|
沙发

楼主 |
发表于 2008-5-23 12:10:00
|
只看该作者
二氧化钛(钛白粉)
二氧化钛(钛白粉)8 Z- b) b/ D. W& T% I
0 m) u# D( M: @ H5 rJECFA关于二氧化钛(钛白粉)的结论
# N+ t* `+ [# A8 y9 G) `' z& H5 n: u) ?' a; M
摘要: 2006年JECFA关于二氧化钛的结论
" y% G# `% }+ [. F7 G% C5 w) N+ o# aADI值:不作限制。
8 a& |+ E/ v" w) Q% Y功能:着色剂" C$ n+ t5 j3 E4 E) ]
1 I& A- Q; j0 n! Z" k5 gTITANIUM DIOXIDE+ S. I8 J7 ]2 ~- ]( M' T+ U
Prepared at the 67th JECFA (2006) and published in FAO JECFA% a( {) }7 M6 ^* h) B
Monographs 3 (2006), superseding specifications prepared at the 63rd
% M# i# M0 k" Y) W$ _JECFA (2004) and published in FNP 52 Add 12 (2004) and in the U% `) l- C1 J$ |0 k
Combined Compendium of Food Additive Specifications, FAO JECFA
1 D* C8 E( Z E% b$ N2 ~Monographs 1 (2005). An ADI “not limited” was established at the 13th
9 B) t g8 p5 C6 z# ~) ?; BJECFA (1969).
2 V- o# n1 }; r' U: eSYNONYMS. @3 d9 N* ^+ C, s' A' y3 z6 V
Titania, CI Pigment white 6, CI (1975) No. 77891, INS No. 1718 c( g1 |6 x& c7 W8 H
DEFINITION$ u4 Q. B; O" I' N. f5 v, Y- d1 P
Titanium dioxide is produced by either the sulfate or the chloride6 \7 G* b+ Z0 C S1 y s
process. Processing conditions determine the form (anatase or rutile+ x- i# j4 M( }# g4 |
structure) of the final product.
9 X& H" F$ k, N& m) hIn the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)# _: i* T4 F$ r# f
or ilmenite and titanium slag. After a series of purification steps, the5 z9 W/ _* {! x
isolated titanium dioxide is finally washed with water, calcined, and
5 ?/ o3 \- i8 X2 {1 imicronized.
" F. d f9 ?' b8 ^In the chloride process, chlorine gas is reacted with a titaniumcontaining. b6 d" d7 @9 s/ y/ [) a1 }7 L
mineral under reducing conditions to form anhydrous
! Q, F- H8 h2 J* x& z) D1 r3 Q2 l- q0 Ctitanium tetrachloride, which is subsequently purified and converted to: Y* u1 o, k; s5 G( j3 B8 b; r1 O" b
titanium dioxide either by direct thermal oxidation or by reaction with8 h4 z B! p" \
steam in the vapour phase. Alternatively, concentrated hydrochloric
7 e' I( W, V+ r! ?* e0 X! }) F! Wacid can be reacted with the titanium-containing mineral to form a C; ]! K/ r' p# V( J2 G O" X5 ~8 v
solution of titanium tetrachloride, which is then further purified and
9 p6 D8 x) g$ gconverted to titanium dioxide by hydrolysis. The titanium dioxide is
7 W" G' g' ]; [7 W; @$ t8 rfiltered, washed, and calcined.
' ]* R8 D9 c% x) z( TCommercial titanium dioxide may be coated with small amounts of6 ^& P8 o5 I C& g$ V( A$ W
alumina and/or silica to improve the technological properties of the
' q4 d0 |% s* R+ Oproduct.
