NAT'L INST. OF STAND & TECH

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PUBLICATIONS

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NIST SPECIAL PUBLICATION 260-141

U.S. DEPARTMENT OF COMMERCE/Technology Administration

National Institute of Standards and Technology

Standard Reference Materials:

Secondary Ferrite Number

Reference Materials

Gage Calibration and Assignment of Values

QC

100

.U57

NO.260-141

2000

Counterweight

White Dial

Balance

Magnet

Steel Mass

C. N. McCowan, T. A. Siewert,

D. P. Vigliotti, and C. M. Wang
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NIST Special Publication 260-141

Standard Reference Materials:

Secondary Ferrite Number

Reference Materials

Gage Calibration and Assignment of Values

C. N. McCowan, T. A. Siewert,

D. P. Vigliotti, and C. M. Wang

Materials Reliability Division

Materials Science and Engineering Laboratory

National Institute of Standards and Technology

325 Broadway

Boulder, Colorado 80303-3328

U.S. DEPARTMENT OF COMMERCE, William M. Daley, Secretary

TECHNOLOGY ADMINISTRATION, Dr. Cheryl L. Shavers, Under Secretary of Commerce for Technology

NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY, Raymond G. Kammer, Director

Issued February 2000
National Institute of Standards and Technology Special Publication 260-141

Natl. Inst. Stand. Technol. Spec. Publ. 260-141, 87 pages (Feb. 2000)

CODEN: NSPUE2

U.S. GOVERNMENT PRINTING OFFICE

WASHINGTON: 2000

For sale by the Superintendent of Documents, U.S. Government Printing Office, Washington, DC 20402-9325
Contents

1. Introduction 2

2. Secondary Specimens 2

3. Gage Calibration 3 3.1 Frequency 3 3.2 Determination of Tearing Force 4

3.3 Primary FN Calibration 5

3 .4 Calibration Errors and Variables 12

3.5 Force Calibration 16

3.6 Summary of Primary Calibrations 18

4. Measurement of Secondary Reference Materials 21

4.1 Measurement Procedure 21

4.2 Data Analysis 21

4.3 Data Trends 22

5. Certification of Secondary Reference Materials and Discussion of Errors 27

5.1 Uncertainty Analysis 27

6. Microstructure 30

6. 1 Grain Size 35

6.2 Ferrite Content 35

6.3 X-ray Evaluation 36

6.4 Solidification Flaws 37

6.5 Atomic Force Microscopy 38

7. Information on the Reference Material 39

8. Plans 39

9. References 39

Appendix A. Primary Calibration Data 40

Appendix B. Summary Data for the Secondary Reference Materials 43

Appendix C. Raw Data for the Secondary Reference Materials 51

Appendix D. Round-Robin Data for Primary FN Standards 79

iii

Secondary Ferrite Number Reference Materials:

Gage Calibration and Assignment of Values

C.N. McCowan, T.A. Siewert, D.P. Vigliotti, and CM. Wang

Materials Reliability Division, Materials Science and Engineering Laboratory

National Institute of Standards and Technology

Boulder, CO 80303-3328

Ferrite Numbers (FN) were assigned to blocks of stainless steel that serve as secondary ferrite

reference materials (RM 8480 and 8481) and these specimens were placed in our Reference

Materials inventory.* These reference materials are used to calibrate several types of instruments

used to measure the FN, which is proportional to the ferrite content in stainless steel welds. The

ferrite content influences the physical and mechanical properties of stainless steel welds. This

report documents the procedures used to measure the reference materials and the results of our measurements. Appendices are included to document our primary gage calibrations (Appendix

A), the measurements made on the FN reference materials (Appendices B and C), and other

supporting measurements made for the study (Appendix D).

Our initial effort was devoted to finding and reducing sources of uncertainty in the gages

(instruments for measuring FN) and in the calibration procedures. After improving our gages and

procedures, we found that our calibration lines were nearly linear over the range of 0 to 100 FN

and that the gages compare well to gages used by The Welding Institute (TWI), which had

assigned the certified FN values to secondary specimens produced in the past.

The measurements on the reference materials showed that the standard deviations in FN for the

secondary specimens were typically less than 0.5 FN for the 0 to 30 FN range, and less than 3 FN

for the 30 to 100 FN range. The microstructure was found to be a finely dispersed and

homogeneous mixture of ferritic and austenitic phases, with a percent ferrite area fraction that

was nearly equivalent to the FN assigned to the reference materials (up to about 60 FN).

Key words: inspector gage, ferrite, feritscope, ferrite content, ferrite detector, ferrite number,

Magne-Gage, reference material, stainless steel.

*Trade names are included for clarity only; no endorsement or criticism is implied.

1
1. Introduction

Austenitic weld metals usually contain a small but controlled amount of ferrite to reduce the

tendency for cracking during solidification. Duplex ferritic-austenitic stainless steel welds contain

a balance of austenitic and ferritic phases to optimize their mechanical properties. Quantitative

measurement of the ferrite content is an important commercial issue, as ranges are commonly

specified in contracts and production standards. In the U.S., the amount of ferrite is usually

measured magnetically according to the American Welding Society AWS A4.2 standard,

Standard Proceduresfor Calibrating Magnetic Instruments to Measure the Delta Ferrite

Content ofAustenitic and Duplex Austenitic-Ferritic Stainless Steel WeldMetal [1].

The AWS A4.2 standard specifies procedures for both primary and secondary calibration of the

instruments. Primary calibration is based on reference materials of coating thickness, such as the

National Institute of Standards and Technology Standard Reference Materials (SRMs) 1361 to

1364, while secondary calibration is based on certified specimens of stainless steel. In section 3.2,

the standard describes the importance of secondary reference materials as: the only way of

calibrating instruments for which no primary calibration method exists, the most appropriate

standard for in-process checks, and being much more durable than the primary reference

materials.

At least three different companies or organizations have produced specimens, assigned values,

and sold sets of secondary reference materials during the past 30 years [2]. One of our goals

during development of our internal procedures was to assure ourselves that our calibration scale

was comparable to those used previously. Also, we worked closely with Commission II of the

International Institute of Welding and with the Welding Research Council's Subcommittee on

Welding of Stainless Steel, to assure that our procedures would maintain, if not raise, the

accuracy of the measurements.

2. Secondary Specimens

The specimens were produced in Russia from centrifugal castings of chromium-nickel-iron alloys.

The ferrite content (magnetic phase) is varied by adjusting the composition of the alloy. The cast specimens approximate the ferrite distribution in a weld deposit and have solidification structures

similar to those in welds. Like ferrite in welds, the magnetic response of the ferritic phase varies

with alloy composition (Cr, Ni, Mo).

The dimensions of the specimen are approximately 10 mm * 12 mm x 20 mm, as shown in Figure

1. The secondary specimens are sold in sets: (a) a lower-range set with eight specimens

distributed over the range of 0 to 30 FN, and (b) a higher-range set of eight specimens distributed over the range of 30 to 120 FN. The specimens are marked by engraving identification numbers on the 12 mm x 20 mm face opposite the measurement surface.

2
The ferrite content is measured in terms of an arbitrary quantity, the Ferrite Number (FN). The

FN of the specimen is determined using a gage that measures the force required to pull a magnet

of known strength off the surface of the specimen. We used a transfer-standard technique to

assign numbers to the new reference materials. We first calibrated gages (as described in the

following sections), then used them to assign FN values to the secondary reference specimens.

The FN is expected to be approximately equal to the percent ferrite in stainless steel welds up to

about 15, but at higher than 15 FN the true percent of ferrite in welds is overestimated by the FN

numbers. (These concepts are described in more detail in AWS A4.2.)

3. Gage Calibration

The gage used to assign FNs to the secondary specimens is shown schematically in Figure 2. It is essentially a balance, referred to as a Magne-Gage-type instrument in AWS A4.2. The white dial

winds a spring as it is turned and this applies a gradually increasing force to lift the magnet off the

surface of the specimen. Counterweights can be hung on one side of the balance to increase the

applied force. To calibrate this type of gage, a primary coating-thickness standard is used to

determine a relationship between FN (calculated for each coating thickness) and white-dial values

for the gage. We use the average FN of two gages to assign certified values to the reference

materials in our program. The calibration data are given in Appendix A.

