Designation: E1409 − 13

Standard Test Method for

Determination of Oxygen and Nitrogen in Titanium and
Titanium Alloys by Inert Gas Fusion1
This standard is issued under the fixed designation E1409; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope analyzers typically measure both oxygen and nitrogen simul-

1.1 This test method covers the determination of oxygen in taneously or sequentially utilizing parallel measurement sys-
titanium and titanium alloys in mass fractions from 0.01 % to tems.
0.5 % and the determination of nitrogen in titanium and 4.2 The test sample, plus flux, is fused in a graphite crucible
titanium alloys in mass fractions from 0.003 % to 0.11 %. under a flowing inert gas stream at a temperature sufficient to
1.2 This standard does not purport to address all of the release oxygen and nitrogen. Oxygen combines with carbon to
safety concerns, if any, associated with its use. It is the form carbon monoxide (CO) and nitrogen is released as N2.
responsibility of the user of this standard to establish appro- Depending on instrument design, the CO may be oxidized to
priate safety and health practices and determine the applica- carbon dioxide (CO2). The CO or CO2, or both, are swept by
bility of regulatory limitations prior to use. Specific warning the inert gas stream into either an infrared or thermal conduc-
statements are given in 8.8. tivity detector. The detector response generated by analysis of
the test sample is compared to the response generated by
2. Referenced Documents analysis of reference materials and the result is displayed as
2.1 ASTM Standards:2 percent oxygen. The nitrogen is swept by the inert gas stream
E50 Practices for Apparatus, Reagents, and Safety Consid- into a thermal conductivity detector. The detector response
erations for Chemical Analysis of Metals, Ores, and generated by analysis of the test sample is compared to the
Related Materials response generated by analysis of reference materials and the
E135 Terminology Relating to Analytical Chemistry for result is displayed as percent nitrogen.
Metals, Ores, and Related Materials 4.3 In a typical instrument for the determination of nitrogen,
E173 Practice for Conducting Interlaboratory Studies of the sample gases are swept with inert gas through heated rare
Methods for Chemical Analysis of Metals (Withdrawn earth/copper oxide that converts CO to CO2 and hydrogen (H2)
1998)3 to water (H2O). The CO2 is absorbed on sodium hydroxide
E1601 Practice for Conducting an Interlaboratory Study to impregnated on clay, and the H2O is removed with magnesium
Evaluate the Performance of an Analytical Method perchlorate. The nitrogen, as N2, enters the measuring cell and
the thermistor bridge output is integrated and processed to
3. Terminology display percent nitrogen.
3.1 Definitions—For definitions of terms used in this 5. Significance and Use
method, refer to Terminology E135.
5.1 This test method is primarily intended as a test for
4. Summary of Test Method compliance with compositional specifications. It is assumed
4.1 This test method is intended for use with automated, that all who use this test method will be trained analysts
commercially available, inert gas fusion analyzers. These capable of performing common laboratory procedures skill-
fully and safely. It is expected that the work will be performed
in a properly equipped laboratory.
1
E01 on Analytical Chemistry for Metals, Ores, and Related Materials and is the
direct responsibility of Subcommittee E01.06 on Ti, Zr, W, Mo, Ta, Nb, Hf, Re. 6. Interferences
Current edition approved Oct. 1, 2013. Published November 2013. Originally
approved in 1991. Last previous edition approved in 2008 as E1409 – 08. DOI: 6.1 The elements usually present in titanium and its alloys
10.1520/E1409-13. do not interfere but there is some evidence to suggest that low
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or purity flux can cause some adsorption of the released oxygen.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on 7. Apparatus
the ASTM website.
3
The last approved version of this historical standard is referenced on 7.1 Instrument—Fusion and measurement apparatus, auto-
www.astm.org. matic oxygen and nitrogen determinator consisting of an

