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二氧化钛(钛白粉)
二氧化钛(钛白粉)
& B! H, A" b0 H/ M# x% J* ?) e1 q0 |2 R" A J* J# m
JECFA关于二氧化钛(钛白粉)的结论2 X6 R. k, S" p1 D) P5 A
9 x! ]& a: P. J! l$ G: N& E0 G
摘要: 2006年JECFA关于二氧化钛的结论8 h2 d6 Q6 R4 @- \+ r. P
ADI值:不作限制。- i! r! H) W+ [: y( k
功能:着色剂0 P, ? P a+ c% Y& l) T9 {$ V& @
6 U, j; W8 E3 r
TITANIUM DIOXIDE
( _1 h, `+ ^ ~" r; KPrepared at the 67th JECFA (2006) and published in FAO JECFA( A, j/ x( P- k
Monographs 3 (2006), superseding specifications prepared at the 63rd: o5 M1 v6 Q& b
JECFA (2004) and published in FNP 52 Add 12 (2004) and in the
5 Y6 y9 ?+ C( j7 ICombined Compendium of Food Additive Specifications, FAO JECFA
1 D+ n% \' ?6 M! U" b% m% F1 VMonographs 1 (2005). An ADI “not limited” was established at the 13th6 @$ c1 H$ f* {5 a6 R) {
JECFA (1969).- ]. {) F+ c' y& {8 f
SYNONYMS
+ ]* I+ L) F* {9 t9 y( [Titania, CI Pigment white 6, CI (1975) No. 77891, INS No. 1719 o$ O% t5 ~" j; t
DEFINITION
) P3 o; o( V( kTitanium dioxide is produced by either the sulfate or the chloride6 a+ ?( L% O- V4 _' W
process. Processing conditions determine the form (anatase or rutile& d0 x/ Z. c% e$ v
structure) of the final product.( l" V! }" m. L
In the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)
! C+ R, o, T5 W zor ilmenite and titanium slag. After a series of purification steps, the" Q! n9 ~$ p; u- s" S
isolated titanium dioxide is finally washed with water, calcined, and
; l& \3 E5 Z- Pmicronized.! j' q0 i) L1 G4 ^! M
In the chloride process, chlorine gas is reacted with a titaniumcontaining
3 f3 }8 r/ O+ l/ o* @9 T' g8 ~* jmineral under reducing conditions to form anhydrous
7 D# P" ^. @1 K! {4 V& Xtitanium tetrachloride, which is subsequently purified and converted to7 ~" X9 k6 h! s; Z5 U
titanium dioxide either by direct thermal oxidation or by reaction with
7 \2 Y9 j& D8 @steam in the vapour phase. Alternatively, concentrated hydrochloric. r1 |9 k1 w, h/ K
acid can be reacted with the titanium-containing mineral to form a
5 L4 k6 O* b8 P* nsolution of titanium tetrachloride, which is then further purified and
7 S1 u( T# t# |" J# Uconverted to titanium dioxide by hydrolysis. The titanium dioxide is1 F/ L. C1 o, Y, K
filtered, washed, and calcined.
; i6 E4 C4 ~0 x/ M! F' W9 V/ E7 HCommercial titanium dioxide may be coated with small amounts of; u0 P/ I! u) ~, {8 a
alumina and/or silica to improve the technological properties of the
+ r; g( s8 ^3 R2 R. G a- vproduct.6 `; U ?2 z! T3 s
C.A.S. number 13463-67-7' ~8 [ w7 B% @( R. u2 [0 R
Chemical formula TiO2
\( O' t' C* OFormula weight( @/ E# c. ]# l& N
79.88
0 P4 J7 H) ]' o% \Assay/ U5 ~0 I, p0 w
Not less than 99.0% on the dried basis (on an aluminium oxide and- ]# W5 l/ i# ~- I% A9 w+ x f
silicon dioxide-free basis)* ^ t, E( j4 E5 y1 |3 j- ]' |
DESCRIPTION
, X7 C6 H+ h T+ tWhite to slightly coloured powder
) [3 T7 m; o- ]5 xFUNCTIONAL USES% V, D5 O, o8 x% g7 w# { y8 g
Colour: e6 J6 {5 ^, o! U9 J' o
CHARACTERISTICS8 J2 d& G+ B. M0 j1 L4 {
IDENTIFICATION
' b H s/ E# A/ [7 O- @Solubility (Vol. 4) v3 L: \3 a! i& @) ]
Insoluble in water, hydrochloric acid, dilute sulfuric acid, and organic- x$ R5 s4 Y3 m0 A; E, g
solvents. Dissolves slowly in hydrofluoric acid and hot concentrated
* M! k1 X) ~; m4 Gsulfuric acid.1 x6 N" @+ Q/ W) K, m
Colour reaction: j" p% A0 j$ R. s
Add 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of
" s8 n2 C$ ?3 k psulfuric acid appear, then cool. Cautiously dilute to about 100 ml with& n/ F. }% Q$ M2 Z
water and filter. To 5 ml of this clear filtrate, add a few drops of