3.1 Frequency

The calibration for a gage is valid for a maximum period of one year, as specified by AWS A4.2.

When making measurements to assign values to secondary reference materials, we checked the

gage calibration at the beginning of each day. The check was made by measuring three primary

3
White Dial

Specimen

Figure 2. Schematic diagram showing the general

features of the gage.

reference materials in the range of interest and comparing these results to those recorded for the same primary reference materials during the initial calibration. If this check indicated that a

recalibration of the gage (or maintenance) was needed, the full calibration procedure was

implemented.

3.2 Determination of Tearing Force

The magnet used for FN measurement is required by AWS A4.2 to have a tearing force of 510

±5 1 FN per newton (5 ±0.5 FN per gram-force). Using a magnet that is too weak will result in

falsely high FN values, and using a magnet that is too strong will result in falsely low FN values

(with respect to the standardized method).

Traditionally, the magnet's strength is measured on Magne-Gage-type instruments by suspending

a five-gram iron weight from the magnet. The dial reading at the time the weight is lifted just past

the balance point of the gage is divided by the weight to yield the tearing force. Using this

procedure, tearing forces of 490 and 541 FN per newton (4.8 and 5.3 FN per gram-force) were

determined for gages 1 and 2.

The magnet's strength can be determined directly from the slope of the calibration line if a torsion

balance is used, or a Magne-Gage-type instrument is used that has been calibrated in terms of

force. We calibrated our gages using a digital scale to determine the force associated with the

white-dial readings. To do this, a steel mass was positioned below the magnet, as shown in

Figure 3. As the white dial on the gage was turned to load the spring on the gage, the force on

the mass was recorded. The steel mass was sufficiently large that it would not be lifted off the

scale over the range of measurement. Once the white-dial was correlated to force (linear

regression), the force was substituted for the white-dial data and correlated to FN (see section

3.5). The slopes of the FN/Force regression lines for gages 1 and 2 were found to be 541 and 561

4
White Dial

Figure 3. Schematic of the set-up used for force

calibration measurements.

FN per newton (5.3 and 5.5 FN per gram-force), respectively. The procedures yield different

results, but all values are within the 510 ±51 FN per newton (5 ±0.5 FN per gram-force) required

by AWS A4.2.

3.3 Primary FN Calibration

Primary reference materials for coating-thickness were used to calibrate the gages. The FN of the

reference materials were calculated using an equation from AWS A4.2:

ln(FN) = 1.8059 - 1.1189»ln(7) - 0.1774-[ln(7)]2 - 0.0350«[ln(7)]3 - 0.0037- [ln(7)]

4

, (1)

where T is the thickness of the coating in millimeters.

The specific reference materials used to calibrate the gages are given in Table 1 . The coating

thicknesses are distributed through the range of 0.01 to 1.9 mm, which corresponds to a range of

0 to 130 FN (from eq (1)). To calibrate a gage, each reference material listed in Table 1 was

measured a minimum of five times and the lowest repeatable white-dial readings from these

measurements were taken as the calibration value. (The lowest value is taken, as recommended in AWS A4.2, to screen out values associated with premature detachments of the magnet.) Two

operators independently calibrated each gage, and the average of the two white-dial values serves

as the final calibration value for each standard. The calibration data for the gages used in this

study are given in Appendix I.

An example of a typical calibration plot is shown in Figure 4 for the gage 2 data. The 0 to 30 FN

data and two sets of extended FN data are plotted as separate lines (0, 7, and 14 g

5
counterweights). Typically, three or more

calibration lines would be needed to cover the range

of 0 to 100 FN. According to AWS PA. 2, two lines can be fitted to the data in the 0 to 30 FN range, and

above 30 FN, separate lines are fitted to data for

each counterweight.

AWS A4.2 requires that the slopes of the various

calibration lines be similar, and specifies the

maximum variations allowed between the fitted lines

and the FN assigned to the primary reference

materials. The allowed variations are as follows:

Table 1: Primary coating-thickness

±0.40

±0.50

±0.70

±0.90

± 1.00

±5%

Oto 5 FN,

5 to 10 FN,

10 to 15 FN,

15 to 20 FN,

20 to 30 FN,

30 to 90 FN.

The requirement that the slopes of the various

calibration lines be similar helps ensure that the

estimates of FN calculated from the calibration lines are more or less continuous over the 0 to 100 FN

range. If the slopes are very similar and the

intercepts are correct, this approach serves as an

accurate calibration procedure. It is awkward,

however to justify why sets of discontinuous data

are used to develop independent equations for the

calculation of FN, particularly when Hooke's law

says the slopes should be the same. For this reason, we

used offsets to produce a white-dial calibration that was

FN.

TJ A.' (T J* Identification Thickness FN

SKJVL 1364a-93.082 1.901 2.729 bKM 1364 1.800 2.943 CDA K 1 1 £ A 1.700 3.180 bKM 1364a-yi.U82 1 1 1.63

1

3.360 5KM 1364 1.070 5.637 oKM 1364a-y3.Uoz 1.006 6.045 SKM l364a-y3.(J5z O.o20 *7 C A O 7.548 oKM 1364 A Oln O.olO 7.646

oKJVL I363a-yj.zy3 0.613 10.092 iSKM I363a-y3.zy3 0.496 12.359 oKM 1313 c\ in i 0.3/1 I5.y©2

aKM 1313 0.2/7 20.369

ISKM 1363a-y3.2y3 A 1 0.251 22.035 JNBb-LDff 154107 0.208 25.544

SRM 1312 0.195 26.780

JNBS-LC # 154107 0.137 34.671 NB55-L-B # 15410/ A AO A 0.084 AO T1A 48.730

CDTk / ion bKM. 1321 A r\A o 0.048 69.054

JNrJo lbjo AU 0.048 69.357

SKM 1321 A A/1 A 0.044 /3.29/

IQO/i A 44 1C/11A"7 iyo4-UAff 1J41U/ A A1C 0.038 /y. /42

SRM 1321 0.037 79.971 SRM 1321 0.035 83.674

NBS 7656 AD 0.028 94.184

NBS 7656 AD 0.014 130.250

took a slightly different approach and

continuous over the range of 0 to 100

The offsets can be determined in several ways. One way is to measure a primary standard using

two counterweights. For example, measuring SRM 1313 (Table 1) on gage 1 produced a white

dial value of 45.75 with no counterweight, and a white-dial value of 150.75 with a 7 g

counterweight. The offset for gage 1, 105, is the difference between the two values. The offset

for gage 2 was determined to be 118. Another way to find the offset is to use a digital scale to

determine the white-dial reading that corresponds to equal forces for various counterweight

configurations. This approach was used to construct the continuous data sets for gages 1 and 2

that are shown in Figures 5 and 6.

6
150

75 100 \ Q

o

50

i—i—i—

r

•

t—

r

• 7 g Counterweight

o g

Counterweight

1 i .

14 g Counterweight

%

y

k

J I I I 0

0 10 20 30 40 50 60 70 80 90 100

FN

Figure 4. Calibration data for gage 2. The three sets of data show the typical appearance

for calibration lines over the range of 0 to 100 FN. Calibration lines are determined

separately for the 0, 7, and 14 g counterweights, respectively.

7
200

100

0 V

Q-100 -

ii± ^-200

-300 \

-400

-500

V

50 100 150

FN

Figure 5. Calibration data for gage 1 using offset white-dial values

to allow a continuous linear fit of data over the 0 to 100 FN range.

200

50 100 150

FN

Figure 6. Calibration data for gage 2 using offset white-dial values

to allow a continuous linear fit of data over the 0 to 100 FN range.

8
Although this offset procedure is not mentioned in AWS A4.2, it clearly follows the intent of the

standard to have similar slopes. From a statistical standpoint, it is hoped that this procedure will

improve the calibration, because more data are included and the data are continuous over the

region of interest, 0 to 100 FN. However, the deviation allowed by AWS A4.2 between the FN

assigned to the primary reference materials and the calibration line is small, so fitting a single

calibration line over the whole FN may not always be possible.

For this study, we decided that each gage would be calibrated for two FN ranges: 0 to 30 and 30

to 100 FN. To minimize the error at very low FN, only calibration data within the 0 to 30 range were used for the linear regression fits. To retain some of the advantages discussed above, all the

calibration data (0 to 100 FN) were used for calibration between 30 and 100 FN.

