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二氧化钛(钛白粉)

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发表于 2008-5-23 12:09:00 | 只看该作者 回帖奖励 |倒序浏览 |阅读模式
二氧化钛(钛白粉) , A: R' F; W- v

* j0 J6 N" h: x4 U
! i& U4 w% c  \! f7 q, n( A% p& KCAC关于二氧化钛(钛白粉)的使用规定) ^* E: u. n) M$ A/ d& t
GSFA Online
  S5 |1 ?* d/ e; i( Z4 jFood Additive Details
, o( @; R5 }! c+ ETitanium Dioxide (171)
( N! \8 y7 f5 h/ V( w2 tNumber Food Category  
/ A! q% S5 k5 X0 X: M  01.1.2 Dairy-based drinks, flavoured and/or fermented (e.g., chocolate milk, cocoa, eggnog, drinking yoghurt, whey-based drinks)  % S$ a8 e; ?8 c1 [$ e7 _7 F7 X. a
  01.3 Condensed milk and analogues (plain)  / [3 ^6 v8 p, G4 ?
  01.4.3 Clotted cream (plain)  
7 s1 N, h$ z* n* P/ b6 P  01.4.4 Cream analogues  ! Q% @% f6 q; j- V
  01.5 Milk powder and cream powder and powder analogues (plain)  . p, y/ C0 u1 y
  01.6 Cheese and analogues  
% C& J" R7 \8 [- N6 G+ W  01.7 Dairy-based desserts (e.g., pudding, fruit or flavoured yoghurt)  " m! Q  C5 U6 |' W2 _
  01.8 Whey and whey products, excluding whey cheeses  
2 t# y) Z; {5 O% {' I* \7 C+ [" f  02.2.1.2 Margarine and similar products   6 m8 h5 C0 ?+ X: d
  02.2.1.3 Blends of butter and margarine  6 L. j* V: ?+ X7 t6 b3 K! D, q0 O
  02.2.2 Emulsions containing less than 80% fat   
* {* Q$ x) Y. A. |, b$ B! l0 x  02.3 Fat emulsions maily of type oil-in-water, including mixed and/or flavoured products based on fat emulsions   0 f! o$ l3 [0 X9 s7 u* W% i% o' Y
  02.4 Fat-based desserts excluding dairy-based dessert products of food category 01.7  + X) A3 P. D+ D# h
  03.0 Edible ices, including sherbet and sorbet  ; S; I9 d) |' d4 Y0 c
  04.1.2 Processed fruit  ( b$ i: A. P' ^/ u3 J: ]7 v
  04.2.2.2 Dried vegetables (including mushrooms and fungi, roots and tubers, pulses and legumes, and aloe vera), seaweeds, and nuts and seeds  
0 x. N8 `" v6 e; f  04.2.2.3 Vegetables (including mushrooms and fungi, roots and tubers, pulses and legumes, and aloe vera) and seaweeds in vinegar, oil, brine, or soy sauce  . R5 D  M0 p7 I. L. T. q) G5 A
  04.2.2.4 Canned or bottled (pasteurized) or retort pouch vegetables (including mushrooms and fungi, roots and tubers, pulses and legumes, and aloe vera), and seaweeds  
* c# o/ Q# G$ K& U% c$ W  04.2.2.5 Vegetable (including mushrooms and fungi, roots and tubers, pulses and legumes, and aloe vera), seaweed, and nut and seed purees and spreads (e.g., peanut butter)  
/ r/ i6 x+ s; O. f  04.2.2.6 Vegetable (including mushrooms and fungi, roots and tubers, pulses and legumes, and aloe vera), seaweed, and nut and seed pulps and preparations (e.g., vegetable desserts and sauces, candied vegetables) other than food category 04.2.2.5  
( Z1 j( R4 a$ T  04.2.2.8 Cooked or fried vegetables (including mushrooms and fungi, roots and tubers, pulses and legumes, and aloe vera), and seaweeds  ( [4 V3 D; J. N
  05.0 Confectionery  
6 G& d, t' E( ~* p  06.3 Breakfast cereals, including rolled oats  
- ]7 ]" c" Y5 A  06.4.3 Pre-cooked pastas and noodles and like products  * K! M# {1 G# ], Y( D) U
