- D& T3 a: a( n $ t1 Q4 e* X' R4 N: e7 S作者: 1123456789 时间: 2008-5-23 12:10 标题: 二氧化钛(钛白粉) 二氧化钛(钛白粉) ! q* R& h: v+ H5 v9 L$ G ) z, q( ~7 ?" z, F9 f& A0 qJECFA关于二氧化钛(钛白粉)的结论% t2 y8 {2 @. |$ m5 [- C
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摘要: 2006年JECFA关于二氧化钛的结论3 ?9 N) U2 |5 f- L, K
ADI值:不作限制。 7 F5 g9 g" q [: z( K3 U0 l功能:着色剂, o3 n" J) b6 g5 c% u8 x+ `
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TITANIUM DIOXIDE # R( `2 B1 r( Z' n) `, SPrepared at the 67th JECFA (2006) and published in FAO JECFA 1 ^. j( t/ Q. B1 [" ]Monographs 3 (2006), superseding specifications prepared at the 63rd 5 _3 i% @9 F$ n: wJECFA (2004) and published in FNP 52 Add 12 (2004) and in the , z6 k( E/ m' m$ e8 _4 bCombined Compendium of Food Additive Specifications, FAO JECFA % L1 h2 d! @; J# f* N3 |) {0 W0 zMonographs 1 (2005). An ADI “not limited” was established at the 13th$ v+ D* J1 W9 s' w5 |7 m' S
JECFA (1969).# ^6 h" v4 ^: U& i6 i* ?
SYNONYMS/ |3 v3 }' I% x( w) y" V1 D9 v
Titania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171 & i% H9 {: t/ C/ b# l( qDEFINITION9 v) L% U+ A, r. q* i
Titanium dioxide is produced by either the sulfate or the chloride & H+ ^- S1 g0 {' xprocess. Processing conditions determine the form (anatase or rutile0 U& k) ?0 M: \7 z- ^( {0 z
structure) of the final product. * _( | c1 t) s7 ?* PIn the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3) $ ]+ F/ p9 f+ U2 ?: A: Xor ilmenite and titanium slag. After a series of purification steps, the : i0 R; s1 m# b$ w4 G9 |isolated titanium dioxide is finally washed with water, calcined, and - x& K9 ^, a: x* B- Q( I8 L4 e9 kmicronized.8 O; C% k3 E2 m3 h) x2 m: w
In the chloride process, chlorine gas is reacted with a titaniumcontaining . j) Y8 K9 `& u& D1 W: t8 w3 N% Vmineral under reducing conditions to form anhydrous 2 k, s* s- }9 ^/ ntitanium tetrachloride, which is subsequently purified and converted to + Y: O1 G. ~1 c% [3 dtitanium dioxide either by direct thermal oxidation or by reaction with ; h( [- d( w$ ?" y- Lsteam in the vapour phase. Alternatively, concentrated hydrochloric ) Z/ l$ Q, b& B( K9 v; kacid can be reacted with the titanium-containing mineral to form a 5 h& w* _4 \! I P2 Xsolution of titanium tetrachloride, which is then further purified and / Y" U4 o% V& Cconverted to titanium dioxide by hydrolysis. The titanium dioxide is: ?6 C" }+ Z( g4 U9 }
filtered, washed, and calcined.2 y$ S" n4 p" k' `- f0 U1 x+ ]4 n4 q- T
Commercial titanium dioxide may be coated with small amounts of : s2 }, X, }* f6 J+ p+ i, balumina and/or silica to improve the technological properties of the 3 _) e: q* H4 U8 T4 }product. ( f% s, S1 Y* s7 D4 h3 SC.A.S. number 13463-67-7 ; r/ l5 d0 b( c2 }2 R& J- MChemical formula TiO29 u, V+ ~. B4 [4 \, u- L/ W
Formula weight 2 y! w3 f& u. G0 C! f79.88 % u0 t% i5 u- d5 jAssay 4 r" Z* o; [' h: fNot less than 99.0% on the dried basis (on an aluminium oxide and 2 C: U: W* e6 fsilicon dioxide-free basis)6 B7 U# }- Y! Z
DESCRIPTION- P9 ^/ ^4 ?$ U, N% t
White to slightly coloured powder & G9 { e& r0 W! XFUNCTIONAL USES6 d* f, s) i' e& M j
Colour % ]/ w& O& t' o+ R M5 ^CHARACTERISTICS, u8 ^ |4 F; s6 R7 l
IDENTIFICATION" t" e2 q: |; V
Solubility (Vol. 4)9 \$ M2 @8 B" F* |" [6 T% T
