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二氧化钛(钛白粉)
二氧化钛(钛白粉)
; L" x$ n/ Y3 C7 P
9 _! `* W! s+ P7 }; rJECFA关于二氧化钛(钛白粉)的结论
4 G0 R5 d: w4 D/ i: S! R2 W* c7 p. J" D4 ~+ t, G
摘要: 2006年JECFA关于二氧化钛的结论
y: ?& r6 Q7 k6 Q9 qADI值:不作限制。8 p: L& @7 a; d
功能:着色剂4 d) q3 x( Z% E. q
. N# {' I: C# w7 [; K# oTITANIUM DIOXIDE
: F! u' c8 ~# sPrepared at the 67th JECFA (2006) and published in FAO JECFA N. @/ h3 K4 A! ~
Monographs 3 (2006), superseding specifications prepared at the 63rd
# m9 C2 |' y' P. [ l6 YJECFA (2004) and published in FNP 52 Add 12 (2004) and in the- T% R( r% V; D' y) ]
Combined Compendium of Food Additive Specifications, FAO JECFA7 E+ h& C# H- J* d1 }& y0 x
Monographs 1 (2005). An ADI “not limited” was established at the 13th4 f6 ]$ P/ U% k7 _: v9 Y# t0 l
JECFA (1969).9 l! k3 o) R4 K, F
SYNONYMS4 o# x- i* U& R! n7 c7 n
Titania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171
. c {8 P3 Y& y; |% N) |DEFINITION7 H# m. H6 T4 h8 C0 r$ o( r- T' d
Titanium dioxide is produced by either the sulfate or the chloride
# H$ U% W7 L" ]2 t% s0 }8 Yprocess. Processing conditions determine the form (anatase or rutile# m9 ]* L" a( I- b+ O
structure) of the final product.
( C( _* \ o. g! v, T1 IIn the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)
7 m5 }9 O" F* H; i1 o; t& k; _or ilmenite and titanium slag. After a series of purification steps, the/ t0 g# z7 p" ]. F2 U) X' G- r3 Z: c
isolated titanium dioxide is finally washed with water, calcined, and6 [9 V. w4 E, ^& X* O
micronized.
! Q! K2 D2 c/ i L w+ BIn the chloride process, chlorine gas is reacted with a titaniumcontaining8 u2 B+ S. J- P+ m8 W/ f3 ~+ Z
mineral under reducing conditions to form anhydrous- e: m" B1 H2 J
titanium tetrachloride, which is subsequently purified and converted to0 W- w' n2 Z* S1 ]
titanium dioxide either by direct thermal oxidation or by reaction with
6 a% B$ u/ i8 a' x s0 Esteam in the vapour phase. Alternatively, concentrated hydrochloric; i; F) v3 ?0 i0 l- I0 X5 N, c7 j
acid can be reacted with the titanium-containing mineral to form a- N9 ]8 j) T' a. ^
solution of titanium tetrachloride, which is then further purified and7 r+ s/ N, x! D6 g3 ?8 B5 R% |
converted to titanium dioxide by hydrolysis. The titanium dioxide is$ E9 l3 D% e2 D3 I9 h6 h
filtered, washed, and calcined.* K$ W( G0 D" C, Y5 X. X" [& h* ]
Commercial titanium dioxide may be coated with small amounts of4 z9 W( x" F% {# n
alumina and/or silica to improve the technological properties of the' {+ E% @' V( A" P; M* C7 T
product. b; x0 a# m$ d4 v4 Z1 [. b
C.A.S. number 13463-67-7$ N- K8 d& ~! B+ E0 n$ J4 s% ]
Chemical formula TiO2
; ?; e# ]/ [ F+ {2 xFormula weight
9 L0 B6 n/ f$ H; x' [79.880 T6 K; Q- g9 s3 ] `0 Y
Assay) Q8 T |! ~7 @" H( B: ]7 u
Not less than 99.0% on the dried basis (on an aluminium oxide and
; A) s/ _/ R& z2 H% z% o- Jsilicon dioxide-free basis)& O8 @- H) W( r) Y/ i/ o# ~0 x
DESCRIPTION
1 R4 {8 u! m' H3 h3 fWhite to slightly coloured powder
* c! w- X5 ~( R* w3 x g$ XFUNCTIONAL USES
) L0 H- E( D/ I+ {9 ^! YColour! e. N; `. u4 y9 _
CHARACTERISTICS5 T" n- H/ A- l& ^: |$ w) x
IDENTIFICATION7 q* J, g% Y$ i4 t$ x# t
Solubility (Vol. 4)
2 L0 _+ k0 E3 _% A0 a; [. }0 l5 LInsoluble in water, hydrochloric acid, dilute sulfuric acid, and organic
/ h. ^# n8 h3 {+ z9 Lsolvents. Dissolves slowly in hydrofluoric acid and hot concentrated
1 n! v4 F, C& P3 Z& _sulfuric acid.
