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二氧化钛(钛白粉)
二氧化钛(钛白粉)
) @7 Y# k1 D) R2 M3 o, n7 I+ \0 K9 R; X+ A) A# c7 E
JECFA关于二氧化钛(钛白粉)的结论
) W7 R2 X2 c) @( X- e7 F: I3 K: g8 E# F7 w4 M9 [; r l7 A
摘要: 2006年JECFA关于二氧化钛的结论
[9 S% a: d# b% N6 CADI值:不作限制。3 V: W( q# }9 c/ f# r9 N
功能:着色剂, c+ h$ p8 n$ n& H
. ?. M; r2 y" t
TITANIUM DIOXIDE
, Z0 J% G4 |6 Z' @" N0 `* w5 o% pPrepared at the 67th JECFA (2006) and published in FAO JECFA% H" l9 w& {* l% C+ p' |- c4 ]% L5 S
Monographs 3 (2006), superseding specifications prepared at the 63rd
+ G2 w1 Q: S) ]5 ]) PJECFA (2004) and published in FNP 52 Add 12 (2004) and in the3 r- l4 g0 @4 w2 e7 a" W& J8 d6 z; O
Combined Compendium of Food Additive Specifications, FAO JECFA
" a+ z3 C8 n( x1 ~# N8 n; MMonographs 1 (2005). An ADI “not limited” was established at the 13th3 h/ L! c. \9 h1 |$ u
JECFA (1969).
* ]4 v% X/ i) ]9 |( h9 M' o+ PSYNONYMS
: ]# F& x1 W# \" @Titania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171 ?, b* \! a$ X1 y( |8 m
DEFINITION
" `6 q% y) {# f/ cTitanium dioxide is produced by either the sulfate or the chloride
; T9 {8 p# D! f/ ~process. Processing conditions determine the form (anatase or rutile
" e: I* H* c% _) rstructure) of the final product.. R) ~6 K" O x( M. p
In the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)
9 S ^- j1 F1 }0 c# j( gor ilmenite and titanium slag. After a series of purification steps, the& }+ |; F. m" F6 G5 a
isolated titanium dioxide is finally washed with water, calcined, and
' u! [8 `- o+ \' m! M' hmicronized.
' c5 g# x. H( g. K, e( ]In the chloride process, chlorine gas is reacted with a titaniumcontaining6 @ O0 L) h" ~; C0 b
mineral under reducing conditions to form anhydrous2 M$ M1 O, X, y2 J9 ^
titanium tetrachloride, which is subsequently purified and converted to
3 ~4 `" P: @3 h( Btitanium dioxide either by direct thermal oxidation or by reaction with8 ?# T/ o4 |0 V
steam in the vapour phase. Alternatively, concentrated hydrochloric
2 j4 C8 q+ R& @7 C# Yacid can be reacted with the titanium-containing mineral to form a" p1 R/ {2 }$ v$ [* ?0 B$ {$ i! h: p
solution of titanium tetrachloride, which is then further purified and# k7 N1 S! Q- G; M$ J& x+ l5 I
converted to titanium dioxide by hydrolysis. The titanium dioxide is3 y6 u; ]$ ?3 j& w' f
filtered, washed, and calcined.
2 Z+ b, |% a7 B1 k, t* \Commercial titanium dioxide may be coated with small amounts of1 J2 ~! t. n' |$ r1 @/ x+ h) ]
alumina and/or silica to improve the technological properties of the
& e9 `' p/ D. G6 e4 Wproduct.
6 W1 D) G% F: i, ~# A: X2 `C.A.S. number 13463-67-74 @- k8 M. Z" x" y4 J9 G4 w/ W- K3 b
Chemical formula TiO2( Z& R m8 }- F! E0 F" L! S2 E
Formula weight
5 X; E) M: u q5 y& {, _4 d79.88
9 y Q r' {2 P0 j: \1 vAssay5 @( ^$ v) w1 E4 v4 e* u
Not less than 99.0% on the dried basis (on an aluminium oxide and6 g4 c8 A. v4 Z
silicon dioxide-free basis)
% [6 ~" o5 E, a5 `" J) C. mDESCRIPTION
$ W0 H0 `$ G8 f+ X& D0 }/ nWhite to slightly coloured powder: P! f0 x5 v6 ]: M* t0 f
FUNCTIONAL USES
0 y1 r* V; A8 E, I7 k8 P; sColour
/ B. |% o% T% g V. XCHARACTERISTICS* f [7 v0 S' P- H
IDENTIFICATION' m+ i" _; S8 d3 b) F( G
Solubility (Vol. 4)
$ p- Q- A3 m9 _+ P6 M( ~* E& GInsoluble in water, hydrochloric acid, dilute sulfuric acid, and organic* Z4 W# A9 e9 v/ ^) ~, m
solvents. Dissolves slowly in hydrofluoric acid and hot concentrated1 Y% O- j+ ?1 i8 j9 d1 i
sulfuric acid.