The equations that best fit the calibration data for gage 1 and gage 2 are given in eqs (2) to (5):

Gage 1 FN = 27.35 - 0.247 (WD) for 0 to 30 FN, (2)

FN = 28.30 - 0.261 (WD) for 0 to 100 FN, (3)

Gage 2

FN = 26.33 - 0.244 (WD) for 0 to 30 FN, (4)

FN = 27.04 - 0.252 (WD) for 0 to 100 FN, (5)

where WD is the white-dial reading of the gage.

Overall the fits are good, as indicated by the relatively small differences between the predicted and

assigned FN values for primary reference materials (Figures 7 through 10). The standard errors

for the slopes of eqs (2) through (5) were typically 0.001. The R-squared values for the equations

all exceeded 0.999.

Both eq (3) and eq (5) come very close to satisfying the tolerances required by AWS A4.2 over

the range of 0 to 100 FN. However, neither equation fully meets the allowed tolerance of ±0.40

FN between 0 and 5 FN. The largest error for eq (3) in the 0 to 5 FN range is -0.5 1 FN. For eq

(5), all calibration points meet the required tolerances of AWS A4.2, except the 0 FN point which

has an error of -0.58 FN. The errors are reasonable, but the lack of full compliance for the

extended FN equations (eqs (3) and (5)) makes it necessary to use eqs (2) and (4) for FN

calculations within the 30 FN range. These equations are both well within the required tolerance

of AWS A4.2.

The two equations that best fit the 0 to 30 FN data (eq (2) and eq (4)) have slightly lower slopes

than the equations developed for the higher FN range (eq (3) and eq (5)). This suggests that the

calibrations are not ideal. (The error plots in Figures 8 and 10 show trends at low FN, confirming

that the data are better fit by two lines having slightly different slopes. But, six calibration points

for gage 2 between 0 and 10 FN have errors very near to 0).

9
1.0

0.5

Li.

o" 0.0

«_

l. LU

-0.5

-1.0

0 10 20 30

FN Assigned to Primary Standard

Figure 7. The difference in the FN assigned to the primary

reference materials and FN calculated from eq (2) for the range 0 to

30 FN (gage 1).

0 50 100 150

FN Assigned to Primary Standards

Figure 8. The difference in the FN assigned to the reference

material and FN calculated from eq (3) for the range 0 to 100 FN

(gage 1). Only data of 100 FN or less were used for fitting.

10
1.0

0.5

o 0.0

l_ LU

-0.5

%

0 10 20 30

FN Assigned to Primary Standard

Figure 9. The difference in the FN assigned to the standard and FN

calculated from eq (4) for the range 0 to 30 FN (gage 2).

6

0 50 100 150

FN Assigned to Primary Standard

Figure 10. The difference in the FN assigned to the standard and

FN calculated from eq (5) for the range 0 to 100 FN (gage 2).

11
3.4 Calibration Errors and Variables

The major contributors to errors in the calibration of the gages include: operator measurement

error (and bias), uncertainty in the thickness of the primary reference materials (±5 % of the

coating thickness), errors due to the gage, errors due to magnetic effects, and errors associated

with the coefficients determined for the line fits.

Some differences in the measurements made by the two operators are apparent in the data. As

shown in Figure 1 1, one operator tends to measure the FN slightly lower than the other.

Hopefully, the average of the measurements for the two operators is near the average that would

be found for a larger population of operators measuring the samples. Since these differences are

to be expected for users of the reference materials, we did not change our measurement

procedures or attempt to train the operators to produce more similar results. These data,

however, show that the magnitude of the difference between operators is significant in relation to

the maximum error allowed by AWS A4.2, and some influence of the gages and samples on the

magnitude and sign of the differences are also apparent.

Sources of error due to the primary thickness reference materials used to calibrate the gages were

evaluated by comparing the calibration measurements to the measurements from the 5 1 other

primary reference materials (gathered from various sources, see Appendix D). All of the

reference materials were measured by the same operator on the same gage, and then compared to

the calibration data for the gage. As shown in Figure 12, there are no significant outliers in the

data. Equations for lines fit to the calibration data and the independent data (5 1 other primary

reference materials) are virtually identical. We conclude that all the primary FN standards used

for our calibrations are within the ±5 % thickness tolerances expected of them.

z

ll

S2o*=* (0

8—m

a, O

c

.ft I

®

.a

0)o

?' |

1.0

0.5

0.0

-0.5

1.0

a a e

-ffl» B

CI

D €>

O Gage 2 ® Gage 1L10 20

FN

30

Figure 11. The difference between the measurements for operator

1 and 2 is shown for the two gages.

12
200

100

CO Q

CD § -100

-200

i—i—i—

r

t—i—i—

r

j i i i i L -300

0 10 20 30 40 50 60 70 80 90 100

FN

Figure 12. The primary reference materials used for the calibration

of gage 1 (shown as solid dots here) are compared to 5 1 other

primary reference materials.

2000

<D

+-» E

2 1500

1

co" cog 1000

o

!c

\—

D) 500

c

COo

O

- •

1 1 1—

T

Primary Standards

JL I I J *l l ^ • 0 10 20 30 40 50 60 70 80 90

FN

Figure 13. The relationship of the coating thickness of the primary

reference materials to the FN calculated by eq (1).

13
The difference in the 0 FN measured for the gages (Figures 7 and 9) and the lowest FN primary

reference materials measured is typically greater than 0.2 FN, which is large, considering that only

a ±0.4 FN error is allowed in the 0 to 5 FN range for primary gage calibrations. Although better

agreement in this critical low FN range would be desirable, the lowest FN primary reference

materials used for our calibration are well within ±5 % uncertainties certified for their thicknesses.

At 2.5 FN (2 mm coating thickness), for example, a ±5 % error in the thickness of the standard

translates to about a 0.4 FN difference. This points out the importance of determining accurate 0

FN data for these gages (to help weight the calibration data), and indicates that primary reference

materials with lower uncertainties in the very low FN range are needed to more accurately

calibrate the commercially important 0 to 10 FN range.

Accurate measurements of the thickness of the nonmagnetic coatings become more difficult as the

thickness decreases. Fortunately, the relationship between the thickness of the primary reference

materials and FN (Figure 13) is more tolerant of measurement errors as thickness decreases (FN

increases). Although small differences in thickness have a more pronounced effect on FN, a

larger error in FN can be tolerated in this region (high FN range). This is because the accuracy of

the measurement is less critical to the performance and properties of high FN alloys.

150

50

b

<b

±f -50

150

I I I I I I 1 1 "

* » B Gage #2

\

i B '!!

e

•

> c

a

* e m b « ® A

i i I i i i

P

»

B

i i

' -250

0 10 20 30 40 50 60 70 80 90

FN

Figure 14. The white-dial versus FN for the A, B, and C magnets are shown for Magne-Gage #2.

14
150

<5 h

-150 -

0 10 20 30 40 50 60 70 80 90

FN

Figure 15. The white-dial versus FN for the A, B, and C magnets for

Magne-Gage #1. The A, B, and C magnets are all #3 magnets.

50 100

FN

150

Figure 16: The effect of using #2, #3, and #4 magnets on gage

calibration data (magnetic strength increases with magnet number).

15
The strength of the magnets used on the gages also affects the calibrations. As shown in Figures

14 and 15, using #3 magnets of slightly different strengths (all within the tolerance allowed for #3

magnets) results in different calibrations for the gages. As long as the calibration data is linear,

this does not present a problem. However our evaluation of significantly stronger magnets (#4

magnets) indicated that magnet strength has an effect on the linearity of the calibration data. In

Figure 16, the calibration data for a #4 magnet is shown to diverge from the line drawn to fit the

low FN data (FN < 20). As already discussed, the data for the #3 magnets (our calibration data)

are also best fit by two lines, but are quite linear over the 0 to 100 FN range compared with data

for #4 magnets. It appears, however, that magnet/sample interactions effect the linearity of the

calibration, and this would tend to increase the uncertainty of the calibration. The changes in

slope of the data tend to occur at around 15 to 20 FN for the #4 magnets, and at 20 to 30 FN for

the #3 magnets (on both of our gages). These FN ranges correspond roughly to the knee of the

FN/coating-thickness in Figure 13.

