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二氧化钛(钛白粉)
二氧化钛(钛白粉)
3 h+ ~5 y" P5 L8 b* B, }" \: T8 }2 ^
JECFA关于二氧化钛(钛白粉)的结论
9 F) Z* O$ _, Y+ `4 a [8 x5 Y' U4 K4 b/ h4 z
摘要: 2006年JECFA关于二氧化钛的结论
/ b |( Q$ m y. _6 qADI值:不作限制。
& ^% M( @- w; z/ J0 U/ A功能:着色剂
5 B3 T4 X( O% h) ^9 k7 t; ^5 A0 _3 i
TITANIUM DIOXIDE6 K0 k- m' _0 v* s' k3 G6 \' n
Prepared at the 67th JECFA (2006) and published in FAO JECFA
! D1 W+ J" D3 Q9 `/ b. ]2 R6 UMonographs 3 (2006), superseding specifications prepared at the 63rd
- d" p5 n, q& A' P7 p$ \& ^JECFA (2004) and published in FNP 52 Add 12 (2004) and in the
2 a- z4 S; ^5 X5 c# aCombined Compendium of Food Additive Specifications, FAO JECFA5 I% k$ s9 ]. f9 q1 |) p6 q- p( s
Monographs 1 (2005). An ADI “not limited” was established at the 13th4 q1 ]- C' e) U, ]1 ^
JECFA (1969).
0 Q; J! B$ D3 I& M" A: jSYNONYMS
( c* n R0 ?- _) c K, V) mTitania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171
# p/ e$ f- ]: C# D( f3 ~DEFINITION
8 D: w+ r+ y" lTitanium dioxide is produced by either the sulfate or the chloride
4 B) A+ h( a5 }2 J- ^; h3 B! lprocess. Processing conditions determine the form (anatase or rutile4 U$ e# `, n9 Z! ^0 g+ `' Z4 I
structure) of the final product.
2 y+ V, S' }. ~: O. sIn the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)
4 V ^4 A* Q w B% V6 d8 Y5 b* Q( kor ilmenite and titanium slag. After a series of purification steps, the
/ Z7 z: `8 w6 B) Gisolated titanium dioxide is finally washed with water, calcined, and
8 x5 r: j! m+ ~/ S3 G( smicronized.2 w- Y/ R( q% Y* o
In the chloride process, chlorine gas is reacted with a titaniumcontaining. K0 p/ ` n1 N4 d2 m
mineral under reducing conditions to form anhydrous* C. [. U7 u/ G6 L
titanium tetrachloride, which is subsequently purified and converted to$ E* c/ A2 Y1 }5 n
titanium dioxide either by direct thermal oxidation or by reaction with ?2 d5 ^$ p. s; m$ [- _
steam in the vapour phase. Alternatively, concentrated hydrochloric
, K3 b4 S) a- a9 c& V1 `4 w0 }# a4 Macid can be reacted with the titanium-containing mineral to form a
; l1 v% ` O$ q6 k! Q ?7 `solution of titanium tetrachloride, which is then further purified and
- i9 ~) x0 f/ y4 f( Vconverted to titanium dioxide by hydrolysis. The titanium dioxide is
2 R7 S: F; W& M7 zfiltered, washed, and calcined.9 G2 U( P7 W1 ^. S0 ~8 `# T
Commercial titanium dioxide may be coated with small amounts of! f% @. ]# Y& H8 z" E4 t
alumina and/or silica to improve the technological properties of the
% Y1 h3 d9 Y4 P7 ~: E, M# xproduct.* E2 I! T+ {3 U4 y
C.A.S. number 13463-67-7
8 d# ?5 Z4 i0 n% s- RChemical formula TiO29 F: k( D. J# u
Formula weight
" Q: y2 w" f5 S& s79.88
1 f4 r% T U' {Assay
: a- \) r* E5 x# @; l0 w0 y) tNot less than 99.0% on the dried basis (on an aluminium oxide and7 c$ T2 q& v* n1 h' C
silicon dioxide-free basis): e6 {$ `5 J; ~) Q* a
DESCRIPTION
y) _* f( x) m/ A: \1 N. WWhite to slightly coloured powder5 e/ L4 h, ^+ X ~1 I: F2 C3 c
FUNCTIONAL USES
: ?5 w% u. k) U# G7 xColour
5 O" k& B* @0 ]( a- q, I: X) pCHARACTERISTICS0 J. _$ U! a. M% g4 C/ S
IDENTIFICATION, n6 E5 D4 m) q! \9 O, C: m/ x
Solubility (Vol. 4); J1 j# J* ~8 y' j
Insoluble in water, hydrochloric acid, dilute sulfuric acid, and organic9 O& c$ m3 }# u& C6 @
solvents. Dissolves slowly in hydrofluoric acid and hot concentrated1 e( a. q9 K5 t' S) d
sulfuric acid.
