R. W.

H i n t o n I

Interlaboratory Evaluation of ASTM Practice for X-Ray Determination of Retained Austenite in Steel with Near-Random Crystallographic Orientation (E 975)

REFERENCE: Hinton, R. W., "Intedaboratory Evaluation of ASTM Practice for X-Ray Determination o1 Retained Austenlte in Steel with Near-Random Crystallographic Orientation (E 975)," Journal of Testing and Evaluation, JTEVA, Vol. 15, No. 2, March 1987, pp. 95-100. ABSTRACT: A standard practice (ASTM E 975) was developed by Task Group E04.0602 for the X-ray diffraction determination of retained austenite in steel. Results of interlaboratory studies of retained austenite samples performed before and after the practice was developed are described. The final interlaboratory study using ASTM E 975 and ASTM E 173 as a guide to the study resulted in an estimate of repeatability within the same laboratory of 37o retained austenite for a 95% confidence limit, and an estimate of reproducibility between laboratories of 4% retained austenite for a 95% confidence limit. KEY WORDS: retained austenite, X-ray diffraction method, interlaboratory study, ASTM E 975, NBS retained austenite standards

In 1948, Harris [1] and Averbach and Cohen [2] published X-ray diffraction integrated intensity ratio procedures for determining the relative amount of retained austenite in steel. Since that time a variety of X-ray diffraction integrated intensity ratio methods have been used to determine retained austenite in steel; some of these methods are described in Refs 3 to 10. National Bureau of Standards personnel have produced mechanical mixtures of austenitic (Type 310) stainless steel and ferritic (Type 430) stainless steel to provide standards for retained austenite. However, these mechanical alloy mixtures produce different X-ray diffraction intensities and peak shapes than either medium carbon-alloy steels or tool steels in the heat-treated condition. Although austenite is visible in the polished and etched microstructure of highly alloyed stainless steels such as austenitic (Type 300 series) stainless steel, retained austenite is not usually visible in the microstructure of heat-treated medium carbon-alloy steels and tool steels where it may have detrimental effects on the performance of those steels. To develop a relatively simple practice for the determination of retained austenite using X-ray diffraction methods, ASTM Task Group E04.0602 of Subcommittee E04.06 on X-ray Methods agreed to use scattering factors for iron without attempting to adjust for the scattering factors of alloy additions. A near-random crystallographic condition was agreed upon by the Task Group Manuscript received 4/23/86; accepted for publication 9/10/86. 1Owner, R. W. Hinton Associates, Center Valley, Box 413, PA 18034. 1987 by the American Society for Testing and Materials 95

that was based upon a minimum-to-maximumratio of two different X-ray diffraction peaks for austenite (ratio 220 to 200) and ferrite (ratio 211 to 200). The method would apply to steels that met this near-random condition, and all these steels would be analyzed using the scattering factors for elemental iron. An initial interlaboratory survey of existing X-ray diffraction procedures for the determination of retained austenite was made by heat treating a medium-carbon alloy steel and circulating those samples to ten laboratories. Many of the participants in that initial study became members of ASTM Task Group E04.0602. An X-ray diffraction procedure for the measurement of retained austenite was developed by those Task Group members, presented by Subcommittee E04.06 to Committee E-4, and received Society approval in 1984 as ASTM E 975. Two subsequent interlaboratory studies were completed using ASTM E 975 practices. The final study provided samples prepared from the same heat-treated bar of steel to each laboratory to evaluate ASTM E 975 including sample preparation.

Interlaboratory Study of a Variety of Historic Retained Austenite Practices

A description of retained austenite samples for the first interlaboratory study is presented in Table 1. Samples were heat treated and prepared by Laboratory 1 to provide three different aim levels of retained austenite. A near-random crystallographic orientation using chromium radiation and austenite X-ray diffraction peak ratios of 220 to 200 for the three standards were all within a ratio of 1.3 to 1.7, which was the Task Group's near-random requirement at that time. No near-random crystallographic requirement for ferrite peak ratios was used at that time. Organizations that participated in the first interlaboratory study are listed in Table 2. A detailed summary of the first interlaboratory study including the X-ray methods used by each participant is provided in Table 3. Participating laboratories are identified by a code number. Measurements of Samples 1-10 and 2-5 are plotted in Fig. 1 and in some cases show bias within the same laboratories; that is, high or low values of retained austenite were determined for both samples by the same laboratory, especially in the case of Laboratory 3 (low values) and Laboratory 7 (high values). The general conclusions concerning the interlaboratory measurements that can be drawn from these near-random samples containing retained austenite are: 0090-3973/87/0003-0095502.50

