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二氧化钛(钛白粉)
二氧化钛(钛白粉)
( U" f! [( J/ D" R1 g6 ~9 ^) q8 t+ U
JECFA关于二氧化钛(钛白粉)的结论" o1 r, H# }# Q/ T
3 Z- ]% H- `( _5 l1 J( X3 S$ o" X摘要: 2006年JECFA关于二氧化钛的结论
9 M: V- n+ h6 I" hADI值:不作限制。
7 n# K) z/ _. u5 l1 ?功能:着色剂
* S! `& w* M7 N" h C. Z% k* b1 a8 w( K3 ^) Z
TITANIUM DIOXIDE
- q* ]' g N* s/ }4 lPrepared at the 67th JECFA (2006) and published in FAO JECFA
' C0 s/ h) v0 S* R0 Y& a6 V8 SMonographs 3 (2006), superseding specifications prepared at the 63rd9 T4 X) r/ |1 B$ y7 K$ S5 i5 ?0 F! g
JECFA (2004) and published in FNP 52 Add 12 (2004) and in the1 |5 P2 P9 `* f
Combined Compendium of Food Additive Specifications, FAO JECFA' d, `: \ _8 w; q
Monographs 1 (2005). An ADI “not limited” was established at the 13th' s5 n2 }2 Z* q3 v- |0 B
JECFA (1969).1 Y7 B6 @6 L# O/ G% Q
SYNONYMS9 G( \; |8 {3 s8 `3 f
Titania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171: B3 {! d% e* F, h1 d
DEFINITION
7 O1 T d0 f$ r* Q1 bTitanium dioxide is produced by either the sulfate or the chloride0 ^9 F) E' D l9 u
process. Processing conditions determine the form (anatase or rutile* @) c& k& X2 ~; C* R
structure) of the final product.
- N) _9 P- {8 J8 z zIn the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)% g9 g" D% T2 t
or ilmenite and titanium slag. After a series of purification steps, the- o8 j8 s- h/ [* R& c$ p/ P& \5 v
isolated titanium dioxide is finally washed with water, calcined, and: \( F0 ]* ?* G; A/ ]: O0 A6 }% z
micronized.
- F t( L, S8 N& A: @( {In the chloride process, chlorine gas is reacted with a titaniumcontaining# X# F6 B( k; B' y
mineral under reducing conditions to form anhydrous, \; @1 l; H: b7 i* Y; K
titanium tetrachloride, which is subsequently purified and converted to) v8 x1 I1 N$ q1 Z/ n
titanium dioxide either by direct thermal oxidation or by reaction with- V6 `( a" r, [: v# P
steam in the vapour phase. Alternatively, concentrated hydrochloric3 P1 d# D6 f8 P* D3 e
acid can be reacted with the titanium-containing mineral to form a; e: z$ V+ |+ C1 ]/ o
solution of titanium tetrachloride, which is then further purified and
/ C3 b8 w# W' J+ _( b2 N" p: dconverted to titanium dioxide by hydrolysis. The titanium dioxide is L, k4 G& {% A+ i
filtered, washed, and calcined.0 x8 Y9 ], u& a* c1 x( X6 e" ?' s
Commercial titanium dioxide may be coated with small amounts of
& w5 G' W* r( p, c$ d' Zalumina and/or silica to improve the technological properties of the
3 N# u \5 u* A0 f$ S7 Nproduct.
. M! Z8 A- L! H9 \; ZC.A.S. number 13463-67-7* ~: _7 `7 B2 [0 [8 r6 j4 U
Chemical formula TiO2( \% z) e9 ~/ B& f) e! y, ^
Formula weight2 r9 U: v5 B- X0 Y2 _
79.88
* i& j; z; s) q b: Z8 |: |$ LAssay% {+ n# ]$ C0 i9 j8 o5 L, E
Not less than 99.0% on the dried basis (on an aluminium oxide and
; { ~, A6 _5 L/ P& V1 asilicon dioxide-free basis)& Y2 h% c! {$ l- c, V, z3 i
DESCRIPTION6 R, \2 b' o$ s0 {3 ^# A
White to slightly coloured powder; J1 Z* w: J8 e
FUNCTIONAL USES5 \* H; h5 u! ~
Colour2 X9 E& `4 ]8 A6 b1 ^
CHARACTERISTICS
% u6 M- I B, n5 h' E# QIDENTIFICATION
^- v4 r" S% e$ f$ ?' s- z* KSolubility (Vol. 4)# ~7 K |( T# `8 Y# O
Insoluble in water, hydrochloric acid, dilute sulfuric acid, and organic
) T( x; }1 E' A6 |) S7 J% ?solvents. Dissolves slowly in hydrofluoric acid and hot concentrated6 h1 W# `7 V1 A( D- L/ F6 \8 }5 m
sulfuric acid.