0 J* ?% s) G. fhydrogen peroxide; an orange-red colour appears immediately., x: W8 ~2 h+ H7 V7 S
PURITY& M6 n1 f. L& q( i9 z% G
Loss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)
; K0 V" h; R2 LLoss on ignition (Vol. 4)% ^1 I- b4 S. P" g0 h: ~
Not more than 1.0% (800o) on the dried basis
1 L( U3 }4 t0 e5 N/ T' RAluminium oxide and/or/ q' q$ h6 T' Q$ e
silicon dioxide H; G4 U* a- c% N
Not more than 2%, either singly or combined
# {; d) W( e5 P" l$ Y, K X9 gSee descriptions under TESTS
- w7 Y6 A5 f3 h- h6 }4 G2 d. ~Acid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing( r6 u3 X! `1 \6 {% f* n
alumina or silica.) ]3 t: ]+ D, ^, u5 _3 X6 @' W
Suspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and
' \! f5 I; p2 }- ?9 h8 e5 t! zplace on a steam bath for 30 min with occasional stirring. Filter
. W8 N f+ a* fthrough a Gooch crucible fitted with a glass fibre filter paper. Wash; g8 j$ c! I2 [4 n# {
with three 10-ml portions of 0.5 N hydrochloric acid, evaporate the
" Y3 j0 p3 w' o, ^) R2 Z9 Icombined filtrate and washings to dryness, and ignite at a dull red4 o, D* i/ ?% e' t' b
heat to constant weight.0 J' \7 P- b" _& @7 s1 q
Water-soluble matter
5 p, Y# A9 a$ U+ x7 a( d3 i(Vol. 4)( I* N9 S' t' T
Not more than 0.5%0 [/ y k* Y0 I0 R6 v1 |
Proceed as directed under acid-soluble substances (above), using( h( [4 j- m" `% a9 M* ?. t1 \
water in place of 0.5 N hydrochloric acid.* j8 x. u" g8 Z
Impurities soluble in 0.5 N/ a) m& v4 n7 W
hydrochloric acid1 h# Y5 q ~: o; R3 c5 s' {! O% E$ [
Antimony Not more than 2 mg/kg* h; u6 I, P- L& f" n
See description under TESTS
4 k; E Y9 U7 q( [& \- E) R( ]- JArsenic Not more than 1 mg/kg& \3 w; T: r- |4 t9 T8 q! N
See description under TESTS
$ d5 T% s I* z# z! \Cadmium Not more than 1 mg/kg7 F/ A2 C/ f% n2 {3 N
See description under TESTS
6 S5 N8 U% @3 C& C1 JLead
/ E: Q9 u% C* b3 H' M3 y# q" _' ANot more than 10 mg/kg; `9 D6 _ w9 k* E( Y$ e! T
See description under TESTS
& o1 \" E b2 u5 u ~1 WMercury (Vol. 4) Not more than 1 mg/kg K% {" s) D2 S2 I4 k
Determine using the cold vapour atomic absorption technique. Select a9 x, t" U. G8 \+ F
sample size appropriate to the specified level# b0 a2 W8 N( }9 t* I8 X
TESTS
6 g( w3 H5 W- M) a; X( t. i8 WPURITY TESTS b, y8 }5 y' @' Y% {( A' d
Impurities soluble in 0.5 N
2 ? T y% p# i0 d: n0 nhydrochloric acid
5 c! D9 P! _ _+ U( m: E3 pAntimony, arsenic,; x/ r6 N/ r8 ?* `% e9 T% K/ g
cadmium and lead
/ Q# k0 ]6 C# E C! T(Vol.4)
7 e5 C9 k3 c. _7 q! O- E4 bTransfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N
3 L' _0 r& t$ X( B4 h0 Phydrochloric acid, cover with a watch glass, and heat to boiling on a2 d$ O; L0 @0 H
hot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml
. L5 q: T$ x9 u' q8 [5 j- Z# kcentrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved
# N0 S2 A! Z. M4 z! X2 @' Amaterial settles. Decant the supernatant extract through a Whatman0 W- w: m- b/ n7 h6 ~. ~
No. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml8 @7 Y/ n7 Q- r4 b \# j, k
volumetric flask and retaining as much as possible of the undissolved6 a$ l! u+ ?4 c: W5 q* C
material in the centrifuge bottle. Add 10 ml of hot water to the original
@- E$ e$ Y9 @- G) G1 Q" \beaker, washing off the watch glass with the water, and pour the0 A/ q" B& ] j
contents into the centrifuge bottle. Form a slurry, using a glass stirring2 t c4 p* ]. z& f
rod, and centrifuge. Decant through the same filter paper, and collect7 }) G. m+ ~2 _1 b% `5 |; d4 y
the washings in the volumetric flask containing the initial extract.