9 ?) Y8 x! u) L: H7 e. f; _Colour reaction8 F# D! c; J4 P
Add 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of
5 d; Q& a% P5 E8 Z) c! ] gsulfuric acid appear, then cool. Cautiously dilute to about 100 ml with
) X; w8 |' h1 w8 twater and filter. To 5 ml of this clear filtrate, add a few drops of, ^/ D( }6 X0 r4 O/ X3 T6 Y
hydrogen peroxide; an orange-red colour appears immediately.
M6 x! s# |4 O1 T9 DPURITY9 n9 g4 W; j5 [7 E0 v
Loss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)
8 z/ g9 e" U% d3 `1 F# L1 X' _- MLoss on ignition (Vol. 4)* K7 g5 X4 U m$ J4 `9 V
Not more than 1.0% (800o) on the dried basis9 E- |$ t+ J2 _! e% k4 z/ u6 T
Aluminium oxide and/or1 ^/ u8 G; F* N9 |
silicon dioxide
/ Q' ~ D7 f; B TNot more than 2%, either singly or combined! [" m2 f+ k, t$ e" _2 X
See descriptions under TESTS4 ^2 D! | g5 |% ^$ c. o& j& i
Acid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing
5 [8 v" h9 U: n- ^ l& Valumina or silica.% m' p- y D$ ?9 q- z
Suspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and/ y: _0 r7 O: @$ |# L) \6 M; p( g
place on a steam bath for 30 min with occasional stirring. Filter
0 }8 k6 x7 B+ Vthrough a Gooch crucible fitted with a glass fibre filter paper. Wash- i1 {% i, d" L, l/ _
with three 10-ml portions of 0.5 N hydrochloric acid, evaporate the
( M$ G% M5 k+ G, O" U1 L# X/ qcombined filtrate and washings to dryness, and ignite at a dull red/ E. t& q$ l8 h+ B) x3 y/ S" ^
heat to constant weight.
2 d" a' H$ H7 R+ |Water-soluble matter
6 p( r' a \4 ?(Vol. 4)
+ W) T+ e' y$ X& @; R! }* T& ^Not more than 0.5%
/ Q& Z/ z1 W1 s1 b* h1 t: t2 FProceed as directed under acid-soluble substances (above), using
) F" x7 O5 |& ^' \3 S3 c/ H2 pwater in place of 0.5 N hydrochloric acid.
