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二氧化钛(钛白粉)
二氧化钛(钛白粉)/ {- A, n& Z7 O, p( Y
' ]' z6 e4 ^0 O; }( g/ B; h
JECFA关于二氧化钛(钛白粉)的结论, Q- e8 j6 Q/ y; F3 x2 r0 w
& `- I: ~+ M* ? _& x* U摘要: 2006年JECFA关于二氧化钛的结论+ Y! @( F/ v. ]0 e. T
ADI值:不作限制。- z2 z9 [0 \1 H8 V6 }
功能:着色剂
6 b( o% G: W, d# b. V$ _% u, G, I% P2 x. Q
TITANIUM DIOXIDE* a& g3 N+ H( @' } ?: [& M
Prepared at the 67th JECFA (2006) and published in FAO JECFA0 X$ |$ w; y" F* O* x- Y3 b) m) H
Monographs 3 (2006), superseding specifications prepared at the 63rd: a& ~$ W7 z% F+ S3 f% E- \. Q
JECFA (2004) and published in FNP 52 Add 12 (2004) and in the B9 p) `% v3 `8 f: I3 a
Combined Compendium of Food Additive Specifications, FAO JECFA0 i5 Q6 |. q! P) U4 }
Monographs 1 (2005). An ADI “not limited” was established at the 13th# P" W: [1 ~$ `6 t9 y# Y
JECFA (1969).
0 I" f1 W; p6 B- s+ o( M- ASYNONYMS) t+ Z% v5 I* L# I! }3 [$ w$ A
Titania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171+ B, \- r- `& z3 i+ _, ~
DEFINITION. `% Q1 \# _$ [4 X+ c9 |5 p6 A
Titanium dioxide is produced by either the sulfate or the chloride
9 D/ r/ F; U' {- iprocess. Processing conditions determine the form (anatase or rutile+ j/ W# v4 B% ~, ^: ?
structure) of the final product./ W) x+ r6 _. S/ h6 \ i6 I/ a
In the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)$ w0 M2 ^% g) k( ]/ F, r, Y6 G4 h+ [+ |
or ilmenite and titanium slag. After a series of purification steps, the1 u% g! p7 {; S# G- c1 V
isolated titanium dioxide is finally washed with water, calcined, and
- H0 R7 q1 W |* ^, ^micronized.# t( ^5 _ L. x3 u
In the chloride process, chlorine gas is reacted with a titaniumcontaining
2 \6 \3 N; e* l6 n) b6 T4 v Amineral under reducing conditions to form anhydrous( D) W- o \+ }+ I9 J
titanium tetrachloride, which is subsequently purified and converted to
& o D. w- U+ @0 ]$ T$ A; C/ Ytitanium dioxide either by direct thermal oxidation or by reaction with! y0 J1 s( v) A" ^$ q: ?3 o
steam in the vapour phase. Alternatively, concentrated hydrochloric6 F) g# L4 P5 }/ _' L8 ^
acid can be reacted with the titanium-containing mineral to form a& y6 K7 `1 L; A# _
solution of titanium tetrachloride, which is then further purified and
8 v. M5 o* T$ Pconverted to titanium dioxide by hydrolysis. The titanium dioxide is0 M- T$ q3 v1 ~) c/ c* V( S( K+ A5 F- B
filtered, washed, and calcined.
8 [& ?6 c! n G1 \2 ~( ECommercial titanium dioxide may be coated with small amounts of! f; W0 Z1 v" p L8 _! [! u
alumina and/or silica to improve the technological properties of the" i$ P0 C" |+ |7 T2 q+ k
product.
