Oxygen in Copper and

®
Copper Alloys
LECO Corporation; Saint Joseph, Michigan USA

Instrument: O836*
*O/ON/OH/ONH836 also applicable

Introduction
Copper is the most important material in the
electrical conductor wire industry due to its high Accessories
benefit-cost ratio. Copper provides admirable surface 776-247 Graphite Crucibles; 501-073 Graphite Powder;
quality, mechanical properties and high conductivity 611-351-182 Lower Electrode Tip for 776-247 Crucibles
at a cost much less than silver or gold. Aluminum is without automation; 611-351-181 Lower Electrode Tip for
the only metal that is routinely substituted for copper, 776-247 Crucibles with automation.
but only in applications where weight is a major
Note: The 611-351-181 Lower Electrode Tip is only required
factor. One of the most important factors when
if the instrument is equipped with automation.
grading copper is the level of residual impurities,
primarily the oxygen level. Oxygen levels in electrical
conductor wires typically range from 5-10 ppm (OF –
oxygen free, OFE – oxygen-free electronic grades) to
Calibration Samples
around 650 ppm (ETP – electrolytic tough pitch LECO 501-147, 501-148, 501-149, 501-990 One-Gram
grade). Oxygen levels of up to 200 ppm can actually Nickel Plated Copper Pins with O content determined;
improve conductivity as it acts as a scavenger NIST, BCR or other suitable reference materials.
element that forms metal oxides with metal Note: Most LECO copper calibration materials are plated
contaminants. Too much oxygen has been associated with nickel for stability and oxidation resistance. Sample
with an increase in hydrogen embrittlement preparation is not required and the samples are suitable for
problems. use straight from the bottle. Refer to the certificate of
analysis for details.
Oxygen determination by the inert gas fusion infrared
detection method is the most widely used and Sample Preparation
reliable method for broad range and high precision 1. Prepare the samples according to the standard method
oxygen determination in copper and copper alloys. in ASTM E2575 for the analysis of Oxygen in Copper.
LECO Corporation offers several configurations of 2. If conformance to ASTM E2575 is not required, the
fusion determination for this analysis. The following samples may be abraded with a file before analysis.
application note outlines the process from sample

Inorganic Application Note

Note: Take care when abrading samples to not heat the
generation to data. samples. Analyze the samples within four (4) hours of
abrading.
Sample Preparation
The sample preparation of copper for oxygen analysis Analysis Procedure
is important due to the oxidation properties of 1. Prepare the instrument as outlined in the operator's
copper. There are two methods of sample instruction manual.
preparation that are frequently used for the analysis 2. Determine the instrument blank.
of oxygen in copper. The standard method according a. Login a minimum of 3 Blank replicates.
to ASTM E2575 uses chemical etching to remove b. Press the Analyze button on the instrument screen.
impurities from the surface of the copper. After a short delay, the loading head slide-block will
Subsequently the prepared sample is washed in a open.
suitable solvent such as methanol and dried with c. Press the Analyze button on the instrument screen
warm air. Another method of preparation that is not again; the loading head slide-block will close and
included in the standard method is physical abrading. the lower electrode will open.
The sample can be cut and abraded with a file to d. Remove the crucible and clean the upper and lower
remove the surface impurities. Care must be taken to electrode either manually or, if applicable, press the
not overheat the sample and change the chemistry of Analyze button again to clean with the
the copper. The prepared sample may be washed in a automatic cleaner.
suitable solvent such as methanol. Both methods e. Add approximately 0.05 g of 501-073 Graphite
require immediate analysis of the prepared sample to Powder to the 776-247 crucible.
minimize the oxidation of the prepared copper. f. Firmly place the graphite crucible on the lower
electrode tip.
g. Press the Analyze button on the instrument
screen; the lower electrode will close and the
analysis sequence will start and end
automatically.
 Method Parameters
Delivering the Right Results General Parameters
Sample Introduction Automated Sample Drop
Analysis Delay 25 s
Auto Analyze on Mass Entry No
Outgas Before Mass Entry No
Wait for User to Load Sample Yes
Vacuum On Time 18 s
Element Parameters Oxygen
Integration Delay 5s
Starting Baseline 2s
Use Comparator No
Integration Time 30 s
Use Endline Yes
Ending Baseline 2s
Range Select Auto
Range Lower Limit 800
Range Upper Limit 950
Furnace Control Mode Power
Outgas Furnace Settings
Cycles 2
Power Mode Constant
Power 5800* W
Time 20 s
Cool Time 5s
Surface Oxide Removal
Remove Surface Oxide No
Analyze Furnace Settings
Step 1 Power Mode Constant
Power 4825* W
Approximate Cycle Time 3.5 Minutes
*May vary, depending on line voltage. Level can be adjusted to facilitate recovery and/or reduce crucible burn-through.