: K& f+ `# Z6 Q; HRepeat the entire washing process two more times. Finally, wash the
8 J$ Y6 t+ \: G. Xfilter paper with 10 to 15 ml of hot water. Cool the contents of the flask
' U3 j" k3 r6 j3 Y6 ?+ ato room temperature, dilute to volume with water, and mix.
9 E2 y1 C' s; i' [; w, z3 w( iDetermine antimony, cadmium, and lead using an AAS/ICP-AES
" S1 L- ?$ v. ^7 ] E4 ]+ ^: ]+ ~- r) htechnique appropriate to the specified level. Determine arsenic using the \7 H4 ~3 M/ y# d4 v9 V
ICP-AES/AAS-hydride technique. Alternatively, determine arsenic using4 S% F: L, L: E
Method II of the Arsenic Limit Test, taking 3 g of the sample rather than
. F& Z# i" K, `1 `' }$ i, f1 g. The selection of sample size and method of sample preparation6 L7 j1 ?: p! n. C1 ], ]1 e
may be based on the principles of the methods described in Volume 4., r' _4 O0 m1 ]
Aluminium oxide Reagents and sample solutions7 N# ?% j1 R: e% T8 Y
0.01 N Zinc Sulfate
$ }' J+ f4 q+ ^1 NDissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to8 ]# _0 l1 ?, u$ c+ V2 P
make 1000 ml. Standardize the solution as follows: Dissolve 500 mg' \. \2 f& D" @
of high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of
! ~' |3 L) }+ m7 u4 dconcentrated hydrochloric acid, heating gently to effect solution, then9 z0 n; v. c) l3 j( [" B7 b# c
transfer the solution into a 1000-ml volumetric flask, dilute to volume
6 V+ i2 u z, X, |9 [2 @with water, and mix. Transfer a 10 ml aliquot of this solution into a 5009 s( x5 q) E( S2 j) a' c4 V
ml Erlenmeyer flask containing 90 ml of water and 3 ml of ?! E. W h- G5 Z0 b+ B
concentrated hydrochloric acid, add 1 drop of methyl orange TS and
1 G/ @; u; k: n9 U$ I1 d25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,
$ ^9 G& t- V8 d8 }9 [dropwise, ammonia solution (1 in 5) until the colour is just completely
& \/ E/ G# v+ Qchanged from red to orange-yellow. Then, add:* g' Z" n1 K7 j5 ?' z9 H
(a): 10 ml of ammonium acetate buffer solution (77 g of [5 ?1 y; @& C* i; B# W
ammonium acetate plus 10 ml of glacial acetic acid, dilute to- B. }8 n# w6 A( w% F7 J
1000 ml with water) and* c$ \8 _0 U6 r! c- \+ ?5 R3 r
(b): 10 ml of diammonium hydrogen phosphate solution (150 g2 q8 m1 L/ x/ u3 L+ M! A/ w
of diammonium hydrogen phosphate in 700 ml of water,7 K$ K# f, {3 E
adjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,
9 {4 T- p3 |# ^9 g2 P! V5 w$ ]- cthen dilute to 1000 ml with water)." M1 ?# @ D0 w% ~3 L) M1 ?
Boil the solution for 5 min, cool it quickly to room temperature in a! `4 G7 q% L& a ^6 I- ~- O
stream of running water, add 3 drops of xylenol orange TS, and mix.