  06.5 Cereal and starch based desserts (e.g., rice pudding, tapioca pudding)  
; ?& m' m+ G' v2 _  06.6 Batters (e.g., for breading or batters for fish or poultry)  ; w9 o& f) W/ A2 ^" y+ x* T
  06.7 Pre-cooked or processed rice products, including rice cakes (Oriental type only)  
8 [+ y1 u- V% W  o" y% B  06.8 Soybean products (excluding soybean products of food category 12.9 and fermented soybean products of food category 12.10)  & U6 s* r- ^: V- `5 y7 G8 [
  07.0 Bakery wares  
" @/ E, M* A+ @  08.2 Processed meat, poultry, and game products in whole pieces or cuts  
8 {% G$ f: O& l  l7 j& @. ~  08.3 Processed comminuted meat, poultry, and game products  
+ J- d9 }9 ?6 _6 ~% o8 u1 u  08.4 Edible casings (e.g., sausage casings)  
! x2 x/ W$ J; f; S  09.3 Semi-preserved fish and fish products, including mollusks, crustaceans, and echinoderms  
7 l/ |* o# A) I. E, \9 X3 l1 N# o  09.4 Fully preserved, including canned or fermented fish and fish products, including mollusks, crustaceans, and echinoderms  / p- B0 c/ C, l# |3 d' Q8 i- j+ y' V
  10.2.3 Dried and/or heat coagulated egg products  
  b, P, K( }6 `( f1 l: k1 q  10.3 Preserved eggs, including alkaline, salted, and canned eggs  0 M1 J0 O5 R5 \; |; d
  10.4 Egg-based desserts (e.g., custard)  4 j# c' {) ]6 X8 }
  11.6 Table-top sweeteners, including those containing high-intensity sweeteners    A- f7 a  G2 }
  12.2.2 Seasonings and condiments  7 _4 W$ |& p0 w$ A' j
  12.3 Vinegars  2 o7 ]* s' |- b2 ?( R% Y2 V
  12.4 Mustards  
% B5 \# K$ Y" ]. |/ l1 \  12.5 Soups and broths  ) l, T4 |) N5 N- ]
  12.6 Sauces and like products  
7 `/ @7 [, ~4 n* G7 I  12.7 Salads (e.g., macaroni salad, potato salad) and sandwich spreads excluding cocoa- and nut-based spreads of food categories 04.2.2.5 and 05.1.3  ; C; z% z, J: F, Z; }5 t1 ]
  12.8 Yeast and like products  
8 E+ j) s, _* M1 Y* c2 }, ^  12.9 Protein products  
7 d0 N6 a/ W0 k  12.10 Fermented soybean products  
: m7 h' }- z7 D. V  13.3 Dietetic foods intended for special medical purposes (excluding products of food category 13.1)  " [6 p5 U# v) h$ `- S1 z* k" y% O4 z
  13.4 Dietetic formulae for slimming purposes and weight reduction  
% x* l/ z; i  J  13.5 Dietetic foods (e.g., supplementary foods for dietary use) excluding products of food categories 13.1 - 13.4 and 13.6  
4 F* a" P/ s* ?$ A6 V( e6 k' b  13.6 Food supplements  
6 Z6 G$ j- P2 @; Y! N$ b: u  14.1.1.2 Table waters and soda waters    U# C& b* f; Q7 J+ _# ^. q
  14.1.4 Water-based flavoured drinks, including "sport," "energy," or "electrolyte" drinks and particulated drinks  
$ t) P6 g* N' P$ h' h3 }  14.2.1 Beer and malt beverages  . x# Y0 N, ?# L) N- |6 G( V
  14.2.2 Cider and perry  
# R0 C) G# d) L2 ~; ^% ^7 z8 }  14.2.4 Wines (other than grape)  
1 C9 c) B+ A6 r8 M6 x$ Q  14.2.5 Mead  
* d  q7 P3 W0 b( Z( c  14.2.6 Distilled spirituous beverages containing more than 15% alcohol  9 u+ @0 ]  u' ], d# n- s
  14.2.7 Aromatized alcoholic beverages (e.g., beer, wine and spirituous cooler-type beverages, low alcoholic refreshers)    x7 g+ l/ m  G1 ?
