This article discusses the steps and setting necessary to evaluate the sulfur level in ore concentrates using the CS/S844. The efficiency of the concentration process can be determined using the sulfur level of the ore concentrate as a quality control measure. It can also be used to obtain an estimate of the metal-in-concentrate.
The CS/S844 sulfur by combustion analyzer, equipped with an easy-to-use touch-screen interface and a broad sulfur detection range, can be used in all mining operations laboratories.
Sample Preparation
Prior to analysis, samples must be crushed to a uniform powder form.
Accessories
LECOCEL II (502-173 or 501-008); 528-018 or 528-018HP Crucible; 773-579 Metal Scoop; 502-231 Iron Chip or 501-077 Accelerator; 761-929 Tongs
To obtain optimal sulfur precision, ceramic crucibles can be pre-baked in a tube furnace (LECO TF1/TF-10) at ≥1250°C for a minimum of 15 minutes, or in a muffle oven at ≥1000°C for a minimum of 1 hour. The crucibles are removed from the muffle oven/tube furnace, allowed to cool, and then transferred to a desiccator for storage.
Clean tongs must be used while handling the baked crucibles to avoid contamination.
Calibration
502-085 Zinc Sulfide Reference Material or other appropriate ore concentrate reference materials.
Method Parameters
General Parameters |
|
Purge Time: |
10 s |
Delay Time: |
20 s |
Sample Cool Time: |
0 s |
Furnace Mode: |
Constant |
Furnace Power: |
100% |
Element Parameters |
Sulfur |
Integration Delay: |
0 s |
Starting Baseline: |
2 s |
Use Comparator: |
No |
Integration Time: |
55 s |
Use Endline: |
Yes |
Ending Baseline: |
2 s |
Range Select: |
Auto |
Range Lower Limit: |
800 |
Range Upper Limit: |
950 |
Procedure
1. Following the instructions in the operator's instruction manual, prepare instrument for operation.
2. Determine the instrument Blank.
- Login at least three Blank reps.
- Add one 773-579 Scoop (~0.8 g) Iron Chip and one 773-579 Scoop (~1.2 g) of LECOCEL II.
- Put the crucible on the furnace pedestal (or suitable autoloader position if applicable), and start analysis.
- Repeat steps 2b through 2c at least three times.
- Follow the procedure described in the operator's instruction manual to set the blank.
3. Drift/Calibrate Correct
- Login at least three standard/drift reps.
- Weigh ~0.15 g of 502-085 zinc sulfide reference material or other appropriate calibration/drift material into the crucible. Enter the identification and mass of the reference material.
Note: For multi-mass calibration linear, use ~0.05 to ~0.20 g (three reference material reps at every mass) as alternate calibration.
- Add one 773-579 Scoop (~0.8 g) Iron Chip and one 773-579 Scoop (~1.2 g) of LECOCEL II.
- Place the crucible on the furnace pedestal (or suitable autoloader position if applicable) and begin analysis.
- Repeat steps 3b through 3d at least three times for every calibration/drift reference material intended for calibration/drift.
- Follow the procedure described in the operator's instruction manual to calibrate/drift correct.
4. Sample Analysis
- Login a sample with suitable number of reps.
- Weigh ~0.05 to 0.20 g of ore concentrate sample in the crucible. Enter the identification and mass.
Note: 60 mg sulfur is the maximum instrument range.
- Add one 773-579 Scoop (~0.8 g) Iron Chip and one 773-579 Scoop (~1.2 g) of LECOCEL II.
- Place the crucible on the furnace pedestal (or suitable autoloader position if applicable), and begin analysis.
Typical Results
Sample |
Mass (g) |
% Sulfur |
502-085 |
0.0508 |
32.62 |
Zinc Sulfide |
0.0498 |
32.99 |
32.91% Sulfur |
0.0503 |
32.98 |
|
0.1012 |
33.12 |
|
0.1024 |
32.95 |
|
0.1000 |
33.02 |
|
0.1513 |
32.79 |
|
0.1493 |
33.01 |
|
0.1520 |
32.84 |
|
0.2001 |
33.60 |
|
0.2006 |
33.28 |
|
0.2020 |
33.61 |
|
Avg = |
33.07 |
|
s = |
0.30 |
CCU-1c |
0.0515 |
33.56 |
Copper Concentrate |
0.0523 |
33.59 |
33.3% Sulfur |
0.0490 |
33.32 |
|
0.1025 |
33.71 |
|
0.0997 |
33.58 |
|
0.1000 |
33.29 |
|
0.1506 |
33.63 |
|
0.1496 |
33.34 |
|
0.1511 |
33.23 |
|
0.2011 |
33.32 |
|
0.1998 |
33.25 |
|
0.2003 |
33.40 |
|
Avg = |
33.44 |
|
s = |
0.17 |
This information has been sourced, reviewed and adapted from materials provided by LECO Corporation.
For more information on this source, please visit LECO Corporation.