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States

1
 E1409 − 13
electrode furnace, provision for scrubbing impurities from NOTE 3—In 2004, alternative sample preparation procedures (Section
analytical gas stream; infrared or thermal conductivity mea- 12) were tested by seven laboratories. Three laboratories processed the
sample materials by pickling their samples in HF-H2O2 (8.8). Two
surement system(s), or both, and auxiliary gas purification laboratories utilized the HF-HNO3 alternative pickle solution (8.8). Two
systems (Note 1). laboratories utilized abrasion (in this case diamond saw and shear) in
accordance with 12.2. The prepared samples were distributed among the
NOTE 1—Several models of commercial oxygen and nitrogen determi-
laboratories for analysis. Six laboratories analyzed these samples in
nators are available and presently in use by industry. Each has its own
random order under a single operator, single-day, single calibration sample
unique design characteristics and operational requirements. Consult the
run. The results of this testing are given in Tables X1.1 and X2.1 for
instrument manufacturer’s instruction manual for operational details.
oxygen and nitrogen, respectively. In both cases, the analysis of variance
7.2 Graphite Crucibles—The crucibles must be made of (ANOVA) indicates that there is no significant difference at the 95 % level
high-purity graphite and be of the dimensions recommended by of confidence for either oxygen or nitrogen due to the preparation
the instrument manufacturer. technique.

7.3 Flux—Flux must be made of high-purity nickel. If 9. Hazards

nickel baskets are used, the dimensions must meet the require- 9.1 Use care when handling hot crucibles and operating
ments of the automatic sample drop, if present, on the furnaces to avoid personal injury by either burn or electrical
instrument. (See Note 2.) Ultra high-purity nickel flux is shock.
commercially available and may eliminate the need to clean the
flux before using it. 9.2 For precautions to be observed in the use of HF and
other reagents in this test method, refer to Practices E50.
NOTE 2—In some instruments, nitrogen and oxygen are run sequentially
and platinum is the required flux for nitrogen. High-purity platinum can be 10. Preparation of Apparatus
substituted for nickel in the same ratio of flux to sample.
10.1 Assemble the apparatus as recommended by the manu-
7.4 Tweezers or Crucible Tongs, made of solvent and acid
facturer. Make the required power, gas, and water connections.
resistant material.
Turn on the instrument and allow sufficient time to stabilize the
equipment.
8. Reagents
10.2 Change the chemical reagents and filters as required.
8.1 Acetone—Low residue reagent grade or higher purity.
Test the furnace and analyzer to ensure the absence of leaks
8.2 Graphite Powder (optional)—High-purity as specified (Note 4). A minimum of two test runs using a sample as
by the instrument manufacturer. directed in 14.3 and 14.4 is recommended to condition the
8.3 Inert Gas—Use the purity and type specified by the newly changed filters. This should be done before attempting
instrument manufacturer. to calibrate the system or to determine the value of the blank.
8.4 Magnesium Perchlorate, Anhydrous4—Used in the in- NOTE 4—Typical leak checks should be 0.0 mm Hg to 1.5 mm Hg. The
strument to absorb water. Use the purity specified by the maximum allowable leak check should follow the manufacturer’s recom-
mendation.
instrument manufacturer.
8.5 Nickel Flux Cleaning Solution—An acid solution ca- 11. Nickel Flux Preparation
pable of removing surface contamination from the nickel flux. 11.1 Ultra high-purity nickel is commercially available that
A solution made by combining 75 mL of acetic acid, 25 mL of does not require the nickel cleaning procedure below. Its
HNO3, and 2 mL of HCl has been found suitable for this sufficiency must be verified by satisfactory blank determina-
purpose. tions. If ultra high-purity nickel is not used, the nickel must be
8.6 Copper Oxide or Rare Earth/Copper Oxide—Reagent cleaned to remove contamination (11.2).
used in some instruments to oxidize CO to CO2 for detection. 11.2 Immerse the flux in freshly prepared nickel flux clean-
Use the purity specified by the instrument manufacturer. ing solution for 50 s to 60 s, then rinse in running water for 2
8.7 Sodium Hydroxide on Clay5—Reagent used in some min to 3 min. Pour flux onto paper towels to remove excess
instruments to absorb CO2. Use a purity specified by the water. Place flux in sealable glass container, rinse with acetone
instrument manufacturer. and decant. To prevent new oxidation from forming, the flux
may be stored under fresh acetone until used. (See Note 5.)
8.8 Titanium Sample Pickle Solution—Three parts 30 %
hydrogen peroxide (H2O2) and 1 part 48 % HF. Other pickle NOTE 5—The fluxing agent must be of proper size to be introduced
solutions may be substituted if there are data supporting the through the sample drop mechanism and into the graphite crucible.
effectiveness of the solution on removing contaminants. For
12. Sample Preparation
example, substituting concentrated HNO3 for 30 % H2O2 has
been found effective (see Note 3). (Warning—HF causes 12.1 Remove the surface of the sample either mechanically
serious burns that may not be immediately painful; refer to the (12.2) or chemically (12.3). Start with a sample of sufficient
paragraph about HF in the Hazards Section of Practices E50.) size that the final sample after surface removal will be between
0.100 g and 0.150 g.
12.2 To mechanically remove the sample surface, abrade
4
Known commercially as Anhydrone. with a clean file or similar abrasive device to remove contami-
5
Known commercially as Ascarite II. nation. Other methods, such as shearing, saw cutting, or