3.5 Force Calibration

It is difficult to directly compare the gages used for FN measurement. The comparison can be

simplified, however, by replacing the arbitrary white-dial values of the calibration plot with a

force. By calibrating the white-dial scale in this manner, only the uncertainty in accuracy of the

primary standard and the difference in the strength of the magnet used on the gage remains.

As shown in Figures 17 and 18, the relationship of the white dial to the force measured on the

digital scale is linear, as would be expected by Hooke's law. This result is comforting and serves

as an excellent check on the gage overall. For example, gage 2 (Figure 18) shows a slight

undulation in the data, which is a result of a slight imperfection in the spring on this gage.

The overlaps in the data for the various counter weights used (0, 7, 14, 21, and 25 g) are also

apparent in Figures 17 and 18. At any point within these overlaps, the offset of the data sets can be determined. We also found that the zero for the gage was most consistently determined from

force data, because much of the operator bias was removed from the measurement.

Rearranging the the terms of the linear equations developed from the white-dial and force data

(Figures 17 and 18) we find that:

Equations (6) and (7) show that for a given white-dial value, gage 1 applies more force at the

sample than gage 2. Here, there is no effect of magnet strength, because the magnet never

detaches from the steel mass. As the white dial is turned, the force lifting the mass is measured on

a digital scale (see Figure 3).

Linear equations were developed for the force data and used to calculated the force for the whitedial values taken during the primary calibrations of the gages (primary reference materials

Force = 5.48 - 0.0494(WD)

Force = 5.01 - 0.0457(WD)

Gage 1 Gage 2

(6)

(7)

16
-400

0 10 20 30

Force, gram-force

Figure 17. The relationship of the white-dial reading to the force

measured using a digital scale for gage 1

.

200

-500

0 10 20 30

Force, gram-force

Figure 18. The relationship of the white-dial reading to the force

measured using a digital scale for gage 2.

17
calibration). The force data were substituted for the white dial data and plotted against the FN

data for the primary calibrations in Figures 19 and 20. The result is a plot for which both the X

and Y axes are traceable to calibration standards. The arbitrary white-dial scale has been

eliminated.

In terms of force, the data in Figures 19 and 20 show that a greater force is needed to pull the

magnet off a sample of given FN for gage 1 . This difference is attributed to the stronger magnet on gage 1 than on gage 2.

In terms of FN, the magnitude of the slopes for the data reverses:

These slopes, 541 and 561 FN per newton (5.27 and 5.52 FN per gram-force), for gages 1 and 2

respectively, are defined as the detachment force by AWS A4.2, but are actually a calibration

factor. A decrease in the calibration factor relates to an increase in magnet strength. At an FN of

80, for example, the calibrations indicate a 1560 N (15.3 g-force) is needed to detach the magnet

on gage 1, and a 1490 N (14.6 g-force) is needed to detach the magnet on gage 2. The

differences in the applied force needed to detach the magnets decrease with decreasing FN.

The intercepts for the lines in Figures 19 and 20 are not equal to 0. Both lines have intercepts of

0. 1 1, which we attribute to chance. (Note that fitting only the low FN data would result in

different slopes for both gages, and these lines would intercept nearer to 0 FN.) These results

simply reflect that the changes in slopes apparent in the calibration data plotted in Figures 5 and 6

remain after the force calibration.

3.6 Summary of Primary Calibrations

Overall we conclude that the gage calibrations are within the accuracies required by AWS A4.2,

and that we can certify secondary reference materials using these gages and calibrations which will

have accuracies that will meet or exceed those of past producers of these materials. This

conclusion is supported by practical verifications we performed to check the performance of our

gages. For example, when the FNs calculated using gages 1 and 2 are compared (Figure 21), only

slight differences are apparent and the FN values calculated for these gages are in good agreement

throughout the 0 to 100 FN range. To verify that our gages compared well to gages previously

used for certifying these materials, FN was measured on TWI secondary reference materials. As

shown in Figure 22, FN measurements made on our gage 1 agree well with the certified values

assigned to the specimens by TWI. The agreement for the gage 2 data showed a similar trend.

This result indicates there will be continuity between the FN values that assigned by NIST and

those assigned by TWI.

FN =-0.57 + 5.27 (Force)

FN =-0.61 + 5.52 (Force)

Gage 1, Gage 2.

(8)

(9)

18
20 1—i—i—i—i—i—i—i—i—

r

Figure 20. The relationship of force to FN for gage 2.

19
0 20 40 60 80 100

Gage 2, FN

Figure 21. The FN calculated using eqs (2) and (3) for gage 1 and eqs (4)

and (5) for gage 2.

0 20 40 60 80 100

TW! Certified Value, FN

Figure 22. The FN measured by gage 1 plotted versus the FN

certified by TWI.

20
Clearly, the use of commercial gages and the current calibration practices are not ideal for use in our FN reference material program. At this point, there is not an adequate understanding of the

variables contributing to calibration error, particularly those influencing the linearity of the

calibration. However, we are satisfied with the performance of our gages and our calibration

procedures (for now).

We find several of the calibration procedures that we incorporated into our program useful, and

suggest that they be considered as requirements (or recommendations) in AWS A4.2.

Specifically, we find that adding the extra procedural step of force calibration is useful and plan to continue to track the performance of the gages in this manner. It provides detailed information on

the linearity of the gages, a way to separate magnetic coupling variables from mechanical

variables, and a means to better compare the gages to one another. Torsion balances have been

evaluated in the past for FN measurement, so this more direct approach is not new [3]. But, by

simply adding a force calibration to the existing procedure for calibrating white-dial gages, the

best of both types of measurement devices can be realized: the accuracy and design of the MagneGage-type gages, and the traceability of the force calibration for the true torsion balance.

In addition, the determination of 0 FN using a balance (rather than operator judgement) and the use of continuous 0 to 100 FN data for the calibration of gages for high FN measurements should

be considered in AWS A4.2. The use of a balance to determine 0 FN is simple and removes

operator bias for this critical datum. The use of continuous data in the calibration of extended FN

ranges is more consistent with the principles on which the calibrations are based (linear), and will

likely help reduce variations in slopes obtained when fitting smaller groups of calibration data (for

various counterweights) independently.

4. Measurement of Secondary Reference Materials

4.1 Measurement Procedure

Measurements were made on the secondary reference materials in five positions, by two operators

using two gages. As shown in Figure 23, the five positions are clustered about the center of the

specimen face. At each position, five measurements are made (by each operator on each gage),

but only the lowest repeatable measurement of the five is retained. (This portion of the procedure

is to screen out measurements for which the magnet detaches prematurely, in accordance with

AWS A4.2.) In all, 100 measurements were made on each standard, but only 20 were retained

for the permanent data record and the calculation of the certified FN value.

4.2 Data Analysis

The data for a secondary standard are evaluated by calculating the mean and standard deviation

(STD) for each gage and operator combination, and each specimen position. In the example data

record shown in Table 2, these calculations are shown by row and column, respectively.

21
Typically, the STD is lowest for measurements performed by the same operator on the same gage

(row). This STD is the best indicator of variation in FN for the sample, because it is primarily due

to differences in FN measured at the five specimen locations. These values are deemed

particularly characteristic of the specimen when the STD for the four conditions (two gages, two

operators) show similar variation. In this example, the measurements made with gage 2 by

operator 1 have much higher variation than the other three conditions. This likely indicates a measurement error, and this is one approach used to check the data. The mean values are also

helpful in detecting measurement errors, assuming the means for a given gage are similar if the

operators have made good measurements. The mean and STD for the measurements made at a

single specimen location (column) include variation due to the differences between the gages and

operators. These values are the best indicator of how closely a customer measuring the standard

might expect to match our measurement at a given sample location. (Users of the reference

materials are instructed to make their measurements at the center of the sample face.) Therfore,

the mean for specimen position 5 is defined as the certified value for the secondary standard.

A grand average and STD, and a pooled STD are also calculated. The grand average and STD

for the 20 measurements made on the specimen provide our best overall estimate of the FN, and

variation in FN because differences in FN due to sample location are also included. The pooled

estimate of the variation in the specimen, S, is our best estimate of the variation in FN due solely

to the sample. S is calculated as shown in eq (10), where Si to s4 are the standard deviations

calculated for the five measurements for each of the four operator-gage combinations.