5 C4 K/ M# Y: |6 U% f# T8 rC.A.S. number 13463-67-7& C( d( d) ?3 `1 O" i
Chemical formula TiO29 [4 @5 a* D5 u3 |, C4 W5 ~" V* V
Formula weight
8 f+ D( v( G( S: a; u7 L H79.88( M, Y( p" O" v! c: w4 g# g3 s* R
Assay) I% ?- h! L. m2 @4 y
Not less than 99.0% on the dried basis (on an aluminium oxide and
: M7 j" l _. asilicon dioxide-free basis)
9 ~, H. i% {5 q y7 @3 S+ i5 yDESCRIPTION
4 k, r( P! \7 O# j+ {1 dWhite to slightly coloured powder$ [" e2 a! V8 G" X* \
FUNCTIONAL USES% ^- G" c+ t! F ?. {) O
Colour! G; l! |! x7 |0 S4 m
CHARACTERISTICS
5 ?" ^9 |% S6 Z& H/ K2 [0 H5 C% yIDENTIFICATION% C4 u' c$ m6 [/ P' \ O# k! b9 S( T2 D
Solubility (Vol. 4)) [% J0 W8 F: O5 q3 O2 L$ h
Insoluble in water, hydrochloric acid, dilute sulfuric acid, and organic
5 N; N" }$ j/ k, H, \solvents. Dissolves slowly in hydrofluoric acid and hot concentrated, T( O* b( p4 m3 Y+ \
sulfuric acid.! }/ k0 @" T7 [) e4 [0 B& N
Colour reaction
E4 F7 Y! C8 d% g& AAdd 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of, d, X. y3 @& P; w1 ~
sulfuric acid appear, then cool. Cautiously dilute to about 100 ml with
" `& K; A6 o" n) _7 pwater and filter. To 5 ml of this clear filtrate, add a few drops of
; q- m# Q0 A1 b4 x: S" T, Dhydrogen peroxide; an orange-red colour appears immediately.
- y2 Q$ h( B" {: R1 A7 @PURITY: w0 w/ A( P! V* \$ W5 ?
Loss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)
6 h) f( C) G5 m3 jLoss on ignition (Vol. 4)
2 D( G {; O% L3 y+ KNot more than 1.0% (800o) on the dried basis
: V! R5 K% h2 h FAluminium oxide and/or; M* h) W/ F& b) e1 s7 ]$ l8 g
silicon dioxide
, V' E* l5 Z' C/ ~6 {! @8 K; CNot more than 2%, either singly or combined6 Y6 o. d+ F7 S% u, M6 M3 c
See descriptions under TESTS
" `% z4 q( J4 V6 X; j0 bAcid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing
+ b, c3 P' e) B9 l+ galumina or silica.
a4 Y! k. M2 ]+ |; ISuspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and
4 n' T. D, P. ?: I1 `3 _; splace on a steam bath for 30 min with occasional stirring. Filter
. H Y6 {& t7 b: d! x4 Rthrough a Gooch crucible fitted with a glass fibre filter paper. Wash
6 l! p! X: v" J8 H' B# F$ Pwith three 10-ml portions of 0.5 N hydrochloric acid, evaporate the
' X! W) @3 u5 i8 Hcombined filtrate and washings to dryness, and ignite at a dull red
0 r' _( }2 l2 X y) gheat to constant weight.
4 x; n3 l: Z# g3 P( kWater-soluble matter
( J; k- B, A% d9 g) H8 P9 J0 ^% t(Vol. 4)
1 d- S# q6 v6 D: d. Q; G! L4 O$ }Not more than 0.5% k/ F7 \$ w4 E, o; A% O t
Proceed as directed under acid-soluble substances (above), using
2 D5 B5 O& w% f* A3 r( X. dwater in place of 0.5 N hydrochloric acid.* k2 x: }- Z1 k F9 b6 r# w
Impurities soluble in 0.5 N
7 _6 X, F0 h; g; Lhydrochloric acid0 \$ J. c: L& U' M4 B- V0 u
Antimony Not more than 2 mg/kg7 }, e9 O, U3 ~1 h
See description under TESTS; I0 g( G7 N/ r% d$ B
Arsenic Not more than 1 mg/kg% K# A5 K+ {8 b. j& y( g2 J) Q
See description under TESTS s9 B5 Z0 s h, P: A- c
Cadmium Not more than 1 mg/kg
3 v# \/ b/ Z- S/ _! ^/ e$ DSee description under TESTS; P1 U9 Y9 U4 V( p1 f
Lead
! w7 @7 L8 a) f! B6 v) ONot more than 10 mg/kg2 r4 m" y% {2 R; m1 G' v/ f
See description under TESTS
$ {3 k: |; |4 L" I; M5 e/ ]* `- vMercury (Vol. 4) Not more than 1 mg/kg9 ` f( H- q: k N
Determine using the cold vapour atomic absorption technique. Select a$ q0 S4 D9 L1 K" b; p
sample size appropriate to the specified level7 Q8 W# X) h; J# b
TESTS+ F9 I B3 N% _ G
PURITY TESTS5 b1 W# o4 V0 p/ s! M& i" `
Impurities soluble in 0.5 N- Q# z6 w+ r4 z0 ?1 ]
hydrochloric acid4 L3 q5 `/ h+ ^* U
Antimony, arsenic,
6 Q. k Y9 w7 mcadmium and lead
. l0 I! `7 F; x(Vol.4)
7 |. s7 H2 L& k8 N; f: aTransfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N