3 C4 ]1 a* t/ \' t, Q! q# B- r1 XColour reaction
+ e( g) C) W! E ` S( x6 ? rAdd 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of
) k4 ?/ D) ]3 {sulfuric acid appear, then cool. Cautiously dilute to about 100 ml with
- i3 U5 | F: |, Cwater and filter. To 5 ml of this clear filtrate, add a few drops of/ B2 F1 O5 ^8 c0 B* H3 p) H
hydrogen peroxide; an orange-red colour appears immediately.
( m2 s, U( n" d4 e0 M. t/ E1 M. ?5 r! rPURITY" n" ~( e, F- U$ s! `9 X: P
Loss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)$ i7 R# U1 ?$ R3 W5 K5 }( b
Loss on ignition (Vol. 4): m4 a; m. Q% b" K N7 z: v2 L
Not more than 1.0% (800o) on the dried basis
" V, Z% ?2 M0 p2 V* p" N6 j; xAluminium oxide and/or) @- j& _: c7 i& j, K1 t4 l
silicon dioxide7 {$ z. n; o) c( O7 }
Not more than 2%, either singly or combined
7 \1 v c' H/ H% Y DSee descriptions under TESTS& z9 O) S/ l J& m( v. [- h O
Acid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing
6 u! P$ S/ l! H, M; l0 C/ s2 Ialumina or silica. J8 F, U! g+ W6 I1 }5 A. P9 R
Suspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and
+ E$ Y4 G1 z$ q- p% `place on a steam bath for 30 min with occasional stirring. Filter$ L. ~. M( d) p, H! @
through a Gooch crucible fitted with a glass fibre filter paper. Wash
3 D" B7 C* P; N( J: s. r9 Vwith three 10-ml portions of 0.5 N hydrochloric acid, evaporate the. _; E- E, |5 w8 I
combined filtrate and washings to dryness, and ignite at a dull red
. k7 ~8 H8 d4 c6 t! Gheat to constant weight.4 a' l! r6 M7 ~% v% v
Water-soluble matter7 c! m4 }! R7 Y; W+ ~! ~8 f
(Vol. 4): _' b2 b2 X3 |: m3 J3 R2 D: x
Not more than 0.5%, x! W1 I5 ^ v' v6 f1 J
Proceed as directed under acid-soluble substances (above), using
6 D. a/ U, Q* twater in place of 0.5 N hydrochloric acid.
( u" M, {' i' r' ^Impurities soluble in 0.5 N2 o) o$ A Q) W9 l
hydrochloric acid# Q3 u! Z( Y/ T2 `
Antimony Not more than 2 mg/kg9 P& T5 Y# h& ~4 t
See description under TESTS
# R( V- e, U t" q' XArsenic Not more than 1 mg/kg1 a& H. f9 i7 a9 z
See description under TESTS
5 E% a% H4 A$ F9 N; N+ }Cadmium Not more than 1 mg/kg$ N o. |" A7 S' ]$ X$ ?
See description under TESTS! f% v& E. m( P. H, G( S2 h* N
Lead) p. w; l" i7 s [4 Y% K. C
Not more than 10 mg/kg
% ^: C6 d8 ]( R1 y' H- W8 i$ PSee description under TESTS R* B! @+ u6 z( @3 \7 v
Mercury (Vol. 4) Not more than 1 mg/kg& ^" T4 D, x+ _& U
Determine using the cold vapour atomic absorption technique. Select a
7 y- \0 N" k! C7 {7 t5 `sample size appropriate to the specified level1 d! U5 S* w Z" X3 G
TESTS
4 e4 j5 A5 V- E4 z+ [% T* VPURITY TESTS- q9 V$ Q; F: Q$ O) l
Impurities soluble in 0.5 N0 a3 o" `( Q0 O% Z
hydrochloric acid' _8 r2 b5 c0 A2 M4 A
Antimony, arsenic,* [" _8 R% i/ m
cadmium and lead8 n, G6 v+ h7 l L* F
(Vol.4)2 J& P, F( E. ?5 E) G1 X# ?
Transfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N
4 \* \% G& i6 b: T3 p( t1 Thydrochloric acid, cover with a watch glass, and heat to boiling on a4 l% l* I6 Q$ t# i
hot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml
0 ?$ J) ^/ {( Z: H* w) I kcentrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved" [ }6 G, c, \& { D- Z- M
material settles. Decant the supernatant extract through a Whatman, |+ M: B! N9 F D1 X: l7 j% [
No. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml: c {+ ~# _& q0 `" m
volumetric flask and retaining as much as possible of the undissolved- n' V, l) W+ C: w& f' c: a/ h
material in the centrifuge bottle. Add 10 ml of hot water to the original! D/ s) c) i1 k- \% S2 [ o
beaker, washing off the watch glass with the water, and pour the
. I" G5 _6 O& O( D/ S- _1 Vcontents into the centrifuge bottle. Form a slurry, using a glass stirring
& H2 I$ T9 k f7 C3 i3 Mrod, and centrifuge. Decant through the same filter paper, and collect+ R O8 O: ~: v* |( B( v
the washings in the volumetric flask containing the initial extract.8 D0 j! [4 O+ H+ U- F
Repeat the entire washing process two more times. Finally, wash the
* k- J' |4 U: G+ z7 d" v- v* @filter paper with 10 to 15 ml of hot water. Cool the contents of the flask( v9 W# R4 y" ?1 S4 y
to room temperature, dilute to volume with water, and mix.. d" Q6 h+ U3 q. W
Determine antimony, cadmium, and lead using an AAS/ICP-AES4 ~/ |: C* y: E9 `
technique appropriate to the specified level. Determine arsenic using the
4 m3 W+ Q y4 |! |: WICP-AES/AAS-hydride technique. Alternatively, determine arsenic using
x9 q& c: {- o$ Z: c% r& sMethod II of the Arsenic Limit Test, taking 3 g of the sample rather than
3 U) V+ ~0 v9 J5 \ ?8 g, |1 g. The selection of sample size and method of sample preparation
. w3 F" v! g; P1 p" G# p6 pmay be based on the principles of the methods described in Volume 4.% Q! d G9 h7 w+ x/ N
Aluminium oxide Reagents and sample solutions/ Q3 V2 i8 O4 H$ S$ `+ q
0.01 N Zinc Sulfate
3 w+ P4 F( y0 {0 K$ ?! x- eDissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to
5 Z* I, H) t! |( imake 1000 ml. Standardize the solution as follows: Dissolve 500 mg
8 _) p7 `" K2 Y8 }5 R; sof high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of
! U. d1 z( o# I7 D/ v1 W: \$ r& vconcentrated hydrochloric acid, heating gently to effect solution, then9 L7 [) y- N- ]$ E( b6 L
transfer the solution into a 1000-ml volumetric flask, dilute to volume
9 ?8 f5 C2 ? O" j$ t3 y" I; j6 cwith water, and mix. Transfer a 10 ml aliquot of this solution into a 500, ]6 l W, n" H# Z0 g4 h) u
ml Erlenmeyer flask containing 90 ml of water and 3 ml of w0 c. p7 K3 d; y
concentrated hydrochloric acid, add 1 drop of methyl orange TS and* N) q5 |* a4 I1 E% L3 K A
25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,
Y9 `, J9 ~ R7 {4 z2 D# Z# Rdropwise, ammonia solution (1 in 5) until the colour is just completely& p. a3 Q, \8 q
changed from red to orange-yellow. Then, add:
9 p" x& }3 X: j( g$ ?(a): 10 ml of ammonium acetate buffer solution (77 g of
( z' M. c$ \; a. o# C S- z+ Uammonium acetate plus 10 ml of glacial acetic acid, dilute to
( V0 u% ^3 N& w6 K. H) l; }6 E1000 ml with water) and
, p" \: L/ I7 `3 E% a* Q4 s(b): 10 ml of diammonium hydrogen phosphate solution (150 g& C4 ?! c: i" g6 Z& Q, F
of diammonium hydrogen phosphate in 700 ml of water,* M& x" ]5 Y; z! B% |+ t$ F
adjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,
1 S4 d. o8 K5 T) h# Bthen dilute to 1000 ml with water).1 Y! x0 ?0 J! W( J5 r# N. W$ W