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TABLE l--Description of A S T M retained austenite interlaboratory samples. = Sample Code 2-10 Companion Code 2-11 Aim Level RockwellC of Retained Hardness Austenite 60 2.5%

Heat Treatment (1600F)austenitize, oil quench, refrigerate at --28C (--18F) temper at 177, 238, and 221C (350, 460, and 430F) 871C (1600F) austenitize, oil quench, refrigerate at --23C (--I0F), temper at 177 and 227C (350 and 440F) 871C(1600F) austenitize, oil quench, temper at 93C (200 F)

1-10

1-9

61

5%

2-5

2-4

65

15%

=Samples of hardened steel roll 2.3 cm (19 in.) square and 1.0 cm (014 in.) thick were prepared by P. M. Giles, Bethlehem Steel Corporation, Homer Research Laboratories, Bethlehem, PA. The samples were polished to 6 #m diamond, etched in nital (2%), repolished with Linde A, and etched in nital (2%). Sample composition: 0.82 C, 0.39 Mn, 0.25 Si, 0.21 Ni, 1.81 Cr, 0.09 V, and 0.24 Mo.

TABLE 2--Participating laboratories in the first interlaboratory study. Armco Steel Corporation Allegheny Ludlum Steel Corporation Bethlehem Steel Corporation Carpenter Technology Crucible Steel General Electric (2 locations) Union Carbide Corporation United States Steel Corporation Universal-Cyclops Specialty

I0

ot-

-7~ s ,,,g
.2

~z tLI a:

(I 8

There is reasonable agreement between laboratories, considering the wide variation in techniques. Development of a standard practice should improve interlaboratory agreement compared with these results. Results of the stability study by Laboratory 1 and effects of surface preparation on retained austenite measurements are listed in Table 4. The lower austenite content reported for the 2-10 austenire sample after some of the laboratories evaluated the same sample was caused by corrosion and corrosion products on its surface. Therefore, repolishing all samples by mechanical and chemical means after the interlaboratory study resulted in measurements of retained austenite similar to measurements by the preparer before the interlaboratory study. This shows that retained austenite was stable during the study except for the corroded surfaces of Sample 2-10. Results of Sample 2-10 were not used because of the effect of corrosion on the measurement of retained austenite during the interlaboratory study. Development of a Standard Practice for Retained Austenite Task Group objectives for the standard practice included: A relatively simple X-ray diffraction method that could be performed with a standard diffractometer using chromium or molybdenum radiation and integrated peak intensity (area under the X-ray diffraction peak above background).

IO

12 14 16 18 RETAINED AUSTENITE,percent SAMPLE 2 - 5

FIG. l--Plot of retahwd austenite measurements for 5 and 15% aim samples.

Calculated theoretical intensities (R values) should be based upon the scattering factors for pure iron with no adjustment for the effect of alloy content in the steel on X-ray diffraction intensities. The method should apply to carbon and alloy steels with nearrandom crystallographic orientation of both ferrite and austenite phases. Desired minimum sensitivity for the method was 1% austenite. X-ray diffraction peak interference from other crystalline phases such as carbides should be eliminated from the ferrite and austenite peak intensities. Preparation of the sample for analysis should be in accordance with ASTM E 3 practices. The standard practice for retained austenite that resulted from the Task Group, Subcommittee, and Committee efforts became ASTM E 975, a standard X-ray diffraction method for the determination of retained austenite in steel containing austenite and ferrite