$ y$ W! W% k3 h$ yhydrochloric acid, cover with a watch glass, and heat to boiling on a
7 V2 s7 i; r' z1 q' Z- K" ehot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml
8 a* M9 \; [) V6 Q) M2 S/ n' Qcentrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved
. f+ X9 M5 x2 @4 z: h% Tmaterial settles. Decant the supernatant extract through a Whatman
5 |& }) [! Y, a: U- u9 @No. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml' m( O: r* G; s
volumetric flask and retaining as much as possible of the undissolved+ T- r& Y, O, ~9 ~( v: t$ K: b5 T' j: i
material in the centrifuge bottle. Add 10 ml of hot water to the original
; P2 O) m$ k; ?4 q' cbeaker, washing off the watch glass with the water, and pour the
# U8 k1 S- s0 J q5 Zcontents into the centrifuge bottle. Form a slurry, using a glass stirring
" h) y: A' U3 O/ z$ trod, and centrifuge. Decant through the same filter paper, and collect
- H2 g# M; Q7 y# h( c6 e; wthe washings in the volumetric flask containing the initial extract.% ^5 u6 B* Q& o) b/ }0 e- }
Repeat the entire washing process two more times. Finally, wash the$ J- h" l5 ]5 a! l( R" M, T* J
filter paper with 10 to 15 ml of hot water. Cool the contents of the flask
. U; v- v0 R9 z$ `1 z# e7 {0 ^( C2 f9 sto room temperature, dilute to volume with water, and mix.) ?- x4 z) V% t: Z) c6 H
Determine antimony, cadmium, and lead using an AAS/ICP-AES# [2 P! x$ q2 n9 q; e
technique appropriate to the specified level. Determine arsenic using the7 U3 D5 @! r+ j
ICP-AES/AAS-hydride technique. Alternatively, determine arsenic using
. a6 B. [7 {2 h8 J; w$ V2 l4 XMethod II of the Arsenic Limit Test, taking 3 g of the sample rather than+ M5 @" G- g+ ^: x0 W5 C$ G
1 g. The selection of sample size and method of sample preparation
' R1 A+ l q0 X' K5 ^7 j' W8 a; tmay be based on the principles of the methods described in Volume 4.
+ D* ^8 ~# e2 P4 L+ QAluminium oxide Reagents and sample solutions- i+ _# K ^9 R: Y. k. M7 ?& R4 Z
0.01 N Zinc Sulfate D1 d+ e" P! @
Dissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to
% i5 l8 w+ ~7 Emake 1000 ml. Standardize the solution as follows: Dissolve 500 mg2 o8 P" a- B0 F* v; w
of high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of$ o( E- X9 h& {
concentrated hydrochloric acid, heating gently to effect solution, then' H! {( o/ ~$ Q$ r2 H$ q+ G
transfer the solution into a 1000-ml volumetric flask, dilute to volume2 _( f( q* K8 n4 u2 N
with water, and mix. Transfer a 10 ml aliquot of this solution into a 5003 ?* b3 l Y; H9 d& S
ml Erlenmeyer flask containing 90 ml of water and 3 ml of
. f2 q$ `* a! Xconcentrated hydrochloric acid, add 1 drop of methyl orange TS and
+ n9 o1 @$ \" k5 R6 e: _. P4 m; u* w6 m25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,
Q; V) |3 V3 G) G( \1 ydropwise, ammonia solution (1 in 5) until the colour is just completely* J Q B# {4 ~, E8 ~8 n# M; m& B# G: `
changed from red to orange-yellow. Then, add:
$ S5 Z3 t- Z+ J3 \5 W(a): 10 ml of ammonium acetate buffer solution (77 g of
% V$ ^/ u" s5 Rammonium acetate plus 10 ml of glacial acetic acid, dilute to& J$ ^* _" O% O, `, C" {
1000 ml with water) and
9 i" W# `' q$ T$ Z/ V) X(b): 10 ml of diammonium hydrogen phosphate solution (150 g* U3 B. h7 X: C9 K0 u) p; K! u5 U
of diammonium hydrogen phosphate in 700 ml of water,* N' h+ v9 C; r# x% {+ ^7 h
adjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,
7 x( b) w: L! X. ^then dilute to 1000 ml with water).! O- @+ s k/ T) I; Z( f
Boil the solution for 5 min, cool it quickly to room temperature in a
, s* O6 e. z+ [# ?* q ^stream of running water, add 3 drops of xylenol orange TS, and mix.
