flaming of the filter paper, first heat the cover from
2 X# j' x! {* sabove, and then the crucible from below.
8 y+ g) M: ?3 M. W% T2 d6 \) KWhen the filter paper is consumed, transfer the crucible to a muffle
- t1 W* N, j+ p# M9 u& wfurnace and ignite at 1000o for 30 min. Cool in a desiccator, and
1 @) U$ {( e: ]& W+ y$ Uweigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated: J" s) g3 p6 v# C3 N3 N6 ?+ J
hydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first9 O, I4 g. g, b: p3 k
on a low-heat hot plate (to remove the HF) and then over a Bunsen
1 e# {+ z5 C. S8 d) q" aburner (to remove the H2SO4). Take precautions to avoid spattering,9 k% t7 o6 y" W& q6 P4 E, s) e7 i
especially after removal of the HF. Ignite at 1000o for 10 min, cool in a
- V/ l, N0 t' y, p$ vdesiccator, and weigh again. Record the difference between the two3 M+ m+ J( Q/ d& p% K+ @
weights as the content of SiO2 in the sample.% W6 p% i8 V3 A+ E+ [* X
METHOD OF ASSAY
8 R! T9 V5 `1 jAccurately weigh about 150 mg of the sample, previously dried at 105o6 C5 }5 b/ W5 Y! l
for 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water
$ f5 d* C' c0 v4 B6 `3 {8 Cand shake until a homogeneous, milky suspension is obtained. Add 301 |% r" v) r' k p A
ml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially2 `0 t& Y: }* F- B
heat gently, then heat strongly until a clear solution is obtained. Cool,% b% P4 h" s. K; z- a& `. q
then cautiously dilute with 120 ml of water and 40 ml of hydrochloric
7 { B; D# T+ R' Y& k0 m$ Dacid, and stir. Add 3 g of aluminium metal, and immediately insert a* K. J" _: c) K3 Q( ?5 U) A
rubber stopper fitted with a U-shaped glass tube while immersing the$ p/ L: v2 j, u5 ^: C; F# S: i
other end of the U-tube into a saturated solution of sodium
k7 ]7 j! q8 s( W# abicarbonate contained in a 500-ml wide-mouth bottle, and generate; i! I! T+ ?$ y' x, K5 V
hydrogen. Allow to stand for a few minutes after the aluminium metal
9 o+ r5 W1 E' v+ L; @5 j+ Hhas dissolved completely to produce a transparent purple solution.
* f! d1 A" p% Q6 P# v: tCool to below 50o in running water, and remove the rubber stopper
& U; l2 J& ]! e# K _3 Dcarrying the U-tube. Add 3 ml of a saturated potassium thiocyanate1 E, o3 j5 Q1 m8 x0 C
solution as an indicator, and immediately titrate with 0.2 N ferric* B7 I+ R$ a! q4 V6 I$ R2 h. I
ammonium sulfate until a faint brown colour that persists for 30
% l8 ^, R2 l; f% ]) \: E8 y2 yseconds is obtained. Perform a blank determination and make any
4 E f' o# D- N* r. y0 anecessary correction. Each ml of 0.2 N ferric ammonium sulfate is
4 r/ I( T$ D9 w: W/ P8 Iequivalent to 7.990 mg of TiO2.
' C7 }+ Q3 ]7 r8 \$ F |
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