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HINTON ON INTERLABORATORY EVALUATION OF ASTM E 975

97

TABLE 3--Results of round-robin retained austenite measurements. Retained Austenite, vol%, for Sample: Laboratory No. 1 Cr-K~ (Preparer) X-Ray Method a(200) vs. 7(200) and 7(220) with use of Bierwirth's table; % austenite vs. integrated intensity by counting a(200) and c~(211) vs. 3`(200) and 7(220); 90 sample rotation for average ct(200)and ct(211) vs. 3'(220) and 3`(311); sample tilting stage and integrated intensity by counting ct(ll0), (200), (211) vs. 7(111) (200), (220); integrated intensity by Plainimeter method c~(200)vs. 3"(220); Rigaku integrated intensity by counting tx(200)vs. 3'(200) and 3'(220); intensity by Plainimeter Unknown procedure Cr-Ko c~(200)vs. 3'(200) and 3'(220); film--densitometer trace intensity by Plainimeter Monochromator; tx(200), (211), (222) vs. 3'(200) (220), (311); intensity by counting a(200) vs. 3'(220); intensity by counting 1-10 6.0 2-10 3.2 2-5 13.5

Cr-K~

4.7

2.5

14.0

Mo-K,

4.8

2.0

12.3

Cr-K~

5.9

3.2

15.3

Cr-K~

5.5

2.2

14.5

6 7 8

Cr-K~

6.9 6.6 4.0

4.5 1.0 1.2

14.2 17.8 13.0

Cu-K~

6.0

1.0

16.0

10

Cr-K~ Average

4.6 5.7 1.0

2.1 2.3 1.1

11.7 14.2 1.8u

Standard Deviation, % "Standard deviation without the 17.8 value is 1.4%.

or martensite phases in the near-random crystallographic condition.

Interlaboratory Evaluation Using ASTM E 975

After ASTM E 975 was established, companion samples to those listed in Table l prepared by Laboratory 1 were sent to each participating laboratory. The same three samples were passed from laboratory to laboratory. Those laboratories participating in this second interlaboratory study are listed in Table 5. Laboratory code numbers were the same for those laboratories participating in both studies. Results of the second study are listed in Table 6 and plotted (X) in Fig. 2, which shows less bias in the measurement for most laboratories using A S T M E 975. Laboratories 3 and 7 show the most bias in retained austenite. One standard deviation of retained austenite for all laboratories using chromium radiation ranged from 0.8 to 1.25% for the three samples (Table 6). Only one laboratory used molybdenum radiation, and those values were relatively low compared with results of the laboratories using chromium radia-

tion. Results of the eighth laboratory were not used because of an electronic measurement instability that was identified by that laboratory after the measurements had been made. Laboratory 7 submitted the average of three of the five determinations listed in Table 7 for each sample. A single standard deviation from their results for one of the five samples is higher than the standard deviation for the second interlaboratory study, which is unexpected unless other individual laboratories were submitting averaged results. In contrast, the three individual results of Laboratory l listed in Table 8 have a relatively small standard deviation compared with the standard deviation of the interlaboratory study of ASTM E 975. Laboratory 5 reported two-peak and four-peak results (Table 9), with a substantial difference in the results for Sample 2-11. The four-peak method is preferred over the two-peak method because the use of additional peaks should help average the effect of preferred crystallographic orientation on the retained austenite determination. Although this study has shown relatively good agreement between laboratories, there are questions about repeatability within

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JOURNAL OF TESTING AND EVALUATION

TABLE 4--Preparer laboratory measurement of retained austenite before and after the first interlaboratory study was completed, a Retained Austenite, vol%, for Sample: Time Period Before Round-Robin (RR) After RR (as-received) After RR (repolished) Orientation EffecP Parallel Perpendicular After RR (HF chemical polishy 1-10 6.0 6.1 5.5 5.4 5.6 6.0 2-10 3.2 2.6 3.3 3.4 3.1 3.3 2-5 eZ 13.5 13.8 14.3 14.4 14.2 14.3

IO

E
7 x
6 o a O S ~ 4 ~

6 ;~ V ~ " ~ e 7 LABORATORY
~ - ~ l ~~ l

2N6
Jr'~ n W ~Z_4 UJ
2 t I I I I

el

L..-:~'4

NUMBER"

e~.o3~o2

eS~

eB

I0

"See Table 3 for X-ray method used by Laboratory 1. bOrientation is defined as a direction from the coded side to the opposite side of the sample. This direction is either parallel or perpendicular to the goniometer axis. CMetallographic preparation to a final 600-grit SiC grind was done before chemically polishing 0.08 mm (0.003 in.) from the surface using 14 mL HF, 100 mL H202 and 100 mL H20. Because hydrofluoric acid (HF) is hazardous, it is not recommended for routine application.