" _" q% y9 @: e5 a+ l7 CImpurities soluble in 0.5 N
; O) [4 l7 t) C# i' Chydrochloric acid
0 ?% M& b6 o( B% q t7 T8 ~Antimony Not more than 2 mg/kg& N4 j8 o# P% ~% W1 c4 c+ I
See description under TESTS+ `$ `7 h% F% b& n! w8 b3 h- I7 c3 q
Arsenic Not more than 1 mg/kg
8 v( R+ P# [3 R {8 t: i* O6 JSee description under TESTS
% Z7 ^8 |+ U, u6 O- M; WCadmium Not more than 1 mg/kg
+ A& A" v1 r& G% f- S1 tSee description under TESTS6 |3 m: F( z, s! T3 s4 o& V! [
Lead u; d! _5 x0 G; Z* R
Not more than 10 mg/kg0 [$ Y1 Q( i" b# G
See description under TESTS
- D- f" ~7 j- v4 i8 ZMercury (Vol. 4) Not more than 1 mg/kg
4 }0 u( E) b0 \# F9 wDetermine using the cold vapour atomic absorption technique. Select a1 B" Z( E: n5 j& t% q* Y
sample size appropriate to the specified level( b+ P6 L% v2 s5 z
TESTS
# L* M/ U# s! BPURITY TESTS: U/ r$ m) w4 f* n. v, R
Impurities soluble in 0.5 N
6 t c4 \$ {6 C" Xhydrochloric acid' u8 m: ? e8 K( T4 @8 l
Antimony, arsenic,
z: b& a5 S) x- x4 [& rcadmium and lead
D$ w3 o3 I+ I! p, w) {(Vol.4)2 { O5 z! N5 v s; j/ ^
Transfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N" l; Q# V" m( @# H
hydrochloric acid, cover with a watch glass, and heat to boiling on a6 c* I4 [1 j) P4 l+ r: E
hot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml9 F# k5 p# H" | F0 t
centrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved
; K+ |9 [! z0 R" D/ Pmaterial settles. Decant the supernatant extract through a Whatman" p! [- h( C- F t) p1 d" ]
No. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml n. v5 n3 t4 S2 d P% y' v
volumetric flask and retaining as much as possible of the undissolved
- r5 \+ \: z$ [4 Z6 q+ Gmaterial in the centrifuge bottle. Add 10 ml of hot water to the original+ C- t" U( Q9 a% }( J0 W* O0 H9 Y
beaker, washing off the watch glass with the water, and pour the/ N0 T) X6 |' H7 U$ f
contents into the centrifuge bottle. Form a slurry, using a glass stirring
0 Z I/ H9 U: f% Yrod, and centrifuge. Decant through the same filter paper, and collect
5 F# e7 s5 V4 I' |- lthe washings in the volumetric flask containing the initial extract." i0 M6 N8 k% i- J: {0 q
Repeat the entire washing process two more times. Finally, wash the
5 {1 O; d1 D5 e4 {( L& Tfilter paper with 10 to 15 ml of hot water. Cool the contents of the flask! ]! O1 v3 @2 K, F8 J
to room temperature, dilute to volume with water, and mix.
; J }5 U/ f6 M# B' [3 ]1 S. `# kDetermine antimony, cadmium, and lead using an AAS/ICP-AES6 w \: V1 S) D/ a5 y
technique appropriate to the specified level. Determine arsenic using the
" u: H; k; R1 ?) M5 [1 ^& @: wICP-AES/AAS-hydride technique. Alternatively, determine arsenic using7 }& r" u2 Q& W) ^- p3 m, n" U; w' {
Method II of the Arsenic Limit Test, taking 3 g of the sample rather than
4 r& k5 {0 |, _2 L7 [1 g. The selection of sample size and method of sample preparation
" b: B& [: P) l/ ?: Z9 cmay be based on the principles of the methods described in Volume 4.' \5 U- G- G$ J1 L0 X" s! c: m' ?