2 2 2 2 sl + s2 + s3 + s4 (10)

4.3 Data Trends

As we developed the certification data on the secondary reference materials, we were able to determine a representative measure of the standard deviation in the measurements for the batch.

An overview of the data is presented in Figures 24 through 29. The various symbols used in these

figures represent the rings from which the samples were taken.

In Figure 24, the grand standard deviations of the secondary reference materials are shown to

increase with increasing FN. This trend is apparent in Figures 26 and 28 as well. However, the

pooled standard deviations shown in Figure 26 indicate that the FN variation in the specimens do

not necessarily continue to increase with increasing FN. The pooled standard deviations for the

specimens show that above about 50 FN, the variation might be expected to remain below 3 for

good specimens. Several specimens have high standard deviations, compared with other

specimens of similar FNs. In particular, there is a group of specimens between about 50 and 60

FN that appear to be outliers. These data were reviewed for errors, and the specimens were

remeasured. Most outlying measurements were found to be repeatable and had higher than

average variation, so these specimens will not be used as secondary FN reference materials.

22
Figure 23. Measurements are made in the five positions shown, on

the face of the standard that is opposite the identification number.

Table 2. Example data for a secondary FN standard. Statistics for

each of the five positions (Plthrough P5) are shown (units are FN).

Gage PI P2 P3 P4 P5 Mean STD

(Operator)

Gage 1,(1) 51.79 51.53 52.57 52.31 51.53 51.94 0.47

Gage 1,(2). 52.75 52.75 53.50 53.00 53.00 53.00 0.31

Gage 2,(1) 51.26 49.96 51.53 53.09 52.57 51.68 1.22

Gage 2, ( 2) 53.00 53.25 53.00 53.50 52.75 53.10 0.29

Mean 52.20 51.87 52.65 52.97 52.46 52.43 STD 0.82 1.47 0.84 0.50 0.65

23
120

Figure 24. The grand standard deviation (STD of 20

measurements) for the batch of secondary specimens.

120

Figure 25: The grand standard deviation normalized by FN

showing the larger relative variation for lower FN specimens.

24
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Figure 26. The pooled standard deviation for the batch of

secondary FN reference materials showing variation similar, but

often lower than the grand standard deviation for the specimens.

120

Figure 27. The pooled standard deviation normalized by FN.

25
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40 80 120

FN

Figure 29. The standard deviation for the measurements made at position 5, normalized by FN.

26
In Figures 25, 27, and 29, the data are normalized with respect to FN. In Figures 25 and 29 the

relative variation in FN is shown to be highest within the 0 to 5 FN range, indicating that the

influence of different gages and operators on the FN measurements is most significant at low FN.

The pooled statistics, Figure 27, show that the variation in the low FN specimens is less than half

those that include gage and operator effects (Figures 25 and 29). This 10 % variation for the

normalized pooled statistics (Figure 27) best represents the FN variation inherent to the specimens

in the 0 to 5 FN range.

Since this is the first batch of secondary specimens for which these statistical data have been

compiled, we can not compare the quality of these specimens with thoses of specimens produced

in the past. The variation in the FN of the specimens does appear to be reasonable, considering

the various requirements for measurement accuracy in AWS A4.2. These and future data will be

used to develop better documentation on the quality of secondary FN reference materials. The

data will also be used to support and to update the requirements of AWS A4.2.

5. Certification of Secondary Reference Materials and Discusion of Errors

Each set of FN reference material (RM) contains eight individual specimens. A table that

accompanies the set provides three types of data on each specimen and a plot reflecting the

calibration error. As shown in Tables 3 and 4 (examples of high and low FN sets), the average

and STD for position 5, the pooled statistics, and the grand values are given for each specimen.

The FN value at the center of the sample (position 5) is defined as the reference value. The

pooled statistics and grand averages are provided for information only, to more fully describe the

variation in FN measurement within a specimen. The additional data are provided because the

specimens will be used to calibrate several different types of instruments and it is not clear at this

time which statistics may best support the users of these instruments.

5.1 Uncertainty Analysis

Measurement Repeatability (Wr): The Type A uncertainty in FN measurements taken at a single

location (position 5) is due to differences in operators, gages, and magnets used on the gages.

Here, uRis equal to the STD at position 5. Example wR data are given in Tables 3 and 4 for lowand high-range reference materials.

Calibration Error (wc): The Type B uncertainties in FN measurements due to sources of bias

include: (1) uncertainty due to variation in the thickness of the coating thickness reference

materials used to calibrate the gage, (2) the uncertainty of the dial readings on the gage, and (3)

the uncertainty related to the fit of the calibration curve.

The calibration errors shown in Figures 30 and 3 1 were determined by simulation. A triangular

distribution (±0.5) was used to model the thickness of the primary standard, and another

triangular distribution (±0.5) was used to model the error of the dial readings from the gage. The

27
Table 3. Example certificate for a 0 to 30 FN reference material set.

Level Specimen ID

Reference Values

average and standard

deviation (FN, position 5)

Pooled statistics ofspecimen positions

(FN)

Grand average and standard

deviation

(FN)

Avg u. Avg S Avg StD

1 16 - 1002 0.7 0.14 0.7 0.06 0.7 0.12

2 17 - 762 2.5 0.09 2.5 0.08 2.5 0.12

3 15-222 3.6 0.07 3.4 0.13 3.4 0.13

4 18-153 83 0.10 8.3 0.21 8.3 0.20

5 7-1127 11.6 0.25 11.5 0.17 11.5 0.24

6 19-156 14.8 033 14.8 0.11 14.8 0.32

7 26- 1653 18.2 0.26 18.1 0.24 18.1 0.29

8 27-1071 26.2 0.52 27.1 0.81 27.1 0.75

Figure 30. Simulated calibration error for 0 to 30 FN.

28
Table 4. Example certificate for a 30 to 100 FN reference material set.

Level Specimen ID

Reference Values

Average and Standard

Deviation (FN, position 5)

Pooled Statistics of Specimen Positions

(FN)

Grand Average and Standard

Deviation

(FN)

Avg u. Avg S Avg St.D.

9 10-300 313 0.72 31.3 0.47 31.3 0.74

10 29 - 2044 38.4 0.48 37.2 0.93 37.2 1.11

11 30 - 2052 46.6 0.94 46.8 0.81 46.8 1.10

12 12-713 53.4 0.98 53.6 1.05 53.6 1.31

13 11-622 62.7 1.13 62.3 1.14 62.3 1.43

14 14-446 77.6 1.51 76.1 1.76 76.1 1.77

15 14 - 866 88.9 1.84 87.4 2.07 87.4 2.44

16 13 - 563 107.9 2.36 108.4 2.29 108.4 3.34

Figure 31. Simulated calibration error for 30 to 100 FN.

29
root-mean-square error of the calibration result, based on 10 000 Monte Carlo samples, was used

as the calibration error.

Combined Standard Uncertainty (u): The two standard uncertainties (wR and uc) can be

combined by quadrature addition to obtain the combined standard uncertainty (combined

uncertainty). To determine the overall uncertainty for a given specimen, the measurement

repeatability for the specimen given in Table 3 or 4 and the calibration error estimated for the FN

level of the specimen in Figure 30 or 3 1 are combined using eq (1 1). For example, the combined

standard uncertainty for sample 27-1071 (Table 3) is:

u = ^ul + uc

= \j0.52

2 + 0.172 = 0.55. (11)

6. Microstructure

We have examined the microstructures of secondary reference materials, selected over a broad

range in FN. The samples chosen for these destructive evaluations also had high variation in FN.

These samples are used to provide characteristic examples of microstuctures for the various FN

levels selected and to identify microstructural features that might explain the high variation in FN

measured for the samples. Example microstructures for these specimens are shown in Figures 32

through 40. The specimens were prepared for both light microscopy and atomic force

microscopy evaluations. The primary features of interest for these evaluations were the ferritic phase content and uniformity, the "grain size," magnetic domain size, and solidification flaws.

Figure 32. Light micrograph of sample 14-888, 10 mm equal to 50 //m.

30
Figure 33. Ring 7, specimen 1268, FN = 9.9.

Figure 34. Ring 27, specimen 1732, FN = 26.