- p* @# c$ B* E* D5 SColour reaction1 M$ i9 K! W6 q4 S8 n. k
Add 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of- m8 [+ j2 z& A- F
sulfuric acid appear, then cool. Cautiously dilute to about 100 ml with
( l3 d) I) `4 y5 E6 S$ Q/ J* dwater and filter. To 5 ml of this clear filtrate, add a few drops of- H" i+ H. W# F! l! u
hydrogen peroxide; an orange-red colour appears immediately.
( [/ ^/ B2 n B, JPURITY' f! Z7 d4 u7 A, j r4 Z3 Q9 }
Loss on drying (Vol. 4) Not more than 0.5% (105°, 3 h), c+ x0 G' f. n
Loss on ignition (Vol. 4) c7 Q+ m, L- q" s
Not more than 1.0% (800o) on the dried basis; G I5 V! i0 e% M/ |2 ~" `! v* @4 T
Aluminium oxide and/or2 S* |& p' j* j5 z; H' {
silicon dioxide2 Q c( e- p1 T+ Y8 |' r) B0 S
Not more than 2%, either singly or combined. U! J7 D5 r4 v$ a# u! R8 l
See descriptions under TESTS- o2 n, _; b, I8 |9 t$ n# |
Acid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing5 C9 Y% A/ W) F$ E0 E/ _
alumina or silica.5 Y! v0 F' U: i, a
Suspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and
0 F* n P$ j' A% c+ @place on a steam bath for 30 min with occasional stirring. Filter
5 N( }7 Y6 z5 v/ `1 tthrough a Gooch crucible fitted with a glass fibre filter paper. Wash
/ O" X4 B6 f7 w& @' F2 vwith three 10-ml portions of 0.5 N hydrochloric acid, evaporate the
5 d+ N6 e' u2 w9 a6 J! ]combined filtrate and washings to dryness, and ignite at a dull red
* e/ o$ F5 T1 _( O2 K+ I7 W* ^heat to constant weight.
g- V1 |* N' j3 qWater-soluble matter i5 K w2 J- C8 h: h
(Vol. 4)
3 t6 _& D4 W4 f9 Y. t, h; L: |( s- BNot more than 0.5%! q' g$ i' ]- n$ j. H1 b g# k
Proceed as directed under acid-soluble substances (above), using# g- [ E4 S( H
water in place of 0.5 N hydrochloric acid.
. `7 W b3 Q% |Impurities soluble in 0.5 N4 e K& p- ^7 C6 O+ L8 l
hydrochloric acid7 z5 m; F) T- [
Antimony Not more than 2 mg/kg5 r5 Z6 _+ M- x7 f0 k! {1 o
See description under TESTS3 u- `6 ]% Q ~ a: K( }) ]" v& t
Arsenic Not more than 1 mg/kg
; U7 w9 G+ n5 Q. HSee description under TESTS% ~. T6 s* G- o! h+ F1 Y( }
Cadmium Not more than 1 mg/kg
( ]$ Y- ?+ |7 c! P3 z# y) b. l6 B6 }See description under TESTS8 h0 |! n7 C& f. m
Lead
Q9 O' m' h0 E; f2 ]Not more than 10 mg/kg( ^' B/ s6 i$ ?: u9 g9 z3 X
See description under TESTS
, a' y! n1 ?# {6 j3 VMercury (Vol. 4) Not more than 1 mg/kg
R7 i( w! A2 C& zDetermine using the cold vapour atomic absorption technique. Select a
4 m- _6 t$ {9 j5 y* {: Y4 ?sample size appropriate to the specified level
8 d+ p6 O1 w& N; N$ lTESTS0 R; M+ t1 A) W7 ~
PURITY TESTS
, A2 r+ n- z- J/ a4 KImpurities soluble in 0.5 N$ H: }2 T$ |: q) m( U+ x8 [
hydrochloric acid& j9 C3 o1 {( `% ?* B9 I$ J
Antimony, arsenic,) i+ I; `5 P2 t! L/ r" T# H
cadmium and lead
: z# o/ _( {. a(Vol.4)
6 j" \ T, j( g3 m. ?+ o- E/ w. UTransfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N
% q$ n# p- K+ F& u: a2 t, ]: bhydrochloric acid, cover with a watch glass, and heat to boiling on a8 M1 W% A$ W/ s* A* G
hot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml
: R. i, {# l) P1 Z' tcentrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved
- }- ~7 f! u& B# x* H( B% Jmaterial settles. Decant the supernatant extract through a Whatman5 K8 O% y6 f W2 x' @9 H6 m5 e, f
No. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml5 d/ r4 K3 \4 G, C7 Y
volumetric flask and retaining as much as possible of the undissolved. l0 P" T3 ^. D4 Z" k h! I. W
material in the centrifuge bottle. Add 10 ml of hot water to the original
% E; l8 e3 e, _6 j$ S2 sbeaker, washing off the watch glass with the water, and pour the& X$ O8 Z7 Z7 a$ `, x
contents into the centrifuge bottle. Form a slurry, using a glass stirring
! Z2 w& X% ]! m7 u* }0 ?" ]: V4 Crod, and centrifuge. Decant through the same filter paper, and collect( [3 w9 d* h" N. y
the washings in the volumetric flask containing the initial extract.1 K1 F$ O& T: {. L9 w
Repeat the entire washing process two more times. Finally, wash the5 ] G, {% t: M" i- n. _( |
filter paper with 10 to 15 ml of hot water. Cool the contents of the flask1 s4 u" c) z* w; F
to room temperature, dilute to volume with water, and mix.
0 R4 I' X* L. x' bDetermine antimony, cadmium, and lead using an AAS/ICP-AES9 K. B& n$ _4 \% m( l# `
technique appropriate to the specified level. Determine arsenic using the
1 V) [7 a9 O* G# wICP-AES/AAS-hydride technique. Alternatively, determine arsenic using* V! X' L# e# `
Method II of the Arsenic Limit Test, taking 3 g of the sample rather than
& u h) ?. @" R. [ b1 g. The selection of sample size and method of sample preparation7 W3 U" V6 {; ?7 f: W4 |
may be based on the principles of the methods described in Volume 4.
* [0 e8 x' y g% q* c6 k6 ]Aluminium oxide Reagents and sample solutions
) Y1 @' r' m+ E# ^. {0.01 N Zinc Sulfate
1 {: E5 `* V# U- i$ \Dissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to9 l W4 [' ^! U0 d
make 1000 ml. Standardize the solution as follows: Dissolve 500 mg; ?: j! b: y( k( [- h6 \& J8 g1 b% k
of high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of
: ^% J( e& Z* O, W+ G( y0 C. h- i& Zconcentrated hydrochloric acid, heating gently to effect solution, then! c9 P9 E+ w& U1 S
transfer the solution into a 1000-ml volumetric flask, dilute to volume- w# c+ p/ ?- M
with water, and mix. Transfer a 10 ml aliquot of this solution into a 500
; n% F% X* z; v5 q; Gml Erlenmeyer flask containing 90 ml of water and 3 ml of
5 B+ V# z; a3 o( J2 fconcentrated hydrochloric acid, add 1 drop of methyl orange TS and
" A$ b, |+ L; f4 H2 W" r25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,
7 L C% V6 x! g5 x7 |5 E9 g+ d) s, rdropwise, ammonia solution (1 in 5) until the colour is just completely, q1 G$ l3 d) M& q
changed from red to orange-yellow. Then, add:
- o+ x( U# Q7 c) U* o! T9 U' w(a): 10 ml of ammonium acetate buffer solution (77 g of
5 e- L+ d' E K1 Mammonium acetate plus 10 ml of glacial acetic acid, dilute to
$ l: B! j6 x+ K1000 ml with water) and: X& F6 O' @: F
(b): 10 ml of diammonium hydrogen phosphate solution (150 g; S, C1 D* [2 E( N7 k
of diammonium hydrogen phosphate in 700 ml of water,( U! e5 t5 v6 i' v8 \
adjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,
; ?) f+ }# q& h; y: X0 E: W( zthen dilute to 1000 ml with water).+ Q# F9 }9 |6 S4 d3 ]
Boil the solution for 5 min, cool it quickly to room temperature in a! n" a" `: K5 G$ x% O, U, K9 q
stream of running water, add 3 drops of xylenol orange TS, and mix.