Boil the solution for 5 min, cool it quickly to room temperature in a% B; ^7 o' t, P' z, B4 B1 f6 W' v
stream of running water, add 3 drops of xylenol orange TS, and mix., T9 I1 F; b2 K- `' I; H8 A
Using the zinc sulfate solution as titrant, titrate the solution to the first
; S2 N0 P& I7 C% X' u& j2 |yellow-brown or pink end-point colour that persists for 5-10 sec. (Note:% X0 ^! x" `/ \/ U$ O7 S! T
This titration should be performed quickly near the end-point by: L& t2 R9 \- x0 d: ]: M
adding rapidly 0.2 ml increments of the titrant until the first colour
e1 B2 i3 W Y8 S1 e5 p0 [$ ?change occurs; although the colour will fade in 5-10 sec, it is the true( e( }' B4 m q% B2 G
end-point. Failure to observe the first colour change will result in an6 A1 X7 V3 C; _0 m& o+ E
incorrect titration. The fading end-point does not occur at the second: l& Q A3 ?; Y+ c7 O' A% \
end-point.)* D3 e, t& P4 `& b3 t8 k
Add 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a4 v: n' U5 l% u
stream of running water. Titrate this solution, using the zinc sulfate
0 _7 n( C& O0 @8 ~- i6 Qsolution as titrant, to the same fugitive yellow-brown or pink end-point
: F; F( V6 j, O1 x! X( {: `as described above.5 p# Z2 r1 K4 n8 ^
Calculate the titre T of zinc sulfate solution by the formula:
: J# ^! D+ x R- U2 r- E0 ET = 18.896 W / V2 [8 J' N T& x' \& L; D" h
where
]1 q p/ s5 h& U! K5 m* E, r/ UT is the mass (mg) of Al2O3 per ml of zinc sulfate solution
% z0 d% E1 t; i' B$ k, CW is the mass (g) of aluminium wire
6 b3 `( l, f& T' OV is the ml of the zinc sulfate solution consumed in the
- r+ p: X# @) p8 N! G- Qsecond titration
! R; S; Y; W+ j9 x# P6 v* m18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and" Z8 e: I9 c- x; _' o
R is the ratio of the formula weight of aluminium oxide to
5 y, R/ q+ R* B! m/ F6 T' v. g5 k; Tthat of elemental aluminium.
) q# |! Z) ?; ~( Q fSample Solution A
$ ]/ H( y9 B3 cAccurately weigh 1 g of the sample and transfer to a 250-ml high-silica
9 U0 b5 B' G% ~! _% aglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
; {) S* W* U" b, Y3 D$ u9 ]7 m(Note: Do not use more sodium bisulfate than specified, as an excess! }8 S4 k% J; J
concentration of salt will interfere with the EDTA titration later on in the6 G: r# H n5 F/ z! j6 S
procedure.) Begin heating the flask at low heat on a hot plate, and, w, E9 A! N6 p
then gradually raise the temperature until full heat is reached.1 q4 q8 s8 _/ t& A5 L* j1 P* o# [/ ]1 W
(Caution: perform this procedure in a well ventilated area. ) When' F+ B- y5 ~$ l; x0 ~
spattering has stopped and light fumes of SO3 appear, heat in the full
5 l# ~/ v5 }; t' kflame of a Meeker burner, with the flask tilted so that the fusion of the. p6 E5 \1 l5 K2 F" s5 M# I, _
sample and sodium bisulfate is concentrated at one end of the flask.6 {/ `# k' A: e$ C2 T! _
Swirl constantly until the melt is clear (except for silica content), but2 w" J! O9 O3 |. i$ s, g
guard against prolonged heating to avoid precipitation of titanium( ^ m" ?. N* Q g; E" E5 \7 m3 c
dioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until
@0 p$ ~4 R* \) R5 E$ ithe mass has dissolved and a clear solution results. Cool, and dilute to
! P8 R' r1 b+ d120 ml with water. Introduce a magnetic stir bar into the flask.
4 b. }# b- T+ d( j; PSample Solution B" l! H7 V4 n/ `- V4 F" I
Prepare 200 ml of an approximately 6.25 M solution of sodium
* L4 U, {7 Z% o) C" hhydroxide. Add 65 ml of this solution to Sample Solution A, while7 j$ J0 o2 H" b& D
stirring with the magnetic stirrer; pour the remaining 135 ml of the% `! V3 S" e# [) Q. |
alkali solution into a 500-ml volumetric flask.