8 J9 V0 \# d7 j9 |C.A.S. number 13463-67-7
# @) `2 s; e9 _, r- sChemical formula TiO2
& _8 v ^5 r8 ~% w) X' V R* mFormula weight8 f% ~- h+ \8 i! \% F3 v. T; u$ k2 K X
79.880 ?. ~8 u9 ~" W0 Y: \- r4 U
Assay5 _3 @. B0 @/ o# j$ Q3 ~
Not less than 99.0% on the dried basis (on an aluminium oxide and( o. C" J8 }+ @+ b
silicon dioxide-free basis)9 ^6 f( m! f( w$ j* I
DESCRIPTION- X% M# I; ]2 y- d
White to slightly coloured powder% q* i. y2 L) | \$ W& E! N! P4 c5 }
FUNCTIONAL USES" _! c% Y' N: L* \0 {
Colour
- I' J2 O! G1 I& d( WCHARACTERISTICS
0 O$ y) @0 g* D9 e2 O; DIDENTIFICATION
1 l2 f3 s; i0 I6 |# T9 B' e& b+ tSolubility (Vol. 4)
$ N* q0 G8 W) W8 K8 sInsoluble in water, hydrochloric acid, dilute sulfuric acid, and organic# I0 e% `/ \1 C! u( _
solvents. Dissolves slowly in hydrofluoric acid and hot concentrated
* P; U# P+ _6 j- s0 osulfuric acid.: ?6 }" f& |+ j3 C7 T2 P
Colour reaction$ ~7 w- R7 _/ L/ r! u
Add 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of( ~8 R. y( G/ V, l; t
sulfuric acid appear, then cool. Cautiously dilute to about 100 ml with
0 D0 {* a0 C4 Cwater and filter. To 5 ml of this clear filtrate, add a few drops of" D/ m9 R' K g- G. p1 p2 Z" x
hydrogen peroxide; an orange-red colour appears immediately.& G7 [! g1 K1 Q2 e7 u
PURITY g$ y/ |8 j6 P8 y
Loss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)
% f8 N7 `% [7 j+ Z* T9 Z: ~Loss on ignition (Vol. 4)
( K `. b/ E5 s4 w2 h6 lNot more than 1.0% (800o) on the dried basis: T3 R1 J3 V4 A9 |4 I( ^
Aluminium oxide and/or
6 B) _7 Z6 z' j3 X' bsilicon dioxide4 O) _+ n+ a/ J0 @5 w2 i' Q; F+ G+ w
Not more than 2%, either singly or combined; ^, B A/ Y. Z& h: {4 y7 y% B
See descriptions under TESTS
( Q# p; Y/ e( v8 K7 J/ bAcid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing
& B5 d$ J* |0 w, ralumina or silica.9 ~: n1 F& @& x9 @2 d. j
Suspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and1 g* a2 M; V; Z1 n, G( ^
place on a steam bath for 30 min with occasional stirring. Filter
/ y5 e5 }2 X" Y" A4 pthrough a Gooch crucible fitted with a glass fibre filter paper. Wash2 F& n4 P A: _& ?% |9 G m, @. R
with three 10-ml portions of 0.5 N hydrochloric acid, evaporate the
) o: ^& N* D: `# u8 v1 Acombined filtrate and washings to dryness, and ignite at a dull red+ N' ?, g4 @& x! z$ d5 L. _
heat to constant weight.