Aluminium oxide Reagents and sample solutions
2 N1 V; k7 S, x, |' \0.01 N Zinc Sulfate
1 J9 ~1 @* y! r2 Y0 f; kDissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to0 n' k6 T, t J L3 G5 ~( w1 D* @
make 1000 ml. Standardize the solution as follows: Dissolve 500 mg. R4 V$ Q) e I2 T
of high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of
5 T0 v& y" o, \# y; ~* X( ]concentrated hydrochloric acid, heating gently to effect solution, then# @1 d( L3 @- |1 @9 ~6 z/ |
transfer the solution into a 1000-ml volumetric flask, dilute to volume
1 p9 G4 \( \( R/ @$ vwith water, and mix. Transfer a 10 ml aliquot of this solution into a 500
' v5 ?& x7 G! c: M j% H' Wml Erlenmeyer flask containing 90 ml of water and 3 ml of6 l+ F! h+ t9 G
concentrated hydrochloric acid, add 1 drop of methyl orange TS and
2 }' L; h! v/ G9 E+ X25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,
, g2 ]% `9 i1 ]1 a5 Zdropwise, ammonia solution (1 in 5) until the colour is just completely! _. }, d9 a3 r: E$ H8 A% j+ m; ^
changed from red to orange-yellow. Then, add:
# f8 ?- P7 b, v(a): 10 ml of ammonium acetate buffer solution (77 g of
' T8 S: B8 o$ n2 F6 y; pammonium acetate plus 10 ml of glacial acetic acid, dilute to
9 ^3 H2 x& C. h7 g( R0 Y1000 ml with water) and: @. {* a6 A3 z4 O
(b): 10 ml of diammonium hydrogen phosphate solution (150 g
. O) V! Y5 ^* M# v& x. pof diammonium hydrogen phosphate in 700 ml of water,8 `8 @ w9 l6 R K/ k# q3 |8 X
adjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,
. E6 ?8 M" U. F& t7 othen dilute to 1000 ml with water).
# S+ M; c x [Boil the solution for 5 min, cool it quickly to room temperature in a/ @ @% v% [; _, m& N
stream of running water, add 3 drops of xylenol orange TS, and mix.# Z: d. g5 [/ d2 f1 W) v( M4 Q, u8 p l
Using the zinc sulfate solution as titrant, titrate the solution to the first
/ ~* |' g: d4 u# `8 C* qyellow-brown or pink end-point colour that persists for 5-10 sec. (Note:
0 O i4 P' a5 _4 mThis titration should be performed quickly near the end-point by
' R. r/ n3 f# y" l2 ~adding rapidly 0.2 ml increments of the titrant until the first colour
2 K+ `& K$ b# Q9 dchange occurs; although the colour will fade in 5-10 sec, it is the true
; ~4 F X/ f( x0 L5 z9 i/ wend-point. Failure to observe the first colour change will result in an G" O+ R9 V$ v7 @1 [0 ^* F. E
incorrect titration. The fading end-point does not occur at the second
' [+ }1 H! ^1 u3 }' U9 Z5 nend-point.)
2 h. {; b) x$ W! n1 @" qAdd 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a! m, t% E% x1 \1 I+ @- P/ T
stream of running water. Titrate this solution, using the zinc sulfate3 z/ A- `" }' B4 z# F8 g
solution as titrant, to the same fugitive yellow-brown or pink end-point- }/ Y2 N* a) L: s: l0 j' _
as described above.3 Z0 R' c1 K" q+ b3 U
Calculate the titre T of zinc sulfate solution by the formula:9 u% ^) y) o, }. T& j4 R8 r- S
T = 18.896 W / V7 n$ r9 T3 P. X# i: w) ~
where
a6 ?$ Z2 d; kT is the mass (mg) of Al2O3 per ml of zinc sulfate solution- _) T4 W4 W1 v
W is the mass (g) of aluminium wire
0 M! A, a7 L$ r/ VV is the ml of the zinc sulfate solution consumed in the/ b3 z9 u8 `/ ]* W8 ]
second titration* w( H8 u. B6 ~, w2 V: O' e6 @5 |
18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and |: Q. G' e" M, U0 ~9 p' y
R is the ratio of the formula weight of aluminium oxide to8 M; Y: l( y- ?8 {9 a
that of elemental aluminium.