12 14 16 18 RETAINED AUSTENITE, percent SAMPLE 2 - 5 2-4

Laboratories that are numbered |, 2, 3, O, and 6 are the same laboratories for both studies. Original sluoy without a standard practice.

x Currenl study using the ASTM E975 practice.

FIG. 2--Comparison of retained austenite measurements with and without A S T M E 975.

TABLE 5--Participating laboratories in the second interlaboratory study. Armco Steel Corporation Allegheny Ludlum Steel Corporation Bethlehem Steel Corporation Carpenter Technology Corporation Cummins Engine Corporation Ingersoll Rand Corporation United States Steel Corporation Universal-Cyclops Specialty

each laboratory. This study also does not address the variation in sample p r e p a r a t i o n from one laboratory to another, because all samples for this second study were p r e p a r e d by Laboratory 1. Final lnterlaboratory Evaluation Using A S T M E 975 To determine the repeatability a n d reproducibility for retained austenite m e a s u r e m e n t s by different laboratories using A S T M E 975, different sections of a heat-treated b a r of steel were sent to eight laboratories for sample p r e p a r a t i o n a n d m e a s u r e m e n t . Five of the original eight laboratories participated in this t h i r d a n d final i n t e r l a b o r a t o r y study. T h e results of this final i n t e r l a b o r a t o r y

TABLE 6--Results of the second interlaboratory study." Two- or Four-Peak Method? 4 4 4 4 4 4 Average 3 Mo Standard Deviation, % 4 Average Retained Austenite, rot%, for Sample: 1-9 6.5 6.8 5.6 5.9 7.8 6.1 6.4 0.8 4.7 2-4 15.8 17.7 15.1 14.6 17.4 15.3 15.9 1.3 11.5 2-11 4.5 3.6 3.4 3.4 6.0 6.1 4.6 1.2 2.9

Laboratory NumbeP 2 4 5 1 7 6

Radiation Used Cr Cr Cr Cr Cr Cr

"ASTM E 975 was used to measure austenite in samples prepared by Laboratory 1. hLaboratory results are listed in chronological study order of retained austenite measurement. Laboratories 1, 2, 3, 4, and 6 have the same code numbers as in the first interlaboratory study.

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HINTON ON INTERLABORATORY EVALUATION OF ASTM E 975 TABLE 7--Variation of retained austenite measurement (ASTM E 975) within Laboratory 7 during the second interlaboratory study. Retained Austenite, vol%, in Sample: Measurement Sequence 1 2 3 4 S Average Standard Deviation, % 1-9 8.59 6.26 8.88 7.73 7.58 7.97 1.04 2-4 20.29 16.53 15.78 16.35 17.94 16.94 2.07 2-11 6.4 7.33 5.62 5.35 5.23 5.23 0.91

99

TABLE lO--Results of final A S T M interlaboratory study of retained austenite (volume percent) in steel, a Laboratory First 6.9 7.4 8.0 8.8 10.5 Second 7.3 8.4 7.9 7.0 9.4 Third 8.1 7.2 7.4 8.3 11.5 Average 7.4 7.7 7.8 8.0 10.5

1 2 5 7 8b

"A bar of steel was heat treated to produce retained austenite. Samples from this bar were submitted to each laboratory to cut, prepare, and measure retained austenite three times in accordance with ASTM E 975 and to submit those three results to Task Group E04.0602. hSince Laboratory 8 had an instrument stability problem, these results were not included in the analysis.

"The four-peak method of ASTM E 975 was used.

