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二氧化钛(钛白粉)
二氧化钛(钛白粉)' z& s2 @9 ]4 a2 q
/ I8 W/ T# {2 y) @
JECFA关于二氧化钛(钛白粉)的结论
0 Y3 G- M; c9 e! B7 O5 k3 T
" X; ]% L2 B" E& `+ I. h5 i/ W摘要: 2006年JECFA关于二氧化钛的结论
) _) V- \! _8 Z- J2 a5 pADI值:不作限制。
4 d' W) v1 g$ Q' W* H2 t7 c功能:着色剂* y3 G! M. H& O2 q& r3 l
8 e' l4 @" t' I' a
TITANIUM DIOXIDE
* B; c d6 p- i+ J4 VPrepared at the 67th JECFA (2006) and published in FAO JECFA' j* w6 N* a4 b" W. Y
Monographs 3 (2006), superseding specifications prepared at the 63rd
2 t M, c3 p2 r" y' K. Q+ nJECFA (2004) and published in FNP 52 Add 12 (2004) and in the
7 ]2 g1 h4 m# T: eCombined Compendium of Food Additive Specifications, FAO JECFA
: D& l) R2 M- W/ \Monographs 1 (2005). An ADI “not limited” was established at the 13th
l: h7 E" a1 I& j" a& rJECFA (1969).4 t m# ~/ H% g
SYNONYMS
" R+ u7 g) j2 r+ V) F& JTitania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171. d9 \* u0 V8 }3 Z
DEFINITION
% z! H3 Y; ?1 N/ B/ |( I2 mTitanium dioxide is produced by either the sulfate or the chloride9 p( `2 X: c& z
process. Processing conditions determine the form (anatase or rutile
) n# z6 @8 \+ fstructure) of the final product.7 c" o) _) W% X) N6 _
In the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)0 ~# F0 {9 J1 h! Q j2 ^9 C/ e
or ilmenite and titanium slag. After a series of purification steps, the
$ Y" ?0 ^/ H7 T9 f) b5 e, q! ~isolated titanium dioxide is finally washed with water, calcined, and
7 l8 ~5 i4 _! J* Y0 Emicronized.+ U- n, G% X5 C2 R
In the chloride process, chlorine gas is reacted with a titaniumcontaining/ y% q( j2 H- p1 G! d+ P
mineral under reducing conditions to form anhydrous. W# t; {1 {( m. b3 p
titanium tetrachloride, which is subsequently purified and converted to
) M5 c% l" U4 L' S7 Htitanium dioxide either by direct thermal oxidation or by reaction with; K. q3 G% g, x9 k& f5 r: s
steam in the vapour phase. Alternatively, concentrated hydrochloric
4 r& }8 }# f6 m& b* yacid can be reacted with the titanium-containing mineral to form a0 l! m, p: M1 L) R1 ^1 q( v
solution of titanium tetrachloride, which is then further purified and% J7 ^9 p0 Z. X: Z8 h
converted to titanium dioxide by hydrolysis. The titanium dioxide is
+ h+ r. D! F5 ?9 F+ efiltered, washed, and calcined.
) ]5 Q; I! X2 e2 j1 U+ VCommercial titanium dioxide may be coated with small amounts of- }# }; Z. V! x: S3 a" e
alumina and/or silica to improve the technological properties of the
& i' z$ G7 R! Uproduct.4 P& j l0 ]) B
C.A.S. number 13463-67-7
+ R$ Y( Y0 F+ i9 rChemical formula TiO2
9 Y/ v/ t" n' f; J8 [/ PFormula weight
! O+ H. h0 r5 O2 }79.88
; D: M% T5 E- m; |! g. u' \* kAssay- O. T; t- Q" @) s' c/ Z
Not less than 99.0% on the dried basis (on an aluminium oxide and
! x) t" m& r g% L- k+ x) vsilicon dioxide-free basis)7 [; { ^+ k6 o5 {$ H$ ^! i
DESCRIPTION
0 L" q" Z# F. e8 \- ]: M8 @! YWhite to slightly coloured powder, ^- i% h) |" }- K& H" |
FUNCTIONAL USES
# M) F# m8 T$ }- R1 FColour0 j* L* s, a' f K! _: M1 A8 }
CHARACTERISTICS6 {" x2 L- D# L. E: y1 v: {; U1 m$ [
IDENTIFICATION, g1 Q/ Z# l3 N0 z# {; y
Solubility (Vol. 4)8 z& k# S) y7 u% Z7 A4 b! u% [# ~, t9 ?