31
Figure 35. Ring 10, specimen 2029, FN = 35.
Figure 37. Ring 1 1, specimen 242, FN = 51.9.
Figure 39. Ring 24, specimen 1581, FN = 73.6.
6.1 Grain Size

The "grain size" (cell or dendrite packet size) is difficult to quantify in many of these

microstructures. However, the grain size, which is delineated by differences in dendrite orientations, can be estimated qualitatively in many of the

samples (particularly for specimens of 30 FN or more). Etching to enhance grain contrast was used

occasionally to help delineate the boundaries

(Figure 32), but in many of the alloys (Figure 35,

for example) an almost continuous austenitic phase

(white) marks the grain boundaries well enough to roughly estimate the grain size for our purposes.

The changes in the ferrite/austenite morphology

within the boundaries reflect variations in dendrite

orientations, and this apparent grain size is clearly a good measure of the critical repeating

micro structural features in the specimens.

Figure 41. Example of a deeply etched

microstructure for the specimens. Ring 12,

specimen 697 (160 by 160 urn area).

The micrographs in Figures 33 through 40 are digital images (light microscope) that show typical

grain morphologies for the specimens. The figures show regions of microstructure that are approximately 800 by 800 urn in size. The apparent grain diameters for the specimen shown in

Figure 35, for example, range from about 100 to 300 um. This range in grain diameter appears to

be common to the specimens that were evaluated, and it is likely that the average grain size for

the specimens is well below 300 um. Assuming that the magnetic measurements made with the

FN gage cover microstructural regions of near 1 mm 2

, then the relative scale of the ferrite/austenite

morphologies are reasonable, particularly for

specimens of less than 50 FN.

6.2 Ferrite Content

The ferritic phase content of the specimens was

estimated using light microscopy and image

analysis. The measurements were made on planes

parallel to, and just below the plane on which the

FN measurements were made. The specimens were lightly ground (800 grit) and polished to

remove surface damage, then etched using a Beraha

II solution for the evaluations. Area fraction

counts were made at 2 different magnifications, and

for each count 100 adjacent fields were measured.

100

TO

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80

60

u. 40

20

0

! |

•

i i

s

• * i :

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•

20 40 60 80 100

Ferritic Phase, Area Fraction (%)

Figure 42. Area fraction of ferrite

measured for the specimens. Values are the average of at least two counts (100

fields each).

35
For the lower magnification used, the total area of each count was about 2.5 mm2 and for the

higher magnification the total field area was about 0.64 mm2

.

Typically, several counts were made at each of the two magnifications. The influence of the etch

(light versus deep etching condition) on the area counts was significant in some cases, as is always

the case. However, with appropiate thresholding similar area fractions were counted for both

conditions. The deeply etched samples (Figure 41) were found to provide excellent contrast for

the analysis, particularly for the higher FN levels.

The results of the area fraction counts were somewhat surprising. As shown in Figure 42, we

found a 1: 1 correlation between FN and the ferrite area fraction measured (up to at least 50 FN).

It was expected that above 10 FN, the two measurements would start to diverge, and by 50 FN be

significantly different.* We remeasured several of the samples to check the result, and believe the

results to be accurate (within about 5 %).

Three of the samples were evaluated by X-ray diffraction to determine whether they might contain

sigma phase, which is non-magnetic and could be incorrectly identified (and counted) as ferrite in

the light microscopy results. No sigma phase was present in the samples.

6.3 X-ray Evaluation

The secondary FN specimens were X-rayed prior to beginning our FN measurements to help screen out any samples that contained serious casting flaws. No specimens were excluded for use based on these results, but some characteristic differences in the specimen were apparent. As

shown in Figure 43, some specimens have a much grainier, more textured appearance than others.

This may be a result of compositional differences, which can change the primary solidification

mode or influence the relative segregation of compositional elements in the cast. The different

appearances may also be due to crystallographic alignment (texture) or networks of small casting

defects, which might have characteristic differences due to the specific solidification conditions

(and composition) of the ring from which the group of samples was taken.

Figure 43. X-ray images of some of the ferrite reference samples.

* Area fraction counts of the percent ferrite in stainless steel weld have shown the percent ferrite and FN to be

aproximately equal up to 10 % ferrite. At levels of more than 10 % ferrite, FN measurements have been shown to over

estimate the percent ferrite in welds (AWS A 4.2).

36
6.4 Solidification Flaws

Microstructural evaluations showed that the centrifugal cast FN specimens have solidification

flaws, as might be expected. As shown in Figure 44 , these flaws can be quite minor and would

not be expected to result in significant deviation for FN measurements. Larger flaws, however,

such as those shown in Figure 45, would likely result in variation for FN measurements. We

expect that these types of flaws were the main reason for unacceptable variation in a few of the

reference specimens. These specimens were rejected and used only for the microstructural

studies.

Figure 44. Solidification flaws in a sample from ring 14 - 898. Bar

equal to 100 um.

i » A.

Figure 45. Solidification flaws in a sample from ring 7 - 1268. Bar

equal to 100 um.

37
6.5 Atomic Force Microscopy

The microstructure (by atomic force microscopy (AFM)) and the magnetic fields (by magnetic

force microscopy (MFM)) for a low FN specimen and one with an FN near 42 have been

evaluated. These evaluations showed that the phases delineated in light microscopy, AFM, and

MFM are the same phases: Magnetic domain images show the magnetic ferritic phase is correctly

and clearly revealed by light microscopy and AFM.

The characteristic microstructural features (austenite islands, bordered by ferrite) are closely

spaced, as shown in Figure 46. The width of the austenitic phase separating the magnetic ferrite

phase is typically less than 25 um wide in this example. This fine structure means that many

dendrites are included in each measurement by the 1 mm diameter magnet of the gage. Also,

these dimensions are similar to those found in welds, indicating their suitability for use as secondary reference materials. The magnetic force image shows that the magnetic domains in the

ferrite phase have characteristic dimensions near 2 or 3 (am, giving more information on the fine

distribution of the magnetic fields through these specimens.

Figure 46. MFM image of the magnetic domains in a secondary FN standard sample. The larger, white

regions show the morphology of the austenite phase.

The black-and-white striped regions show the ferritic phase, indicating the size and orientation of magnetic

domains. Units in micrometers.

38
7. Information on Reference Material

Twenty-five sets of secondary specimens are in inventory and can be ordered from the NIST

Standard Reference Materials program by phone at (800) 975-6776, by fax at (301) 948-3730, by

email at srminfo@nist.gov, or on the net at http://ts.nist.gov/srm. Information on the inventory can be obtained from Rob Gettings by phone at (301) 975-5573 or by email at gettings@nist.gov.

Technical information can be obtained from Tom Siewert at (303) 497-3523 or siewert@nist.gov

and Chris McCowan at (303) 497-3699 or mccowan@boulder.nist.gov.

8. Plans

Over the next few years, we will calibrate additional sets, so we can achieve a stock of equal

numbers (50) of sets in each range. In addition to calibrating these sets as secondary reference

materials according to the internationally recognized procedure (AWS A4.2, based on NIST

reference materials for coating thickness), we propose to develop a primary calibration system

which will be traceable to primary electrical quantities. The most likely basis for the system will be

dc magnetic measurements. Initial work will determine the actual magnetic properties of the

existing secondary standard materials at both the macro- and micro-magnetic levels. Conventional

metallography will play a significant role in this phase of the work. Magnetic force microscopy

and vibrating specimen magnetometry will be used along with superconducting quantum

interference device (SQUID) magnetometry as necessary to characterize the ferrite magnetics.

The ultimate goal will be the development of a portable, easily used, standard magnetic

measurement device suitable for accurate determination of ferrite concentration. This standards

development activity will occur parallel to the assignment of values according to the existing

standard, and will be performed in close collaboration with experts in WRC, AWS, and IIW

Commission II, so the users group will be ready to adopt this primary calibration technique when

it is ready.

We thank D.J. Kotecki (The Lincoln Electric Company) for his comments on this manuscript and

for his active role in helping us obtain the samples from Russia.

9. References

1 . Standard Proceduresfor Calibrating Magnetic Instruments to Measure the Delta Ferrite

Content ofAustenitic and Duplex Austenitic-Ferritic Stainless Steel WeldMetal, American

Welding Society Standard A4.2-91, American Welding Society, Miami, Florida, 1991.

2. B.J. Ginn, T.G. Gooch, D.J. Kotecki, G. Rabensteiner, and P. Merinov, Weld Metal Ferrite

Standards Handle Calibration of Magnetic Instruments, Welding Journal 76:59; September 1997.