& p- N& \/ a3 X$ A. @* n2 rWater-soluble matter
5 F% Q" A. \8 r. z F(Vol. 4)
4 U1 W' C* S8 tNot more than 0.5%7 |! | @+ ]! r
Proceed as directed under acid-soluble substances (above), using1 H' V! T2 N* A# s$ U# d. y8 [
water in place of 0.5 N hydrochloric acid.% x+ G" W6 w* D1 k5 \3 Y
Impurities soluble in 0.5 N0 { ^4 A6 A4 ^' \: H
hydrochloric acid$ h }, d5 k7 P W, b" b3 |' k
Antimony Not more than 2 mg/kg) @8 O$ `' b4 a
See description under TESTS& G, |) i* I5 Y3 N
Arsenic Not more than 1 mg/kg
+ R/ w2 D, Y8 t( f$ K4 NSee description under TESTS
9 F$ v( r s6 uCadmium Not more than 1 mg/kg
5 Z, D1 Z( ~7 n; Z# [" XSee description under TESTS
C8 I( N: Y3 _! B+ ~1 TLead1 P7 u8 W2 ^0 M+ L
Not more than 10 mg/kg
; Z) w% `+ A9 f9 b6 ^See description under TESTS( w8 n0 y9 u0 f) M& {! ~
Mercury (Vol. 4) Not more than 1 mg/kg
1 O r# ~, v+ |* SDetermine using the cold vapour atomic absorption technique. Select a
, L& O ]8 h4 ^7 x) r" ?" Hsample size appropriate to the specified level3 q8 b b4 f% k' r3 j% Q
TESTS8 S6 H _" w, m+ ~. y8 _' D
PURITY TESTS/ `6 h. {, J" A$ s% w* H2 _" G
Impurities soluble in 0.5 N
" e5 U6 X% h+ f7 ?6 p2 P& I. |! `hydrochloric acid+ G: t$ A/ ~' R8 Y
Antimony, arsenic,# {0 h, J) _9 n4 S* V8 _$ e( H
cadmium and lead
; V0 x! v: I# a3 s3 u2 }6 v(Vol.4)/ a4 y5 O$ ~# H" V
Transfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N& c$ E; G( a# }6 w; R
hydrochloric acid, cover with a watch glass, and heat to boiling on a) u6 \) [7 {! B
hot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml! ]" {$ S% }6 a, u4 u
centrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved
# Q2 c, f2 c* l: f) vmaterial settles. Decant the supernatant extract through a Whatman/ n5 c3 W+ U+ g. [ }9 P+ r( }+ m" O: y
No. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml
% e4 Q; j- c) U* Q1 }volumetric flask and retaining as much as possible of the undissolved
V7 h5 u# R0 Umaterial in the centrifuge bottle. Add 10 ml of hot water to the original
h5 g" o# F& dbeaker, washing off the watch glass with the water, and pour the* ]6 O _! R# o1 ?' m
contents into the centrifuge bottle. Form a slurry, using a glass stirring
6 F( n6 B- l' P+ ^rod, and centrifuge. Decant through the same filter paper, and collect
$ v0 ^) o2 Y `$ w" x2 Athe washings in the volumetric flask containing the initial extract.. K4 t9 a, F$ ~& e) k' m3 [
Repeat the entire washing process two more times. Finally, wash the! ?# C2 x5 K; g# q! r. w4 V- G
filter paper with 10 to 15 ml of hot water. Cool the contents of the flask- y, i6 a% `" V. R2 O" E/ ]5 E1 T
to room temperature, dilute to volume with water, and mix.
1 ^" \0 I: B- i2 o% p' Y3 |, e8 yDetermine antimony, cadmium, and lead using an AAS/ICP-AES, O9 W+ d# W, Z! ~" K8 |
technique appropriate to the specified level. Determine arsenic using the
5 e( w5 W1 w: Y7 u( z* gICP-AES/AAS-hydride technique. Alternatively, determine arsenic using' s2 M( o: A/ `' t+ }- G+ D
Method II of the Arsenic Limit Test, taking 3 g of the sample rather than& n/ D. I3 A# B8 ]- f, @, |% ]
1 g. The selection of sample size and method of sample preparation7 m: Q( w! z1 M, N J/ ]
may be based on the principles of the methods described in Volume 4.