) l. {8 q+ B4 x: ?0 PSample Solution A
3 m# g. P, L' n. i! p m( J& aAccurately weigh 1 g of the sample and transfer to a 250-ml high-silica
0 W% i) h( ]6 i, M, L# I7 K3 d9 ?glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).+ G* A2 h3 o+ D: H5 {/ q
(Note: Do not use more sodium bisulfate than specified, as an excess
! E' \# T. c, J6 M% H1 econcentration of salt will interfere with the EDTA titration later on in the+ ]8 o2 N8 ]4 o" B' V6 ]/ T
procedure.) Begin heating the flask at low heat on a hot plate, and9 i& p% ^/ ]# D( w/ b8 n, Z7 q
then gradually raise the temperature until full heat is reached.
9 C/ |' G. I' ~# v(Caution: perform this procedure in a well ventilated area. ) When
/ a7 J' U- c, U% R9 l1 Rspattering has stopped and light fumes of SO3 appear, heat in the full9 @: C$ c! c3 u# w$ |8 B
flame of a Meeker burner, with the flask tilted so that the fusion of the
) l5 v- e3 {% Y3 ~& M6 J3 Osample and sodium bisulfate is concentrated at one end of the flask.
1 g/ Z7 T# T$ @& _; L3 ^; xSwirl constantly until the melt is clear (except for silica content), but
; R+ l3 Q$ E, Mguard against prolonged heating to avoid precipitation of titanium4 a- a9 t" a2 _' J" ~
dioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until/ i8 o0 O) r8 O; x
the mass has dissolved and a clear solution results. Cool, and dilute to) x6 c5 j# Q" H, A( Z6 U+ G, k" l" M
120 ml with water. Introduce a magnetic stir bar into the flask.+ r" a* Q* d; S- i5 T4 y) E
Sample Solution B. S# z. f9 r( O7 l# I& _7 e2 }
Prepare 200 ml of an approximately 6.25 M solution of sodium, g R2 { U0 x0 n! ]
hydroxide. Add 65 ml of this solution to Sample Solution A, while9 G' C7 f/ v) ^. ]. i
stirring with the magnetic stirrer; pour the remaining 135 ml of the8 V) E8 v# k9 z* B* D e* L; y* ]
alkali solution into a 500-ml volumetric flask.
' Q4 |. ]6 ]) O7 x7 z7 F, WSlowly, with constant stirring, add the sample mixture to the alkali) v' Q& W& S' @. {
solution in the 500-ml volumetric flask; dilute to volume with water,
, m" A- I! C2 o* R8 T! vand mix. (Note: If the procedure is delayed at this point for more than- j+ @" u. o1 E9 b# Q
2 hours, store the contents of the volumetric flask in a polyethylene
' r* ~0 i) b! _+ s7 i, p) U+ w% q' Cbottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),5 Q8 _. q- v2 b! }' H- M( Y" c
then filter the supernatant liquid through a very fine filter paper. Label; k8 K9 g' a0 ^3 y* n5 H
the filtrate Sample Solution B.
9 T3 o* A7 |. w# y$ u' C- t2 @9 f# oSample Solution C
2 r0 p4 X! I1 ETransfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer
" y7 } {4 D) i4 d2 sflask, add 1 drop of methyl orange TS, acidify with hydrochloric acid; |+ n. b& s' H" ^( j9 k
solution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02
0 Y9 \2 b a5 |/ r6 [M disodium EDTA, and mix. [Note: If the approximate Al2O3 content is0 I/ L) h9 d$ \8 x L. q
known, calculate the optimum volume of EDTA solution to be added6 _4 J3 P- h3 h1 U* J( F
by the formula: (4 x % Al2O3) + 5.]( i5 U- D$ p0 G
Add, dropwise, ammonia solution (1 in 5) until the colour is just
2 B' F. C; _1 ]/ ycompletely changed from red to orange-yellow. Then add10 ml each
9 S- e; V. b0 e5 m: Fof Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to3 V. U2 U) y" ~3 Q! L$ [& |3 W! o
room temperature in a stream of running water, add 3 drops of xylenol f5 V' d6 m; i/ k& N
orange TS, and mix. If the solution is purple, yellow-brown, or pink,/ M# s* I5 J( H( [
bring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired% p# K2 O/ s T' `3 U3 B
pH, a pink colour indicates that not enough of the EDTA solution has" X7 Z* W. P. v0 d/ _5 }& T
been added, in which case, discard the solution and repeat this* J4 u5 Q) _% a0 u) ]: I B
procedure with another 100 ml of Sample Solution B, using 50 ml,4 q( F4 v/ `% s8 t* O% z- X
rather than 25 ml, of 0.02 M disodium EDTA.