3 M, l! s5 o7 T! ]" |% G$ b/ C1 E9 C: uUsing the zinc sulfate solution as titrant, titrate the solution to the first
3 P( ~: c5 V* ^* C- Z" n" Fyellow-brown or pink end-point colour that persists for 5-10 sec. (Note:8 s; y' E% ?$ l$ b0 `7 K
This titration should be performed quickly near the end-point by4 `# r9 m7 c- ^ P. b) G+ P
adding rapidly 0.2 ml increments of the titrant until the first colour
6 t/ p0 j z; h% Ochange occurs; although the colour will fade in 5-10 sec, it is the true
" T. T# o |8 q9 } r% C8 Rend-point. Failure to observe the first colour change will result in an
$ U1 M7 S! g1 e. u$ [incorrect titration. The fading end-point does not occur at the second
& P j% Q- j. p* ^' }end-point.)3 _6 o2 w& s- _7 s
Add 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a4 _3 K/ s n: L3 q, ?4 `! i
stream of running water. Titrate this solution, using the zinc sulfate
/ B1 H. h, X% k) W) Q8 o) l: Dsolution as titrant, to the same fugitive yellow-brown or pink end-point
5 Y( h e2 t6 d/ @as described above.
" @) }! t5 O7 K6 g/ S. GCalculate the titre T of zinc sulfate solution by the formula:5 e Q& o6 c' I# w" n* B) w; j
T = 18.896 W / V
* {1 x* I. b) ], m% Nwhere9 h3 Z' n( m, S4 b. j5 T5 M
T is the mass (mg) of Al2O3 per ml of zinc sulfate solution3 \( v8 R M5 k$ ` q4 v8 T
W is the mass (g) of aluminium wire' P* I6 J @/ s, w) \) v
V is the ml of the zinc sulfate solution consumed in the
2 X* j) P! H+ O( S+ B- psecond titration
4 _. w2 ]; v8 Q. F' G: _18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and
, h$ r4 w9 f! k: iR is the ratio of the formula weight of aluminium oxide to5 w6 E2 g/ t: g% J% u
that of elemental aluminium.2 C3 N+ w$ e% t" m% C
Sample Solution A# y5 g0 n3 W7 b @/ d0 F
Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica$ B. y" Z# v' e3 e5 L0 }2 r
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
?, Z: d! o: Y9 y: [(Note: Do not use more sodium bisulfate than specified, as an excess
" v: E/ O5 t" A! Gconcentration of salt will interfere with the EDTA titration later on in the
, S" s3 g) G eprocedure.) Begin heating the flask at low heat on a hot plate, and
9 [7 ~6 P5 ]9 r7 g7 n- jthen gradually raise the temperature until full heat is reached.
4 j4 l5 x& L5 ^0 V: r! h. q5 E" ?(Caution: perform this procedure in a well ventilated area. ) When9 C* d- J3 W- j9 g6 K. Y! z/ h
spattering has stopped and light fumes of SO3 appear, heat in the full% Z5 l. z# a l& K5 e
flame of a Meeker burner, with the flask tilted so that the fusion of the/ l$ i9 ^+ K5 {. A; P
sample and sodium bisulfate is concentrated at one end of the flask.! [5 e# @& d. y! W b
Swirl constantly until the melt is clear (except for silica content), but
9 T e6 g5 Y6 J. V7 p9 Cguard against prolonged heating to avoid precipitation of titanium
( N' Y! Q1 ?6 Q# |. p6 Ddioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until
1 Z' ^' r; a3 _0 {the mass has dissolved and a clear solution results. Cool, and dilute to: s- A, o4 H" p& O
120 ml with water. Introduce a magnetic stir bar into the flask.