TABLE 8--Variation of retained austenite measurement (ASTM E 975) within Laboratory I during the second interlaboratory study. Retained Austenite, vol%, in Sample: Measurement SequencC 1-9 5.6 6.2 5.8 5.9 0.2 2-4 15.1 13.9 14.7 14.6 0.6 2-11 3.4 3.4 3.9 3.4 0.1

1 2 3 Average
Standard Deviation, %

From one laboratory to a n o t h e r the estimate of reproducibility is 4 % retained austenite for a 9 5 % confidence limit. These values represent the range of values within a confidence limit, b u t they are obviously not valid n e a r the detection limit of a b o u t 2 % for this method. A S T M R e c o m m e n d e d Practice for Use of the T e r m s Precision a n d Accuracy as Applied to M e a s u r e m e n t of a Property of a Material (E 177) was not used, because a n i n d e p e n d e n t m e t h o d to determine the exact value of retained austenite in each sample was not available.

"The four-peak method of ASTM E 975 was used.

Differences Between NBS Retained Austenite and ASTM E 975 Values

National Bureau of S t a n d a r d s personnel have m a n u f a c t u r e d retained austenite s t a n d a r d s by mixing powders of AISI Type 310 (austenitic) stainless steel a n d AISI Type 430 (ferritic) stainless steel. Since b o t h of these stainless steels are highly alloyed, X-ray intensities are changed by the alloy content c o m p a r e d with the theoretical X-ray intensities or " R - v a l u e s " for iron t h a t were used in A S T M E 975. Also the X-ray diffraction peak shape of these relatively strain-free NBS s t a n d a r d s are different t h a n those X-ray diffraction peak shapes of m e d i u m carbon-alloy steels in the heattreated condition. For comparison, some NBS retained austenite s t a n d a r d s were evaluated using A S T M E 975; the results are listed in Table 11. Although some of the A S T M E 975 m e a s u r e m e n t s are relatively close to the actual NBS retained austenite content, there is a large relative difference between the m e a s u r e d a n d actual retained austenite values in at least four of the seven measurements. T h e results listed in T a b l e 11 emphasize the h a z a r d of applying A S T M E 975 to highly alloyed steels. In general, the m e a s u r e m e n t of retained austenite in steels with a total (cumulative) alloy content of over 15% using A S T M E 975 is not r e c o m m e n d e d .

TABLE 9--Comparison of two- and four-peak A S T M E 975 practice by Laboratory 5 durhzg the second interlaboratory study. Retained Austenite, vol% ASTM Sample No. 2-11 1-9 2-4 Two-Peak Method 2.6 5.2 14.6 Four-Peak Method 3.4 5.6 15.1 Relative Difference, % 23 8 3

study are listed in T a b l e 10. Each laboratory was asked to repeat the m e a s u r e m e n t three times to establish a measure of repeatability within t h a t laboratory. Results listed in T a b l e 10 were analyzed in accordance with A S T M R e c o m m e n d e d Practices for Conducting Interlaboratory Studies of M e t h o d s for Chemical Analysis of Metals (E 173). Alt h o u g h the m e a s u r e m e n t of retained austenite is not a chemical analysis, the same principles apply. However, the exact a m o u n t of retained austenite in these samples could not be determined by an i n d e p e n d e n t m e t h o d to consider the accuracy of the method.

Summary
Historically, a variety of X-ray diffraction (integrated intensity ratio) methods have been used to determine retained austenite in m e d i u m carbon-alloy steel a n d tool steels. A survey of these methods via an interlaboratory study showed a single s t a n d a r d deviation between laboratories to b e 1.8% retained austenite for a steel sample containing 14.2% retained austenite.

Statement of Precision and Bias

From A S T M E t 73, the estimate of repeatability within the same laboratory is 3 % retained austenite for a 95% confidence limit.

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TABLE l l--Actual and measured retained austenite contents within NBS solid mixtures of stainless steel. Measured Actual Retained NBS Retained Austenite Actual Austenite, (ASTM E 975), Difference, vol %" vol %b vol % 32.84 14.41 15.05 5.66 4.55 2.20 2.63 35.5 14.3 12.5 4.1 3.6 2.1 2.0 +2.66 --0.11 --2.55 -- 1.56 --0.95 --0.10 --0.63

Acknowledgments

NBS No.