1 \/ y2 R4 V0 w. s5 F; B2 B2 ]0 |Procedure
1 s1 Y! z* f1 e( G/ y* `Using the standardized zinc sulfate solution as titrant, titrate Sample
2 Q6 x2 u: A. K* PSolution C to the first yellow-brown or pink end-point that persists for' C, l( f5 s- ]9 A9 ~. g# U
5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first1 ?+ _1 h2 y2 i3 B7 i, {
titration should require more than 8 ml of titrant, but for more accurate+ N2 i& G- F% n/ z$ u+ ~( ]0 @
work a titration of 10-15 ml is desirable.
9 R" l8 z' l0 o; U3 C: w! i. tAdd 2 g of sodium fluoride to the titration flask, boil the mixture for 2-57 I/ Z; ^. l. B0 s* E
min, and cool in a stream of running water. Titrate this solution, using
7 h! X$ U, l" i5 M: h5 Mthe standardized zinc sulfate solution as titrant, to the same fugitive: [7 k- N& `# K' t B
yellow-brown or pink end-point as described above.: Z: u% v! r; A g
Calculation:+ V. i2 u& L5 Y" R; M/ u6 i
Calculate the percentage of aluminium oxide (Al2O3) in the sample
* T, a3 w6 w6 C3 h8 ^taken by the formula:
0 @& l3 ~* P9 B& l) t. N% Al2O3 = 100 × (0.005VT)/S
( S/ m+ a6 k" j9 y0 Kwhere
7 x4 v8 u3 q# _, r( V& ~V is the number of ml of 0.01 N zinc sulfate consumed in
4 @9 P) z* N, W0 ?0 r; rthe second titration,
6 c* g8 y# G3 H2 P) o! e" p' F! _2 h% p- GT is the titre of the zinc sulfate solution,# p6 L( j$ I" m3 C" P6 h9 U p
S is the mass (g) of the sample taken, and
# D2 b' s! E% H! c" d5 I4 G0.005 = 500 ml / (1000mg/g × 100 ml).5 E: k- t* k3 z# N( S4 Z# U! h
Silicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica
: d7 s5 _$ c4 w \$ g8 oglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).- h r0 I- `6 E% n
Heat gently over a Meeker burner, while swirling the flask, until
; S" E0 D1 U; ~5 S% p# p9 N$ K. J% adecomposition and fusion are complete and the melt is clear, except/ u6 p R: M: e( k! G7 Q
for the silica content, and then cool. (Caution: Do not overheat the
- y5 H( w/ D( p7 rcontents of the flask at the beginning, and heat cautiously during2 _0 I2 k S( W2 z, F a& a
fusion to avoid spattering.)