Insoluble in water, hydrochloric acid, dilute sulfuric acid, and organic
. E1 s. _& h/ B% v h/ g! h$ Fsolvents. Dissolves slowly in hydrofluoric acid and hot concentrated
5 x$ H6 R E; H, J& ^9 d: [sulfuric acid.! H/ o9 x# |2 p
Colour reaction7 Z3 }7 Z. |/ m+ M) |0 C
Add 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of Z9 B p! ]4 K# d8 G
sulfuric acid appear, then cool. Cautiously dilute to about 100 ml with
/ k+ ~- K" h! r1 d3 mwater and filter. To 5 ml of this clear filtrate, add a few drops of, p' L; a: k9 U5 @
hydrogen peroxide; an orange-red colour appears immediately.! \! @' @6 I# d" N% z- I5 l
PURITY+ A) [# `0 x( Y" T' `1 ]
Loss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)# F- y1 ?9 o- \( A4 ?5 X+ j
Loss on ignition (Vol. 4)
; l4 a% x+ V( q( B Y* r0 }+ }& HNot more than 1.0% (800o) on the dried basis$ }6 e+ `# o: [0 _" m" S4 w2 C& c# n2 a
Aluminium oxide and/or; W, M* J! R$ P4 L
silicon dioxide
: E" h0 V) J( z% c* Z. i/ \Not more than 2%, either singly or combined7 {9 K( v* Q. P5 x4 m
See descriptions under TESTS# L7 E! z1 _3 L
Acid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing
* A) \/ R$ Q, J( D- ~3 y, X6 balumina or silica.& F- C1 o6 _7 h0 X
Suspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and! n6 y( }/ m$ C" G6 D7 N1 t
place on a steam bath for 30 min with occasional stirring. Filter5 |( O& ~' M* l& c
through a Gooch crucible fitted with a glass fibre filter paper. Wash: k6 V# n2 e D- E: M% M0 ~
with three 10-ml portions of 0.5 N hydrochloric acid, evaporate the7 @( s* Y; I2 s1 D T
combined filtrate and washings to dryness, and ignite at a dull red; i" i! h) J$ ~: ^ z8 T: a. C
heat to constant weight.' x) d. h Y, k; A* k5 I+ u8 h
Water-soluble matter8 L) d+ |1 ?6 \. g D
(Vol. 4)
- `3 p) {: l* f7 S) {& [5 SNot more than 0.5%
& c9 J1 J* W kProceed as directed under acid-soluble substances (above), using0 d! i# J. r ~- b$ h
water in place of 0.5 N hydrochloric acid.
( N J1 }. a1 b5 tImpurities soluble in 0.5 N2 K' h( H5 P% e; S
hydrochloric acid
! {8 I% y/ R1 }! a/ CAntimony Not more than 2 mg/kg9 l' j) W, n8 S% [$ m9 l) w
See description under TESTS
1 m; I, F% b1 e1 V: M/ mArsenic Not more than 1 mg/kg2 ]/ u' d6 L; N! C j- y
See description under TESTS
% C+ ]3 M: I( d- Q- L- I" e' ^Cadmium Not more than 1 mg/kg) d( r2 w8 v, h+ N" _
See description under TESTS/ E- n8 J& }! _9 I6 n
Lead5 ?8 [6 k3 q* Z e, l) \ q
Not more than 10 mg/kg
, k& P: U) A; Y3 A( v$ |# \See description under TESTS1 e* p1 b' e$ g7 K* u0 N/ p8 p
Mercury (Vol. 4) Not more than 1 mg/kg. D- ~* h0 e$ s0 ?8 P
Determine using the cold vapour atomic absorption technique. Select a* t$ }2 Z' O; F. A: K6 n. a* V
sample size appropriate to the specified level
: o3 x( t2 S9 |: ~( t6 PTESTS7 z- ` V5 z3 k+ f0 B2 D5 }# V. E
PURITY TESTS4 L/ _" x" _# {& z' G/ Q& B
Impurities soluble in 0.5 N2 z& d! [+ {8 ~4 L% P
hydrochloric acid" V1 n H! |' H x
Antimony, arsenic,
4 a. V& |8 d/ I/ X' w, icadmium and lead
9 V: |0 ^, j2 J% T- [' I(Vol.4)+ v2 A) \2 n4 Y1 y) S
Transfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N3 L% T" @0 ~- C* L6 h
hydrochloric acid, cover with a watch glass, and heat to boiling on a4 L- L8 b6 z& X# s
hot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml& @6 K! b* x$ n7 c3 e- j' ?) a
centrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved. o7 o+ G1 H3 m( u/ N