Insoluble in water, hydrochloric acid, dilute sulfuric acid, and organic) }6 c% ]6 U* ~8 K1 q& p& K
solvents. Dissolves slowly in hydrofluoric acid and hot concentrated& T7 ~$ l% F2 v
sulfuric acid.5 v. t0 i1 R, X6 ]( V
Colour reaction, h3 y: y& D Y- k7 ?/ K( n9 U3 ^
Add 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of d9 p7 }# z$ n) ]
sulfuric acid appear, then cool. Cautiously dilute to about 100 ml with - v1 }! v* w# @ `water and filter. To 5 ml of this clear filtrate, add a few drops of 1 ^$ Z9 P! t; t, y4 Ohydrogen peroxide; an orange-red colour appears immediately. - u7 F" \" s; K- \! V- SPURITY( L5 T7 }9 _8 ~0 V/ t5 I
Loss on drying (Vol. 4) Not more than 0.5% (105°, 3 h) % Q# `7 \0 T7 G! ALoss on ignition (Vol. 4)# k* P" o# A- P. \& q
Not more than 1.0% (800o) on the dried basis! U, U: r5 e# W5 d. S- r" J: p9 s/ {
Aluminium oxide and/or $ d, ]- U: K+ {5 Gsilicon dioxide 8 y- l) j. w( M- lNot more than 2%, either singly or combined , v P6 `( L0 D6 P3 LSee descriptions under TESTS$ p. X$ a' Z8 F0 J1 Y
Acid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing, ~" w5 I2 h Q* j. Z
alumina or silica. . O" B" S: F6 P' Y; e$ |+ }Suspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and1 q- ^) l' p0 l
place on a steam bath for 30 min with occasional stirring. Filter7 D7 ^, @8 o% p+ X
through a Gooch crucible fitted with a glass fibre filter paper. Wash + j, l! b5 v) }. w: a. pwith three 10-ml portions of 0.5 N hydrochloric acid, evaporate the - A* o, W k7 T+ o% f! rcombined filtrate and washings to dryness, and ignite at a dull red % J' D" V1 f6 c; @% W# ?heat to constant weight.# @& i; I; M0 g6 P7 V+ U( p: N4 E
Water-soluble matter ! D3 j$ z- [$ Y$ J/ h; b. Q2 N(Vol. 4)) Q# Q9 U% X1 G$ P0 O/ }/ [8 ~- O
Not more than 0.5% ) Q- Q- ]; N( ~9 NProceed as directed under acid-soluble substances (above), using ; {* G0 i$ [- r- A. s, _water in place of 0.5 N hydrochloric acid. ) W- q. J# M* g; T( E9 HImpurities soluble in 0.5 N % W, k0 q! ^8 phydrochloric acid. K: z7 e6 y7 ?1 n: p* z
Antimony Not more than 2 mg/kg' ^+ E( S% \, r8 a4 I% P
See description under TESTS* I- u# `: j# F L2 {% t" t3 e
Arsenic Not more than 1 mg/kg ) u8 _) J( @+ y; L/ ZSee description under TESTS * _' Q5 m% g$ k" U! JCadmium Not more than 1 mg/kg$ H& z* J+ ]' F: X" d/ [1 G
See description under TESTS 4 r( X: a* o1 M; l, oLead ' U! J! t2 W+ x+ t; UNot more than 10 mg/kg3 m: L8 R+ l3 k @9 W) O
See description under TESTS1 E* Z9 P$ S& E. Z3 x$ m
Mercury (Vol. 4) Not more than 1 mg/kg; ]# i- I/ |7 g. T
Determine using the cold vapour atomic absorption technique. Select a 4 f( i* o, L1 |+ Z- nsample size appropriate to the specified level 1 A: `5 H% W+ S4 n1 j7 j' X) zTESTS- d! y0 A- \" [% e0 U5 M* v8 y
PURITY TESTS : l3 N6 p# N4 lImpurities soluble in 0.5 N' l j2 ]; @% o7 H
hydrochloric acid 2 z4 W9 h/ h; t9 h( JAntimony, arsenic, . X7 S9 Q6 Z& o* ^! y( Dcadmium and lead$ ~; E# q5 @. O/ i, c
(Vol.4)1 Z) }2 x( j( A
Transfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N t7 M; i' {4 g/ O/ w$ |+ {
hydrochloric acid, cover with a watch glass, and heat to boiling on a ) L' C. @6 R5 O1 y3 zhot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml, O, N( [* _; D0 T9 @' M
centrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved , D7 m% s3 n3 q/ X" u0 Tmaterial settles. Decant the supernatant extract through a Whatman ; J/ W' M* S$ I1 I9 Z7 o2 u* dNo. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml 6 u3 S& L) A( a7 r# Jvolumetric flask and retaining as much as possible of the undissolved/ q8 f+ i4 K3 t" ~* ~# X; H/ S
material in the centrifuge bottle. Add 10 ml of hot water to the original L# m2 D w+ d1 rbeaker, washing off the watch glass with the water, and pour the $ j) Z( B% }8 _1 G/ B) P; l, wcontents into the centrifuge bottle. Form a slurry, using a glass stirring, P" C, r# M$ k! v
rod, and centrifuge. Decant through the same filter paper, and collect 9 A k: z! |4 Z* q' Qthe washings in the volumetric flask containing the initial extract.; d G5 S5 h8 S M# s2 W X- I
Repeat the entire washing process two more times. Finally, wash the' P* t8 x1 A+ W6 E. x
filter paper with 10 to 15 ml of hot water. Cool the contents of the flask8 c/ D9 C# _4 t+ p7 B: R6 u0 E
to room temperature, dilute to volume with water, and mix.7 ~( B0 l1 E; W, e+ {
Determine antimony, cadmium, and lead using an AAS/ICP-AES " B: E0 K5 i7 B0 G; a; _( C/ H& ttechnique appropriate to the specified level. Determine arsenic using the7 t: }9 g8 l- Q9 g
ICP-AES/AAS-hydride technique. Alternatively, determine arsenic using$ r+ P4 a7 @# X% ]8 D6 e* S
Method II of the Arsenic Limit Test, taking 3 g of the sample rather than# \. B. e1 E7 a6 o4 j S+ L
1 g. The selection of sample size and method of sample preparation ! l A* s: r1 p" f6 dmay be based on the principles of the methods described in Volume 4. 0 L6 J, c" w2 w* \! B4 [' kAluminium oxide Reagents and sample solutions8 G0 W+ {0 } [4 ^' h, N
0.01 N Zinc Sulfate $ N6 |* R. T: a; bDissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to 9 Z, V% Z, Y/ `/ lmake 1000 ml. Standardize the solution as follows: Dissolve 500 mg% x7 Y) i0 c$ |! d5 G
of high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of4 ?. \- o8 y' O% l" u; ?3 n
concentrated hydrochloric acid, heating gently to effect solution, then j5 Q# y1 ^7 E/ s7 Z5 p* T" {transfer the solution into a 1000-ml volumetric flask, dilute to volume- {+ W! e3 W5 C0 i5 j, x9 U
with water, and mix. Transfer a 10 ml aliquot of this solution into a 500 ( f' f) M- ^9 Gml Erlenmeyer flask containing 90 ml of water and 3 ml of% ?2 h/ ] u! o$ D- Q+ m
concentrated hydrochloric acid, add 1 drop of methyl orange TS and i% @* t' ]* y$ h( V25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add, 2 }9 k2 L1 k2 _2 A* x: D/ D0 ddropwise, ammonia solution (1 in 5) until the colour is just completely' L% d) B- d. h5 N0 d
changed from red to orange-yellow. Then, add: 6 C9 A+ t8 @, @) ](a): 10 ml of ammonium acetate buffer solution (77 g of 9 O0 ~: U, \3 I* a* n7 nammonium acetate plus 10 ml of glacial acetic acid, dilute to, I: G/ l4 T* v& y! M+ r
1000 ml with water) and9 s, e. F) Q. q# v9 ^
(b): 10 ml of diammonium hydrogen phosphate solution (150 g . k9 V5 M/ M1 n* D- N; o+ Sof diammonium hydrogen phosphate in 700 ml of water, ! ?, H1 i0 U3 q; U3 K5 J: A: vadjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid, 1 j# l. U$ ^; c" B4 ~0 vthen dilute to 1000 ml with water). . e& f* I. e7 J1 Y SBoil the solution for 5 min, cool it quickly to room temperature in a , ~5 G5 }+ g Z9 Ystream of running water, add 3 drops of xylenol orange TS, and mix.- W4 R7 [" q5 X/ p
