PERMFILE131137

• Permit No: C1980005
• IBM Index Class Name: Permit File
• Doc Date: 12/11/2001
• Doc Name: LABORATORY PROCEDURES
• Section_Exhibit Name: TAB 06 APPENDIX 6-2
• Media Type: D
• Archive: No

DETERMINATION OF TOTAL SULFUR IN OVERBURDEN MATERIALS
with a
LECO INDUCTION FURNACE AND AUTOMATIC TITRATOR
Solution Preparation:
1. Potassium Iodate (KIO3):0.444g/L. This solution is
direct reading for lg samples. For 0.5g samples
multiply the buret reading by 2, for O.lg samples
by 10, etc. (Stronger solutions may be employed
with the correct factors being applied to the buret).
2, Hydrochloric Acid solution: 15 ml conc. HC1/L and
lOg/L sodium azide (complexes chlorine liberated from
the sample which has the same bleaching effect on
the indicator solution as the titrated 502). Handle
with extreme caution as sodium azide liberates poison
gases in acid solutions.
3. Starch Solution: Add 2 g arrowroot starch to 50 ml
water; stir well. Spearately boil 150m1 water and to
this slowly add the 2g starch solution, stirring
constantly. Cool and add 6g potassium iodide (KI)
to the solution. Transfer the solution into the
starch dispenser. Do not use starch solution over
5 days old.
Sample Preparation:
1. Place one 0.2m1 scoop, level full, of iron chip
accelerator into crucible.
2. Weigh O.SOOg of -60 mesh sample into crucible.
(Sample size and. accelerators may have to be adjusted
to come into the buret and titrant range.)
3. Place one 0.2 ml scoop tin metal accelarator on copper
ring.
4. Place 1 copper ring on top of sample.
5. After adding each component, gently shake the crucible
to evenly cover the bottom.
6. Place porous cover on crucible.
Instrument
1.
2.
3.
ration:
Turn filament and high voltage switches on (grid tap
in high position).
Turn on titrator.
Set timer switch to on with timer adjusted to
(or a time sufficient to satisfy instructions
I,
I,
//
8 minutes
10 and 11).
6-57