& q$ j# S/ ?4 g: mColour reaction
2 E& o3 b/ {7 [5 }) Y6 f* w! v3 \2 eAdd 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of
* \! f5 D* i! q- F1 W" usulfuric acid appear, then cool. Cautiously dilute to about 100 ml with
. y$ E% {. p, J" Y9 w- n* V* Nwater and filter. To 5 ml of this clear filtrate, add a few drops of
6 R! r& n# U& R9 c: |% u* Rhydrogen peroxide; an orange-red colour appears immediately., Y- c; T; d, ?, `# t& r1 Y
PURITY3 ?$ w% r" {- A4 e% ]' l6 }
Loss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)3 g$ o& h; c. L' c$ R& H3 c
Loss on ignition (Vol. 4)
* J# s- m2 t2 r) _Not more than 1.0% (800o) on the dried basis
9 q, O$ U: N" G, s; ~+ }0 OAluminium oxide and/or6 K, s: n: m8 P/ H) G: ~; H" |
silicon dioxide
; H% ^# E+ n# l- }% b! [Not more than 2%, either singly or combined
% ~( x r$ y% G/ h. L; [See descriptions under TESTS
, u) c3 o8 K& R+ J2 \& _1 TAcid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing6 i0 [( T5 S- x+ n4 o O9 \) z* ?$ P
alumina or silica.- w/ {6 k$ ~, a2 S
Suspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and
: g+ N2 _* X6 F6 }place on a steam bath for 30 min with occasional stirring. Filter
P' B( \* g& t% i" ]through a Gooch crucible fitted with a glass fibre filter paper. Wash
2 S8 l' ? P- O% M, ]4 r+ gwith three 10-ml portions of 0.5 N hydrochloric acid, evaporate the
0 \! I% Y. r0 H* w, Scombined filtrate and washings to dryness, and ignite at a dull red' B3 X; q5 Y. \
heat to constant weight.
1 J4 V P& s' d: q4 c$ t! l' GWater-soluble matter7 n( i+ k; e2 L; Q8 ?
(Vol. 4)
# `5 X. ]1 f+ _" [% ~( u( v+ xNot more than 0.5%4 H7 ]" G& H" G2 V7 I( q
Proceed as directed under acid-soluble substances (above), using
8 a1 D1 c" C3 M" Q. Z- m9 L8 dwater in place of 0.5 N hydrochloric acid.
1 K# X6 | z0 o0 _Impurities soluble in 0.5 N
. I9 ?( u( P1 [: d, H2 K; hhydrochloric acid* L* X/ \# O6 [" R2 Z
Antimony Not more than 2 mg/kg6 u/ k3 Q) Y2 ]/ I0 i* {$ U% r* ]5 w
See description under TESTS3 g7 p, h7 h& K: i5 n" O! i
Arsenic Not more than 1 mg/kg% ~( a# R) y. H C9 G% X
See description under TESTS) F( q. D# L6 G
Cadmium Not more than 1 mg/kg6 z- c5 e0 }3 b2 n1 s( x- P
See description under TESTS0 Z6 ]5 G' c4 f/ p6 {
Lead! c2 p, i0 h9 ?; P" r+ U
Not more than 10 mg/kg2 |) O2 @6 l B% E! ]1 y- k+ l
See description under TESTS
% Q+ k+ a7 }, j: }1 EMercury (Vol. 4) Not more than 1 mg/kg4 Y; z5 | r( ?; ]
Determine using the cold vapour atomic absorption technique. Select a! N* f* y: `0 f I
sample size appropriate to the specified level9 ^7 @6 f" C& z9 _' Q
TESTS. @1 r% z4 {% G0 `. q( H
PURITY TESTS
: S1 u) c) j/ P9 V* e* w' RImpurities soluble in 0.5 N
! M- @' j( d* G# |4 a2 \hydrochloric acid! Q& N. S; V+ }# b2 t
Antimony, arsenic,
6 c L: S9 H% w: y5 \4 q) ~$ F$ }cadmium and lead
6 X" [) C0 J/ T: X5 ]0 q5 D(Vol.4)
7 V; {- ?# ?, x3 A4 N2 rTransfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N @) P! O. ?5 R; g7 Z, Z e
hydrochloric acid, cover with a watch glass, and heat to boiling on a4 z/ @2 K2 L6 c h. K
hot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml0 u4 @$ K" J, o& |* Y
centrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved0 F( |" O9 ]& j N8 r1 y0 _
material settles. Decant the supernatant extract through a Whatman( }2 u9 J/ k& I6 I7 e* @
No. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml
% U& l; _) K4 ~ q1 l& yvolumetric flask and retaining as much as possible of the undissolved
% J4 y& o% i5 G7 l( jmaterial in the centrifuge bottle. Add 10 ml of hot water to the original% A. U( a' A2 e* M) u; P9 f
beaker, washing off the watch glass with the water, and pour the" s" V8 ^5 k8 E- z8 w G
contents into the centrifuge bottle. Form a slurry, using a glass stirring
1 S5 s) X! r7 k. d* m& [! B4 srod, and centrifuge. Decant through the same filter paper, and collect
" G. U0 l+ W- v- ]6 p. [ G0 G7 l( jthe washings in the volumetric flask containing the initial extract.
