Organic Application Note

Sulfur and Carbon in Cement, Fly Ash,

Limestone, Soil, and Ore
Instrument
SC632

Sample Preparation
A representative, uniform sample is required. Samples
should be ground to pass a No. 100 (150 micron) sieve.
Samples should be dried to a constant weight.

Accessories
528-203 Ceramic Boat, 502-321 Com-Cat™

Calibration Samples
NIST or other suitable cement, fly ash, ore, or limestone reference materials

Method Parameters*
Description
Nominal Mass 1.0000
Furnace Temperature 1450oC
Lance Delay Time 20 seconds
Elements to Analyze Sulfur and Carbon

Element Parameters Sulfur Carbon

IR Analysis Stabilize Comparator 2.00 2.00
Manual Load Baseline Delay Time (seconds) 3 3
IR Baseline Time (seconds) 1 2
Auto Detect Data Missed Time (seconds) 5 5
Endline Time (seconds) 1 1
Minimum Analysis Time (seconds) 120 60
Maximum Analysis Time (seconds) 360 360
Comparator Level (%) 0.30 1.00
Conversion Factor 1.00 1.00
Significant Digits 5 5
Range Selection Automatic Automatic
Automatic Range Switch Level 3500.0 4000.0
Automatic Range Switch-Back Level 3000.0 3500.0

System Parameters
Gas Conservation Timeout 5 minutes
Auto Increment Sample Name Disable
Lance Limits 50000
Furnace Standby Temperature 1050oC

*Refer to the SC632 operator's instruction manual for method parameter definitions.

SC632
Procedure
1. Prepare instrument for operation as outlined in the operator's instruction manual.
2. Condition the system by analyzing three to five ~0.25 g coal samples.
3. Determine blank.
a. Enter 1.0000 g mass into Sample Login (F3) using Blank as the sample name.
b. Add ~1 g of 502-321 Com-Cat™ into a 528-203 Ceramic Boat.
c. Initiate the Analysis Sequence (F5), when “Load Sample into Furnace” message appears on the
display, slide crucible into the combustion tube until it reaches boat stop. Alternately, place
crucible onto the appropriate position of carousel if equipped with autoloader system.
d. Repeat steps 3a through 3c a minimum of five times.
e. Set the blank following the procedure outlined in the operator's instruction manual.
4. Calibrate/Drift Correct.
a. Weigh ~0.1 to 0.35 g of calibration sample into a 528-203 Ceramic Boat, enter mass and
sample identification into Sample Login (F3).
b. Add ~1 g of 502-321 Com-Cat™ to the crucible and thoroughly mix with the sample.
c. Initiate the Analysis Sequence (F5), when “Load Sample into Furnace” message appears on
screen, slide crucible into the combustion tube until it reaches boat stop. Alternately, place
crucible onto the appropriate position of carousel if equipped with autoloader system.
d. Repeat steps 4a through 4c a minimum of five times for each calibration/drift sample used.
e. Calibrate or Drift Correct the instrument following the procedure outlined in the operator's
instruction manual.
5. Analyze Samples.
a. Weigh ~0.1 to 0.35 g sample into a 528-203 Ceramic Boat and enter mass and sample
identification information into Sample Login (F3).
b. Add ~1 g of 502-321 Com-Cat™ to the crucible and thoroughly mix with the sample.
c. Initiate the Analysis Sequence (F5), when “Load Sample into Furnace” message appears on
screen, slide crucible into the combustion tube until it reaches boat stop. Alternately, place
crucible onto the appropriate position of carousel if equipped with autoloader system.

Typical Results*
Sample Mass g %S %C
NIST 0.1031 1.083 0.14
SRM 0.1054 1.070 0.12
1889 0.1016 1.086 0.12
Cement 0.1059 1.081 0.12
1.072%S 0.1042 1.064 0.12
X= 1.077 0.12
s= 0.009 0.01

NIST 0.2196 0.143 0.42

SRM 0.2057 0.147 0.41
2690 0.2062 0.148 0.38
Coal 0.2013 0.147 0.39
Fly Ash 0.2125 0.154 0.40
0.15% S X= 0.148 0.40
s= 0.004 0.01

NIST 0.2531 0.367 3.31

SRM 0.2505 0.357 3.32
8704 0.2437 0.360 3.31
River 0.2501 0.366 3.31
Sediment 0.2510 0.364 3.32
3.35% C X= 0.363 3.31
s= 0.004 0.005

continued on next page

*Results based on multipoint, multi-standard calibration using NIST and LECO soil, ore, cement, and fly ash reference materials.
Typical Results* (continued)
Sample Mass g %S %C
502-318 0.2455 0.736 0.50
Ore Tailing 0.2563 0.754 0.52
0.73% S 0.2487 0.744 0.50
0.50% C 0.2530 0.740 0.52
0.2575 0.715 0.49
X= 0.738 0.51
s= 0.015 0.01

LECO 0.2212 4.31 4.09

502-320 0.2042 4.29 4.16
Ore Tailing 0.2139 4.32 4.10
4.31% S 0.2121 4.31 4.12
4.11% C 0.2067 4.36 4.06
X= 4.32 4.11
s= 0.02 0.04

LECO 0.2175 0.122 10.14

502-309 0.2077 0.126 10.15
Soil 0.2190 0.126 10.15
0.126% S 0.2133 0.127 10.15
10.14% C 0.2217 0.125 10.14
X= 0.125 10.15
s= 0.002 0.005

LECO 0.2507 0.022 3.00

502-308 0.2499 0.022 2.96
Soil 0.2533 0.022 3.00
0.022% S 0.2626 0.021 3.03
3.00% C 0.2574 0.021 3.04
X= 0.022 3.01
s= 0.001 0.03

*Results based on multipoint, multi-standard calibration using NIST and LECO soil, ore, cement, and fly ash reference materials.

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