Using the zinc sulfate solution as titrant, titrate the solution to the first5 Q4 C7 o0 d5 c, o" k/ I# V
yellow-brown or pink end-point colour that persists for 5-10 sec. (Note: : |7 Y0 q( U2 G8 W, B% oThis titration should be performed quickly near the end-point by " h# e d! V; P1 b% s( C/ yadding rapidly 0.2 ml increments of the titrant until the first colour $ j, T: i! j. Kchange occurs; although the colour will fade in 5-10 sec, it is the true8 C h& z. i0 m, J$ R
end-point. Failure to observe the first colour change will result in an4 u& e! \7 |8 L4 d
incorrect titration. The fading end-point does not occur at the second C R h( I8 ^! S6 y1 Mend-point.)4 A' C" c1 k9 x
Add 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a ) }9 j: o/ Y" Z U# mstream of running water. Titrate this solution, using the zinc sulfate9 S& M) Q1 j8 k
solution as titrant, to the same fugitive yellow-brown or pink end-point2 f1 d2 ]3 O/ Q
as described above. - M$ @' v6 ^. ^% F+ ^8 B; UCalculate the titre T of zinc sulfate solution by the formula: * l/ X+ J* ?0 D2 wT = 18.896 W / V + C$ I% f- W7 F- Vwhere6 d4 ?" P& X( E9 c( Y* V
T is the mass (mg) of Al2O3 per ml of zinc sulfate solution 1 n* o5 A3 X" C5 p; _: PW is the mass (g) of aluminium wire $ \+ C: A: v9 ^. K' b1 B! PV is the ml of the zinc sulfate solution consumed in the " v; r! _- t; P9 Y/ |" {second titration 9 e% U8 F! J; t; N/ q18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and4 }( K$ ~) T( f* z3 @, h4 e
R is the ratio of the formula weight of aluminium oxide to: } U) X7 \4 J' h' q
that of elemental aluminium./ ^- Y' w7 u; {4 `2 X
Sample Solution A , P$ ~- A8 @, d) A) CAccurately weigh 1 g of the sample and transfer to a 250-ml high-silica / h$ k4 {: u7 y7 p$ Eglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O). 8 e! T# M8 O. U- ?(Note: Do not use more sodium bisulfate than specified, as an excess! q1 N$ ]1 f7 m! Y
concentration of salt will interfere with the EDTA titration later on in the9 N) h4 ?5 d" }' i
procedure.) Begin heating the flask at low heat on a hot plate, and8 C# N9 ]$ E3 s
then gradually raise the temperature until full heat is reached. , i; x5 e8 C7 N(Caution: perform this procedure in a well ventilated area. ) When , L; O* N; g' ]2 B8 v3 W q) Jspattering has stopped and light fumes of SO3 appear, heat in the full- `3 q$ x: o+ u% N( {2 m& b
flame of a Meeker burner, with the flask tilted so that the fusion of the6 c/ h$ e& B- D
sample and sodium bisulfate is concentrated at one end of the flask.6 Z7 A) O. W7 {' _( A0 z$ Q
Swirl constantly until the melt is clear (except for silica content), but% A# R$ j2 s m# s1 D' z
guard against prolonged heating to avoid precipitation of titanium - Z, n' H. e$ R- y9 W3 A5 Hdioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until : d6 F% B6 D& Sthe mass has dissolved and a clear solution results. Cool, and dilute to) j9 w, k6 n% _! [; f
120 ml with water. Introduce a magnetic stir bar into the flask. % e9 ?: |0 S5 y0 SSample Solution B T' c7 r* F4 J- a* fPrepare 200 ml of an approximately 6.25 M solution of sodium4 o! l0 {& y: @% O9 {' Q( U) L
hydroxide. Add 65 ml of this solution to Sample Solution A, while7 M# Y& f0 J: \; t' P' X1 b% o