8 I4 W. ?- D7 rUsing the zinc sulfate solution as titrant, titrate the solution to the first
2 e0 V9 |$ O$ U& d0 X6 }yellow-brown or pink end-point colour that persists for 5-10 sec. (Note:
/ i2 i& v$ ]4 j( }/ Y% DThis titration should be performed quickly near the end-point by
- t6 V$ i0 d" A) ?adding rapidly 0.2 ml increments of the titrant until the first colour
+ V1 d0 O5 @) C5 p, L4 tchange occurs; although the colour will fade in 5-10 sec, it is the true
2 H! @/ a6 x0 q/ P: P+ pend-point. Failure to observe the first colour change will result in an. C! i8 R* V9 t S- ^& U
incorrect titration. The fading end-point does not occur at the second
4 Q* a @. D$ z0 @; q8 Vend-point.) i: A( E2 K0 m+ w6 j
Add 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a4 A5 C3 u, C' G" }/ |8 m h
stream of running water. Titrate this solution, using the zinc sulfate
* N1 {( f& D M7 v9 d: Lsolution as titrant, to the same fugitive yellow-brown or pink end-point6 t2 c, F$ Q5 k& B# J: A9 S+ S& ^
as described above.+ |" Y! y% {* e& H
Calculate the titre T of zinc sulfate solution by the formula:
& c& u( a/ ~- r! c8 MT = 18.896 W / V, s9 }! @8 P: o
where
3 d* A8 ~$ \9 GT is the mass (mg) of Al2O3 per ml of zinc sulfate solution: y5 X& G' H% {4 F# I$ c
W is the mass (g) of aluminium wire0 Y' i% m! q1 I/ A0 P
V is the ml of the zinc sulfate solution consumed in the( a0 n6 D8 T' p% @
second titration
) J$ F/ s. W/ t" v18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and
* h! i( P! v; `' x0 D* x/ @R is the ratio of the formula weight of aluminium oxide to
% I- s) M% h F$ \0 hthat of elemental aluminium.
5 |; K1 b4 _9 z$ I0 ]. pSample Solution A, Z+ {% Q. O$ Y9 {1 p" i
Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica
Q, ?* b( s- s; ^6 W* Wglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).8 G! {, i: {* k: Q
(Note: Do not use more sodium bisulfate than specified, as an excess
- e# A! o+ \0 l- V! }. ?9 Rconcentration of salt will interfere with the EDTA titration later on in the% i2 ^6 V! w) ]# H
procedure.) Begin heating the flask at low heat on a hot plate, and
0 [# `: b1 d4 s2 Q3 U7 b5 jthen gradually raise the temperature until full heat is reached.
' y- C+ E2 E1 c/ `9 m(Caution: perform this procedure in a well ventilated area. ) When8 ^( a6 B# q# n( T
spattering has stopped and light fumes of SO3 appear, heat in the full- L! J3 s3 P% R9 u5 q8 U
flame of a Meeker burner, with the flask tilted so that the fusion of the
' q( \! X- |* g9 rsample and sodium bisulfate is concentrated at one end of the flask.- Y! m3 M2 o; o l: X
Swirl constantly until the melt is clear (except for silica content), but) r% {, [0 G# j: B- }" `, _
guard against prolonged heating to avoid precipitation of titanium
7 w+ { J3 n) _8 S! V3 t4 T9 Wdioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until
$ p! E# B$ u9 e; w1 ^) Wthe mass has dissolved and a clear solution results. Cool, and dilute to
- r b* l' r/ X2 o120 ml with water. Introduce a magnetic stir bar into the flask.# i, D$ n+ I' A; D8 k9 w
Sample Solution B
- k" `7 T. n% jPrepare 200 ml of an approximately 6.25 M solution of sodium. J: q5 Y. `$ d7 v
hydroxide. Add 65 ml of this solution to Sample Solution A, while4 [1 I) }! K1 ~6 l
stirring with the magnetic stirrer; pour the remaining 135 ml of the
5 e2 y0 O& r7 j- Z dalkali solution into a 500-ml volumetric flask.