! n9 X7 a) s5 K/ H1 ^2 m9 GRepeat the entire washing process two more times. Finally, wash the( B8 K: h- O1 E+ ~
filter paper with 10 to 15 ml of hot water. Cool the contents of the flask) C ?' l Q; N& u
to room temperature, dilute to volume with water, and mix.
4 d- V& m0 P2 N9 A. t* ZDetermine antimony, cadmium, and lead using an AAS/ICP-AES
# R( b, t6 _/ c+ ]technique appropriate to the specified level. Determine arsenic using the7 @! `6 E* Q: p3 U; y
ICP-AES/AAS-hydride technique. Alternatively, determine arsenic using& a: y1 p: v0 b8 i) |' s- f! t
Method II of the Arsenic Limit Test, taking 3 g of the sample rather than' c p- d5 g# q; j9 c, o2 z
1 g. The selection of sample size and method of sample preparation
A2 K' x3 B5 G! Smay be based on the principles of the methods described in Volume 4.
9 ~1 b" u6 B9 b, uAluminium oxide Reagents and sample solutions
& C, B/ \$ O# f n0.01 N Zinc Sulfate
% }8 O. u/ F* w+ k+ MDissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to
+ {+ |* k$ P7 M" Q* @2 f' \make 1000 ml. Standardize the solution as follows: Dissolve 500 mg+ E( |& U: t. B1 O9 ~0 E( M6 Z
of high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of( |7 |1 D2 U \* z: g5 `
concentrated hydrochloric acid, heating gently to effect solution, then9 M% B8 u- z5 T8 d( O
transfer the solution into a 1000-ml volumetric flask, dilute to volume( [; |' b1 m' k" }7 U9 b5 x' W
with water, and mix. Transfer a 10 ml aliquot of this solution into a 500+ H8 m) ?7 @) Y' z6 `& h
ml Erlenmeyer flask containing 90 ml of water and 3 ml of
# U }# \5 ^# `concentrated hydrochloric acid, add 1 drop of methyl orange TS and- ?; V7 _% t8 \2 ]4 y6 z8 A$ Z
25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,
8 T6 {( @: s3 l' bdropwise, ammonia solution (1 in 5) until the colour is just completely
3 ^1 m0 |+ Q; ?" cchanged from red to orange-yellow. Then, add:
2 f& M" n e% \(a): 10 ml of ammonium acetate buffer solution (77 g of
/ d. U' |0 v+ @1 n3 k( Wammonium acetate plus 10 ml of glacial acetic acid, dilute to
2 n! ~4 D3 p- p# a1000 ml with water) and
4 @' J- b+ W' |(b): 10 ml of diammonium hydrogen phosphate solution (150 g( P3 d. A7 H) d% a ?' a( s
of diammonium hydrogen phosphate in 700 ml of water,
! n }- H, R4 M5 x9 I& padjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,8 R5 y1 A7 x# Q9 _7 H, J