2
 E1409 − 13
turning down on a lathe, may be employed for reducing sample 13.4 Determination of Blank—Proceed as directed in 14.2
size and removing the surface of the sample. Regardless of the and 14.3 with a graphite crucible containing graphite powder
method used, the sample must not be allowed to overheat, as (Note 1 and Note 6) and analyze the nickel flux without a
this will adversely affect the results of the analysis. Indications sample. Determine the average blank of three to five individual
that the sample has overheated while being worked may runs and enter this value into the appropriate mechanism of the
include discoloration of the metal or the sample becoming too analyzer. If each individual result is within 5 µg of the average,
hot to handle without tools. Rinse the sample in acetone and air the blank is acceptable. Alternatively, a maximum value may
dry. Weight to 60.001 g. Proceed to 12.4. be used. Values of 0.0005 % for oxygen and 0.00007 % for
12.3 To chemically remove surface contamination, follow nitrogen have been found adequate. Higher limits may be
12.3.1 and 12.3.2. appropriate, particularly for reporting results that are not near
12.3.1 Leach the test sample in the titanium sample pickle the lower end of the scope. If other values are used, data
solution. (Warning—See 8.8.) (see Note 3) until the surface is showing that they are acceptable must be on file. Problems
clean. This will normally require approximately 5 s from the with inconsistent or high blank values must be corrected before
time of the initial vigorous reaction between the sample and the the analysis can be continued. If the unit does not have
solution. provision for automatic blank compensation, then the blank
12.3.2 Immediately remove the reacting test sample and value must be manually subtracted from the total result prior to
rinse it twice with water and once with acetone and allow to air any other calculation. Refer to the manufacturer’s instructions
dry. Weigh to 60.001 g. for proper blanking procedures (Note 6).
12.4 All subsequent operations on the test sample and flux 13.5 Calibration—Follow the calibration procedure recom-
must be done without introducing contamination to either. Use mended by the manufacturer using titanium reference materi-
only clean tweezers or crucible tongs and never let the test als.
sample or flux contact the analyst’s skin. In the event this does 13.5.1 For each non-zero calibration point, weigh a titanium
happen, rinse the sample and nickel with acetone and air dry reference material to the nearest milligram, place it with nickel
before analysis. flux into an outgassed graphite crucible containing graphite
13. Calibration powder if appropriate (Note 6).
13.5.2 Proceed as directed in 14.3 and 14.4.
13.1 Reference Materials—Select only titanium or titanium
alloy reference materials such that the high point on the 13.5.3 Repeat 13.5.1 and 13.5.2. Analyze three to five
calibration curves will represent an amount of oxygen and specimens of each titanium reference material. For each
nitrogen that is approximately equal to or greater than the reference material used to calibrate, calculate the average of
amount expected in the samples. The accuracy of the test these results, and compare the average to the certified value for
method is dependent upon the accuracy of the methods used to the reference material. Adjust the instrument output to match
certify the oxygen and nitrogen values of the reference the certified value unless the average already agrees with the
materials, as well as upon their homogeneity. Thus, wherever certified value within the range of the uncertainty given on the
possible, reference materials used to confirm instrument cali- certificate. (Note 7.)
bration should be traceable to certified reference materials from NOTE 7—Some instruments have expanded computer capabilities that
a national or international metrological institute. allow multi-point calibration which may improve the accuracy of the
calibration over the single point calibration as tested in the current
13.2 Gas Dosing—Automatic and manual gas dosing, rec-
interlaboratory study (ILS). Either calibration type may be used.
ommended by some manufacturers, can be used to calibrate the
instrument, but instrument response must be verified by cali- 13.5.4 Confirm the calibration by analyzing another speci-
bration with titanium reference materials because of the fusion men of the reference material after the calibration procedure is
characteristics of the furnace/sample combination. complete. The result should agree with the certified value
within a suitable confidence interval (Note 8). If the result
13.3 Initial Adjustment of Measurement System (that is,
“warm-up”)—Place a titanium material (not necessarily a agrees with the certified value within the uncertainty provided
titanium reference material) with nickel flux into an outgassed on the certificate of analysis, the calibration is acceptable.
graphite crucible containing graphite powder (optional, see Alternatively, if the certified value falls within an interval
Note 6). Proceed as directed in 14.3 and 14.4. Repeat in calculated as described in Eq 1, the calibration is acceptable.
duplicate. (Outgassing is accomplished automatically either as NOTE 8—The procedure outlined in the original version of 13.5.4
part of the continuous analysis cycle used with the automatic required the test result to “fall within the maximum allowable limit of the
sample drop, or as the first step in a two-stage cycle associated standard” typically interpreted as the range defined by the certified value
with the manual addition of the sample to the crucible.) 6 its associated uncertainty. The original version was utilized in the
generation of the data in this method’s Precision and Bias statements
NOTE 6—The use of graphite powder is optional. In some instruments (Section 16). The current method for confirming the standardization is
the addition of graphite powder (0.01 g to 1.0 g depending on crucible size statistically rigorous and should be used in general practice. As an option,
and style) is designed to optimize furnace performance and facilitate the the laboratory may obtain an estimate of s from a control chart maintained
release of nitrogen from the test sample. Refer to the instrument as part of their quality control program. If the control chart contains a large
manufacturer’s instructions for recommended graphite powder additions number of measurements, t may be set equal to 2 % at the 95 %
(Note 1). If graphite powder is used, it must be employed consistently for confidence interval. At its discretion, the laboratory may choose to set a
blanks, samples, and reference materials. smaller range for the acceptable test result.