  15.0 Ready-to-eat savouries  
3 Z4 x" Y7 N2 J- @  16.0 Composite foods - foods that could not be placed in categories 01 – 15" G0 @% x2 X: F: U) o5 \, `4 q

% f& I. v% ^7 m6 k' y& p" ?6 ]* a  l9 N6 V' @% i# J
部分译文:
0 V! H1 X( a8 V% Q% |% |8 @
' o! v6 G' d8 K2 d  I( K1 X食品添加剂通用规则# L8 k, y9 ]* k1 C( l# B$ d+ y- C
食品添加剂
6 n4 f6 f( X7 C& i                    二氧化钛(171)
! [) o# y2 r# g7 W+ O. V食品类别:
5 w3 z& J% E& M3 B) G, ~1 n  h: g06.3 早餐谷类,包括燕麦片: C, i' K" N6 f3 ?; E) M
06.4.3面条及类似产品5 G6 D& t! N$ ]% @* h. ^, ~
06.5 谷类,淀粉甜点(包括:米粉布丁,木薯布丁)
: K( S0 B0 [  a: H3 `06.6 面团
$ N: o" W, \3 T5 e- ?( T06.7 预煮的或加工的米产品,包括年糕(只包括中式的)06.8 Soybean products
; Z# J& Y. g% h4 I: I. n3 o( M  \07.0 烘焙类9 ^& J* A3 x1 f0 o! G1 r
07.1 面包,普通烘焙类,以及其混合物8 Q; B2 ~, ]7 _, o& h0 `# }
07.1.1 面包,面包卷. n# [% B. F# e8 M  p
07.1.1.1 酵母发酵面包及特殊面包
0 L1 b5 b' c7 L' k2 V; h4 |& X4 ?! v0 i07.1.1.2 苏打面包
4 I- Y4 H( z1 X8 x8 F7 `" ?2 s' v0 H% I
1 B) M6 ~+ R8 {# N" z+ g; u
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 楼主| 发表于 2008-5-23 12:10:00 | 只看该作者

二氧化钛(钛白粉)

二氧化钛(钛白粉)
, B9 |3 T; _1 |" E. D# v: K6 k& [- o( G6 \( u5 y  d
JECFA关于二氧化钛(钛白粉)的结论5 k% ~5 Q) Q% W# D: }# @5 J

  H$ O2 Z( O! t8 v4 }6 @/ e" ~摘要: 2006年JECFA关于二氧化钛的结论2 M% I6 t+ y0 H9 q8 A# ^
ADI值:不作限制。: |- A4 |& u3 o5 p, |$ a
功能:着色剂
$ U" e% b% ]& \+ \/ P5 n* P  Q, E' P. q4 o7 |
TITANIUM DIOXIDE, m" m; Q, `5 F% I9 x, n, M& |
Prepared at the 67th JECFA (2006) and published in FAO JECFA3 @$ g" O8 F3 f
Monographs 3 (2006), superseding specifications prepared at the 63rd. o; K# H  c7 E# ?, m5 |( P7 i, Z
JECFA (2004) and published in FNP 52 Add 12 (2004) and in the
3 h7 W# Y' y6 G  Y% {' WCombined Compendium of Food Additive Specifications, FAO JECFA6 G5 s0 H8 Q: t# e+ l9 B/ o9 m
Monographs 1 (2005). An ADI “not limited” was established at the 13th
  c0 O- K/ z1 Q0 y; X# b8 V8 {JECFA (1969).; O* P; ]7 a5 f, ^) y. [
SYNONYMS( U9 V6 P7 A2 a6 F
Titania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171
+ p0 D: ^6 L+ y/ x& _DEFINITION
! D- v4 @5 e$ w  @5 b9 P# @! L* LTitanium dioxide is produced by either the sulfate or the chloride6 }5 {3 C$ M( l+ d& s. g6 {! }
process. Processing conditions determine the form (anatase or rutile
4 T$ T3 ~9 j4 [$ \& ~; istructure) of the final product.
: Y6 K2 a* ~. k9 [! |In the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)
' z3 I6 d& r) ]or ilmenite and titanium slag. After a series of purification steps, the% z8 I4 n' y% [) d2 y' [
isolated titanium dioxide is finally washed with water, calcined, and" A7 x% m0 T  @' s
micronized." t: N" ]6 V7 _7 V% d
In the chloride process, chlorine gas is reacted with a titaniumcontaining
4 n8 j" `- m1 g2 ?; S  R' c3 umineral under reducing conditions to form anhydrous
* B0 S; j; g  |0 }titanium tetrachloride, which is subsequently purified and converted to
5 |6 w* U5 n' C8 C" W3 h) ltitanium dioxide either by direct thermal oxidation or by reaction with+ I+ P. }- S; E4 x9 P2 F4 f
steam in the vapour phase. Alternatively, concentrated hydrochloric
  G9 i6 x4 K( {2 a. Q% cacid can be reacted with the titanium-containing mineral to form a
8 C1 u5 w9 I; z, g0 Q3 h, ~/ ksolution of titanium tetrachloride, which is then further purified and) i8 t' y0 `( M+ J3 }- R: [
converted to titanium dioxide by hydrolysis. The titanium dioxide is/ \6 y4 Q# ~: I' n3 x
filtered, washed, and calcined.