then dilute to 1000 ml with water).7 s `, G% f \& i8 T3 |) F
Boil the solution for 5 min, cool it quickly to room temperature in a
3 K0 Z' }. n; L/ y- Astream of running water, add 3 drops of xylenol orange TS, and mix.
0 C3 Y) Q' H2 L8 Q. @( b0 NUsing the zinc sulfate solution as titrant, titrate the solution to the first; `; I9 ]. G) b- [) [6 K4 @2 \
yellow-brown or pink end-point colour that persists for 5-10 sec. (Note:) m" B0 u+ Y5 M9 C( V0 G
This titration should be performed quickly near the end-point by2 G9 g9 ^4 \+ s' Y9 i. B7 K
adding rapidly 0.2 ml increments of the titrant until the first colour
! }3 I& I& H* X8 i: v( nchange occurs; although the colour will fade in 5-10 sec, it is the true
( i0 g9 [- b3 ^% u0 Hend-point. Failure to observe the first colour change will result in an
) |- d4 n/ S1 s9 aincorrect titration. The fading end-point does not occur at the second
U- G( S8 x9 }end-point.)
" d, B# _/ e; k) z" m* q7 E5 U# @Add 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a5 ~" N% O+ f/ Z3 t9 v i- w; F
stream of running water. Titrate this solution, using the zinc sulfate
- [+ A3 i' r* N& t7 s& O' _solution as titrant, to the same fugitive yellow-brown or pink end-point( O0 R2 P* `5 T8 ~
as described above.
' C& r; L) N) z+ Z+ e; P0 [7 @Calculate the titre T of zinc sulfate solution by the formula:$ q' e; H3 P5 Q6 G
T = 18.896 W / V# c# s5 Z* m+ Y0 t
where
- a* D8 z& ~+ Q2 E# ?& IT is the mass (mg) of Al2O3 per ml of zinc sulfate solution7 B! h8 n* b! E, U) w( Y
W is the mass (g) of aluminium wire
7 A! d1 t4 x5 dV is the ml of the zinc sulfate solution consumed in the
) g7 u! q/ T4 P2 asecond titration
5 g) p2 J1 ~0 r) C18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and
+ G J" z2 y# d9 ~R is the ratio of the formula weight of aluminium oxide to
+ Q. _- ?* S4 R$ I/ P3 {: uthat of elemental aluminium. s: L' z. D/ X7 r a
Sample Solution A# `' b8 e) f1 m1 O
Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica9 n) I! U9 X- O, Y
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).& z/ q# d) l2 B
(Note: Do not use more sodium bisulfate than specified, as an excess
5 b7 i: k# e) k* H! m: k$ y, w2 ?concentration of salt will interfere with the EDTA titration later on in the0 X/ o% B( z9 ]8 I
procedure.) Begin heating the flask at low heat on a hot plate, and
4 ?+ X. o6 j( G- r0 x/ i$ H* @then gradually raise the temperature until full heat is reached.
( e& Q' E$ u2 @) B9 N2 x(Caution: perform this procedure in a well ventilated area. ) When- D0 X; G4 R Z6 I/ T1 ^
spattering has stopped and light fumes of SO3 appear, heat in the full9 ^- @, B" x$ n2 ]
flame of a Meeker burner, with the flask tilted so that the fusion of the
% E4 j5 e% D* q) P' }$ F+ ksample and sodium bisulfate is concentrated at one end of the flask.
$ W6 e# `( G- f/ c5 @& uSwirl constantly until the melt is clear (except for silica content), but
7 }9 u- Q$ u# kguard against prolonged heating to avoid precipitation of titanium9 e" W. @. G, j( l
dioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until! T' D8 p9 k7 e% S) G
the mass has dissolved and a clear solution results. Cool, and dilute to6 ~; ~; h9 ^, w% H
120 ml with water. Introduce a magnetic stir bar into the flask.8 I1 J2 R& [- z" M- u+ v" }
Sample Solution B; a1 r0 r! U9 J( t6 b5 L
Prepare 200 ml of an approximately 6.25 M solution of sodium {8 o4 w- A f# i) w- A E
hydroxide. Add 65 ml of this solution to Sample Solution A, while" D& ?: y8 @3 z+ k5 ~- {, e* \
stirring with the magnetic stirrer; pour the remaining 135 ml of the8 ^! U( q% {( U: h' N. T: \% ~
alkali solution into a 500-ml volumetric flask.! v8 U7 V- @3 f
Slowly, with constant stirring, add the sample mixture to the alkali- r& h* ?/ k" `" n& |
solution in the 500-ml volumetric flask; dilute to volume with water,' F- K2 Q3 s4 ] E- w) ^
and mix. (Note: If the procedure is delayed at this point for more than
7 z; {/ O( x3 \4 H6 \, d& h2 hours, store the contents of the volumetric flask in a polyethylene
3 ]. \! A% I( R6 ~/ H# `# ebottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),
4 q8 I8 X( N" cthen filter the supernatant liquid through a very fine filter paper. Label
1 |9 X5 K" }* {7 M7 X# Pthe filtrate Sample Solution B.+ T6 v5 T$ j+ \5 o0 b
Sample Solution C
3 S+ i' \3 p" c, ATransfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer3 i) B. d; B$ ^7 r$ }6 D0 U) V" _
flask, add 1 drop of methyl orange TS, acidify with hydrochloric acid% A ]8 e7 A& J5 M" }' ?; K
solution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02' D# P# H3 [0 W) e" O
M disodium EDTA, and mix. [Note: If the approximate Al2O3 content is
/ s5 _: @+ g% h. Q" aknown, calculate the optimum volume of EDTA solution to be added* Z8 }/ E2 b% n6 J9 j! Z' c; }) ~5 _
by the formula: (4 x % Al2O3) + 5.]