3
 E1409 − 13
TABLE 1 Statistical Information—Oxygen in Titanium
ILT
Published Minimum SD Reproducibility SD Reproducibility
Certified Analyzed Diff.
Test Material ID Uncertainty (Sm, Practice (SR, Practice Index (R, Prac- Rrel %
(Wt. %) Mean (%)
(Wt. %) E1601) E1601) tice E1601)
(Wt. %)
GBW–02603A 0.119 0.115 0.004 0.005 0.0027 0.0043 0.012 10.4
GBW–02604A 0.273 0.274 -0.001 0.008 0.0038 0.0054 0.015 5.5
BCR No. 24B 0.0608 0.0632 -0.002 0.0023 0.0026 0.0047 0.013 20.8
BCR No. 59B 0.175 0.179 -0.004 0.007 0.0073 0.0074 0.021 11.6
LECO 501–653C 0.044 0.044 0 0.004 0.0028 0.0032 0.009 20.4
Lot 290–103
TIMET 0.239 0.238 0.001 0.009 0.0044 0.0083 0.023 9.8
Material BD
LECO 501–664C 0.154 0.153 0.001 0.006 0.0037 0.0051 0.014 9.2
Lot 390–113–1
TIMET (0.0080) 0.0090 ... ... 0.00091 0.0017 0.0048 53.3
HTL 80E
CEZUS (0.35) 0.3309 ... ... 0.0029 0.0092 0.026 7.8
LHF
ATI Allvac C092G NA 0.503 ... ... 0.0112 0.0131 0.037 7.3
A
Certified Reference Material, People’s Republic of China.
B
Certified Reference Material, Community Bureau of Reference, Commission of the European Communities.
C
Calibration samples, Leco Corporation.
D
TIMET, Henderson Technical Laboratory (vacuum fusion technique).
E
TIMET, Henderson Technical Laboratory (Electrorefined Ti, Estimated by Mass Spectrometry), not certified.
F
CEZUS, Internal reference material, not certified.
G
ATI Allvac, Monroe, NC Laboratory (Ti-Nb alloy), not certified.

