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二氧化钛(钛白粉)
二氧化钛(钛白粉)
* m2 B. G8 n: Q# d. x: {/ a; m
e' j9 \2 B2 O: M7 n/ Y! Z$ `JECFA关于二氧化钛(钛白粉)的结论
& @, G3 r: x x3 X; N, f) x+ z) v) {/ b+ z: |
摘要: 2006年JECFA关于二氧化钛的结论
5 a% B6 H8 v6 \. z9 N" J5 W2 ?ADI值:不作限制。1 K3 s* s1 O( n! t
功能:着色剂
$ \! z1 `& x& S; s1 h g& n. O, Q& Q0 O( H6 T& ~2 _
TITANIUM DIOXIDE6 @ O9 \% ~ W0 w# k; d
Prepared at the 67th JECFA (2006) and published in FAO JECFA
- A& F$ ]% }; z g( y9 f7 X" DMonographs 3 (2006), superseding specifications prepared at the 63rd) E _1 @3 X) P% g/ R& }) ~
JECFA (2004) and published in FNP 52 Add 12 (2004) and in the+ r! |* R2 P4 l- A
Combined Compendium of Food Additive Specifications, FAO JECFA
# f/ A1 A1 T, {* ?6 a" xMonographs 1 (2005). An ADI “not limited” was established at the 13th
2 `0 [2 r y* e/ lJECFA (1969).. L* P, \( Q! z5 A) v
SYNONYMS
# K! S; Z' @7 [/ w( \Titania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171
& h, b0 L# a2 k# N( l% K: ~" ODEFINITION% R- ]8 {+ X7 x
Titanium dioxide is produced by either the sulfate or the chloride
7 j5 D6 q5 v5 t. q0 uprocess. Processing conditions determine the form (anatase or rutile
4 T& N4 X6 f4 r$ N0 E$ Cstructure) of the final product.
& A6 v# c) a k/ L) n* t- IIn the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)! X H. V/ M r3 S' u; J
or ilmenite and titanium slag. After a series of purification steps, the/ V( i2 s5 o: n! n
isolated titanium dioxide is finally washed with water, calcined, and
+ b+ T8 o6 I E3 j7 hmicronized.5 g% x6 j& W! \ i" o
In the chloride process, chlorine gas is reacted with a titaniumcontaining
6 B7 D) e% {+ `: s) n" gmineral under reducing conditions to form anhydrous
Z7 i' k* g. b5 u* dtitanium tetrachloride, which is subsequently purified and converted to
: S2 |- C6 r) p- a$ F% ~titanium dioxide either by direct thermal oxidation or by reaction with2 o g3 j9 H- d4 q( G
steam in the vapour phase. Alternatively, concentrated hydrochloric- o( w4 R# I( ^) r- `% g
acid can be reacted with the titanium-containing mineral to form a
7 C. {$ W# ^+ E2 |+ Isolution of titanium tetrachloride, which is then further purified and
/ h, x: A& _9 E, S* U4 C& qconverted to titanium dioxide by hydrolysis. The titanium dioxide is
, y! v; {: d8 Y& E; O: ?filtered, washed, and calcined.4 A: r) ]/ O# @( b+ U
Commercial titanium dioxide may be coated with small amounts of% ]4 D/ M9 k8 I- `8 M1 T/ t+ F0 M. g3 Y
alumina and/or silica to improve the technological properties of the
+ B# ?5 q# [2 \3 o# [+ l" ~product.
& u @) ~5 U! b/ R3 j+ t6 S" gC.A.S. number 13463-67-7: F8 |8 F" x& O, m- R& p
Chemical formula TiO2+ t4 ~1 C. U& V e' l; r* F
Formula weight
7 I$ o, |1 Y0 S7 _79.88$ K1 z' H, m9 n- C2 G( ]& Q N
Assay
, G( V- H, \) Y+ Z5 _9 c' V9 BNot less than 99.0% on the dried basis (on an aluminium oxide and
" n" q( \4 j, K6 Esilicon dioxide-free basis)
) z1 J7 F7 F0 p l% \DESCRIPTION- b) u* R6 K* J8 p o7 ~2 z! J
White to slightly coloured powder; u+ ?. m8 D- D+ |' g. t) a
FUNCTIONAL USES
2 @+ K; ?5 ]4 gColour) l4 N" l. d/ l$ O# a1 U
CHARACTERISTICS
! l' y% T. y3 @ \' K3 ` U7 B8 aIDENTIFICATION
$ J" {. L' m! z: O8 o$ }Solubility (Vol. 4)* V W: J' B1 m, u
Insoluble in water, hydrochloric acid, dilute sulfuric acid, and organic* ~/ X. M' x7 }/ p Q7 [
solvents. Dissolves slowly in hydrofluoric acid and hot concentrated0 ~( k# ?. ~! v( M
sulfuric acid.