/ H; j- r# \/ |1 D" x3 ]Slowly, with constant stirring, add the sample mixture to the alkali
8 @$ m S1 u1 ysolution in the 500-ml volumetric flask; dilute to volume with water,& Z+ f2 B4 o+ U3 N Q5 b
and mix. (Note: If the procedure is delayed at this point for more than
5 @4 Y0 x# \: _9 |# G) i0 n2 hours, store the contents of the volumetric flask in a polyethylene
" W- W0 x" y' qbottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),
: V# Q) S! ]- E/ B ^* ?then filter the supernatant liquid through a very fine filter paper. Label
" O3 n" J+ \8 N5 j# R1 k' mthe filtrate Sample Solution B.. c* h; @) A; v1 v# `/ ?" I3 P
Sample Solution C
5 G% L n* d( _: j0 V& rTransfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer# P3 m+ @, E# h2 c5 o; i
flask, add 1 drop of methyl orange TS, acidify with hydrochloric acid2 A9 G6 N' u% m. e& O! R+ q
solution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02
/ p6 \) J' n1 y/ f3 G: wM disodium EDTA, and mix. [Note: If the approximate Al2O3 content is
" P& p2 L: e' U" g! Yknown, calculate the optimum volume of EDTA solution to be added
6 C# y5 q/ g8 g: vby the formula: (4 x % Al2O3) + 5.]
) x- n0 o& t! @4 O" TAdd, dropwise, ammonia solution (1 in 5) until the colour is just
, r5 i( Q }6 x& G7 pcompletely changed from red to orange-yellow. Then add10 ml each- y+ L, \4 i4 c
of Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to
1 S# k4 w! {/ `/ o: H" S6 Broom temperature in a stream of running water, add 3 drops of xylenol9 l, B9 |, r9 t' e" N5 D5 ]
orange TS, and mix. If the solution is purple, yellow-brown, or pink,
W: r- _ F c8 h; V/ Jbring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired
5 f( o3 N8 T- `* TpH, a pink colour indicates that not enough of the EDTA solution has0 n0 a% b' h% r
been added, in which case, discard the solution and repeat this
6 T/ f3 O) O+ s+ lprocedure with another 100 ml of Sample Solution B, using 50 ml,9 n- j8 Q7 E* B* o( e9 ~
rather than 25 ml, of 0.02 M disodium EDTA.1 R" J9 `8 C4 q3 P2 E" f
Procedure( m- k) t' O& _5 p
Using the standardized zinc sulfate solution as titrant, titrate Sample
( Z' H' {& G9 y! c, `1 A2 PSolution C to the first yellow-brown or pink end-point that persists for. n# ?9 f- \; V0 s |8 `
5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first0 M/ M5 Y! D" M$ O/ P
titration should require more than 8 ml of titrant, but for more accurate
( ?" `( n+ s5 ?$ x' |work a titration of 10-15 ml is desirable.
) p* R0 G8 D. h( F# q5 U/ U! d( FAdd 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5+ v' T4 y- u3 M8 \/ ]; G0 h
min, and cool in a stream of running water. Titrate this solution, using- f! A6 P3 q. v! {
the standardized zinc sulfate solution as titrant, to the same fugitive
3 n, K2 e% }3 c) ]9 ?/ ]yellow-brown or pink end-point as described above.
1 L0 }2 p s ], z* ^6 hCalculation:; X0 ]+ n/ e) C3 j/ x
Calculate the percentage of aluminium oxide (Al2O3) in the sample3 O+ i5 _8 N! C( K# _
taken by the formula:6 o& F' m: {9 |- q3 B3 o8 W0 A/ u6 q
% Al2O3 = 100 × (0.005VT)/S* u( f3 r) W9 o
where
# h p& J/ D. LV is the number of ml of 0.01 N zinc sulfate consumed in2 H, e/ S! Y' m1 L) t* V+ S
the second titration,
9 e o9 E6 ^6 k7 J3 VT is the titre of the zinc sulfate solution,0 K. o* E! E' |# O
S is the mass (g) of the sample taken, and1 P+ q ^+ e$ q& X8 I8 q
0.005 = 500 ml / (1000mg/g × 100 ml).