TABLE 2 Statistical Information-Nitrogen in Titanium

Reproducibility Reproducibility
ILT Published Minimum SD
Test Material Certified Diff. SD Index
Analyzed Mean Uncertainty (Sm, Practice Rrel %
ID (Wt. %) (%) (SR, Practice (R, Practice
(Wt. %) (Wt. %) E1601)
E1601) E1601)
LECO 501–653A 0.002 0.0031 –0.0011 0.001 0.0009 0.0012 0.0033 106
Lot 290–103
BCR No. 24B 0.0117 0.0101 0.0016 0.0013 0.0014 0.0019 0.0053 52.7
BCR No. 59B 0.0172 0.0167 0.0005 0.0027 0.0020 0.0025 0.0071 42.6
TIMETC 0.107 0.116 –0.009 0.006 0.0047 0.014 0.039 34.0
B–10377
TIMET (<0.0010) –0.00008 ... ... 0.00020 0.00062 0.0017 ...
HTL 80D
A
Calibration sample, Leco Corporation.
B
Certified Reference Material, Community Bureau of Reference, Commission of the European Communities.
C
TIMET, Henderson Technical Laboratory, Nitrogen content determined by Kjeldahl distillation-titration method.
D
TIMET, Henderson Technical Laboratory (Electrorefined Ti, Estimated by Mass Spectrometry), not certified.

S
p 5 t· 1 1
= D
1
n
·s (1)
(Note 10) titanium reference material for each analyte. Calcu-
late the average and standard deviation(s) of these results. In
the absence of bias among the reference materials, the average
where: result for this reference material should agree with the certified
p = one-half the prediction interval, value within a prediction interval defined by the repeatability
n = number of replicates used in 13.5.3, of the measurement system at the mid-range of the calibration
t = student’s I chosen for the 95 % confidence level for n (Note 11). This prediction interval may be calculated using Eq
replicate measurements (for example: t = 4.30 when n = 1 and the s and n values for the mid-range reference material.
3, 3.18 when n = 4, 2.78 when n = 5), and If the prediction interval does not encompass the certified
s = standard deviation of n replicates in 13.5.3 (Note 9). value, determine and correct the cause and repeat 13.5.1
NOTE 9—Here, s should be comparable to Sm, the repeatability standard through 13.5.5 (Note 12).
deviation, given in Table 1. If s » Sm, there is evidence that the
repeatability of the particular instrument is not acceptable for use with this NOTE 10—Commercially available reference materials are not always
test method. The user should determine and correct the cause, and repeat available at the compositions required to have a true mid-point check. The
13.5.1 through 13.5.3. mid-range material must have a value that is above the limit of detection,
13.5.5 Confirm calibration linearity by analyzing a mid- but below that of the high calibration point, preferably as close to the
range (Note 10) titanium reference material each for oxygen mid-point of the calibration curve as possible.
and nitrogen (a single reference material may be used if a NOTE 11—Typically, repeatability standard deviation is a function of
the mass fraction of the analyte. Compare the values labeled ILT Analyzed
suitable reference material is available for both analytes), using Mean in Tables 1 and 2 with the values for Minimum SD (Sm) to see a
the limits stated on the certified value as an acceptance range. typical trend for laboratories using this test method. If your results are not
Alternatively, analyze at least three specimens of a mid-range comparable, investigate and correct the cause.