: g% s0 ^5 f8 S* s4 C/ pCommercial titanium dioxide may be coated with small amounts of7 ~' A1 O% m% ?0 j& l  k
alumina and/or silica to improve the technological properties of the
$ y5 i% V4 E+ Q+ ^! Uproduct.1 h( W& |+ `+ ?$ ?- _
C.A.S. number 13463-67-7+ @% a1 j! P, B5 j/ d) D, }
Chemical formula TiO2
. _9 p5 {1 p" f; \Formula weight% s0 S- j9 x: E  W; M
79.88
7 H* U9 y9 t- m8 h' pAssay
* q# P: X4 ]1 c7 f( w# u8 ?Not less than 99.0% on the dried basis (on an aluminium oxide and
) ^, v; E1 `4 q. \/ Msilicon dioxide-free basis)
1 }; \' N# b& `DESCRIPTION/ H5 p$ k. J3 l
White to slightly coloured powder6 B  [+ f* z$ A: A5 I, }/ K
FUNCTIONAL USES2 X) `' _" B+ z3 y; L4 k
Colour
  R6 ]3 r" `  T& u0 W0 PCHARACTERISTICS
% \$ O" B& t. [IDENTIFICATION/ |: G( B$ d2 ?3 w/ u& s
Solubility (Vol. 4)4 N9 r0 m- K' X/ i( j
Insoluble in water, hydrochloric acid, dilute sulfuric acid, and organic  t! u: a8 {. C; j) f
solvents. Dissolves slowly in hydrofluoric acid and hot concentrated- X1 {" A$ X, E# D0 J
sulfuric acid.
  ^9 g6 Z: q5 |9 NColour reaction; h" u% z& Z) y- E
Add 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of
  b  n* C# }: ?* V" Jsulfuric acid appear, then cool. Cautiously dilute to about 100 ml with1 S- ?" S: R1 ~) R& w
water and filter. To 5 ml of this clear filtrate, add a few drops of
1 Y& G! c& b5 Z# Whydrogen peroxide; an orange-red colour appears immediately.8 `% w' j4 `1 ^. Z- ]3 B7 A2 O3 ^
PURITY( j7 q2 A1 Z: z3 V9 e# z
Loss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)% p- ?9 ?" c/ F! U
Loss on ignition (Vol. 4), [" Z; H  Y: O1 a. v; I& X/ B
Not more than 1.0% (800o) on the dried basis  J( M* X+ v, i$ ^
Aluminium oxide and/or
0 J  {/ r# C% Psilicon dioxide
% R5 m3 b: f9 S/ b% b! FNot more than 2%, either singly or combined/ `9 l( R! |( N. _0 K2 J
See descriptions under TESTS
: y" q3 @( y5 k% ~Acid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing
8 |, Y/ v5 R" [' y) ~alumina or silica.1 E! [( B  i8 h& n% _
Suspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and
& r  X" @% p* p7 V9 ?1 vplace on a steam bath for 30 min with occasional stirring. Filter
+ H! o! y8 e" i0 o/ Q2 ?0 gthrough a Gooch crucible fitted with a glass fibre filter paper. Wash
& R# X9 _9 h9 iwith three 10-ml portions of 0.5 N hydrochloric acid, evaporate the5 D5 L# M) p' F3 w) M" w
combined filtrate and washings to dryness, and ignite at a dull red9 w5 s, H; `+ y0 i+ M4 ~
heat to constant weight.
6 b# Z" h- S" [Water-soluble matter
) z3 j4 }2 l4 d) g! l2 x' m(Vol. 4)% ]& ]% B$ X- r) v5 O, T1 M: [
Not more than 0.5%
5 r  Z3 _) o, `" I2 c9 ]Proceed as directed under acid-soluble substances (above), using3 F+ J2 u! q# I
water in place of 0.5 N hydrochloric acid.4 L0 [) C2 M( B4 o$ f" O) N
Impurities soluble in 0.5 N
- Q+ {* N  p/ J- M1 Lhydrochloric acid8 J7 I8 K5 P9 H' l: ?