stirring with the magnetic stirrer; pour the remaining 135 ml of the $ \% H4 D& }! `: z/ Ialkali solution into a 500-ml volumetric flask.- y- f7 p2 R& E( }, G$ z
Slowly, with constant stirring, add the sample mixture to the alkali; T( r3 \" A, l3 L$ v
solution in the 500-ml volumetric flask; dilute to volume with water, 3 \3 L0 ^: z$ n% j2 Sand mix. (Note: If the procedure is delayed at this point for more than6 j @5 W- s% S! q& h
2 hours, store the contents of the volumetric flask in a polyethylene8 j' `: {0 J O7 A5 K
bottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),) z5 _6 F/ u# @2 w' ]; e4 a: P% D
then filter the supernatant liquid through a very fine filter paper. Label3 ~0 t; h+ G0 y8 o! t
the filtrate Sample Solution B.# s2 U4 C5 ]# S Y
Sample Solution C$ t8 K% m% t2 [6 }3 w x+ o
Transfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer & H1 w% Q$ @; j, H* c0 y" }flask, add 1 drop of methyl orange TS, acidify with hydrochloric acid! F) m* r& P5 E9 I( D
solution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02 " g4 P3 w$ o, }6 aM disodium EDTA, and mix. [Note: If the approximate Al2O3 content is, l$ m( _! t2 d* A+ f# A* i; \! C
known, calculate the optimum volume of EDTA solution to be added 9 j; H$ O- F9 e4 qby the formula: (4 x % Al2O3) + 5.] , X) k) c% k% Y% e. i% T1 R4 OAdd, dropwise, ammonia solution (1 in 5) until the colour is just2 N8 b( R+ n! T: p* x0 ^
completely changed from red to orange-yellow. Then add10 ml each " g) ~& a; o& bof Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to 6 N6 A2 k4 I& o4 Zroom temperature in a stream of running water, add 3 drops of xylenol3 E" h) N2 ]$ y6 D9 O
orange TS, and mix. If the solution is purple, yellow-brown, or pink,+ U' F# t( s9 P. F4 a8 Z
bring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired6 a+ S+ ?% o# ~3 b# U
pH, a pink colour indicates that not enough of the EDTA solution has* f6 c/ k4 ^7 `) K
been added, in which case, discard the solution and repeat this0 u5 F6 u* t. k' @: w/ S
procedure with another 100 ml of Sample Solution B, using 50 ml," m# k$ L- w9 C5 U1 e
rather than 25 ml, of 0.02 M disodium EDTA. + v5 v( `. p' L) X; w& D& A- YProcedure' c* @: g+ r) k& U8 v8 m( W
Using the standardized zinc sulfate solution as titrant, titrate Sample6 Q+ H6 Q X9 q' Q$ C
Solution C to the first yellow-brown or pink end-point that persists for0 q) R* }: Z1 R* d+ a7 [
5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first / x$ R( e1 i* l$ j, j8 t$ j) ctitration should require more than 8 ml of titrant, but for more accurate 9 F- j; Z' r! B; a9 B' L/ m: [work a titration of 10-15 ml is desirable. 2 v2 T0 T: S+ p4 t) A @* {& lAdd 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5 ' O) |/ G; _- W+ qmin, and cool in a stream of running water. Titrate this solution, using 9 V# }! y! f$ b' ]2 dthe standardized zinc sulfate solution as titrant, to the same fugitive2 q1 G0 R6 r9 r1 [9 {
yellow-brown or pink end-point as described above.* s! A0 o" H+ J
Calculation: ) g, G9 I! ~( g( A! E. _Calculate the percentage of aluminium oxide (Al2O3) in the sample/ b: w$ @! f* M
taken by the formula: : T \* N' N9 g% y0 }8 I% Al2O3 = 100 × (0.005VT)/S$ I3 {! D! j% p$ V1 R
where 4 S. j/ t/ h3 ]7 W) A h1 TV is the number of ml of 0.01 N zinc sulfate consumed in! O, _' S+ Z9 ?