4
 E1409 − 13
NOTE 12—The presence of bias between the reference material used in 16. Precision and Bias7
13.5.1 and the reference material used in 13.5.5 may cause the calibration
to appear to be non-linear. This cannot be corrected by making adjust- 16.1 Precision—Oxygen:
ments to the instrument. 16.1.1 Eleven laboratories cooperated in testing Samples 1
through 7. The data obtained are presented in Table 1. The
14. Procedure testing was performed in accordance with the provisions of
14.1 Start with an instrument that has been prepared and Practice E173. The results of the testing are recalculated in
calibrated as directed in Sections 10 and 13. accordance with Practice E1601, Plan A.
14.2 Transfer a 0.100 g to 0.150 g titanium test sample with 16.1.2 In August 2004, eight laboratories tested Samples 8
nickel flux to the sample drop port. The weight of nickel should and 9 that were outside the oxygen content range of the original
exceed the weight of sample by at least a factor of 7(Note 13.) testing. The testing was performed in accordance with Practice
The weight tolerance of the titanium test sample must be 61 E1601, Plan A and the results calculated accordingly. The
mg. resultant data are presented in Table 1. The scope of Practice
E1601 reflects this additional testing. The lower scope is
NOTE 13—Research has demonstrated that the effective ratio of flux to calculated as (2)(R) of the lowest analyzed material plus
titanium is 7:1 to 17:1.6 Nickel baskets are commonly manufactured in 1.0
consideration of the 0.008 % material included in the August
g and 1.5 g sizes with the 1.0 g size in common usage among the titanium
producers and users and the weight utilized in this method’s ILS. 2004 ILS.
16.1.3 In October 2007, six laboratories tested one addi-
14.3 Place the crucible containing graphite powder (Note 6)
tional sample for the element oxygen only. The testing was
on the furnace pedestal, raise the mechanism, and start the
performed in accordance with E1601, Plan A and the results
analysis cycle. Refer to the instrument manufacturer’s instruc-
calculated accordingly. The resultant data have been appended
tions for the specific instrument model regarding operation,
to Table 1. As a result of this testing, the scope of this test
entry of sample weight, and blank value.
method has been modified to reflect the new oxygen scope
14.4 One or more continuing calibration verifications must maximum of 0.5 %. Supporting data have been filed at ASTM
be performed prior to and upon completion of a period of Headquarters in Research Report RR:E01-1109.8
continuous operation, and throughout this period with a pre-
16.2 Precision—Nitrogen:
determined minimum frequency to be established by each
16.2.1 Twelve laboratories cooperated in testing Samples 1
individual test facility. The acceptance range for the verifica-
through 4. The data obtained are presented in Table 2. The
tion material may be the limits stated on the certified value for
testing was performed in accordance to the provisions of
the reference material, or may be calculated using Eq 1 and the
Practice E173. The results of the testing are recalculated in
s and n values for multiple analyses of the verification material.
accordance with Practice E1601, Plan A.
If a continuing calibration verification indicates an out of
16.2.2 In August 2004, eight laboratories tested Sample 5
calibration condition, stop analysis. Results must be supported
that was outside the nitrogen content range of the original
by acceptable preceding and subsequent verifications to be
testing. The testing was performed in accordance with Practice
reported.
E1601, Plan A, and the results calculated accordingly. The
14.5 It is the responsibility of the user to document the resultant data are presented in Table 2. The scope of Practice
frequency of blank determination (13.4), routine calibration E1601 reflects this additional testing. The lower scope is
and confirmation (13.5.1 – 13.5.4) and linearity confirmation calculated as (2)(R) of the lowest analyzed material plus the
(13.5.5), and the conditions under which blank determination consideration that a 0.002 % material was included in the
or recalibration, or both, beyond this frequency is required original ILS and a <0.001 % material included in the August
(examples may include changing reagents, beginning use of a 2004 ILS.
new batch of crucibles, changing gas cylinders, or a personnel
16.3 Bias—The accuracy of this test method may be judged
shift change).
by comparing the results obtained from certified reference
15. Calculation materials with their certified values.
15.1 Refer to the manufacturer’s instructions to ensure that 17. Keywords
all essential variables in the analysis have been addressed.
17.1 inert gas fusion; nitrogen; oxygen; titanium; titanium
Because most modern commercially available instruments
alloys
calculate mass fraction directly, including corrections for blank
and sample mass, manual calculations by the analyst are
generally not required. 7
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:E01-1002 for oxygen and Research
Report RR:E01-1024 for nitrogen.
6 8
Method of Analyzing Oxygen or Nitrogen Contained in Titanium Group Metal Supporting data have been filed at ASTM International Headquarters and may
or Alloy Thereof, Okamura, et al., U.S. Patent Number 4,673,655, June 16, 1987. be obtained by requesting Research Report RR:E01-1109.

5
 E1409 − 13

APPENDIXES

(Nonmandatory Information)

X1. PREPARATION ANOVA OXYGEN

X1.1 See Table X1.1.

TABLE X1.1 Preparation ANOVA Oxygen

Lab Code
Treatment
Random A B C D E F
Code
Run Order
bA 2 0.08265 0.0822 0.08178 0.08371 0.08065 0.08413
bA 11 0.08317 0.08177 0.08045 0.08422 0.08320 0.08591
bA 20 0.08162 0.08936 0.08257 0.07965 0.08374 0.08455

eA 6 0.08055 0.08445 0.08096 0.08377 0.08292 0.08476

eA 13 0.08322 0.08559 0.08079 0.08457 0.08266 0.08498
eA 21 0.08103 0.08107 0.08004 0.07952 0.08258 0.08542

fA 1 0.08372 0.08219 0.08036 0.08226 0.08540 0.08507

fA 10 0.08372 0.08265 0.08147 0.08355 0.08388 0.08501
fA 17 0.08140 0.08686 0.08098 0.08340 0.08244 0.08362