9 w2 Z7 P: q O% T3 U, {Slowly, with constant stirring, add the sample mixture to the alkali
8 M: v9 I# j* r r2 {; ^solution in the 500-ml volumetric flask; dilute to volume with water,* w) k! b: g# q( p' b
and mix. (Note: If the procedure is delayed at this point for more than8 l) [! j( K' v* @
2 hours, store the contents of the volumetric flask in a polyethylene
3 d8 [% i7 v$ Nbottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),
6 s1 s3 v0 W( z% q+ q& Mthen filter the supernatant liquid through a very fine filter paper. Label
! o9 i, B1 X7 Q# B& G; `the filtrate Sample Solution B.8 v( o/ n& X1 P: `0 J
Sample Solution C; ^ M9 m' G9 n; m. a
Transfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer! |; E+ X. w, N
flask, add 1 drop of methyl orange TS, acidify with hydrochloric acid; J- {9 X! K, d3 \' |: i. g
solution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02
. N/ ]! ^4 t. zM disodium EDTA, and mix. [Note: If the approximate Al2O3 content is8 M0 D/ D, P5 D
known, calculate the optimum volume of EDTA solution to be added
0 ^& a6 s9 k( w! U) p) ]by the formula: (4 x % Al2O3) + 5.]
1 O4 Y% L/ L, H( K6 B' aAdd, dropwise, ammonia solution (1 in 5) until the colour is just- i* V! J3 h$ Y3 W, o: C5 e4 I% D
completely changed from red to orange-yellow. Then add10 ml each
' ?8 F5 c+ b; |of Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to: [7 C& R" O7 J, i- r
room temperature in a stream of running water, add 3 drops of xylenol
" T! P0 j& _+ `* V3 ~9 morange TS, and mix. If the solution is purple, yellow-brown, or pink, t& b9 P% ~. D
bring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired
/ c% d) [- N; h# o$ ?- spH, a pink colour indicates that not enough of the EDTA solution has4 M4 ]0 H, v- X) ^
been added, in which case, discard the solution and repeat this
: ~2 P) c+ y+ T' w( Iprocedure with another 100 ml of Sample Solution B, using 50 ml,
6 y: Q {$ V2 I$ e+ u1 v9 V8 erather than 25 ml, of 0.02 M disodium EDTA.
# J& c8 Y# l$ S) }* CProcedure
6 Y2 {2 L/ J v7 s! } ]Using the standardized zinc sulfate solution as titrant, titrate Sample+ g# J7 r# P: N0 i# F1 F! A
Solution C to the first yellow-brown or pink end-point that persists for7 E& S( m7 \& K: J" ~/ }4 h
5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first
8 @5 z. ^: J0 Z F [. Utitration should require more than 8 ml of titrant, but for more accurate l" x0 |' Y6 q+ d' }2 N
work a titration of 10-15 ml is desirable.
3 T; ~3 \/ |0 d g" H9 vAdd 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5& U3 b- s! d) x |! R8 ?; m' b
min, and cool in a stream of running water. Titrate this solution, using, }# o+ {* W, H+ _
the standardized zinc sulfate solution as titrant, to the same fugitive! |: e9 q5 L6 N% z9 X
yellow-brown or pink end-point as described above.+ E5 Z! P. I/ W0 z
Calculation:# O4 A3 c5 G: G# I
Calculate the percentage of aluminium oxide (Al2O3) in the sample
! d* Y i% D4 l+ q, \taken by the formula:* N8 t0 y8 ^. U
% Al2O3 = 100 × (0.005VT)/S
8 i; S1 U1 M) H1 s3 gwhere
& T! O: E9 r9 B& z9 d5 B/ \, b( hV is the number of ml of 0.01 N zinc sulfate consumed in8 R3 b- Z+ v( C' D$ L
the second titration,
" |) C* k% q5 q+ A9 K; `- E3 H! L+ V' tT is the titre of the zinc sulfate solution,