; D$ t* v, U6 c/ bColour reaction
% q) n( Y0 F D4 Q+ OAdd 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of- N1 ?* E( K7 {* n
sulfuric acid appear, then cool. Cautiously dilute to about 100 ml with
- y0 G. `, D6 V! P, fwater and filter. To 5 ml of this clear filtrate, add a few drops of- T" }! x: ?0 c. Q3 r
hydrogen peroxide; an orange-red colour appears immediately.
. y. N2 y: @6 n+ F% B: j) HPURITY
8 I! D# Z" F, ^5 H5 RLoss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)0 N& m4 a8 i: Z5 R: B8 `
Loss on ignition (Vol. 4)
+ [4 k& P: y1 U$ M D3 NNot more than 1.0% (800o) on the dried basis" B; V; _9 O H
Aluminium oxide and/or2 R, G/ r: r2 H
silicon dioxide
# ?6 o4 S a7 M1 ^ j! N" Q% {Not more than 2%, either singly or combined
* J2 _$ E2 K1 `& c- L( d3 \See descriptions under TESTS
; A: q! `( W, dAcid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing
; V7 m: b, Y$ Y! l0 ualumina or silica.
+ ?* x% D/ t: sSuspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and
; y! S0 A8 `9 t" L+ a6 oplace on a steam bath for 30 min with occasional stirring. Filter, Q- o3 ?# f5 F7 ?+ A* s |, y1 I8 G
through a Gooch crucible fitted with a glass fibre filter paper. Wash# H& y% t- `2 g
with three 10-ml portions of 0.5 N hydrochloric acid, evaporate the) z7 e/ j' b- T( \
combined filtrate and washings to dryness, and ignite at a dull red
1 T! w0 P0 Y. i; s. N0 H3 a, w4 ~. \( F8 wheat to constant weight.
) X' _- q6 ?% U) hWater-soluble matter8 d& b7 E9 c3 \( N
(Vol. 4)
, m6 Z4 X. k5 q6 @3 _% W0 jNot more than 0.5%/ t/ `9 V" w' J M; w' J
Proceed as directed under acid-soluble substances (above), using
& i" y5 s7 G# n+ l7 L D8 {water in place of 0.5 N hydrochloric acid.+ M$ ?3 ]( P# h9 f7 w( e1 A
Impurities soluble in 0.5 N. @9 {# |* b* E0 |
hydrochloric acid
6 {8 C% Z) ]+ K0 n' c$ u0 PAntimony Not more than 2 mg/kg% w4 R$ }9 F0 |+ I# n
See description under TESTS4 ?$ K8 N: Q1 S: l$ t' p! n
Arsenic Not more than 1 mg/kg
8 i( r0 ~- o$ |) f( Y& D W3 B- zSee description under TESTS
+ S7 N) i, B( \0 R6 m9 ^Cadmium Not more than 1 mg/kg
( c$ {# v3 x( F. I4 f! \& y; g t* T+ iSee description under TESTS
' S9 k# b m c3 _Lead
- p8 e4 R% m$ K5 z+ qNot more than 10 mg/kg/ A0 R$ p) f J2 o, h
See description under TESTS
& R7 d: Q8 b# z6 t( gMercury (Vol. 4) Not more than 1 mg/kg
3 x8 b y0 R( G2 U) k. XDetermine using the cold vapour atomic absorption technique. Select a h- u; } ?" ]. z$ l# S( ~6 v _$ h' w* s
sample size appropriate to the specified level, r# f, y, D' P
TESTS
* z J( }$ G: G# Y$ Q# hPURITY TESTS& e" I+ W$ x2 a: @4 D
Impurities soluble in 0.5 N
3 u6 Y" u6 J4 n6 S$ ohydrochloric acid
. I: c4 U+ d" m# w; JAntimony, arsenic,8 {, x, j6 t9 w+ ?. l
cadmium and lead
; J5 b3 A( g; N H- c(Vol.4)
% G- _! F" b, P* H9 ]) U" G1 |( R6 MTransfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N
6 f$ K; n8 o7 M' u6 q* }7 o) lhydrochloric acid, cover with a watch glass, and heat to boiling on a
2 K7 a" S3 J" h- g+ R0 B! Nhot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml; f! d1 V& P0 a. f( T, ?" N
centrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved
% L+ Q6 n& z; M9 `# Amaterial settles. Decant the supernatant extract through a Whatman
; `- E; }; `. |2 m; i& \1 z+ qNo. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml6 w2 a% y& I' F! D
volumetric flask and retaining as much as possible of the undissolved
; O0 i, P+ o4 E6 Cmaterial in the centrifuge bottle. Add 10 ml of hot water to the original
* L, L# W y3 Pbeaker, washing off the watch glass with the water, and pour the
. d* U% d( {/ \# Rcontents into the centrifuge bottle. Form a slurry, using a glass stirring5 x- d8 `0 }# {! B6 [# v
rod, and centrifuge. Decant through the same filter paper, and collect
" [& X8 g: i: W [the washings in the volumetric flask containing the initial extract.