material settles. Decant the supernatant extract through a Whatman
& |" j9 Q5 H; C. ENo. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml
) q. e( z9 w" Q7 Q9 U3 N) Yvolumetric flask and retaining as much as possible of the undissolved$ E) v" u- q' Q2 E% }3 q" s
material in the centrifuge bottle. Add 10 ml of hot water to the original
# L# F9 ^1 n0 h: e( o9 e V9 ybeaker, washing off the watch glass with the water, and pour the1 Q6 ~/ ]( w1 ^- _- a
contents into the centrifuge bottle. Form a slurry, using a glass stirring
3 a; r( Z& X2 H# z8 h9 _7 \rod, and centrifuge. Decant through the same filter paper, and collect
# {) u E8 o% Q: l+ G N8 {the washings in the volumetric flask containing the initial extract.7 K. ?$ Q' z; |6 J3 L @
Repeat the entire washing process two more times. Finally, wash the
6 O' C0 y4 D7 O7 x& bfilter paper with 10 to 15 ml of hot water. Cool the contents of the flask$ b2 W& F5 Y- A- A, [$ Y
to room temperature, dilute to volume with water, and mix.
( j# a8 \6 |; T( P2 C1 \ BDetermine antimony, cadmium, and lead using an AAS/ICP-AES
H: M" T; Y {/ C" k0 ytechnique appropriate to the specified level. Determine arsenic using the* v* o# S1 E8 t6 ?* V3 c+ w2 q" ]* k
ICP-AES/AAS-hydride technique. Alternatively, determine arsenic using
1 w5 [! f9 c: G/ X: w7 `2 TMethod II of the Arsenic Limit Test, taking 3 g of the sample rather than' t+ |# D" T9 p) ?
1 g. The selection of sample size and method of sample preparation: g" S3 n6 i$ y
may be based on the principles of the methods described in Volume 4.) U) X0 k# m) W) B* F
Aluminium oxide Reagents and sample solutions
9 l& A* X" W9 w6 m0.01 N Zinc Sulfate
/ S, L- x( I j# P- |! Y: VDissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to
& W* p/ j. Q- M, r$ m, ymake 1000 ml. Standardize the solution as follows: Dissolve 500 mg
4 u; ~: \, k& o7 m/ ^' q9 tof high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of+ @; Y6 r4 X3 s6 Q3 j
concentrated hydrochloric acid, heating gently to effect solution, then
3 B4 Q; H6 P3 _transfer the solution into a 1000-ml volumetric flask, dilute to volume }2 C7 B% _7 @: m3 y9 h) L
with water, and mix. Transfer a 10 ml aliquot of this solution into a 500. ?$ b. h2 C0 M' w y4 J
ml Erlenmeyer flask containing 90 ml of water and 3 ml of
; w+ J5 |# Y( W3 P7 ^, A# h# Lconcentrated hydrochloric acid, add 1 drop of methyl orange TS and! h3 Q0 F( G4 l; j: o
25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add, u, r1 W. P# r& M1 f5 z
dropwise, ammonia solution (1 in 5) until the colour is just completely, K; \& p' I$ H6 w8 L/ h+ }& y
changed from red to orange-yellow. Then, add:3 B1 o3 O$ }; u n2 _
(a): 10 ml of ammonium acetate buffer solution (77 g of0 M6 E4 U9 S2 ]/ d7 X0 G$ y
ammonium acetate plus 10 ml of glacial acetic acid, dilute to7 M, G, I4 e: K7 U- Y
1000 ml with water) and
5 _ ^& R: r1 j; O0 X(b): 10 ml of diammonium hydrogen phosphate solution (150 g0 \& E+ A! g* n9 C' k
of diammonium hydrogen phosphate in 700 ml of water,
{( q& H& p0 z# oadjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,* z4 X# \6 }5 {4 y9 H5 A( G# p
then dilute to 1000 ml with water).. m, Z( G$ `* x' Q% J
Boil the solution for 5 min, cool it quickly to room temperature in a
; Z# U \# `* N- Estream of running water, add 3 drops of xylenol orange TS, and mix.