Relative Difference, % 8.1 0.8 16.9 27.6 20.9 4.5 24.0

110 388 280 93 80 C 38 C 232

uThese standards consist of mechanical mixtures of AISI Type 310 and Type 430 stainless steel. Retained austenite contents are based upon light microscope measurements and analytical evaluation of the nickel content representing Type 310 stainless steel. bDetermination made by Laboratory 1. ASTM E 975 values are not accurate because of the alloy effect on the X-ray intensities used to make these determinations. No compensation for alloy effect has been included in ASTM E 975.

In addition to the participants in the interlaboratory study and the members of Task Group E04.0602, a number of individuals have devoted considerable effort to the interlaboratory studies and the development of ASTM E 975. Mr. Peter Morris of Armco was especially helpful in its development and evaluation. Messrs. Marion Longenbach, Albert Brandemart, and Philip Giles of Bethlehem Steel Corporation provided sample preparation and numerous X-ray diffraction measurements during the development and evaluation of this practice. Mr. John Larson of Ingersoll Rand provided liaison between SAE and ASTM representatives and constructive criticism during this study. Mr. Leo Zwell, chairman of A S T M Subcommittee E04.06 on X-ray Methods, initiated the interlaboratory studies and the development of a standard practice for retained austenite in steel. Solid NBS mixtures of stainless steel were provided for the study by Mr. George Hicho of the National Bureau of Standards.
References

A standard practice (ASTM E 975) was developed by the X-ray diffraction determination of retained austenite in steel by A S T M Task Group E04.0602 of Subcommittee E04.06 on X-ray Methods. An interlaboratory study of this practice using ASTM E 173 as a guide resulted in an estimate of repeatability within the same laboratory of 3 % retained austenite for a 95 % confidence limit, and an estimate of reproducibility between laboratories of 470 retained austenite for a 95% confidence limit. Differences were observed between National Bureau of Standards (NBS) standards consisting of known stainless steel mixtures to produce retained austenite standards and the values for retained austenite in those NBS standard samples using the A S T M E 975 retained austenite method. In addition to the normal measurement error, differences were observed for the standards because of the effects of alloy and crystal lattice strains on the X-ray diffraction peaks of NBS standards compared with carbon-alloy steels.

[1] Harris, W. J., Jr., "Comparison of Metallographic and X-Ray Retained Austenite Measurements," Nature, Vol. 161, Feb. 1948. [2] Averbach, B. L. and Cohen, M., "X-Ray Determination of Retained Austenite by Integrated Intensities," Transactions of AIME, Vol. 176, 1948, pp. 401-415. [3] Beu, K. E., "Modification of an X-Ray Method for Measuring Retained Austenite in Hardened Steel," Transactions of AIME. Vol. 194, 1952, pp. 1327-1328. [4] Ogilvie, R. E., "Retained Austenite by X-Rays," Norelco Reporter, May 1959. 15] Erard, H. R., "Technique for Measuring Low Percentages of Retained Austenite Using Filtered X-Ray Radiation and an X-Ray Diffractometer," in Advances in X-Ray Analysis, Vol. 7, Plenum Press, New York, 1963. [6] Miller, R. C., "A Rapid X-Ray Method for the Determination of Retained Austenite," Transactions ofASM. Vol. 57, 1964. [7] Lundgren, R., "On the Accuracy of X-Ray Retained Austenite Measurements," Metals Progress, April 1965. [8] Morris, P. R., "Measurement of Retained Austenite in PrecipitationHardening Stainless Steels," Transactions ofAIME, Vol. 239, 1967, pp. 1506-1590. [9] Leonard, L., Luszcz, S. J., and Meakin, J. D., "Non-Dispersive X-Ray Techniques in Retained Austenite Determinations," American Society for Metals, Metals Park, OH, 1973. [101 Jatczak, C. F., Larson, J. A., and Shin, S. W., RetainedAustenite and Its Measurements by X-Ray Diffraction, Special Publication SP453, Society of Automotive Engineers, Jan. 1980.

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