3. D.J. Kotecki, Extension of the WRC Ferrite Number System, Welding Journal 61: 352-s;

November 1982.

39
Appendix A

Primary Calibration Data

Primary standards and average white-dial values (gage 1 and gage 2):

Case THICK (mm) FN G1AVG G2AVG

1 0.,0 110.25 109.50

2 1. 9010 2 .7293 100.00 96.50

3 1.8000 2 .9429 99.25 95.75

4 1.7000 3,.1795 98.13 94.38

5 1.6310 3.,3595 97.50 94.25

6 1.0700 5.. 6371 88.38 84.50

7 1.0060 6..0448 86.38 82.88

8 0.8200 7.,5475 80.38 76.63

9 0.8100 7..6454 80.13 76.25

10 0. 6150 10., 0917 70.50 67.25

11 0.4960 12.,3590 61.13 58.38

12 0.3710 15.,9824 45.75 44.13

13 0.2770 20. 3685 28. 63 25.50

14 0.2510 22 .0350 19.50 15.88

15 0.2075 25..5438 6.88 2.75

16 0.1950 26.,7801 3.00 -1.50

17 0.1372 34.,6713 -28.88 -34.25

18 0.0836 48..73 -78.25 -82.00

19 0.0481 69.,0539 -156.25 -164.00

20 0.0478 69.,3566 -154.75 -162.00

21 0.0435 73,,2966 -172.25 -178.88

22 0.0376 79. 7415 -191. 63 -204.00

23 0.0374 79..9709 -199.38 -208.00

24 0 . 0345 83, 6737 -211.50 -222.50

25 0.0277 94 , 1840 -255.50 -272.50

26 0.0135 130,.2505 -372.00 -415.00

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p» P> r- en r- cn p> to P* to cn CM cn CM CO CM cn CB P- m to ao in cn «> 00 to p» © CO en o

cn cn cn cn <r °& ^S1 <* ^« «»• in in

cn CO CO m CM cn h H CO m CM CM CM CM cn CM H H 00 H r- o cn m in CM p* p» in in H

H r» r* H in cn p» 10 o CB CM cn m Wj ; p» © w t© h~f =%i cn CM in cn CO P» © cn

in in cn C cn cn r* r- CO to ro CM cn CM to un CM 00 CO r- t» to m to to sn to cn to cn r» p» P- P» en oi °& ««> cn cn °® <* <f «* <*& «* «^ <*

CM H H CM HI CM CM h CM H H CM H CM CM H H CM H CM H CM HI CM HI CM HI CM H HI CM H CM HI H CM CM CM H

u o O u a O a u O Q O Q P 0 U Q U Q u U Q (Q Q Q u u Q O o o, o O P O Q o O a a Q

SB CD m cn m cn cn cn 0» 01 to to to 00 DO 09 CS HI HI H r-l CM CM CM «* ^> CB CB CO 00 en cn cn CM CM cn en vp m in in m r- r» P* r» r~ r» f-» m in in m in m in if) in in in in m m in in m m in <o to GO a ® 00 00 eo 00 IS 80 CO 00 CD CO CO 68 CB 00 o © © a o © o © © © © © © © © © © © © © © o H H H H H <h H H H H H H H H HI H H H CM CM CM CM CM CM CM CM CM CM CM CM CM CM CM CM CM CM CM CM CM CM

O a o O o a © O o o O O a O O o a © © o © © © © © © © © O © © © © © © © © o © ©

cn en cn cn cn rn cn cn cn cn cn cn cn cn <n «n pi rn cn cn cn cn cn cn cn cn cn cn cn <n cn cn cn cn cn cn cn cn <n cn

77
CO H in H <• in CM CM CD CD cn CD CM o

1

A

U J m in 0D cn Ol in iH QQ o Ol cn \0 inu J o o O o O o o ^ H O H o ^i o o o O o

m oi m r- H Ol r- r- Ol r- r- in o

in m en o >H 1*1 10 o CM 10 <ji 10 01 o OJ in o CD oi GO o CD ID Ol rx» o> OD CD '33 o o CD

in in >* ^< ^< LCI in *»<

m O CM r- CB m CM H CM no HI CM cn in

CM o\ *H CM W> CM cn cn Ol o

O Ol 00 oi cn o Ol r Ol as 00 eat o o Ol

in <& in <* in in «#

01 CM cn CM *£> m CM CM 10 r- r- (0 rn

o\ fvt] 01 Oij CI 1 1 001 Ov, fTfi) H m cn o 133 o r- in r- o» o o Ol CD Ol Ol o 00

in in m in

o m H CM 10 Ol m CM m rn a CM rn & m

O _J firs '=© o it Cul r(^,J] (VI '.'! o o en 00 CD r» Ol r- r- o» r» o ea O O o Ol

in «a> in «* in nn in

00 CM p» r- un CM o H 10 m e, r* <H » rn

CM CJD oi 10 p*. cn u> P f

i

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r» "«< r- o» in m rH en cn o m xf CM m

Ol ^« CD Q m CM r> H 10 o ca 00 OS H

Ol ot r- Ol o 00 m CD CD Ol Oi 00 r- o» Ol 00

in <* "*

CM H H CM CM H CM H CM H CM H CM CM H

U U U a a U O u Q O U u o Q o o Q Q

CM CM r- r» r- [- Ol Ol Oi CM CM n rn cn m

10 <£> (0 io 10 10 10 10 «r, r> r- r- r* p. r- o O o o o o o o o O o o o o D o o o

CM CM CM CM CM CM CM CM CM CM CM CM CM CM CM CM CM CM

o © O O o o o O o O O O O O O O O O

m m CI (0 en cn cn n cn n PI n cn m en cn cn cn
Appendix D

Round-Robin Data for Primary FN Standards

Although the calibration data for the NIST gages, shown in Figures 7 to 10, were acceptable, we

wished to reduce the error further. In particular, the error trend seen between 0 and 30 FN did

not seem random, and so we suspected this was some artifact of our measurement technique or equipment. We sought independent data to learn the source of the errors, and so how they might

be reduced.

Our measurement error is the quadrature sum of multiple error sources, such as: operator

technique, primary standards, and gage variables. We were already using two gages, two

operators, and a large number of standards. Additional data would have to come from sources

outside our laboratory, but would have to be compared to it in some way.

We were able to develop this independent data and compare it to our data from Figures 7 to 10,

at a special meeting just before the Spring 1999 meeting of the Welding Research Subcommittee on Stainless Steel, which was attended by other researchers in stainless steel. Frank Lake brought

the Magne-Gage (identified in this report as gage 3) and coating thickness standards that were

regularly used for research by Esab, and Damian Kotecki brought some of his collection of NBS

standards, ones that were selected to supplement the areas where our standards were sparse. This

allowed us to set up a round robin with three skilled operators (one of which was an NIST

operator who contributed to the data in Figures 7 to 10), three Magne-Gages (two from NIST

and one from ESAB, which had not been compared to the two NIST gages before), and 5 1 NBS

and NIST coating thickness standards (which were very well distributed through the range of 0 to 120 FN, and which spanned about 50 years of SRM production). Table D. 1 lists the data from

this round robin. Each standard was measured on three gages. The NIST operator took data

with gage 3, while the other two operators took data on the 2 NIST gages.

Figures D. 1 to D.3 show the calibration data for the three gages. The small scatter of the data

within the error bands indicates that the gages (and operators) have similar accuracies. The data

used to calibrate gage 2 was compared with the data collected for the 51 independent primary

standards (not shown in Figure D.2). It was evident that a similar calibration would be obtained

for gage 2 using either set of primary standards. We think these result indicate that the operators

and standards are not significant contributors to the various trends observed in our calibration

data (between 0 and 30 FN, Figures 7 to 10). The trends seem to be inherent in the NIST gages,

magnets, or the coating thickness-to-FN conversion table in AWS A4.2.

As indicated by the force versus FN plot in Figure D.4, the major differences between the gages

evaluated here are due primarily to the different strengths of the magnets used on the gages. The

magnet strength clearly affects the slope of the fit, as would be expected. It may also have an

influence on the characteristic trends we find in the data for different magnet and gage. Again, this

information has little effect for daily users of the technique, but is important to the calibration

laboratories that are trying to reduce the error in the test to the achiveable minimum.