8 X) b7 \% n. xAdd, dropwise, ammonia solution (1 in 5) until the colour is just& n5 K. g0 |! v8 S
completely changed from red to orange-yellow. Then add10 ml each
' C! t, l2 u2 ~) Fof Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to) F" ?, \9 ~4 ~4 i2 U: k3 G
room temperature in a stream of running water, add 3 drops of xylenol
5 B+ d, b; j2 m" o* m; Oorange TS, and mix. If the solution is purple, yellow-brown, or pink,& A1 x' h7 n/ I8 _! ~7 u
bring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired
7 Y k6 D! h- \) n! M1 r- NpH, a pink colour indicates that not enough of the EDTA solution has X/ [9 l+ a! k& T B2 P
been added, in which case, discard the solution and repeat this3 x% b, F8 G2 m) j4 Q
procedure with another 100 ml of Sample Solution B, using 50 ml,
2 h, L7 V) q1 E" grather than 25 ml, of 0.02 M disodium EDTA.
! g# x+ X* ?- NProcedure
. N! c; h* t) T: [, WUsing the standardized zinc sulfate solution as titrant, titrate Sample
! T/ f* A$ V8 E2 t# L% j2 ?+ xSolution C to the first yellow-brown or pink end-point that persists for
; E8 p: _1 L9 {# ^8 j2 N1 o5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first
. @" Y* M. U0 x0 ntitration should require more than 8 ml of titrant, but for more accurate
2 P! ^9 _$ D0 n. M! g. `, g8 i% ]work a titration of 10-15 ml is desirable.
. N7 o. J, z W6 w2 A7 H4 P3 NAdd 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5) F9 n+ ?! C* f( h* c _
min, and cool in a stream of running water. Titrate this solution, using3 h2 ~; T- E9 r6 Y" |" l
the standardized zinc sulfate solution as titrant, to the same fugitive. v; X" N6 n2 d6 G. |0 K! ?( u& P
yellow-brown or pink end-point as described above.' i! s- [: J7 |+ G, J$ J
Calculation:* p$ E5 V$ h6 |
Calculate the percentage of aluminium oxide (Al2O3) in the sample, p/ I7 S6 t# i
taken by the formula:* S* V1 ^1 m$ O
% Al2O3 = 100 × (0.005VT)/S+ l0 R3 }5 a$ A# n' V% I" p4 I U
where7 v6 F) l5 `- U: `/ r C
V is the number of ml of 0.01 N zinc sulfate consumed in/ T) Q: }* u9 e1 f1 T" l
the second titration," D) L* r; u f X: F/ D5 Q
T is the titre of the zinc sulfate solution,
) P$ x0 u; \+ z* ^: r5 ]- jS is the mass (g) of the sample taken, and
& Q& J2 _+ q# a' j5 a0.005 = 500 ml / (1000mg/g × 100 ml).