( x0 z% g5 x- o+ n0 u- XUsing the zinc sulfate solution as titrant, titrate the solution to the first; d( a1 f. T' O1 [# O8 w
yellow-brown or pink end-point colour that persists for 5-10 sec. (Note:
$ Z: C7 _: O5 I1 x% A5 OThis titration should be performed quickly near the end-point by
' Q1 x! R- M3 O6 V: p6 f6 m5 wadding rapidly 0.2 ml increments of the titrant until the first colour3 `2 O# v! a' V) H3 h( k
change occurs; although the colour will fade in 5-10 sec, it is the true
u: i' i4 r- _# s5 P* U- Cend-point. Failure to observe the first colour change will result in an
; r& c+ B) ~3 L( a2 i* bincorrect titration. The fading end-point does not occur at the second
1 T; w2 M& }# Z0 zend-point.)' Y5 X, `- Z) V+ ]& ~4 ]
Add 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a
0 V, n' D' B3 B ~# sstream of running water. Titrate this solution, using the zinc sulfate" M( ^& ^0 a7 ^* n' E8 D C
solution as titrant, to the same fugitive yellow-brown or pink end-point
; a# c, j( [/ B; h z. y. {3 u$ v5 X* xas described above.
8 z* S$ s* I( n" g* R* VCalculate the titre T of zinc sulfate solution by the formula:
% H0 e: w+ f9 ]. u# M) nT = 18.896 W / V
% r. ], }2 {( D1 @where; d% _! n; H* Y8 O6 u6 }: v
T is the mass (mg) of Al2O3 per ml of zinc sulfate solution/ E7 r3 V( ^) k4 g
W is the mass (g) of aluminium wire
5 x6 v# C. X! V0 |3 d- m$ OV is the ml of the zinc sulfate solution consumed in the
8 h, g# @8 @, b8 c# Ysecond titration
7 Q& y8 z. X* J0 n18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and& f# o5 \) {4 @. ?5 b$ C
R is the ratio of the formula weight of aluminium oxide to2 j- q4 k& U- ~3 m9 p4 P% V! u
that of elemental aluminium.
. ~) t4 V; i) b" |* O% E3 |Sample Solution A) h5 [- ?! t# f9 R" J. \9 |
Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica6 Z8 |. a4 Z9 k+ K8 C0 f9 {
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
. G$ S+ u Z+ e2 \(Note: Do not use more sodium bisulfate than specified, as an excess
1 T+ w1 S, Z9 K+ a" Sconcentration of salt will interfere with the EDTA titration later on in the+ \' W* c% @% @6 @
procedure.) Begin heating the flask at low heat on a hot plate, and0 j5 d4 h3 R5 O+ {# _8 j% f- \
then gradually raise the temperature until full heat is reached.9 z. i1 U8 E" b4 y5 i
(Caution: perform this procedure in a well ventilated area. ) When
' h4 J$ I( B3 D8 m# S$ kspattering has stopped and light fumes of SO3 appear, heat in the full
0 y/ U7 R/ I( G& ~2 a. A; w3 Uflame of a Meeker burner, with the flask tilted so that the fusion of the
8 w; @ w/ {% \. Osample and sodium bisulfate is concentrated at one end of the flask.
6 q. m# _( V3 u; @9 o$ q" `4 RSwirl constantly until the melt is clear (except for silica content), but" A/ x6 N9 N5 u. s# A7 r) i- M
guard against prolonged heating to avoid precipitation of titanium
, r7 G# j. }6 D4 ydioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until
! Q$ F; }- C; S% hthe mass has dissolved and a clear solution results. Cool, and dilute to
. Z# W3 l- w; r120 ml with water. Introduce a magnetic stir bar into the flask.- J5 o6 h) T( I- L
Sample Solution B1 m: n3 y" H! c& ]2 |3 d9 H
Prepare 200 ml of an approximately 6.25 M solution of sodium& B3 h) O- f" L: B r
hydroxide. Add 65 ml of this solution to Sample Solution A, while
: x1 E7 D0 S( Astirring with the magnetic stirrer; pour the remaining 135 ml of the2 g! q& i1 F, F
alkali solution into a 500-ml volumetric flask.
' n( V" P& h( @. k% n+ ~1 |+ e4 eSlowly, with constant stirring, add the sample mixture to the alkali
) C% o$ \! U/ j3 j$ c* C* {8 Qsolution in the 500-ml volumetric flask; dilute to volume with water,
& w; @1 b6 K* c- `5 m- Qand mix. (Note: If the procedure is delayed at this point for more than/ ~' c4 a; }3 l p( I6 B
2 hours, store the contents of the volumetric flask in a polyethylene. E& ]/ Z# B, n3 D
bottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),
0 f$ V: X" i0 J5 F- z) cthen filter the supernatant liquid through a very fine filter paper. Label
- x& o, D6 Y3 dthe filtrate Sample Solution B.