4 ^% o F- P/ k+ y" HRepeat the entire washing process two more times. Finally, wash the P0 }6 }, s% r6 }
filter paper with 10 to 15 ml of hot water. Cool the contents of the flask
" G; M# L( Y! x3 xto room temperature, dilute to volume with water, and mix.
! i$ \/ k4 S% D1 V; H8 D8 QDetermine antimony, cadmium, and lead using an AAS/ICP-AES2 L- {: W% }: v" [8 M# x; Z
technique appropriate to the specified level. Determine arsenic using the
" l* @5 W8 K l: ~ICP-AES/AAS-hydride technique. Alternatively, determine arsenic using* p/ y m% L$ M7 H
Method II of the Arsenic Limit Test, taking 3 g of the sample rather than
F, G* k6 Q: Y1 g. The selection of sample size and method of sample preparation
. g9 Y7 s3 R8 t. Y% R8 Pmay be based on the principles of the methods described in Volume 4.; H3 h N; @: t# q- o! b
Aluminium oxide Reagents and sample solutions
" V: Y) A# ]# C# l0.01 N Zinc Sulfate9 j( O* e7 q, ~/ m" b
Dissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to8 Y; Y; |3 P3 M5 V
make 1000 ml. Standardize the solution as follows: Dissolve 500 mg2 }! E) Y8 V) u B( E
of high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of9 ^ u0 U! W. W
concentrated hydrochloric acid, heating gently to effect solution, then
& ?) @$ M7 }# G& r( b% t, C: E7 btransfer the solution into a 1000-ml volumetric flask, dilute to volume2 y2 C8 M% g; v7 t% J9 K; x
with water, and mix. Transfer a 10 ml aliquot of this solution into a 500( L" t7 S) ^$ u- E& I
ml Erlenmeyer flask containing 90 ml of water and 3 ml of3 ?; T; {9 W1 S. v
concentrated hydrochloric acid, add 1 drop of methyl orange TS and
& W: }/ r; }$ U+ ?& A25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,
/ j+ u- f& {, B5 M/ ]dropwise, ammonia solution (1 in 5) until the colour is just completely# y2 v3 |7 i% k* R0 B6 h' u
changed from red to orange-yellow. Then, add:
$ r8 H# m1 C3 u) E, c* ~4 k(a): 10 ml of ammonium acetate buffer solution (77 g of
& G: u7 M! Y7 }7 Y3 z& [( ~ammonium acetate plus 10 ml of glacial acetic acid, dilute to
, e: T; t( `& ]$ T) ^7 \1000 ml with water) and( J( D. I( s% y; j
(b): 10 ml of diammonium hydrogen phosphate solution (150 g4 v: L E- D8 N( g5 k/ U
of diammonium hydrogen phosphate in 700 ml of water,
5 l7 J, N, ? y: ]; gadjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,
/ d% R" I8 Q9 { A# k" y' {3 w6 rthen dilute to 1000 ml with water).8 W- z4 c* X) S
Boil the solution for 5 min, cool it quickly to room temperature in a; p, @ r) `7 R% ]+ X b
stream of running water, add 3 drops of xylenol orange TS, and mix.