" |1 s2 W; B; z) R- @1 KSample Solution B
: Z3 t& k3 K$ V% APrepare 200 ml of an approximately 6.25 M solution of sodium
$ x5 m4 k, F* Y, n m" ~8 Whydroxide. Add 65 ml of this solution to Sample Solution A, while, U3 p, f! t2 r0 E \; x
stirring with the magnetic stirrer; pour the remaining 135 ml of the
7 W/ A: ?( F P6 v& [alkali solution into a 500-ml volumetric flask., q9 d) J( _2 [3 u* ]
Slowly, with constant stirring, add the sample mixture to the alkali
: X: s! m$ U9 zsolution in the 500-ml volumetric flask; dilute to volume with water,
7 e- t+ Q- p7 m _and mix. (Note: If the procedure is delayed at this point for more than( B( Z0 a) R: s1 w1 s
2 hours, store the contents of the volumetric flask in a polyethylene
7 U: ?! c8 y* p* t* l7 `% @bottle.) Allow most of the precipitate to settle (or centrifuge for 5 min), ~1 d& Y8 n: J N0 m
then filter the supernatant liquid through a very fine filter paper. Label; o/ e# l0 A6 c; g) U
the filtrate Sample Solution B.. ^/ U, e+ `7 T7 S3 S4 f
Sample Solution C
0 b; w' n2 | Y8 aTransfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer3 ~: O; v. G& O
flask, add 1 drop of methyl orange TS, acidify with hydrochloric acid
' f7 N* m; U# |, I$ i% h: osolution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02$ H' \- {: C9 I- p6 f& s
M disodium EDTA, and mix. [Note: If the approximate Al2O3 content is
9 d7 J6 y6 i: P* Cknown, calculate the optimum volume of EDTA solution to be added# r+ C/ h7 y! U; S
by the formula: (4 x % Al2O3) + 5.]% D* v# ]9 b$ M
Add, dropwise, ammonia solution (1 in 5) until the colour is just& `, s# G0 R* d5 {" H# h7 E
completely changed from red to orange-yellow. Then add10 ml each" F+ L; s. v( m; u* M* z, `/ a
of Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to, h3 R; J9 ^9 C2 ~% ]& i6 E6 k
room temperature in a stream of running water, add 3 drops of xylenol T) p* f% A2 K3 Y( V1 N
orange TS, and mix. If the solution is purple, yellow-brown, or pink,! j2 Y: ~' @5 t+ k! |& d
bring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired
1 w* q4 } h' K1 o6 ?pH, a pink colour indicates that not enough of the EDTA solution has- M9 ~7 N2 g7 i$ S& v4 f3 v
been added, in which case, discard the solution and repeat this2 X4 h- H+ H& n' y
procedure with another 100 ml of Sample Solution B, using 50 ml,' r; n: j J/ m* r& p
rather than 25 ml, of 0.02 M disodium EDTA.
! l4 x2 w$ ^0 p: rProcedure
1 L9 y5 @1 O$ q, \Using the standardized zinc sulfate solution as titrant, titrate Sample
c! g+ e5 M# E" o4 }Solution C to the first yellow-brown or pink end-point that persists for4 f2 F& A) y7 P; ^( s( i6 Z/ u9 c; ?
5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first
6 c/ F! u4 T1 u; h. T# s8 Btitration should require more than 8 ml of titrant, but for more accurate7 a* H3 ?$ Z A# p$ s5 f7 j2 s- u9 c
work a titration of 10-15 ml is desirable.
! X: _ A# }/ zAdd 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5 h5 ~, u% D- N# x; s% c
min, and cool in a stream of running water. Titrate this solution, using
/ w: ?2 S0 x. `' l4 Dthe standardized zinc sulfate solution as titrant, to the same fugitive: w* k E$ u6 y* _- ?5 a4 h
yellow-brown or pink end-point as described above.6 G0 D- I9 ?% y! ]. s
Calculation:( I0 A! H1 O# y5 n2 `& q
Calculate the percentage of aluminium oxide (Al2O3) in the sample/ R) a1 T% P! `, S
taken by the formula:
5 K6 z" l' V a" V0 u, }0 U; v% Al2O3 = 100 × (0.005VT)/S& j8 ~: ~ J" E" l# T1 X
where8 V& t$ @4 \4 u& b7 }' q. r
V is the number of ml of 0.01 N zinc sulfate consumed in, y. c' }1 j1 o2 E
the second titration,
3 P: ?6 d" P9 O- VT is the titre of the zinc sulfate solution,
2 ] f& H% u$ S+ V; D. y. s+ t0 D# TS is the mass (g) of the sample taken, and" ?$ K+ B5 x8 g0 s- l. }
0.005 = 500 ml / (1000mg/g × 100 ml).