Antimony Not more than 2 mg/kg
1 M' b; _7 t8 [8 S* O( g/ s9 n; \See description under TESTS
% j3 g3 J- F5 K6 V- CArsenic Not more than 1 mg/kg
/ S+ m% r" ~& [( S- R" m: q* `( ~: @See description under TESTS
2 N, Y% r* @$ B* D; m0 jCadmium Not more than 1 mg/kg
8 x5 W& s6 {6 S1 h' K' x% a1 ]6 pSee description under TESTS1 A% Q/ e) T# R8 Z* l% w
Lead
1 w+ B& l" j& s. G( q1 v  SNot more than 10 mg/kg  V8 g; Z$ w& Q  d7 i. A: B
See description under TESTS
! x' K0 z' R0 r1 ~. h: J! `Mercury (Vol. 4) Not more than 1 mg/kg4 j' n: K6 {; a- l3 d
Determine using the cold vapour atomic absorption technique. Select a
9 N% n# ?+ E/ I- Ksample size appropriate to the specified level
/ R( Z- o8 e1 N+ e8 PTESTS
# I8 a4 n0 I3 I5 D  aPURITY TESTS
3 u; u7 q, J- `, d" XImpurities soluble in 0.5 N
2 R2 Y7 B4 i5 ^% q* Uhydrochloric acid
% k6 }. R( Y9 HAntimony, arsenic,6 {/ \9 |5 s% u5 w7 T0 p
cadmium and lead6 a  `) a, M3 ~1 c
(Vol.4)
4 b" _6 ]! k3 d: c7 b4 FTransfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N
( k+ Q: E  X  ^4 f: i1 n, p; A) shydrochloric acid, cover with a watch glass, and heat to boiling on a
" E! t/ l8 E6 @1 z& t, Ahot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml/ H1 t7 w. Q% l- A
centrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved
; `, I2 A" |5 m: C) ?7 o8 tmaterial settles. Decant the supernatant extract through a Whatman/ M: P" A- w+ d$ n( K
No. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml. y# K* @/ E4 s/ Z8 Y% O
volumetric flask and retaining as much as possible of the undissolved; z1 ~" b5 X4 ^9 u! I
material in the centrifuge bottle. Add 10 ml of hot water to the original0 S% \! O& C  d5 {6 d7 l
beaker, washing off the watch glass with the water, and pour the" L* M& M7 p9 i; t" K0 ]$ U( z
contents into the centrifuge bottle. Form a slurry, using a glass stirring
) r/ z# Z" E3 u" G  irod, and centrifuge. Decant through the same filter paper, and collect
  T% S9 H; i0 k) L) Ythe washings in the volumetric flask containing the initial extract.& q  P) d, [+ C) m& c! O7 p6 U
Repeat the entire washing process two more times. Finally, wash the
% `% V/ Y* b0 i: afilter paper with 10 to 15 ml of hot water. Cool the contents of the flask& Z6 U# I. p6 @" Z: `1 U
to room temperature, dilute to volume with water, and mix.
8 r6 _0 o% ^$ w$ k) p$ R$ fDetermine antimony, cadmium, and lead using an AAS/ICP-AES2 w* W; F( G/ p: P0 Z
technique appropriate to the specified level. Determine arsenic using the# n+ L7 `- t- ?" F
ICP-AES/AAS-hydride technique. Alternatively, determine arsenic using
' k) J* \8 g! ?) jMethod II of the Arsenic Limit Test, taking 3 g of the sample rather than
( D8 D4 x  t5 y0 T% _1 g. The selection of sample size and method of sample preparation
8 A) N/ n0 O# j! ]9 {may be based on the principles of the methods described in Volume 4.
# F( {- @( v. b* PAluminium oxide Reagents and sample solutions  j. g4 c8 t1 s! ^  z- G4 i
0.01 N Zinc Sulfate& v" x& z5 g  h; ?6 r* J
Dissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to! [- x( V) Z5 E6 R2 t) Z0 m
make 1000 ml. Standardize the solution as follows: Dissolve 500 mg9 b( W9 f) O) k% [
of high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of' O" D$ [9 i: a: D3 U& \3 S+ [
concentrated hydrochloric acid, heating gently to effect solution, then( s7 Z5 D0 U/ n7 \; D
transfer the solution into a 1000-ml volumetric flask, dilute to volume% i, r* `& n! c2 L% A
with water, and mix. Transfer a 10 ml aliquot of this solution into a 500
: M: {5 K$ o0 R  }! R9 zml Erlenmeyer flask containing 90 ml of water and 3 ml of
; T  l3 y0 {9 D% [& h, b( fconcentrated hydrochloric acid, add 1 drop of methyl orange TS and2 h1 u$ I5 x+ x
25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,  ~# X. s, M9 H! u9 ]% U) [
dropwise, ammonia solution (1 in 5) until the colour is just completely
. {$ S+ `6 N! E' y! echanged from red to orange-yellow. Then, add:
$ Q+ U0 Q2 `* j7 o6 K8 ?. @- Q(a): 10 ml of ammonium acetate buffer solution (77 g of
; d: f9 o* ?4 V9 i" L# kammonium acetate plus 10 ml of glacial acetic acid, dilute to6 D5 j% D4 p$ a( ]
1000 ml with water) and' R, t% M$ V4 ]% ?$ m6 }1 M3 P$ z
(b): 10 ml of diammonium hydrogen phosphate solution (150 g8 h; B* |# N: B2 Z1 ^& t- f  W
of diammonium hydrogen phosphate in 700 ml of water,
2 M- O9 t% F8 o8 ^: c* c9 I! Padjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,
" I, x0 X* R) @! f1 l6 `2 Gthen dilute to 1000 ml with water).