' G$ z) J7 U# n* w6 FUsing the zinc sulfate solution as titrant, titrate the solution to the first
! o* v5 _+ |) O; j4 `1 {! Gyellow-brown or pink end-point colour that persists for 5-10 sec. (Note:7 w6 T6 S9 J* U
This titration should be performed quickly near the end-point by/ q) B) H. S# r0 ^
adding rapidly 0.2 ml increments of the titrant until the first colour+ F& s3 E! ]0 b# p- `4 N& R$ v
change occurs; although the colour will fade in 5-10 sec, it is the true
: R- s4 A& o( J: L+ e; `3 pend-point. Failure to observe the first colour change will result in an* c4 e% A, c# Y( X' M0 c' g
incorrect titration. The fading end-point does not occur at the second
. j5 }8 S5 H& w6 {end-point.)) Q/ G- q# S) w
Add 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a2 ~# K; f: @6 O9 W( ~
stream of running water. Titrate this solution, using the zinc sulfate& R- _0 F2 ^- `: k
solution as titrant, to the same fugitive yellow-brown or pink end-point
: S' P. ~4 g* n" M' k2 A9 Zas described above.; l* f" v6 L5 t- G3 V! J- P
Calculate the titre T of zinc sulfate solution by the formula:- x; `1 O$ T+ P z" J* m$ z
T = 18.896 W / V
; _1 z# U% v8 i4 f- S- Y$ fwhere7 H/ p$ j6 q: z0 ~8 O/ f- T
T is the mass (mg) of Al2O3 per ml of zinc sulfate solution
E+ I8 x1 s7 G7 G6 }W is the mass (g) of aluminium wire
! P' t# w$ S+ }$ j4 `2 EV is the ml of the zinc sulfate solution consumed in the
% a+ s- o( y2 U6 Nsecond titration2 [, |, |" J6 h! N' C
18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and+ n5 A" Z' j- w y/ @# ~
R is the ratio of the formula weight of aluminium oxide to
) U3 Y- \9 i: }& Mthat of elemental aluminium.+ r# V0 {8 k0 \, B' r X) c
Sample Solution A9 B# l5 J ^* I/ U N5 t
Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica
w7 l* p/ R/ Q1 B$ \1 w& ?glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O). C8 Z- s+ G! O. U0 i
(Note: Do not use more sodium bisulfate than specified, as an excess
+ E$ p; z/ G* h8 n8 [$ ~ n' w. ~! }concentration of salt will interfere with the EDTA titration later on in the6 W. O+ l+ `0 D I
procedure.) Begin heating the flask at low heat on a hot plate, and" x* t( h% {2 L1 f: T$ ~( E! h
then gradually raise the temperature until full heat is reached.
, D4 Y4 _& G |8 L4 l9 D(Caution: perform this procedure in a well ventilated area. ) When
/ o. q N: v6 E& H' {& Gspattering has stopped and light fumes of SO3 appear, heat in the full
/ I _/ @: R- N: q1 r: _4 [flame of a Meeker burner, with the flask tilted so that the fusion of the. ^; M: f9 T6 ^' S1 m
sample and sodium bisulfate is concentrated at one end of the flask.
/ j' u8 m9 F. `Swirl constantly until the melt is clear (except for silica content), but
$ V, c( g* F- b; Zguard against prolonged heating to avoid precipitation of titanium
6 t2 G5 Q: r6 o# ndioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until
5 J3 [" a1 B' `+ S+ nthe mass has dissolved and a clear solution results. Cool, and dilute to q- j+ {3 u; e- c
120 ml with water. Introduce a magnetic stir bar into the flask.+ `1 L3 Z a$ \4 u" t; `" i
Sample Solution B. r2 A( b$ }( Q6 K' H! p9 z8 Q
Prepare 200 ml of an approximately 6.25 M solution of sodium4 U0 y f. L0 J4 y2 v* E# d
hydroxide. Add 65 ml of this solution to Sample Solution A, while
. _, a% J1 M. v6 Pstirring with the magnetic stirrer; pour the remaining 135 ml of the# S, L; P; H) X) m
alkali solution into a 500-ml volumetric flask.5 o3 E/ @: r4 y* V( x
Slowly, with constant stirring, add the sample mixture to the alkali
* Z0 n3 S( t; w4 k+ w, S! usolution in the 500-ml volumetric flask; dilute to volume with water, X3 k! Y% Y. g ^ n0 l
and mix. (Note: If the procedure is delayed at this point for more than" c! J0 }( `' k6 X W- M* [5 P- j
2 hours, store the contents of the volumetric flask in a polyethylene
+ l7 x( ~& ]; R8 Mbottle.) Allow most of the precipitate to settle (or centrifuge for 5 min), F+ B( {: P" @5 C V k. m# Z: v
then filter the supernatant liquid through a very fine filter paper. Label
' X! L, u5 G1 V& o0 B! e, v4 Fthe filtrate Sample Solution B.