1 @$ S% a! m& D6 W: Q* J0 GAluminium oxide Reagents and sample solutions
8 y0 z- V+ ~- n( H3 Z% A4 F" K- A) e0.01 N Zinc Sulfate
9 q2 ~1 b3 V! k1 o' G9 r- z1 e& uDissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to
, e {! J- D* G9 i9 G6 cmake 1000 ml. Standardize the solution as follows: Dissolve 500 mg+ x2 r: q& y" T: }2 P
of high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of7 C- L5 }+ l3 Z. ~1 I s
concentrated hydrochloric acid, heating gently to effect solution, then. I' _* I5 z* s3 J7 r1 r4 ^0 x9 R! e
transfer the solution into a 1000-ml volumetric flask, dilute to volume7 k1 J6 |, T( g2 J5 J0 @
with water, and mix. Transfer a 10 ml aliquot of this solution into a 500
; i! f, M) V) B1 d$ ]ml Erlenmeyer flask containing 90 ml of water and 3 ml of: [& B# w* T( w7 G
concentrated hydrochloric acid, add 1 drop of methyl orange TS and9 ~/ G4 G9 Q, [% Y+ g& {. H
25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,
5 D9 T& b1 |( w( Q5 q' B! b0 tdropwise, ammonia solution (1 in 5) until the colour is just completely* u! f) A1 n0 V7 b/ I# \
changed from red to orange-yellow. Then, add:
0 z' A) z: s4 |& p* {! k(a): 10 ml of ammonium acetate buffer solution (77 g of
2 w0 v7 F& U5 mammonium acetate plus 10 ml of glacial acetic acid, dilute to: H" S: v# v E0 J/ |+ W
1000 ml with water) and0 Z6 ?( S0 k, E- h
(b): 10 ml of diammonium hydrogen phosphate solution (150 g
4 y% L4 O' K9 n- Z; e g# Kof diammonium hydrogen phosphate in 700 ml of water,: I; W% n o$ n* ?
adjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,
9 F$ v4 g$ f" h: ?+ P$ ~: H) Ethen dilute to 1000 ml with water).* y T0 Z! o# Q- x O0 z7 F& ^
Boil the solution for 5 min, cool it quickly to room temperature in a
7 |- W+ a5 ` J( B# U8 g) Cstream of running water, add 3 drops of xylenol orange TS, and mix.
3 Y. b0 L! w3 J. p# Q6 |0 ZUsing the zinc sulfate solution as titrant, titrate the solution to the first" ~) k+ u7 N& p7 f% g5 H4 v* D
yellow-brown or pink end-point colour that persists for 5-10 sec. (Note:
; h& q. Z* k+ s( q2 FThis titration should be performed quickly near the end-point by4 Y4 r5 i& \6 Y2 s& W
adding rapidly 0.2 ml increments of the titrant until the first colour
3 O9 P9 \6 F0 W% }& Y. lchange occurs; although the colour will fade in 5-10 sec, it is the true
. z) ~4 i q" i, @8 send-point. Failure to observe the first colour change will result in an% l* c% i5 i8 ?1 K
incorrect titration. The fading end-point does not occur at the second
& @1 C3 L" _& f* n( P, rend-point.)% C3 I! R( T5 Y
Add 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a$ Y6 q5 n2 v) Z3 e3 E; G: C
stream of running water. Titrate this solution, using the zinc sulfate3 o- o/ [) \* r4 n6 h* v# e
solution as titrant, to the same fugitive yellow-brown or pink end-point0 o: i* v- }% B0 ?/ a
as described above.: D- S* _- I1 G/ }, n; Y- J1 E6 O. \
Calculate the titre T of zinc sulfate solution by the formula:) C$ v$ v' c6 j
T = 18.896 W / V# z- Q# {" X5 k* l! H+ O
where1 G3 s! X/ M2 u
T is the mass (mg) of Al2O3 per ml of zinc sulfate solution
. v. |: ? z5 U: S( V6 SW is the mass (g) of aluminium wire
5 A! A% v5 h, P1 LV is the ml of the zinc sulfate solution consumed in the) B- i4 }# w/ z2 g; S
second titration5 v) j( C% T( D m2 T) d
18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and6 l- u1 N7 I5 \, ?. a; ]
R is the ratio of the formula weight of aluminium oxide to N1 B4 f/ S. u5 B
that of elemental aluminium.