* H* _ `5 ^8 ]Using the zinc sulfate solution as titrant, titrate the solution to the first a# P3 u; n+ i/ T2 }
yellow-brown or pink end-point colour that persists for 5-10 sec. (Note:
: O( t" W6 u. x. X# vThis titration should be performed quickly near the end-point by" [4 @$ ^5 t9 R1 B! O$ C- R8 y4 l
adding rapidly 0.2 ml increments of the titrant until the first colour
% e8 F0 E# ~8 x$ f+ f' Wchange occurs; although the colour will fade in 5-10 sec, it is the true
- b8 X8 V& h% {5 \# Kend-point. Failure to observe the first colour change will result in an" j# \& C7 I$ `8 ^ C9 |
incorrect titration. The fading end-point does not occur at the second
) b' G8 X; V1 v/ fend-point.)
7 b; E: T S+ _Add 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a7 M6 Z* u# {0 I& R! k
stream of running water. Titrate this solution, using the zinc sulfate5 u; R9 _6 `- u* J8 m/ M
solution as titrant, to the same fugitive yellow-brown or pink end-point5 i0 {( ~4 A& B% X% m
as described above./ _ k3 D0 T7 W H \- Q
Calculate the titre T of zinc sulfate solution by the formula:- i ^1 }1 ]; \5 Z( u! d5 I8 {
T = 18.896 W / V! e" Y, M; O, ^" [9 N. M2 u
where* | b) e3 B, y6 W7 Y; F
T is the mass (mg) of Al2O3 per ml of zinc sulfate solution% @8 g, i* @# a+ a1 O
W is the mass (g) of aluminium wire! X' Z2 Y5 V' V8 q% U, H' T
V is the ml of the zinc sulfate solution consumed in the! r3 l& i) ~; `# }6 n2 {4 V d5 v- C
second titration" q8 k( y- M b6 E" l! z
18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and
4 ]/ @+ m2 O& V ER is the ratio of the formula weight of aluminium oxide to
2 p4 W# a* ?8 g# `4 c8 H- G r2 athat of elemental aluminium.
7 p* H3 Y6 o4 ISample Solution A
/ w+ e: i. c7 r8 t- o R0 b/ X. mAccurately weigh 1 g of the sample and transfer to a 250-ml high-silica
& J3 |6 f+ H- }! P8 q3 ]3 yglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
- P6 g0 n; ` V# O2 o' n(Note: Do not use more sodium bisulfate than specified, as an excess* W' n( v/ g& d, P: ^
concentration of salt will interfere with the EDTA titration later on in the
3 q; b: L) j5 g( ^; dprocedure.) Begin heating the flask at low heat on a hot plate, and
8 {( P% {! O$ ?0 t6 _) sthen gradually raise the temperature until full heat is reached.8 |4 r" M/ c. n( h4 Q1 c# D3 d
(Caution: perform this procedure in a well ventilated area. ) When
6 b8 g: s# C8 `spattering has stopped and light fumes of SO3 appear, heat in the full, ^1 ~/ M" [8 Z& N
flame of a Meeker burner, with the flask tilted so that the fusion of the
: f( T# j* O. u$ V# X( H( }5 Ysample and sodium bisulfate is concentrated at one end of the flask.
, I) w( P& X! xSwirl constantly until the melt is clear (except for silica content), but
i8 a& U, L4 e$ Gguard against prolonged heating to avoid precipitation of titanium* M* r, c' j9 V2 M! R
dioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until
! a! x( b1 Y: ^8 }# j" |the mass has dissolved and a clear solution results. Cool, and dilute to: m) C# K) W. u" a" _- I
120 ml with water. Introduce a magnetic stir bar into the flask.
7 m6 g l; t8 YSample Solution B. N7 h" E, l1 |/ o! h
Prepare 200 ml of an approximately 6.25 M solution of sodium8 ^; V! T3 G: W1 W D3 e% |- U) v
hydroxide. Add 65 ml of this solution to Sample Solution A, while0 J3 T/ O& C2 S/ ?5 ]1 B/ k. }
stirring with the magnetic stirrer; pour the remaining 135 ml of the. J. @4 M: v7 E/ m3 |/ K3 E* d" Q0 h
alkali solution into a 500-ml volumetric flask.9 _* R# o; g9 K* f7 l& S3 E
Slowly, with constant stirring, add the sample mixture to the alkali1 H* x4 f* `- Q+ g4 ?4 r8 ^
solution in the 500-ml volumetric flask; dilute to volume with water,4 D. _% _9 K% [+ ~
and mix. (Note: If the procedure is delayed at this point for more than& P1 w, J' w' w" J8 K' w
2 hours, store the contents of the volumetric flask in a polyethylene* X, S1 u7 e8 S: w$ _* v" L
bottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),
- v! v n) Q. K3 s* V& M0 K/ Rthen filter the supernatant liquid through a very fine filter paper. Label
9 y! F! q; }; L# c$ ]' ^) D7 uthe filtrate Sample Solution B.