' [; M }0 Z6 z3 O. P* _: L9 }Sample Solution C/ m1 N! {! d2 M8 k& v1 c5 q2 c
Transfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer
% d) @4 |9 v B; G/ Aflask, add 1 drop of methyl orange TS, acidify with hydrochloric acid
. {6 W- m( G: jsolution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02
0 S1 ^2 @% g3 q2 X2 k; EM disodium EDTA, and mix. [Note: If the approximate Al2O3 content is
- }0 P% N8 G6 U. Z8 ~known, calculate the optimum volume of EDTA solution to be added
6 Q, W* r" y# Dby the formula: (4 x % Al2O3) + 5.]
7 u& ^9 e; N0 J$ ~# u# L5 |Add, dropwise, ammonia solution (1 in 5) until the colour is just ]! ~& C* B5 e9 C
completely changed from red to orange-yellow. Then add10 ml each% [9 l% `' y- Y. g) y; `
of Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to
/ v, t# b7 J. J6 _$ h& M6 kroom temperature in a stream of running water, add 3 drops of xylenol9 ?2 v# V* m$ z' K2 |
orange TS, and mix. If the solution is purple, yellow-brown, or pink,
4 ?" P& U1 j3 h4 Z, Abring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired
0 B( \+ d8 r6 y, Z8 P. C/ PpH, a pink colour indicates that not enough of the EDTA solution has. p5 ~0 n3 T( Y& G. g8 A x& \
been added, in which case, discard the solution and repeat this; f7 \6 Y. I9 d& o
procedure with another 100 ml of Sample Solution B, using 50 ml,1 j2 [9 W& J9 k) o
rather than 25 ml, of 0.02 M disodium EDTA.. K) h9 v) z; W9 U
Procedure7 H+ q5 E- s0 [$ e8 ]/ w. Y
Using the standardized zinc sulfate solution as titrant, titrate Sample
$ S2 |% y/ s. P6 USolution C to the first yellow-brown or pink end-point that persists for4 h" u$ b4 X; ~4 j2 v# }5 n
5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first2 N. B. g! k6 x! Q4 j
titration should require more than 8 ml of titrant, but for more accurate
5 e, r9 V) f. y. } m5 Pwork a titration of 10-15 ml is desirable.
! L$ G& h8 k) {5 w) ZAdd 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5" v! s6 Q/ b- l* u" ?
min, and cool in a stream of running water. Titrate this solution, using1 h* q. ^3 S+ N4 p8 b( L
the standardized zinc sulfate solution as titrant, to the same fugitive z/ ~! k E* t. v* O
yellow-brown or pink end-point as described above.