5 j4 T. ` c! v9 P- Q- I, BSample Solution A
% A8 @; k+ V6 S, C4 KAccurately weigh 1 g of the sample and transfer to a 250-ml high-silica
; l5 j9 v6 [# o/ V) o7 c. x) Cglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
0 b. U/ W5 t% D4 G9 z(Note: Do not use more sodium bisulfate than specified, as an excess
3 k t. b9 ` P; _# N: r, I% \concentration of salt will interfere with the EDTA titration later on in the* Z4 q( p9 M8 t3 u' Q3 N
procedure.) Begin heating the flask at low heat on a hot plate, and
4 k. h0 T4 z, r4 V4 g1 S$ O( Sthen gradually raise the temperature until full heat is reached., D* E# q3 g/ [& t& P$ o' d
(Caution: perform this procedure in a well ventilated area. ) When
, J- Y+ g: g2 |9 Z0 z0 espattering has stopped and light fumes of SO3 appear, heat in the full
1 b5 F- ]/ U) T$ \. q1 d5 s) u+ Hflame of a Meeker burner, with the flask tilted so that the fusion of the
2 f8 v" e- |% T: S# ]sample and sodium bisulfate is concentrated at one end of the flask.
8 B0 c, j% ^. s$ t0 OSwirl constantly until the melt is clear (except for silica content), but
/ K$ S1 r) `1 Z, `$ jguard against prolonged heating to avoid precipitation of titanium
5 ] ^* ~" k2 `2 t+ ^5 O6 Edioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until! l$ I( n- z; ~
the mass has dissolved and a clear solution results. Cool, and dilute to
9 e. Z# A5 S* {3 ]120 ml with water. Introduce a magnetic stir bar into the flask.
3 z' y: m4 p& U& U! c9 ~Sample Solution B
6 @/ q' L) M/ O$ M& U. ?3 WPrepare 200 ml of an approximately 6.25 M solution of sodium8 V, s3 N7 X: u* d+ T; g9 D* O
hydroxide. Add 65 ml of this solution to Sample Solution A, while
) r( w' m& _0 E" ^2 ?' a! jstirring with the magnetic stirrer; pour the remaining 135 ml of the
" @8 ~1 m: d9 Q9 h- |alkali solution into a 500-ml volumetric flask.2 m( \/ q5 V! l M ] S+ O
Slowly, with constant stirring, add the sample mixture to the alkali( Z0 B) M1 u0 W- x
solution in the 500-ml volumetric flask; dilute to volume with water,. \) h, [& Q& f5 a- H! w" h
and mix. (Note: If the procedure is delayed at this point for more than8 u- ]0 R& r4 R0 Z
2 hours, store the contents of the volumetric flask in a polyethylene
, O0 q$ H" K- K0 c$ q5 m gbottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),1 a6 E; S5 P! {; R* s
then filter the supernatant liquid through a very fine filter paper. Label
& [# R- x3 [ S+ k; k) Gthe filtrate Sample Solution B.
2 P$ m9 a/ _, E9 c7 GSample Solution C7 N/ s" R( ]- n% B9 G" N) A
Transfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer, I3 b6 N a* s* M' _/ `+ H. k' z
flask, add 1 drop of methyl orange TS, acidify with hydrochloric acid4 e. Q2 H( X5 N; J) f& Y: A
solution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02
# g' a3 X6 c4 K. h& `5 wM disodium EDTA, and mix. [Note: If the approximate Al2O3 content is
2 s( f+ o6 o1 _) |0 Vknown, calculate the optimum volume of EDTA solution to be added: b9 e1 ^& f) v) ^! u U6 E
by the formula: (4 x % Al2O3) + 5.]