$ v) |$ z( ^5 JBoil the solution for 5 min, cool it quickly to room temperature in a
; c/ @" x- Q. Nstream of running water, add 3 drops of xylenol orange TS, and mix.* _9 u% Z0 X# k) V0 B) ?- {8 G, }
Using the zinc sulfate solution as titrant, titrate the solution to the first
* K: t1 I- G, s* W( P3 Tyellow-brown or pink end-point colour that persists for 5-10 sec. (Note:4 D4 `5 s3 w' Z: P
This titration should be performed quickly near the end-point by
4 ?0 M( [: M" j5 l5 t7 I! k8 Iadding rapidly 0.2 ml increments of the titrant until the first colour9 ~8 s. G$ o( h* U' Y+ @
change occurs; although the colour will fade in 5-10 sec, it is the true
$ M5 C1 \3 j# y, Z" p! gend-point. Failure to observe the first colour change will result in an8 w- o* V! z- Y3 U3 d9 R& P. @3 U
incorrect titration. The fading end-point does not occur at the second
* i3 _; X. R& O. ]" I# P) y  M4 U) I% Send-point.)6 g* b. p3 }5 i/ }0 _
Add 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a+ I2 Y0 [* l$ @" U9 t" j0 Q
stream of running water. Titrate this solution, using the zinc sulfate
/ y8 v2 q8 B  _! j$ Y& nsolution as titrant, to the same fugitive yellow-brown or pink end-point
5 J/ _( @6 p# Was described above.# H, J" ]4 @/ e0 Z' J& t
Calculate the titre T of zinc sulfate solution by the formula:
+ ]4 K( [0 V5 g5 k/ {3 ]T = 18.896 W / V) o9 t6 H  P: ~/ E! I" m
where
, ~6 D; m  r  L' }: R4 C! UT is the mass (mg) of Al2O3 per ml of zinc sulfate solution
" N! l1 l; L1 P! [- S; ZW is the mass (g) of aluminium wire
9 x5 A$ u+ Q7 Z& C" qV is the ml of the zinc sulfate solution consumed in the
  A2 ~. g2 f) Usecond titration% o+ g) A; D5 R7 h8 F
18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and
2 y+ ~4 |' ]+ A& U3 |$ N# fR is the ratio of the formula weight of aluminium oxide to1 D) l. x- f/ l1 P) K- I
that of elemental aluminium.: Q( n9 V2 Y  w6 h7 o
Sample Solution A
5 h1 Z4 `  P6 m  Y& w, kAccurately weigh 1 g of the sample and transfer to a 250-ml high-silica& I, n9 h, y8 P8 h
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).# V( g# K4 y8 G( `( P: ?
(Note: Do not use more sodium bisulfate than specified, as an excess
% D! u* u: B* P5 A3 \concentration of salt will interfere with the EDTA titration later on in the) S, N" A; ~- O& w( i9 Z( d
procedure.) Begin heating the flask at low heat on a hot plate, and) N! s0 o4 V6 x  l& S
then gradually raise the temperature until full heat is reached.
+ C% T6 x$ \. S) b& Y( t3 y(Caution: perform this procedure in a well ventilated area. ) When& G5 d5 i* ^: [, M. D, J
spattering has stopped and light fumes of SO3 appear, heat in the full7 `5 Y. P) O& D+ S8 v4 Q  c7 @6 |) _
flame of a Meeker burner, with the flask tilted so that the fusion of the
$ Q8 C* f; J2 |" U" t9 Usample and sodium bisulfate is concentrated at one end of the flask.
) V9 d1 O7 e2 U! G7 {5 e5 sSwirl constantly until the melt is clear (except for silica content), but
  ~: S# W" D, I1 F8 o4 N4 Zguard against prolonged heating to avoid precipitation of titanium
2 G' }; i) J/ U- v' g. {+ ^* sdioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until5 s! X/ l# U6 W  ~! l7 j
the mass has dissolved and a clear solution results. Cool, and dilute to
8 x/ Z' o) J3 M" G: C7 O; _120 ml with water. Introduce a magnetic stir bar into the flask.  e. X' b% a* z7 L
Sample Solution B
8 d: u7 b: w9 gPrepare 200 ml of an approximately 6.25 M solution of sodium9 j+ x  A$ N- q- A( N; K
hydroxide. Add 65 ml of this solution to Sample Solution A, while5 ~4 O" b6 w; t$ F2 ]0 ^