6 l+ D! Z* f- \( |4 j0 ~5 y* L8 |5 qCalculation:
, q# r- q! e } F T1 iCalculate the percentage of aluminium oxide (Al2O3) in the sample8 k! ^( n: T7 K m# d
taken by the formula:
. M1 v' x" \/ O5 ^" e( Y% Al2O3 = 100 × (0.005VT)/S
/ U* L) j( p7 a# H+ bwhere* ^# k5 G% A8 `) i+ V* ^
V is the number of ml of 0.01 N zinc sulfate consumed in
6 j! q) t' h% H' w( P6 Zthe second titration,& y+ y9 |1 }: `, G P* Y
T is the titre of the zinc sulfate solution,( p9 k# j. j7 q" B% U3 x0 X
S is the mass (g) of the sample taken, and
: c, z% y! Y2 _# P4 R+ k0.005 = 500 ml / (1000mg/g × 100 ml).9 F: k- j, F5 `
Silicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica# @3 j+ M; f7 i- H- i
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).1 B, \& q% |- t$ N: i
Heat gently over a Meeker burner, while swirling the flask, until! m7 m8 y! H8 ~ M
decomposition and fusion are complete and the melt is clear, except( c$ I3 o3 J4 v
for the silica content, and then cool. (Caution: Do not overheat the, j# m: ^" K( @# D- a, k# T
contents of the flask at the beginning, and heat cautiously during
' s; L, d2 Z$ ~' \7 [4 a( kfusion to avoid spattering.)1 N/ m* E8 z& ^3 ^' C3 m9 |
To the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat7 a. q, _# p. t# ^( B/ l' F! e6 p. D( y
carefully and slowly until the melt is dissolved. Cool, and carefully add
8 \& ^! \4 U2 B- C4 _ i150 ml of water by pouring very small portions down the sides of the# G: T/ h- F6 K9 V) M/ T
flask, with frequent swirling to avoid over-heating and spattering. Allow
* v* @5 `3 B: N0 uthe contents of the flask to cool, and filter through fine ashless filter: A6 ~7 J2 ?& R9 \7 M( S; l
paper, using a 60 degree gravity funnel. Rinse out all the silica from; {6 z6 o' \3 H% H) w
the flask onto the filter paper with sulfuric acid solution (1 in 10).& W$ _4 S/ {3 F
Transfer the filter paper and its contents into a platinum crucible, dry in1 s( e9 j* L# H& v. R
an oven at 1200, and heat the partly covered crucible over a Bunsen" Z4 _/ q& ~" }6 M! T
burner. To prevent flaming of the filter paper, first heat the cover from
# `/ S: b. g8 ?9 h+ {. P* G* zabove, and then the crucible from below.! Q: i( H- b1 o, B5 h" V
When the filter paper is consumed, transfer the crucible to a muffle
# L8 g! |7 }! Y; Bfurnace and ignite at 1000o for 30 min. Cool in a desiccator, and0 u! S- X8 H" ]) O
weigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated
- W$ _" Q9 l- X! a6 t! thydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first: a @6 p3 P$ U. N' r5 _. F1 v
on a low-heat hot plate (to remove the HF) and then over a Bunsen
* C1 k2 a% I; w! y: [* qburner (to remove the H2SO4). Take precautions to avoid spattering,8 d, L% e' z* @! j0 m' T* r
especially after removal of the HF. Ignite at 1000o for 10 min, cool in a
; G: K4 c! z" E; N; ]7 \desiccator, and weigh again. Record the difference between the two9 n' A o# d) l1 ], `
weights as the content of SiO2 in the sample.
4 e ~7 b. G! e3 tMETHOD OF ASSAY
a' u% A# ?& W/ J" E) W# KAccurately weigh about 150 mg of the sample, previously dried at 105o H1 F/ J9 G4 y" G
for 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water
( ^9 n9 U0 c! Q" P. Kand shake until a homogeneous, milky suspension is obtained. Add 30% H l& F; D* Y2 w
ml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially; p# z& C& B/ a
heat gently, then heat strongly until a clear solution is obtained. Cool, M0 C W2 D, ^+ x/ z
then cautiously dilute with 120 ml of water and 40 ml of hydrochloric5 ]6 w \- \ b# T0 g. k# s. K
acid, and stir. Add 3 g of aluminium metal, and immediately insert a
7 J" o, I, Z* k2 C2 g6 k+ Z, P, _rubber stopper fitted with a U-shaped glass tube while immersing the2 {% _: L3 k+ ^1 r6 d4 v3 C
other end of the U-tube into a saturated solution of sodium
% |+ Y* Q o" N$ bbicarbonate contained in a 500-ml wide-mouth bottle, and generate
; O0 [ f& c. u# ]" x' L& Nhydrogen. Allow to stand for a few minutes after the aluminium metal
6 V& v. V R4 a6 q. q/ ^has dissolved completely to produce a transparent purple solution. Y+ w8 m w8 N* ?" F- K3 E
Cool to below 50o in running water, and remove the rubber stopper
! {5 g9 B% S4 S. ?carrying the U-tube. Add 3 ml of a saturated potassium thiocyanate
; I! s, v$ K, N% @5 b! \2 Asolution as an indicator, and immediately titrate with 0.2 N ferric
4 ~) i. O" s1 Gammonium sulfate until a faint brown colour that persists for 30
) ?5 D! g: q$ sseconds is obtained. Perform a blank determination and make any
) L2 }& j; @4 j0 T vnecessary correction. Each ml of 0.2 N ferric ammonium sulfate is
s+ s+ o( Z" p- sequivalent to 7.990 mg of TiO2.
/ j* m5 w( N" d |
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