' |1 T' {) w; p+ f& G% S% x1 L7 xSilicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica. k7 o } y% F& c9 C" ~
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
9 l; [, @& G7 h: j a$ XHeat gently over a Meeker burner, while swirling the flask, until
: m8 Q: D6 d2 ?0 T' }/ v+ hdecomposition and fusion are complete and the melt is clear, except
n f; ]5 @3 Gfor the silica content, and then cool. (Caution: Do not overheat the0 X5 k+ \& }: d2 `+ d. d: o h- p
contents of the flask at the beginning, and heat cautiously during
: g$ d* V4 D, ^5 Pfusion to avoid spattering.)7 {3 @- t' a1 x* \
To the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat2 r6 V5 t# l4 q9 R& w
carefully and slowly until the melt is dissolved. Cool, and carefully add
! Q8 U S, S! m$ E- H+ P. ^9 Y150 ml of water by pouring very small portions down the sides of the/ _7 p4 a- D" Z! J m
flask, with frequent swirling to avoid over-heating and spattering. Allow& w; ?( ^) Z* v5 f9 D
the contents of the flask to cool, and filter through fine ashless filter
* |1 f% s" h. v- ~1 [) j6 ^paper, using a 60 degree gravity funnel. Rinse out all the silica from
5 J* }; p0 v1 Othe flask onto the filter paper with sulfuric acid solution (1 in 10).
( z2 }# Y! R0 X8 p% ITransfer the filter paper and its contents into a platinum crucible, dry in
( Y ~- U9 S3 l. ran oven at 1200, and heat the partly covered crucible over a Bunsen$ w/ @4 a* a( m! X
burner. To prevent flaming of the filter paper, first heat the cover from
* m' ?4 l0 H7 J, z# ^9 z& }above, and then the crucible from below.; q7 p5 Y1 C: B! {) R% R
When the filter paper is consumed, transfer the crucible to a muffle
$ S7 u0 z& r) k" T( @5 E. Z, `/ ofurnace and ignite at 1000o for 30 min. Cool in a desiccator, and$ V; u# z9 F, Z# J v
weigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated
6 s# M" T1 t$ k4 q; Fhydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first. X9 s, t7 T# U& A8 \
on a low-heat hot plate (to remove the HF) and then over a Bunsen
- Z: y+ H" ^4 wburner (to remove the H2SO4). Take precautions to avoid spattering,
: \0 l8 _4 {5 F, G( y" Oespecially after removal of the HF. Ignite at 1000o for 10 min, cool in a
2 O' L& b. l1 O$ V% R5 d3 Sdesiccator, and weigh again. Record the difference between the two
$ H$ S4 o2 k0 Y% ~$ y6 eweights as the content of SiO2 in the sample.
7 p8 J7 ~6 W" J: E* X1 M+ N6 OMETHOD OF ASSAY$ V4 B+ v+ Z6 E. T. _- ^4 I
Accurately weigh about 150 mg of the sample, previously dried at 105o
3 q" ]' K9 g ufor 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water8 N$ W6 ?2 I* W
and shake until a homogeneous, milky suspension is obtained. Add 30
! L6 r* e& Y2 B! B/ w9 x* dml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially
# {! W* s# q" S! B' s% Xheat gently, then heat strongly until a clear solution is obtained. Cool,+ z4 g# s9 F& c) e* M
then cautiously dilute with 120 ml of water and 40 ml of hydrochloric+ c! j$ H5 d" B, a5 e1 i
acid, and stir. Add 3 g of aluminium metal, and immediately insert a6 H$ S7 R* b4 L v* I' @( m, ]0 l# J
rubber stopper fitted with a U-shaped glass tube while immersing the9 ~; Z, _: W0 p, F: f
other end of the U-tube into a saturated solution of sodium
2 ?- x+ y/ i1 }) y+ P" |2 Gbicarbonate contained in a 500-ml wide-mouth bottle, and generate9 o$ {$ H& K: s2 S4 Z! e
hydrogen. Allow to stand for a few minutes after the aluminium metal
/ m$ P7 U0 o6 ?has dissolved completely to produce a transparent purple solution." c! a% b& Q0 N/ q" r) u P/ @: s; r
Cool to below 50o in running water, and remove the rubber stopper! F/ x6 s; ^; `7 `5 t1 d% C- f; k. f
carrying the U-tube. Add 3 ml of a saturated potassium thiocyanate
8 K: t3 @& a( I9 R jsolution as an indicator, and immediately titrate with 0.2 N ferric
! ]$ I* e% h) z h2 i+ g4 D" u! V% dammonium sulfate until a faint brown colour that persists for 30
/ x0 W/ K' K% Y# a1 `seconds is obtained. Perform a blank determination and make any
8 [" o2 y: A/ n# u% \necessary correction. Each ml of 0.2 N ferric ammonium sulfate is9 [4 V% @* q: N" T7 x! S6 @! d1 f
equivalent to 7.990 mg of TiO2.) z& @1 w' Q6 j" ?
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