stirring with the magnetic stirrer; pour the remaining 135 ml of the
7 T8 _- d: |4 e# q) D7 n2 P: ~alkali solution into a 500-ml volumetric flask.
0 |3 Z# ~9 ~" ~4 m/ {+ m/ BSlowly, with constant stirring, add the sample mixture to the alkali
5 l4 Z1 h( ]7 ?' fsolution in the 500-ml volumetric flask; dilute to volume with water,
. c6 y; z( b2 u: R& L: F" n" yand mix. (Note: If the procedure is delayed at this point for more than
& F& M; q% D, }. h9 s6 r2 hours, store the contents of the volumetric flask in a polyethylene
- D/ o7 |) U; J3 Zbottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),
! [# j# [" t0 L9 u8 a7 ithen filter the supernatant liquid through a very fine filter paper. Label
& b3 R) s$ C9 Q5 zthe filtrate Sample Solution B.
; W! E; ?* O) ?5 eSample Solution C
) e) n6 ]" _7 ?7 `! A/ n3 c9 _! F8 D/ [Transfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer
8 Y8 u9 e5 ~, W) Q2 w  ^4 }flask, add 1 drop of methyl orange TS, acidify with hydrochloric acid
1 f; Y2 u( \. y3 R* D2 ^" Gsolution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02
9 Q) b& R, }8 N; O% P3 E8 `9 tM disodium EDTA, and mix. [Note: If the approximate Al2O3 content is- V+ \# _- b' c6 K% Z) ~
known, calculate the optimum volume of EDTA solution to be added
3 X7 t9 M* c1 @6 R4 Q1 ^$ hby the formula: (4 x % Al2O3) + 5.]
' x* v# n$ d8 ]) Z) [% @) C: a9 _Add, dropwise, ammonia solution (1 in 5) until the colour is just
# v; F& \$ P" [5 k  l" Bcompletely changed from red to orange-yellow. Then add10 ml each9 K0 Z7 E, e. r
of Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to
- `- f5 G* U6 lroom temperature in a stream of running water, add 3 drops of xylenol- Y- g/ a+ F* V, l
orange TS, and mix. If the solution is purple, yellow-brown, or pink,
8 ?; `! m: l" y; o2 ^bring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired( X* w6 m& j; g% R& o
pH, a pink colour indicates that not enough of the EDTA solution has- ?  X/ X" U( f. U$ u
been added, in which case, discard the solution and repeat this
; D3 H; D, y% K# I# ^1 I  g5 qprocedure with another 100 ml of Sample Solution B, using 50 ml,. d; E3 ?( X& {' |7 z2 @+ K% I
rather than 25 ml, of 0.02 M disodium EDTA.
+ s7 t7 b# U4 \6 R+ T7 K  GProcedure
% _- U4 F' \! u- U' rUsing the standardized zinc sulfate solution as titrant, titrate Sample
' [, d6 u* R. m4 B  X8 v# G1 h! B' mSolution C to the first yellow-brown or pink end-point that persists for8 y9 M- e* n$ Y. t: R, o
5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first) C7 o  [, d% ^% X
titration should require more than 8 ml of titrant, but for more accurate
: f% o, j8 s0 b( J+ U  `2 [work a titration of 10-15 ml is desirable.+ x% I* f3 b+ y% T6 V5 [8 M/ c
Add 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5
, S5 v2 E( S; z! f3 wmin, and cool in a stream of running water. Titrate this solution, using
! o/ h% R! p  V6 R9 L# e  W( Ythe standardized zinc sulfate solution as titrant, to the same fugitive
; u, q- H* H1 C$ G- Byellow-brown or pink end-point as described above.
5 U4 E% I, {5 z) v3 k6 X3 U; Y5 i# ZCalculation:" o) }" T  H& U$ p! L/ t4 l  \& e
Calculate the percentage of aluminium oxide (Al2O3) in the sample7 i/ X1 ?2 L9 H7 |
taken by the formula:. h( O( @9 w2 L+ n- t
% Al2O3 = 100 × (0.005VT)/S$ \( G& W$ p/ L+ l1 Q
where/ U5 t5 u$ o7 h% i
V is the number of ml of 0.01 N zinc sulfate consumed in
; D8 S% I) `; [8 Tthe second titration,$ p0 |1 L9 a* O+ k. C
T is the titre of the zinc sulfate solution,0 ^, U6 d9 n- _
S is the mass (g) of the sample taken, and' s; y- c! c$ Q2 y
0.005 = 500 ml / (1000mg/g × 100 ml).' ~2 ?( O1 J: V+ V. M" |+ i5 ]
Silicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica1 e; a5 m/ s5 S6 k
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).1 }) m; |" K9 Q% p2 i
Heat gently over a Meeker burner, while swirling the flask, until
; `7 o- ~5 n6 @3 [# S5 edecomposition and fusion are complete and the melt is clear, except
6 x: b; F' B& t' v/ Hfor the silica content, and then cool. (Caution: Do not overheat the