2 J0 E$ S" j1 o% dSample Solution C
& H, Y. O% J7 s, i! u! DTransfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer
) L& x1 P- P. z+ _; iflask, add 1 drop of methyl orange TS, acidify with hydrochloric acid+ G+ M z, e, x8 z
solution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.021 p5 M* M4 F8 c" |
M disodium EDTA, and mix. [Note: If the approximate Al2O3 content is
: H$ q$ o4 Y1 e" c7 o' k+ Fknown, calculate the optimum volume of EDTA solution to be added# j: n/ D" v/ ?8 J$ \# ]- z, L3 F
by the formula: (4 x % Al2O3) + 5.]9 w. T+ n! p4 h
Add, dropwise, ammonia solution (1 in 5) until the colour is just3 r' c3 S) \3 t1 b5 }2 V9 C
completely changed from red to orange-yellow. Then add10 ml each
. L3 D) A; ?, }) c/ P: X: ]3 ^6 D& mof Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to. u4 w& h6 g- L( x0 r- Q
room temperature in a stream of running water, add 3 drops of xylenol
& g2 _+ z7 W! s7 T8 |0 Yorange TS, and mix. If the solution is purple, yellow-brown, or pink,6 S P2 S0 ]" ]9 m9 P6 X, R
bring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired
. ~5 ~( ^' V) s# j5 g% ipH, a pink colour indicates that not enough of the EDTA solution has1 L% h9 o& n) H& ^! @* O
been added, in which case, discard the solution and repeat this( V5 I; M# z: N1 J; z
procedure with another 100 ml of Sample Solution B, using 50 ml,
5 V% P% g, F& p4 c/ Grather than 25 ml, of 0.02 M disodium EDTA.
# M* d& _3 Q* Q k: [Procedure2 `6 q; S) i2 n0 u
Using the standardized zinc sulfate solution as titrant, titrate Sample
) E& T! r" ~- aSolution C to the first yellow-brown or pink end-point that persists for
, Y/ G9 a! N: ~& j5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first0 q! ]1 d( w$ O; O) A q
titration should require more than 8 ml of titrant, but for more accurate4 I5 J3 U/ G& K
work a titration of 10-15 ml is desirable.
6 t) U7 o+ x% @! t/ UAdd 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5, {) B, y* ?1 r0 j% {+ k
min, and cool in a stream of running water. Titrate this solution, using0 Z$ F0 y- {. |" R4 ~. W" |$ o
the standardized zinc sulfate solution as titrant, to the same fugitive* M& E& M# V$ W
yellow-brown or pink end-point as described above.# q: M$ g9 q1 E/ s& V
Calculation:; R8 T9 q9 N% F8 J/ U; h
Calculate the percentage of aluminium oxide (Al2O3) in the sample
4 Q8 i4 f! r+ i; d( J; t% e! [taken by the formula:
3 S2 W, F9 P, Y1 z$ u% Al2O3 = 100 × (0.005VT)/S
6 ^/ }- H4 d' H4 r) d1 Ywhere
8 P* s9 ]; c; MV is the number of ml of 0.01 N zinc sulfate consumed in" {7 `/ c6 ]+ |% ]9 @: ]; ?% p( p
the second titration,
G1 f& I& M5 m: MT is the titre of the zinc sulfate solution,
" ]5 d* D/ [+ ? ?5 QS is the mass (g) of the sample taken, and
) q9 d) W" E6 Q, K3 U; g) \% L0.005 = 500 ml / (1000mg/g × 100 ml).& @+ W7 w) U0 d0 h' B$ q2 m! z
Silicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica
6 ]. h* v( _7 _9 E$ x+ z8 x9 i2 ~glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
, P4 l2 y: U2 d8 c/ A' `4 FHeat gently over a Meeker burner, while swirling the flask, until
0 y% j4 H' \! ^5 [- ^ hdecomposition and fusion are complete and the melt is clear, except& V) u" U' K z; K, @
for the silica content, and then cool. (Caution: Do not overheat the$ x2 Y E8 B, s4 m* f- m8 R
contents of the flask at the beginning, and heat cautiously during
5 y! A, U! K, u: b3 ofusion to avoid spattering.)