6 Z/ S5 |% h6 N/ o" V$ SSample Solution C
% s! K! \$ x8 X& GTransfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer
) m5 A# K: \* [9 ]* H* d& Kflask, add 1 drop of methyl orange TS, acidify with hydrochloric acid6 s6 \9 N# }' W' o
solution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02
2 n( k( z1 r5 T5 s8 [M disodium EDTA, and mix. [Note: If the approximate Al2O3 content is
1 o4 S0 }3 G% v, E9 G) ^known, calculate the optimum volume of EDTA solution to be added, u2 s: q# s: W: @
by the formula: (4 x % Al2O3) + 5.]
. h( _' F6 f2 \Add, dropwise, ammonia solution (1 in 5) until the colour is just T' _# z( R3 W* L
completely changed from red to orange-yellow. Then add10 ml each% u# M" s+ q% ~- \( t: b
of Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to
& L$ r9 r |% @room temperature in a stream of running water, add 3 drops of xylenol9 u7 g, {- y$ e' |1 A: v j: D
orange TS, and mix. If the solution is purple, yellow-brown, or pink,! t" R# E' H) e3 e4 o& m0 k
bring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired: _3 ^& W9 ~; Z! |" p' |0 T
pH, a pink colour indicates that not enough of the EDTA solution has9 A/ K0 n3 E) i0 q' |
been added, in which case, discard the solution and repeat this
& j: y+ k/ _! j4 |6 C9 V: |4 k# eprocedure with another 100 ml of Sample Solution B, using 50 ml,% Y4 ^1 ]8 i0 n0 t2 h, `# D
rather than 25 ml, of 0.02 M disodium EDTA.) Q7 b# ?' W- z+ u
Procedure
( p* h2 V. {- K8 w/ p `Using the standardized zinc sulfate solution as titrant, titrate Sample
9 h$ q6 T! E6 O1 ^/ x0 @, GSolution C to the first yellow-brown or pink end-point that persists for* G& j" l* |8 s0 W& d/ g
5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first
: |' s: b3 Z) t) `titration should require more than 8 ml of titrant, but for more accurate
c' C3 ~+ d% Z$ ]# Gwork a titration of 10-15 ml is desirable.
5 y; q2 x8 V+ ^. v' vAdd 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5! x& a# ~, E: r% _1 F* F
min, and cool in a stream of running water. Titrate this solution, using4 T& e5 M6 J$ q7 M# X; _' d
the standardized zinc sulfate solution as titrant, to the same fugitive
% Z# u2 U! t8 P3 N& @. O( Oyellow-brown or pink end-point as described above.
- B5 X1 I8 [/ X" `/ \& R* XCalculation:3 S' }: p% O( Y/ N+ x* D; o
Calculate the percentage of aluminium oxide (Al2O3) in the sample
& P2 ]% g p* f. L9 Otaken by the formula:
1 Y6 }3 i5 Z. O9 J; [% u% Al2O3 = 100 × (0.005VT)/S7 [5 J0 d2 i c9 E5 Q) N+ x" J& \7 ?
where9 U$ U1 R1 F0 G5 U% u
V is the number of ml of 0.01 N zinc sulfate consumed in; U: K: k' S2 \4 g
the second titration,! D- @6 p# X Q
T is the titre of the zinc sulfate solution,$ x) B/ l7 H1 ?8 K% K) H) ?8 z
S is the mass (g) of the sample taken, and
" E. _2 f* \, f0.005 = 500 ml / (1000mg/g × 100 ml).
0 t' Z3 O6 x) M1 iSilicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica0 U; L2 W( i/ Q2 |3 ]
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).$ I( @+ y/ J1 r% ]
Heat gently over a Meeker burner, while swirling the flask, until- @8 J8 X0 L" M6 J# C, @
decomposition and fusion are complete and the melt is clear, except
7 s3 |$ j- \- h$ l1 f0 Q4 {for the silica content, and then cool. (Caution: Do not overheat the$ g' j! _( i' N7 M
contents of the flask at the beginning, and heat cautiously during
* q% P$ h0 ?: [$ g( k g+ Ffusion to avoid spattering.)
