PERMFILE109666

• Permit No: C1981008A
• IBM Index Class Name: Permit File
• Doc Date: 12/11/2001
• Section_Exhibit Name: NH1 TAB 6 APPENDIX 6-3 CHEMICAL ANALYSIS PROCEDURES
• Media Type: D
• Archive: Yes

•
DETERMINATION OF TOTAL SULFUR IN OVERBURDEN MATERIALS
with a
LECO INDUCTION FURNACE AND AUTOMATIC TITRATOR
Solution Preparation:
1. Potassium Iodate (KIO ):0.449g/L. This solution is
direct reading for lgOsamples. 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
1®g/L sodium azide (complexes chlorine liberated from
t1i@ sample which has the same bleaching effect on
the indicator solution as the tit~'ated 50 ). Handle
w:ifh. extreme caution as sodium axida li,beEates poison.
gas_t~~_in acid solutions.
U
3. Starch a3llitican:
water; stir r~d~,~.
this slowly add t
constantly. Cool
to the solution.
starch dispenser.
S days old.
Sample Preparation:
Add 2 g arrowroot starch to 50 ml
Spearately boil 150m1 water and to
he 2g starch solution, stirring
and add 6g potassium iodide (KI)
Transfer the solution into the
Do not use starch solution over
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 FopDer ring on top of sample.
5. After add-ir?~J adch component, gently shake the crucible
to evenly dCYer t1'?%~ bottom.
6. Place porous cover on crucible.
Instrument Operation:
1. Turn filament and high voltage switches on (grid tap
in high position).
r~
L
2. Turn on titrator.
3. Set timer switch to on with timer adjusted to 8 minutes
(or a time sufficient to satisfy instructions 10 and 11).
6-112