3 g$ Y- `: Z9 G) _# wTo the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat' G' b3 W" w8 P7 I- N+ o/ F
carefully and slowly until the melt is dissolved. Cool, and carefully add; W8 O$ M; s! @& T! h
150 ml of water by pouring very small portions down the sides of the
% ]) r" } j; x bflask, with frequent swirling to avoid over-heating and spattering. Allow
+ S' A3 \1 m# N; Ithe contents of the flask to cool, and filter through fine ashless filter6 ^/ H) D$ j' a7 s( \/ `
paper, using a 60 degree gravity funnel. Rinse out all the silica from
. b9 q/ y' X5 ~- d6 s# dthe flask onto the filter paper with sulfuric acid solution (1 in 10).
1 s. X$ l* r9 t& I3 a! G' ~Transfer the filter paper and its contents into a platinum crucible, dry in3 m4 X7 S5 R& a9 v. m; {% Y% l1 v
an oven at 1200, and heat the partly covered crucible over a Bunsen
T% ~5 ^9 [- Uburner. To prevent flaming of the filter paper, first heat the cover from
" M4 N- v9 c. j/ q* l+ g# aabove, and then the crucible from below.
' V4 Q& d v$ g. mWhen the filter paper is consumed, transfer the crucible to a muffle$ {2 j, t3 }1 p: q2 Y: v8 |# a
furnace and ignite at 1000o for 30 min. Cool in a desiccator, and( L; K- t1 Q( d) E3 ^$ f
weigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated
3 Q0 ~) d. q1 K, Z$ r9 E( [. v: Thydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first
4 W, M/ C& [, m0 C% ], Won a low-heat hot plate (to remove the HF) and then over a Bunsen0 Y% r b% U) V8 |, u8 E# Q: f
burner (to remove the H2SO4). Take precautions to avoid spattering,
* y ^* Z1 K3 W1 kespecially after removal of the HF. Ignite at 1000o for 10 min, cool in a N! [/ T* p' k9 c
desiccator, and weigh again. Record the difference between the two
+ F% N/ r3 k" x8 E. qweights as the content of SiO2 in the sample.
7 A; E9 g, k1 m# w. K- K$ h( GMETHOD OF ASSAY
7 h, O8 u+ N9 _4 q, C; x) pAccurately weigh about 150 mg of the sample, previously dried at 105o
* v, B5 M8 C9 Q: Y! Kfor 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water
0 g& W: d+ } Q* Y2 b K0 Rand shake until a homogeneous, milky suspension is obtained. Add 30
9 r1 { o9 J4 T+ q; Y& F" lml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially+ B j* e. |; U
heat gently, then heat strongly until a clear solution is obtained. Cool,6 o2 t! x/ [4 q$ Y4 j0 _
then cautiously dilute with 120 ml of water and 40 ml of hydrochloric
( D3 J& s3 ?. ~0 J* p F' [acid, and stir. Add 3 g of aluminium metal, and immediately insert a1 L$ S9 `$ }% j4 s7 V, H* B
rubber stopper fitted with a U-shaped glass tube while immersing the
/ T3 {- R3 _5 M- `other end of the U-tube into a saturated solution of sodium, Q& \3 ~2 Z1 w% N8 _- S( O
bicarbonate contained in a 500-ml wide-mouth bottle, and generate
9 k9 I, R6 b0 e0 Thydrogen. Allow to stand for a few minutes after the aluminium metal8 A& Y+ p2 S1 j. ]1 u- f
has dissolved completely to produce a transparent purple solution.
3 @9 h; p) T ]+ G: `Cool to below 50o in running water, and remove the rubber stopper d7 ?# g# n* u2 ?9 O1 R
carrying the U-tube. Add 3 ml of a saturated potassium thiocyanate
+ R3 x3 A8 i1 {+ E6 Z) |8 gsolution as an indicator, and immediately titrate with 0.2 N ferric
4 O4 N# D. a( b+ O9 i& pammonium sulfate until a faint brown colour that persists for 30
& W( C; b5 e+ h8 E2 C8 @seconds is obtained. Perform a blank determination and make any1 C& @ D8 w& ]! F
necessary correction. Each ml of 0.2 N ferric ammonium sulfate is
7 V5 K* p0 S% h1 t1 }2 @" e& w) ?' Mequivalent to 7.990 mg of TiO2.
+ N( j( ~; W7 S# e |
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