% B& u& _4 s/ i# u' PAdd, dropwise, ammonia solution (1 in 5) until the colour is just5 E5 ]4 Z! G3 @ S$ v0 C
completely changed from red to orange-yellow. Then add10 ml each+ Z; C, M0 R; n5 `! k* B) _
of Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to
) N; N! V/ }: nroom temperature in a stream of running water, add 3 drops of xylenol
6 }8 L' }" z8 S2 h4 _* {orange TS, and mix. If the solution is purple, yellow-brown, or pink,; z4 [& ?' j) ?8 i& P4 T
bring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired
. k: h2 A6 r/ |; j2 ?& ypH, a pink colour indicates that not enough of the EDTA solution has
5 v/ Y! B3 z4 h* B3 a% u9 Pbeen added, in which case, discard the solution and repeat this1 z+ ]* \* f' M$ s# y3 n8 R
procedure with another 100 ml of Sample Solution B, using 50 ml,2 }8 P% E: ~2 I; U- e9 q) A9 ^1 A
rather than 25 ml, of 0.02 M disodium EDTA.
4 C; y" Y9 p8 R3 ]+ _7 J/ w5 dProcedure5 ?8 p# b4 c& T9 i* ?. L
Using the standardized zinc sulfate solution as titrant, titrate Sample: K9 R3 |" T8 p9 o( U
Solution C to the first yellow-brown or pink end-point that persists for# `$ @* I" Z+ n
5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first
6 G' Q* N. Z# g0 v' ctitration should require more than 8 ml of titrant, but for more accurate
* ]0 Z8 d; X2 _8 o( ~$ Iwork a titration of 10-15 ml is desirable.
* @* n$ r" K/ p. G, wAdd 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5* f( h4 a5 k- J9 H9 V; p0 k
min, and cool in a stream of running water. Titrate this solution, using
8 ?7 i1 { F! t. e: T2 N. m9 ~the standardized zinc sulfate solution as titrant, to the same fugitive! u* ]( f: t8 Y9 H
yellow-brown or pink end-point as described above.
% x2 n/ x1 R. g0 S* p; NCalculation:
3 w! x% u+ A0 e% Y$ y6 x5 M* |% eCalculate the percentage of aluminium oxide (Al2O3) in the sample
& J8 B5 A4 f$ ?$ L _7 ytaken by the formula:
; H! f) n1 ?6 j/ V5 ]6 z% Al2O3 = 100 × (0.005VT)/S
- q. s+ u. p& S9 `7 c8 twhere, ?8 e* O7 w# V% }! N' q
V is the number of ml of 0.01 N zinc sulfate consumed in
( ?9 ]' _9 A3 u! d+ x, |the second titration,
/ I! C$ f8 O+ yT is the titre of the zinc sulfate solution," }! M* _( \7 \- C' k# q. m
S is the mass (g) of the sample taken, and
6 r6 C& F4 a7 H2 c0.005 = 500 ml / (1000mg/g × 100 ml)., Z, a2 k1 L4 O% l! ?0 Y2 `
Silicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica# ]+ k: a/ j- Y0 p+ ?0 `) y S
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
% Q& s3 X( ~7 X- W. Q( fHeat gently over a Meeker burner, while swirling the flask, until! U" x5 n8 }" O, E
decomposition and fusion are complete and the melt is clear, except% ]% l, F) ]0 U% G0 `
for the silica content, and then cool. (Caution: Do not overheat the
! |' [( Z6 E( M% @. `contents of the flask at the beginning, and heat cautiously during
3 a4 s" U* s c" u& i7 xfusion to avoid spattering.)