aB 4 0.08109 0.08366 0.08200 0.08749 0.08360 0.08375

aB 7 0.08173 0.08202 0.08035 0.08428 0.08444 0.08378
aB 14 0.08033 0.08568 0.07878 0.08327 0.08300 0.08460

cB 12 0.08543 0.08221 0.07999 0.08271 0.08475 0.08899

cB 15 0.08023 0.09032 0.08237 0.08468 0.08240 0.08550
cB 19 0.08139 0.08889 0.08384 0.08243 0.08316 0.08575

dC 3 0.08224 0.08265 0.08275 0.08507 0.08448 0.08683

dC 8 0.08413 0.08271 0.08181 0.08509 0.08411 0.08488
dC 18 0.08215 0.08624 0.08233 0.08471 0.08544 0.08407

gC 5 0.08281 0.08621 0.08398 0.08696 0.08487 0.08499

gC 9 0.08437 0.08292 0.08370 0.08622 0.08397 0.08396
gC 13 0.08279 0.08962 0.08114 0.08333 0.08344 0.08682

ANOVA Calculation:
Source of Variance df SS MS F Significance at % of Total Variance
95 % C.L.
Between Lab 5 0.01962 0.00393 12.2 Y 33.4
Between Preps 12 0.00549 0.00046 1.48 N 4.5
Error 108 0.03298 0.00031 ... ... 62.1
Total 125 0.05809 ... ... ... ...
A
Laboratory B, E, F treatments b, e, f respectively: HF-H2O2.
B
Laboratory A, C treatments a, c respectively: HF-HNO3.
C
Laboratory D, G treatments d, g respectively: Abrade.

6
 E1409 − 13

X2. PREPARATION ANOVA NITROGEN

X2.1 See Table X2.1.

TABLE X2.1 Preparation ANOVA Nitrogen

Lab Code
Treatment
Random A B C D E F
Code
Run Order
A
b 2 0.00426 0.00526 0.00423 0.00520 0.00361 0.00335
bA 11 0.00454 0.00388 0.00469 0.00547 0.00362 0.00460
bA 20 0.00325 0.00470 0.00566 0.00466 0.00529 0.00414

eA 6 0.00399 0.00520 0.00409 0.00499 0.00555 0.00328

eA 13 0.00373 0.00461 0.00471 0.00531 0.00522 0.00404
eA 21 0.00332 0.00470 0.00423 0.00490 0.00493 0.00446

fA 1 0.00375 0.00542 0.00450 0.00491 0.00636 0.00426

fA 10 0.00367 0.00543 0.00453 0.00500 0.00552 0.00398
fA 17 0.00417 0.00444 0.00472 0.00425 0.00456 0.00489

aB 4 0.00399 0.00525 0.00432 0.00496 0.00510 0.00312

aB 7 0.00410 0.00476 0.00472 0.00497 0.00503 0.00404
aB 14 0.00352 0.00430 0.00486 0.00474 0.00517 0.00445

cB 12 0.00338 0.00505 0.00486 0.00498 0.00518 0.00414

cB 15 0.00366 0.00516 0.00542 0.00495 0.00416 0.00357
cB 19 0.00398 0.00523 0.00491 0.00557 0.00431 0.00479

dC 3 0.00457 0.00496 0.00537 0.00504 0.00436 0.00420

dC 8 0.00359 0.00541 0.00457 0.00512 0.00497 0.00416
dC 18 0.00345 0.00441 0.00478 0.00485 0.00564 0.00433

gC 5 0.00384 0.00465 0.00489 0.00612 0.00524 0.00387

gC 9 0.00446 0.00532 0.00449 0.00545 0.00551 0.00467
gC 16 0.00425 0.00531 0.00531 0.00529 0.00420 0.00468

ANOVA Calculation:
Source of Variance df SS MS F Significance at % of Total Variance
95 % C.L.
Between Lab 5 0.02514 0.00503 21.8 Y 49.1
Between Preps 12 0.00156 0.00013 0.54 N 0.0
Error 108 0.02612 0.00024 ... ... 50.9
Total 125 0.05281 ... ... ... ...
A
Laboratory B, E, F treatments b, e, f respectively: HF-H2O2.
B
Laboratory A, C treatments a, c respectively: HF-HNO3.
C
Laboratory D, G treatments d, g respectively: Abrade.

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