79
Table D.l. White-dial and force data for 51 primary FN reference materials measured on 3

Magne-Gages by 3 operators.

Case number FN WD1 WD2 WD3 Fl F2

1 o2 . 4 y

i a a c a y d . 30C A 1114. 1 A AOUA u

.

c o 52 0 . C A60 A C C 0.56

o o Q O" y / Q3DO . c a Q A y4 . AOOA 1llz1 o . 3UC A Au

.

Ol 0 . /l A C O 0 . 63

oJ 5 . A R 4 3 OyoC

.

en yz

.

AUUA 111U1 A . AUUA Au

.

IX AU . O 1 81 A O C 0 . 75

A4A4 . o o 2 o yz

.

R n O Q OO . C A 50 1 A T 10 / . A A UU U . 91 0 . 97 0.89

c5

c5 . V! C 4 D

o o 8 8 . a a o o O J . A A 00 1 A O A A UU I . 1 o 1

3

1

.

o o 22 1 1 A 1 . 13

6 5

.

64 88 . 00 83

.

00 101

.

00 1 . 13 1

.

22 1 . 18

7 6

.

78 83

.

00 77 . 00 96

.

50 i . 38; 1

.

49 1 . 40

8 8 . 06 78 . 50 73 . 50 90 . 50 1 . 60 1

.

65 1 . 68

9 9 . A f\ 4 9

O o/ 3 . A00 68 . 00 84 . 50 1 . 87 1

.

90 1 . 97

10 9 . 90 71 . 00 66 . 00 82 . 50 1 . 97 1

.

99 2 . 07

1

1

12 . 1 C 1 6 CObz . c n 30 DO . UU / J . UU 2 . O A 39 2 . O £T 36 2 . 52

1 o 1 o 12 . O A 20 COoz . 0 0 D / . DU / Z . UU o2 . A O 42 A o o 38 O CO 2 . 57

1

3

14 . 94 51 . 50 47 . 50 60 . 00 2 . 9 4 2 . 84 3 . 14

1

4

1 c y lA C 4 6 . 50 4o . UU DDc c . o3 . 1 o 18 -3 . 04 o o ^ 3.36

Id O 1 21 . 1 / Z3o c . A A 0 0 i y

.

UU oU . DU A4 . o c 4 . 14 4.56

16 O "1 21 . 30 O /] 24 . C A 50 17 . 00 30

.

00 A4 . o o 27 4 . 23 4 . 58

17 25

.

88 8 . 50 0 . 0 12

.

00 5 . 06 5 . 01 5 . 44

18 25

.

98 5

.

00 -1

.

00 13

.

50 5

.

23 5

.

06 5 . 37

1 9 26

.

07 7

.

00 -0 . 50 9

.

00 5

.

13 5

.

03 5 . 59

20 29

.

16 -5

.

50 -13

.

00 -7

.

50 5 . 75 5

.

60 6 . 38

21 32 . 36 -18 . 00 -25

.

50 -17

.

50 6

.

37 6 . 18 6 . 85

22 33

.

15 -19 . 50 -28 . 00 -17 . 0 0 6 . 44 6

.

29 6 . 83

o o 2 3o o o o JZ — o o 22 . A A 00 — O A JO . CDOA — o o 2 J . A A 00 o . C O" 5 / 6 . 40 O 1 o 7 . 12

o ^ o. A o. A — tJOR . — o. c u u — OQ nnu u o . 1 c/ 3

cO . ol 7 . 36

O R "3 4 J*i . / u — OK O C. — *3 Q u u — O *7 nu nu o . / O oc

.

1 c/ 3 / . Jl ac cn _ o c; o o nn cO • QA o . O X

"7 fin o "7 a n — A~l cn3 U 3D. u u _ c o 3a . 3U 1 . RO 3

o/ . CT3 / O . 3RQJ

O Q £. 0A R O X au nu / D . u u / 3 . 3U Qo . O ^ o . A A O CO

O Q ^ © . a i / U . cnSU II. A A — OR03 . AU AU Q y o oo . C o. 3 3ix au . nou y

o.n A1 *n _*7 c

/ 3 . 3URD -QA u u OO . cn3U ay

.

Z X Ro . RS3R in o

a

xu . z

o

31 A O 4 8 . 1 A l y -00 . A A 00 — O / . C A 50 -o 1 . C A 50 Ay

.

VI o 43 A

9 . A

1

01 1 A O 1 10.21

32 50 . 23 -84 . 50 -96 . 00 -98 . 50 9

.

65 9 . 40 10 . 73

3 3 C A 50 .

Jl yl 44 -81

.

A A 00 -95A C

. A A 00 -36A c . A A 00 9 . a a 48 9 . o c 35 10 . 61

34 54 . 05 -100 . 00 -109 . 00 -Ill . 00 10 . 42 9

.

9 9 11 . 33

35 58 . o2 6 -113 . C A 50 -123 . 50 -135 IOC . C A 50 11

.

A A 09 10 . 65 12 . 51

3 6

C A 60 . ^ o 62 — 124 . 50 -136 . A A 00 -138 1 o o . A A 00 11

.

c o 63 11 . o o 23 t o ^ o 12 . 63

O O c o DJ . 1 C 1 O -1i o i 31

.

A A 00 -144 1 yl >l

. A A 00 ICO C A 50 11

.

o c 93 i 1 . oy 1 O CI 13 . Ol

38 64 . 08 -136

.

50 -148 . 00 -155

.

50 12 . 22 11 . 7 7 13 . 46

3 9 67 . 30 -148 . 00 -1 62 . A A 00 -17 6 . A A 00 t o 12 . 1 A 79 1 o 4 i

1 A AC 14 . 45

40 67 . 87 -151 . 00 -164 . A A 00 -172 t 1 o. C A 50 1 A 12 . A Jl 94 12 . C A 1 A AO 14 . 28

4 1 69 . 23 -155

.

50 -168 . 50 -181

.

50 13

.

16 12 . 71 14 - 71

42 71

.

19 -163 . 75 -177 . 50 -197 . A A 00 13 . 57 13 . 1 A 12 1 C it c 15 . 45

43 73

.

79 -167 . 00 -188 . 00 -211 . 50 13

.

73 13

.

60 16 . 15

4 4

•—I a 74 . o rv 20 -171 . A A 00 -185 . A A 00 -209 O A A . C A 1 o 13 . A O 93 1 o 1 3 . 46 1 C AC 1 6 . 05

45 76. 08 -191 . 00 -212 . 50 13. 74 16.19

46 76. 19 -191. 00 -210. 50 13. 74 16.10

47 76 . 30 -182 . 00 -192 . 00 -217 . 00 14 . 47 13 . 78 16.41

48 81 . 58 -206 50 -224 . 00 -248 . 00 15. 68 15 . 25 17 . 89

49 84 .49 -21"J1

. 00 -236i. 00 -2621.50 16; . 20 15 .80 18 . 64

50 95. 98 -264 . 30 -280 . 00 -306. 50 18. 54 17 . 81 20.70

51 97 . 10 -261

.

00 -284 . 00 -321

.

50 18 . 37 17 . 99 21 . 41

80
200

100

<5 Q

CD 5-1

-200-

-300

0 10 20 30 40 50 60 70 80 90 100

FN

Figure D. 1 . Data for measurements on gage 1, showing estimated error limits for the

primary samples (±5 % of in thickness, expressed in FN).

81
82
200

100

.-2 -100

i—

r

n—i—

r

v

-Ne-,

"-S.N

XXXJ NX

-200

-300

-400

0 10 20 30 40 50 60 70 80 90 100

FN

Figure D.3. Data for gage 3, and limits for primary standards (±5 % in thickness).

J L J L

83
25.0 I I I I I I I I I 22.5

20.0

17.5

- i _ i

A

5 Gage 3

1 Gage 2

odyc i

/

/

~

^ 15.0

2 12.5

^

10.0

/

7.5 y -

5.0

2.5

0.0

s I I I i i i i i i 0 10 20 30 40 50 60 70 80 90 100

FN

Figure D.4. Force calibration data showing results for all three gages for the 5 1 primary

thickness standards.

Gage 1: FN = -0.75 + 5.3(Force)

Gage 2: FN = -1.22 + 5.5(Force)

Gage 3: FN = +0.54 + 4.6(Force)

84
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