$ I, R" l5 r/ d( T/ g5 ZSilicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica
% m7 @2 v3 ]9 s( |( F' s$ ]glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
P9 h+ ?: ~4 O+ l% w7 hHeat gently over a Meeker burner, while swirling the flask, until
% N) b' w3 ~- C$ udecomposition and fusion are complete and the melt is clear, except4 n2 t* @' K+ |# ?( U4 i5 H
for the silica content, and then cool. (Caution: Do not overheat the
# w8 k# ?( e* P0 s/ P( }0 [contents of the flask at the beginning, and heat cautiously during
' B5 U! d9 [5 p& Z- ]fusion to avoid spattering.)4 i! ^& w0 ?- j$ ?: c' i- @" V9 f
To the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat
) t* w! s' H1 Y9 t- Bcarefully and slowly until the melt is dissolved. Cool, and carefully add
/ l8 Y2 L! _: \; }2 z& \150 ml of water by pouring very small portions down the sides of the
. k D: l" M/ B: h* E$ `2 N3 s4 k. Fflask, with frequent swirling to avoid over-heating and spattering. Allow
! h2 _: F" y# p: c/ v7 k# lthe contents of the flask to cool, and filter through fine ashless filter2 g# f7 W& P9 {& d- I
paper, using a 60 degree gravity funnel. Rinse out all the silica from
: q4 l4 C- ^: m( z/ |the flask onto the filter paper with sulfuric acid solution (1 in 10)." l3 m+ U3 u" v9 \% Q* D- | R
Transfer the filter paper and its contents into a platinum crucible, dry in
# a# r6 z0 Z+ X4 v% U1 |1 Wan oven at 1200, and heat the partly covered crucible over a Bunsen) h; q+ `& ]- s X
burner. To prevent flaming of the filter paper, first heat the cover from# {2 Z" L/ q5 g3 x8 d
above, and then the crucible from below.
+ `6 z( C* W' \) B- h9 V6 sWhen the filter paper is consumed, transfer the crucible to a muffle
/ ]3 g' W. n8 q; V5 Sfurnace and ignite at 1000o for 30 min. Cool in a desiccator, and
! ]& e/ D* |/ h0 z5 A$ kweigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated8 K5 J7 ]8 g, u" H
hydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first# z" v4 U2 W. I! q2 d: h0 e
on a low-heat hot plate (to remove the HF) and then over a Bunsen* c: i0 q! s* _6 z/ m
burner (to remove the H2SO4). Take precautions to avoid spattering,! u2 ~* o8 @; X" A1 {
especially after removal of the HF. Ignite at 1000o for 10 min, cool in a. M5 R- U! Z3 _) y' k
desiccator, and weigh again. Record the difference between the two! H* W9 E& I+ o) ^
weights as the content of SiO2 in the sample.
* l" M5 a; u: I- @METHOD OF ASSAY2 M5 j @$ \, |6 z0 c
Accurately weigh about 150 mg of the sample, previously dried at 105o# ^! h; o# l) H; ?8 y0 m% I' c
for 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water
4 E( Y# r) M2 Hand shake until a homogeneous, milky suspension is obtained. Add 303 ]- ~9 p7 a& x# G$ o2 T% s4 v V
ml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially0 c8 ?4 h8 ~0 V
heat gently, then heat strongly until a clear solution is obtained. Cool,
& n+ t! f1 D, C9 w5 A- dthen cautiously dilute with 120 ml of water and 40 ml of hydrochloric
8 o, x! a4 O) j5 C8 e1 t/ ~acid, and stir. Add 3 g of aluminium metal, and immediately insert a: D; K* ~$ z7 b$ z; x
rubber stopper fitted with a U-shaped glass tube while immersing the: c0 y1 P+ U4 R5 l: C
other end of the U-tube into a saturated solution of sodium
: Q# H7 k# t% O8 i8 j$ n; N6 fbicarbonate contained in a 500-ml wide-mouth bottle, and generate7 b7 M( W, h- x$ Q3 c
hydrogen. Allow to stand for a few minutes after the aluminium metal
, J: }* Y: i# D& S7 r. nhas dissolved completely to produce a transparent purple solution.
2 n: T. r* J0 a' @; h, rCool to below 50o in running water, and remove the rubber stopper
7 U6 `5 H' y1 Ucarrying the U-tube. Add 3 ml of a saturated potassium thiocyanate
6 a% Q0 p" l9 A3 r7 i: rsolution as an indicator, and immediately titrate with 0.2 N ferric9 ~- U0 f% d" w6 Y
ammonium sulfate until a faint brown colour that persists for 300 D& [4 _8 N8 P5 N
seconds is obtained. Perform a blank determination and make any3 L% J! f& w/ G
necessary correction. Each ml of 0.2 N ferric ammonium sulfate is
& D* y' w3 n8 J+ ^" A, A# Pequivalent to 7.990 mg of TiO2. Z( {1 A1 e& n+ @, J* d$ o+ r# Y
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