Automation Parameters (if equipped)

General Parameters
Auto Cleaner State Enabled
Auto Cleaner Mode During Analysis
Clean Time 8s

Procedure (continued)
h. Repeat steps 2b through 2g a minimum of f. Clean the upper and lower electrode either
three times. manually or, if applicable, remove the crucible and
i. Set the blank following the procedure press the Analyze button again to clean with the
outlined in the operator's instruction manual. automatic cleaner.
3. Instrument calibration/drift correction. g. Add approximately 0.05 g of 501-073 Graphite
a. Login a minimum of 3 Standard replicates. Powder to the 776-247 crucible.
b. Weigh ~1.000 gram of a calibration/drift h. Firmly place the graphite crucible on the lower
sample, enter the mass and sample electrode tip.
identification into appropriate replicate fields. i. Press the Analyze button on the instrument screen;
Note: LECO Nickel Plated Copper Pin Reference the lower electrode will close and the analysis
Materials do not require preparation. See the sequence will start and end automatically.
preparation statement on the Reference Material j. Repeat steps 3b through 3i a minimum of three
®

Certificate. times for each calibration/drift sample used.

k. Calibrate/drift following the procedure outlined in
c. Press the Analyze button on the instrument the operator's instruction manual.
screen. After a short delay, the loading head 4. Analyze Samples.
slide-block will open. a. Login the appropriate number of Sample
d. Place the calibration/drift sample into the replicates.
open port at the top of the loading head. b. Weigh ~1.000 gram of sample, enter the mass
e. Press the Analyze button on the instrument and identification into appropriate replicate fields.
screen; the loading head slide-block will close c. Repeat steps 3c through 3i for sample analysis.
and the lower electrode will open.
 ®
Typical Results
Note: LECO Nickel Plated Copper Pin Reference Materials do not require preparation. See the preparation statement
on the Reference Material Certificate.

Sample Mass (g) O% Sample Mass (g) O%

CRM 1.0 g 0.0583 CRM 1.0 g 0.0581
CMO Cu600/I 0.0579 CMO Cu600/I 0.0581
Copper Rod 0.0581 Copper Rod 0.0580
0.0581% O 0.0582 0.0581% O 0.0581
±0.0012% 0.0579 ±0.0012% 0.0580
Etched 0.0578 Abraded 0.0583
0.0584 0.0583
0.0581 0.0583
0.0582 0.0579
0.0580 0.0580
X= 0.0581 X= 0.0581
S= 0.0002 S= 0.0001

CRM 1.0 g 0.0321 CRM 1.0 g 0.0321

NIST 885 0.0318 NIST 885 0.0319
Refined 0.0317 Refined 0.0323
Copper 0.0325 Copper 0.0321
0.031% O 0.0323 0.031% O 0.0321
±0.002% 0.0317 ±0.002% 0.0320
Etched 0.0317 Abraded 0.0318
0.0319 0.0322
0.0319 0.0319
0.0319 0.0320
X= 0.0319 X= 0.0320
S= 0.0003 S= 0.0001

OFHC 1.0 g 0.00010 LECO 1.0 g 0.0238

Inorganic Application Note

Copper Wire 0.00010 501-147 0.0241
Uncertified 0.00009 Nickel Plated 0.0240
Etched 0.00010 Copper 0.0238
0.00009 0.0239% O 0.0238
0.00009 ±0.0003% 0.0237
0.00010 As Received 0.0240
0.00014 0.0237
0.00010 0.0239
0.00015 0.0237
X= 0.00011 X= 0.0238
S= 0.00002 S= 0.0001

Calibrated with CRM CMO Cu600/I utilizing a single standard calibration forced through the origin.

LECO Corporation
3000 Lakeview Avenue • St. Joseph, MI 49085 • Phone: 800-292-141 • Fax: 269-982-8977
[email protected] • www.leco.com • ISO-9001:2008 HQ-Q-994 • LECO is a registered trademark of LECO Corporation.

Form No. 203-821-436 12/12—REV0 © 2012 LECO Corporation