: b3 n2 }0 O) FTo the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat
) O Z4 d. o4 I1 ?7 F Ucarefully and slowly until the melt is dissolved. Cool, and carefully add3 }- }" ^0 g1 }- Y7 a6 C
150 ml of water by pouring very small portions down the sides of the1 l& I I1 {, V" `* S' [
flask, with frequent swirling to avoid over-heating and spattering. Allow
) b* e' w9 N* @" a$ p2 Athe contents of the flask to cool, and filter through fine ashless filter
( i: a# f* @9 Y B7 [paper, using a 60 degree gravity funnel. Rinse out all the silica from
+ @$ [/ q" N8 o% L4 nthe flask onto the filter paper with sulfuric acid solution (1 in 10).7 _% T! I1 r2 q- g& s" s" S$ \
Transfer the filter paper and its contents into a platinum crucible, dry in7 l' O! i5 h" Z) z- U
an oven at 1200, and heat the partly covered crucible over a Bunsen
3 V. k6 o2 G6 l/ V" _burner. To prevent flaming of the filter paper, first heat the cover from/ A2 ^/ F- F. k) r
above, and then the crucible from below.# S- K; d& u4 ]) x2 V3 E3 H( H7 g
When the filter paper is consumed, transfer the crucible to a muffle
; A: V& t: O5 ^; y# I% c- V, Dfurnace and ignite at 1000o for 30 min. Cool in a desiccator, and
5 a9 Y7 L6 O$ q; v5 M& Uweigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated& Q; W# T9 Z$ G% ]) c1 P7 G
hydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first/ l5 a3 L( h3 u' h. z
on a low-heat hot plate (to remove the HF) and then over a Bunsen- d+ o4 p e& G4 r4 [
burner (to remove the H2SO4). Take precautions to avoid spattering,
' S$ T' [" ?- W. p1 Wespecially after removal of the HF. Ignite at 1000o for 10 min, cool in a B9 u8 T E6 P9 I+ k, ?
desiccator, and weigh again. Record the difference between the two2 f- f- H6 H' C" c! U4 O6 B. i \: |
weights as the content of SiO2 in the sample.
! \- |2 T$ b# ~, pMETHOD OF ASSAY& [ |! P1 }4 S1 K, w
Accurately weigh about 150 mg of the sample, previously dried at 105o5 i8 ?2 v; t" f& S0 U U
for 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water
8 D9 I! k" Y1 O5 x% |( ? fand shake until a homogeneous, milky suspension is obtained. Add 30
! u/ k- d! K& A! w& b) Y$ jml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially2 A" C! P! X* _" M" y E6 \% b
heat gently, then heat strongly until a clear solution is obtained. Cool,
6 L- |4 m3 N- ~- Zthen cautiously dilute with 120 ml of water and 40 ml of hydrochloric
- D" b6 j( s4 S% ]8 J2 hacid, and stir. Add 3 g of aluminium metal, and immediately insert a
8 v( [2 H8 z$ D/ \rubber stopper fitted with a U-shaped glass tube while immersing the( I3 }& y& A9 L" q/ L
other end of the U-tube into a saturated solution of sodium
5 I; l% S! v- P! Q" \# W% Lbicarbonate contained in a 500-ml wide-mouth bottle, and generate
$ ^- s4 Q$ n8 X% }( ?' n2 uhydrogen. Allow to stand for a few minutes after the aluminium metal4 q( n8 F( ?# R; C) X6 ~
has dissolved completely to produce a transparent purple solution.
4 \: t D- z% g; }6 @+ cCool to below 50o in running water, and remove the rubber stopper5 b" H9 B$ {1 ~# X7 c
carrying the U-tube. Add 3 ml of a saturated potassium thiocyanate+ f% P5 T ]" _& H' }9 k$ Z- Z( F2 U
solution as an indicator, and immediately titrate with 0.2 N ferric9 C( ^: O- {2 N6 W' U% F) S
ammonium sulfate until a faint brown colour that persists for 30; y! _/ f5 i1 P$ o
seconds is obtained. Perform a blank determination and make any
2 b8 G' _+ g' E4 ~: X% |+ Knecessary correction. Each ml of 0.2 N ferric ammonium sulfate is! v; |- e' F8 H2 R7 M. e$ H% W
equivalent to 7.990 mg of TiO2.
* v) A0 C& j0 g0 d+ G: ?% D |
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