/ w1 k8 w# D, ?' ]# ~+ n% e( C0 vSilicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica$ Q$ B7 @, x/ S
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
& |7 x9 G5 x! Q4 aHeat gently over a Meeker burner, while swirling the flask, until$ ?6 W& Y' e3 j
decomposition and fusion are complete and the melt is clear, except
3 [5 S4 G: R. f( n Tfor the silica content, and then cool. (Caution: Do not overheat the) ?$ c1 `1 `9 E9 @9 I ~4 `- q }( Q
contents of the flask at the beginning, and heat cautiously during* s- F" B/ {- d/ z3 }
fusion to avoid spattering.)9 u! p9 N" j6 s
To the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat
: E- H, J+ ]# X4 x! {carefully and slowly until the melt is dissolved. Cool, and carefully add' \3 N7 [ r& I* U! W8 z
150 ml of water by pouring very small portions down the sides of the* I q5 H/ K. |7 ~* }5 Z
flask, with frequent swirling to avoid over-heating and spattering. Allow
% T( g. a- u1 G, V* Ithe contents of the flask to cool, and filter through fine ashless filter
4 _1 r$ S0 B9 Z- ?1 b" apaper, using a 60 degree gravity funnel. Rinse out all the silica from
7 d/ o* n X- p$ N+ X8 W# w cthe flask onto the filter paper with sulfuric acid solution (1 in 10).
, K) O7 J0 Z) |1 W5 C: v1 bTransfer the filter paper and its contents into a platinum crucible, dry in
0 @/ @ {9 [8 @" N4 s2 T5 D) D* y) Yan oven at 1200, and heat the partly covered crucible over a Bunsen0 k, {$ S! ?1 N' V- L
burner. To prevent flaming of the filter paper, first heat the cover from0 |3 w4 _3 f& H
above, and then the crucible from below.# v, g. _' C! d# f" h; Z
When the filter paper is consumed, transfer the crucible to a muffle; u" V# j9 x3 [. ]$ A- _
furnace and ignite at 1000o for 30 min. Cool in a desiccator, and1 S- i7 f7 t% M; ~( R! M; z
weigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated3 z2 a. |1 ?. m0 w
hydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first7 I m% G: y3 N/ |" K, C
on a low-heat hot plate (to remove the HF) and then over a Bunsen
; E2 r% a- v, V9 c1 r; Nburner (to remove the H2SO4). Take precautions to avoid spattering,6 p0 M, M* X9 D3 }* N6 r5 K
especially after removal of the HF. Ignite at 1000o for 10 min, cool in a
' j! z. `8 y9 x4 \desiccator, and weigh again. Record the difference between the two: r4 C" i5 p3 u6 Q1 A* W x/ N
weights as the content of SiO2 in the sample.1 O/ E0 M9 R8 L- R0 d/ O! x
METHOD OF ASSAY T& J( l, G- M8 N7 b. l0 X) x
Accurately weigh about 150 mg of the sample, previously dried at 105o
: C7 `9 w' L+ K! ~: rfor 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water# I8 S) _# u4 e& H
and shake until a homogeneous, milky suspension is obtained. Add 30
! r% @9 l3 R0 Z" g: [ml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially
- y4 q2 H: V$ W3 C( Iheat gently, then heat strongly until a clear solution is obtained. Cool,( X" p* J5 z" N6 y7 @. |8 Q
then cautiously dilute with 120 ml of water and 40 ml of hydrochloric0 G) s, b$ ]" t6 q
acid, and stir. Add 3 g of aluminium metal, and immediately insert a# W% r& A* @, s+ p
rubber stopper fitted with a U-shaped glass tube while immersing the: r8 t5 Y1 d4 d
other end of the U-tube into a saturated solution of sodium
6 X# i. n1 y+ N% k0 U/ ]3 a/ A$ Gbicarbonate contained in a 500-ml wide-mouth bottle, and generate
1 k6 ]4 ^; t/ x3 Yhydrogen. Allow to stand for a few minutes after the aluminium metal
4 W2 ^: U: x; p/ Ahas dissolved completely to produce a transparent purple solution.
, |3 i/ u( _) {Cool to below 50o in running water, and remove the rubber stopper+ t0 c; y& d8 {% k2 n
carrying the U-tube. Add 3 ml of a saturated potassium thiocyanate& c' F- E p# h$ D& b
solution as an indicator, and immediately titrate with 0.2 N ferric( P" @7 m( t' D$ R' ^
ammonium sulfate until a faint brown colour that persists for 30
s. F0 }* O0 w/ ^" bseconds is obtained. Perform a blank determination and make any0 T& c/ _! U' S) o* W4 [
necessary correction. Each ml of 0.2 N ferric ammonium sulfate is9 R" j+ b: `7 S0 Y2 G
equivalent to 7.990 mg of TiO2.* D: s9 o3 C; u' I
|
|