the second titration," m+ L% D' B9 S4 g p3 h' b4 A2 [
T is the titre of the zinc sulfate solution, ' |% `2 g: m6 ~& b' |% h Y/ a- ^# wS is the mass (g) of the sample taken, and 5 u; Q( F+ ]1 T( M/ x! z0.005 = 500 ml / (1000mg/g × 100 ml).+ o$ B9 u5 |' e* i& N( ~1 T4 s
Silicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica. z# I& H, ^/ N u, e, s6 \' b
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).5 v+ v# U+ j3 p* M [
Heat gently over a Meeker burner, while swirling the flask, until2 z' d+ D$ Y. u0 Z
decomposition and fusion are complete and the melt is clear, except j- m/ w& U1 V/ X$ j" [
for the silica content, and then cool. (Caution: Do not overheat the 2 k, R3 j T5 K6 M1 [# Rcontents of the flask at the beginning, and heat cautiously during & Y" v# E9 Z- yfusion to avoid spattering.) ! O1 R5 m) H- i0 j% FTo the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat0 ~3 I8 [; G& J7 l4 ?4 M/ `9 D
carefully and slowly until the melt is dissolved. Cool, and carefully add" C! g& k f* J' I& V, {/ T
150 ml of water by pouring very small portions down the sides of the" j, P% b0 |8 L' T+ `
flask, with frequent swirling to avoid over-heating and spattering. Allow& B; Q# L H9 I& H
the contents of the flask to cool, and filter through fine ashless filter - T1 J: z: t. I" y. L: `paper, using a 60 degree gravity funnel. Rinse out all the silica from: U4 d* B/ c1 a3 A+ r
the flask onto the filter paper with sulfuric acid solution (1 in 10). - z: |) ?6 x( ?' vTransfer the filter paper and its contents into a platinum crucible, dry in ' z) S3 y8 q+ L: Tan oven at 1200, and heat the partly covered crucible over a Bunsen) n# R) Z! u3 H' |
burner. To prevent flaming of the filter paper, first heat the cover from- U" }' U0 R+ \ I L, h1 _
above, and then the crucible from below.8 s2 S k( \, D+ P$ Z
When the filter paper is consumed, transfer the crucible to a muffle 9 ?' h9 [1 }1 ^furnace and ignite at 1000o for 30 min. Cool in a desiccator, and4 h ]( H9 @8 F' [* m8 W
weigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated : i6 w A& d6 S$ Mhydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first* b) w9 R$ k9 Y5 U; |
on a low-heat hot plate (to remove the HF) and then over a Bunsen + ]) Q: Q% ?& q# bburner (to remove the H2SO4). Take precautions to avoid spattering, + H. `* F! s' m H# ]# P. ], Cespecially after removal of the HF. Ignite at 1000o for 10 min, cool in a; m D0 D1 {4 s. q4 |& B
desiccator, and weigh again. Record the difference between the two * M! e1 k d3 \1 ?weights as the content of SiO2 in the sample. / l0 A# ?/ C$ a( A5 ^ mMETHOD OF ASSAY! N- F: Q( H2 h9 M
Accurately weigh about 150 mg of the sample, previously dried at 105o , M1 g B& \) ofor 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water* m3 ^. [8 c$ I7 z* B% H
and shake until a homogeneous, milky suspension is obtained. Add 30 . s8 q8 Z8 X3 L5 R- B! ], R' Jml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially & ]5 K! u; O# `: Bheat gently, then heat strongly until a clear solution is obtained. Cool,. w. e; n$ G0 b$ g
then cautiously dilute with 120 ml of water and 40 ml of hydrochloric 1 r( C9 t I# f5 N* {9 {acid, and stir. Add 3 g of aluminium metal, and immediately insert a : M6 U0 d/ G6 Drubber stopper fitted with a U-shaped glass tube while immersing the0 l# e; }. q& d* I
other end of the U-tube into a saturated solution of sodium" r, Q M! o5 |1 t
bicarbonate contained in a 500-ml wide-mouth bottle, and generate* i0 @- C1 Y$ \, g3 u6 I
hydrogen. Allow to stand for a few minutes after the aluminium metal h2 c, ^) V- t. h* Yhas dissolved completely to produce a transparent purple solution.0 H5 Z) r* E* F+ K, k5 s$ Q
Cool to below 50o in running water, and remove the rubber stopper , Z* T* |- ]. n' _: W' r b1 \7 S$ Xcarrying the U-tube. Add 3 ml of a saturated potassium thiocyanate; j/ [5 o3 }/ q, V3 i
solution as an indicator, and immediately titrate with 0.2 N ferric ( _+ \# x4 ?/ f! ~8 Uammonium sulfate until a faint brown colour that persists for 30* c1 D' G% V* c& c: ]& T4 O5 l4 n# E4 H
seconds is obtained. Perform a blank determination and make any6 t0 i8 K4 \* K) S( @
necessary correction. Each ml of 0.2 N ferric ammonium sulfate is ' [) L( @8 ^3 a7 z8 b3 ^equivalent to 7.990 mg of TiO2. ( O4 `- V3 a. t3 z; H! A5 `# W) R9 [