- g% ~" \; {; D Y8 vTo the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat" U1 y, y b8 c: _! _, O
carefully and slowly until the melt is dissolved. Cool, and carefully add
# w6 A' Y6 ~2 _150 ml of water by pouring very small portions down the sides of the
& X+ W9 m3 }( P- v2 Z9 s8 ~( V. K/ vflask, with frequent swirling to avoid over-heating and spattering. Allow& m/ K* v$ F+ h2 S' `* s, l( r) r
the contents of the flask to cool, and filter through fine ashless filter
* r4 G: Q" X+ |/ Bpaper, using a 60 degree gravity funnel. Rinse out all the silica from8 ]' T$ Q# C+ f4 g' q' H
the flask onto the filter paper with sulfuric acid solution (1 in 10).) Q/ U9 P& |/ C5 g4 I' H
Transfer the filter paper and its contents into a platinum crucible, dry in
' b4 g6 Q: S) Ran oven at 1200, and heat the partly covered crucible over a Bunsen' g' G. V- k2 b, i2 o. V9 E
burner. To prevent flaming of the filter paper, first heat the cover from
6 x3 b: u9 q# T6 G+ {2 ?above, and then the crucible from below.9 D5 V7 W z8 g3 d( P" T7 m. ]" g5 Z
When the filter paper is consumed, transfer the crucible to a muffle4 V* A7 J+ ^1 b, v0 z
furnace and ignite at 1000o for 30 min. Cool in a desiccator, and! ~- H) K4 _- i# ?# P9 j
weigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated
8 m' \1 v# a( `& c7 Yhydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first
2 \. r' q( n/ ^, Mon a low-heat hot plate (to remove the HF) and then over a Bunsen
7 z" o6 o" {' k4 yburner (to remove the H2SO4). Take precautions to avoid spattering,
6 o# w" P3 U+ Z& x0 T) tespecially after removal of the HF. Ignite at 1000o for 10 min, cool in a* E6 s* I5 b0 Z0 [
desiccator, and weigh again. Record the difference between the two
$ X: ?2 N/ }8 v! w$ tweights as the content of SiO2 in the sample.6 R, Q. w7 j. W, l0 P
METHOD OF ASSAY5 C& Y E# |+ j, H+ i- T
Accurately weigh about 150 mg of the sample, previously dried at 105o
" M' r( Y2 ~: I0 D! Efor 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water
0 H! T! u0 [1 D9 H$ ~6 |. Rand shake until a homogeneous, milky suspension is obtained. Add 30
4 O" j) j; I4 Z! l# o" dml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially
# p7 ^ {3 u5 _* ~# { Iheat gently, then heat strongly until a clear solution is obtained. Cool,/ }1 }% c! _8 C. Y; \
then cautiously dilute with 120 ml of water and 40 ml of hydrochloric- H+ \0 b2 S% e6 g/ u+ B5 G
acid, and stir. Add 3 g of aluminium metal, and immediately insert a
j; M' Z7 F" K, g1 Y' @* B Krubber stopper fitted with a U-shaped glass tube while immersing the4 X" W# m4 H* j
other end of the U-tube into a saturated solution of sodium
# f! Z" G) x% y6 h+ `# _bicarbonate contained in a 500-ml wide-mouth bottle, and generate8 J; X. W$ `. ^% R- w
hydrogen. Allow to stand for a few minutes after the aluminium metal0 J. B6 W N8 X3 s: y
has dissolved completely to produce a transparent purple solution.
3 K/ C9 G8 o7 yCool to below 50o in running water, and remove the rubber stopper
7 P3 [/ j% o+ X; a% ucarrying the U-tube. Add 3 ml of a saturated potassium thiocyanate
! k: N" t8 A/ z, \) Csolution as an indicator, and immediately titrate with 0.2 N ferric
9 {- T8 K* ~& k! @& E* X# z Fammonium sulfate until a faint brown colour that persists for 30
% ^+ z) R; X1 ?/ X$ y1 }# K1 Iseconds is obtained. Perform a blank determination and make any0 b' W% \* p; o7 n, D
necessary correction. Each ml of 0.2 N ferric ammonium sulfate is0 q$ m; n& ]8 Q8 ?
equivalent to 7.990 mg of TiO2./ F5 F1 Y8 r1 ]( D- k
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