4 F5 ~3 X3 P6 L# @) X. |9 X0 vcontents of the flask at the beginning, and heat cautiously during
3 C6 G+ l$ E* s" I7 @7 \8 J4 ifusion to avoid spattering.)
8 Z2 C" P2 C6 q# P" K- ]  pTo the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat
: y: A1 @$ Q" ^; P. k; R8 ~. u& |) e% vcarefully and slowly until the melt is dissolved. Cool, and carefully add
  Z! V( Y! |+ D) k150 ml of water by pouring very small portions down the sides of the+ w# a1 v- m$ q
flask, with frequent swirling to avoid over-heating and spattering. Allow
( b' x) l, m4 B9 X/ b8 O% pthe contents of the flask to cool, and filter through fine ashless filter
8 z$ H! L& d- ]" D; T( H; upaper, using a 60 degree gravity funnel. Rinse out all the silica from
" F. G/ K  U1 b: b; wthe flask onto the filter paper with sulfuric acid solution (1 in 10).
. |- Y3 U% ?/ l  N: }1 v) g- |7 DTransfer the filter paper and its contents into a platinum crucible, dry in5 c+ w8 e" p) \/ |/ K6 F  h! ?
an oven at 1200, and heat the partly covered crucible over a Bunsen
2 H7 N7 G$ m" \burner. To prevent flaming of the filter paper, first heat the cover from$ R7 C2 z- z$ ]
above, and then the crucible from below.
8 b; N' h# g7 L) A! z% C- u7 nWhen the filter paper is consumed, transfer the crucible to a muffle
0 B" J/ |* I/ ~1 w$ tfurnace and ignite at 1000o for 30 min. Cool in a desiccator, and7 p, V" W" `5 {  \% b1 V
weigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated0 c' u  e2 |) c" N4 f
hydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first/ i. I& }* g  Q8 I
on a low-heat hot plate (to remove the HF) and then over a Bunsen
  e1 j+ x5 u6 e) O) T0 N  Pburner (to remove the H2SO4). Take precautions to avoid spattering,
+ b) \7 H4 G' O# e+ l  Hespecially after removal of the HF. Ignite at 1000o for 10 min, cool in a
) A& }' ?, b. h! z; M5 bdesiccator, and weigh again. Record the difference between the two3 @3 ~$ Q& l# z) o; b1 Z
weights as the content of SiO2 in the sample.& |/ Q) H, k- W+ Z
METHOD OF ASSAY
$ G% {1 b/ [" x" W1 IAccurately weigh about 150 mg of the sample, previously dried at 105o; i. ]; \: J# J) R# k" ]9 T
for 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water
' q" J, V/ B" }4 N& H" M1 Cand shake until a homogeneous, milky suspension is obtained. Add 30
" C" ~' c8 l8 B2 d* w9 eml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially: K% `3 b: E9 R
heat gently, then heat strongly until a clear solution is obtained. Cool,: h) z) p: h- D
then cautiously dilute with 120 ml of water and 40 ml of hydrochloric: j5 o7 u# u, \6 b) n2 `: ~  z. s+ z
acid, and stir. Add 3 g of aluminium metal, and immediately insert a
) M7 ~, i( K! xrubber stopper fitted with a U-shaped glass tube while immersing the
3 J; R9 {" h$ ~  M, hother end of the U-tube into a saturated solution of sodium
. p/ }, ]- V1 tbicarbonate contained in a 500-ml wide-mouth bottle, and generate
" y& A1 G4 e2 o* whydrogen. Allow to stand for a few minutes after the aluminium metal, i; N5 D4 |9 l; ^: N
has dissolved completely to produce a transparent purple solution.
: @8 H+ ?- H1 X+ n8 O+ D2 qCool to below 50o in running water, and remove the rubber stopper
2 z4 Z/ t+ g& h2 |carrying the U-tube. Add 3 ml of a saturated potassium thiocyanate9 z& X/ O, f4 u( |; t
solution as an indicator, and immediately titrate with 0.2 N ferric7 b3 @' ^, D8 X1 D" ?2 G
ammonium sulfate until a faint brown colour that persists for 309 H: p9 {- y  |0 s5 m/ }
seconds is obtained. Perform a blank determination and make any5 w% i% ~& x5 S: Z+ [" C
necessary correction. Each ml of 0.2 N ferric ammonium sulfate is
' V4 G* ?; z7 F; W5 M* Qequivalent to 7.990 mg of TiO2.; J2 i% P; r; b' F
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