+ a0 {, K; V9 n+ rTo the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat1 l* P# `# C* j8 Q9 v6 d
carefully and slowly until the melt is dissolved. Cool, and carefully add
0 j$ h+ {! r9 b150 ml of water by pouring very small portions down the sides of the
! h" ~7 ?5 h7 Yflask, with frequent swirling to avoid over-heating and spattering. Allow: N9 y! S' {2 _+ ^
the contents of the flask to cool, and filter through fine ashless filter
; _6 X: G! d) X5 P8 C8 e" upaper, using a 60 degree gravity funnel. Rinse out all the silica from
/ C1 }7 y8 {8 C0 k" X8 rthe flask onto the filter paper with sulfuric acid solution (1 in 10).
8 f5 h- u/ C9 J2 _% ]8 m, o/ {0 B* U9 BTransfer the filter paper and its contents into a platinum crucible, dry in' a2 ~5 ~& B3 N4 _
an oven at 1200, and heat the partly covered crucible over a Bunsen' c2 {3 ?( H9 A6 l+ a
burner. To prevent flaming of the filter paper, first heat the cover from" P m5 F2 @ [7 x9 E2 _, e
above, and then the crucible from below.
" W. i/ l# ]& J4 T _When the filter paper is consumed, transfer the crucible to a muffle. q* U( b: q" s1 W4 D0 w! ^
furnace and ignite at 1000o for 30 min. Cool in a desiccator, and
- h1 R# n( i$ \weigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated. |4 b$ C1 ?) y8 D
hydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first
6 R& C3 d0 M% u! ?1 Oon a low-heat hot plate (to remove the HF) and then over a Bunsen e/ [2 [8 E2 O, M
burner (to remove the H2SO4). Take precautions to avoid spattering,
! P. \9 b% M2 respecially after removal of the HF. Ignite at 1000o for 10 min, cool in a. U! ?3 |% T7 m9 |: j8 ^- |4 M
desiccator, and weigh again. Record the difference between the two
% |5 W8 V- {; F) O9 ]5 ^weights as the content of SiO2 in the sample.9 u5 D1 M5 d( Q4 c1 y8 W- {
METHOD OF ASSAY( U; w' j7 m7 P; W* @5 l' ]% V
Accurately weigh about 150 mg of the sample, previously dried at 105o, P5 g/ L& \) o
for 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water) D+ g+ n% r% S8 c
and shake until a homogeneous, milky suspension is obtained. Add 30% m `! A6 I7 O
ml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially/ F- x5 H7 W% x" v
heat gently, then heat strongly until a clear solution is obtained. Cool,
+ o4 ~( e& y3 ^$ fthen cautiously dilute with 120 ml of water and 40 ml of hydrochloric
& k: C, N; @- d& q! w7 {acid, and stir. Add 3 g of aluminium metal, and immediately insert a& L+ I7 Q6 A: P1 q" @; B9 R* `
rubber stopper fitted with a U-shaped glass tube while immersing the
+ V) U" S6 K* t! I. X9 H; n6 Hother end of the U-tube into a saturated solution of sodium6 |; e: v n; N
bicarbonate contained in a 500-ml wide-mouth bottle, and generate4 ^; C8 R( k0 P5 u ]
hydrogen. Allow to stand for a few minutes after the aluminium metal
9 c3 \6 a. D7 L3 e9 dhas dissolved completely to produce a transparent purple solution.
0 x2 Q# t4 G yCool to below 50o in running water, and remove the rubber stopper% B) K, q4 C! X
carrying the U-tube. Add 3 ml of a saturated potassium thiocyanate
; `" T$ S# }3 y+ P- U: t4 i; xsolution as an indicator, and immediately titrate with 0.2 N ferric/ m/ ~5 `- [: Z6 p
ammonium sulfate until a faint brown colour that persists for 30
! y3 y' y. E% C8 R& G1 y$ b/ P* vseconds is obtained. Perform a blank determination and make any& P+ d# P0 m0 r2 _1 D
necessary correction. Each ml of 0.2 N ferric ammonium sulfate is
; ]& ~. w! }5 e0 S* h4 Fequivalent to 7.990 mg of TiO2.2 w8 j6 y8 n" d
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