7 a/ D1 L# C/ }7 N! ~9 M( PS is the mass (g) of the sample taken, and
1 G7 s, W' _" A! y% C) }: H% Y0 s0.005 = 500 ml / (1000mg/g × 100 ml).
; A5 e0 N. t1 }) pSilicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica& X m, u3 `# V
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).5 u0 ^) v6 ^: u" k( Q
Heat gently over a Meeker burner, while swirling the flask, until l0 B2 B* @( n5 V
decomposition and fusion are complete and the melt is clear, except/ z' i4 w' _! u1 `. A* ~% c
for the silica content, and then cool. (Caution: Do not overheat the6 ?* y9 T- A# w' J ~5 J- ]
contents of the flask at the beginning, and heat cautiously during) E0 {9 _- ^% X5 L% Y" ^; t# D
fusion to avoid spattering.), i, H: p, p: V' }
To the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat8 X- g2 U. l- j; p2 S
carefully and slowly until the melt is dissolved. Cool, and carefully add
: Z; T$ j% E+ m1 C6 w150 ml of water by pouring very small portions down the sides of the! T/ X5 m: a! H0 R; o b% }) @/ Y
flask, with frequent swirling to avoid over-heating and spattering. Allow
$ t8 s, q8 S' c: _. t6 T/ Gthe contents of the flask to cool, and filter through fine ashless filter
. k4 O5 v# g: F9 b4 Gpaper, using a 60 degree gravity funnel. Rinse out all the silica from
8 f& L. X! b& f! M' Z( ^the flask onto the filter paper with sulfuric acid solution (1 in 10).. l) V0 V, p9 U
Transfer the filter paper and its contents into a platinum crucible, dry in, L# ^; g6 i2 }# {; D
an oven at 1200, and heat the partly covered crucible over a Bunsen
9 B& N1 x! E$ _burner. To prevent flaming of the filter paper, first heat the cover from
# n# E: t2 ?+ B$ habove, and then the crucible from below.
; ~( U J' ~- `5 b0 |0 t" b2 O' IWhen the filter paper is consumed, transfer the crucible to a muffle
# I4 P% ?0 X7 [4 hfurnace and ignite at 1000o for 30 min. Cool in a desiccator, and2 ~' C" I" w+ a1 l/ `4 X9 V
weigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated
; w9 r7 D1 X R4 M$ A# H$ Khydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first3 z) i' |7 ?( D0 g
on a low-heat hot plate (to remove the HF) and then over a Bunsen0 s; ~4 J- O1 |! ^9 A- J* \9 w+ u
burner (to remove the H2SO4). Take precautions to avoid spattering,, {+ r6 ?! _5 H; e' d2 g
especially after removal of the HF. Ignite at 1000o for 10 min, cool in a* K% \, ?2 l# Z0 ^! Q- s. Z# R) x. i: `
desiccator, and weigh again. Record the difference between the two5 D' Y3 N5 W' \3 k& m7 n- Y' Z7 @
weights as the content of SiO2 in the sample.. z. o, F/ Y& K* h9 L
METHOD OF ASSAY7 r1 ]; k. _! h$ O
Accurately weigh about 150 mg of the sample, previously dried at 105o
! n" k: l1 h" V( w8 f% C( \% qfor 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water* Y- b/ `7 L& U5 R7 X6 A% g
and shake until a homogeneous, milky suspension is obtained. Add 30
$ Z: S r' d+ f5 q9 o4 ]% \ml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially
) H" ~- b$ F: Z |5 uheat gently, then heat strongly until a clear solution is obtained. Cool,6 U+ v/ L6 w, \: {. ~1 k$ V, N
then cautiously dilute with 120 ml of water and 40 ml of hydrochloric
* C8 a9 T0 Y! M& t0 y1 q- ]7 Cacid, and stir. Add 3 g of aluminium metal, and immediately insert a3 y* `; J. v D. }8 b4 W& i3 b& n9 `; I
rubber stopper fitted with a U-shaped glass tube while immersing the
+ \, G7 k- Z9 n( y3 ^* C aother end of the U-tube into a saturated solution of sodium
; H& T [$ S% T! m2 Vbicarbonate contained in a 500-ml wide-mouth bottle, and generate
) [7 K- P% p& k- |/ b, _ fhydrogen. Allow to stand for a few minutes after the aluminium metal
" t+ `0 u# {. i1 e! v% J+ J# O# u# Zhas dissolved completely to produce a transparent purple solution." h6 }* o" i! F# _$ e7 k5 |
Cool to below 50o in running water, and remove the rubber stopper
0 ]8 z1 A- g R$ M0 Gcarrying the U-tube. Add 3 ml of a saturated potassium thiocyanate; i6 `1 Q& N) l: V7 v
solution as an indicator, and immediately titrate with 0.2 N ferric9 v. H7 |; }9 f5 O. J$ H) q5 p. v
ammonium sulfate until a faint brown colour that persists for 30
( P1 M. F; @* T/ wseconds is obtained. Perform a blank determination and make any
7 C5 r" z0 Q! T0 R" L+ a/ U3 [necessary correction. Each ml of 0.2 N ferric ammonium sulfate is
( K0 F% L u+ x* h) \ w5 Z( sequivalent to 7.990 mg of TiO2.$ m5 v( w) \" u4 k# q# T
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