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An evaluation of ASTM D6200
Article in Materials Performance and Characterization · November 2017
DOI: 10.1520/MPC20170006
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An Evaluation of ASTM D 6200
Criteria for Cooling Curves

D. Scott MacKenzie, PhD, FASM

smackenzie@houghtonintl.com
Agenda
Introduction

Experimental

Discussion

Conclusions
Introduction
• Cooling curves increasing used

New applications

Existing operations – Replacement Oil

Existing Oil – Quality Assurance
 AMS 2759/1 – Quarterly
 NADCAP – Quarterly
 CQI-9 – Bi-Annually
• ASTM D6200 (ISO 9950) is basic method used
ASTM D6200
• Inconel 600 Probe

13 mm diameter

160 mm long

T/C inserted at center

850°C
• Quenchant

1-2 liters (2 liters
recommended)

Temperature variable (60°C
typical)

No agitation
• Transfer

Automated

Manual
ASTM D6200
 ASTM D6200
ASTM D6200 Bias and Precision

Temp. at Temp at Start

Maximum Temp at Start Cooling Rate Time to Time to Time to
Property Max. Cooling of
Cooling Rate of Boiling at 300°C 600°C 400°C 200°C
Rate Convection
Single Operator
Variation (2σ) 2.1 12.7 N/A N/A 8.7% of Mean 0.4 0.5 1.3
Minimum 95.2 606.49 N/A N/A 4.59 6.21 10.39 43.73
Maximum 99.4 631.89 N/A N/A 7.65 7.01 11.39 46.33
Inter-Laboratory
Variation (2σ) 8.6 25.3 N/A N/A 25% of Mean 1.4 2.1 10.1
Minimum 84.7 577.03 N/A N/A 4.02 4.59 8.25 30.33
Maximum 101.9 627.63 N/A N/A 6.70 7.39 12.45 50.53
Experimental
• Three sets of data used

Production data set
 50 Lots of material
 Single operator

Laboratory integrity check
 One lot of material
 131 Curves
 Multiple operators

User Data
 38 Customers
• All using same oil (Houghto-Quench G)
Experimental

All using same Cooling Curves

Three sets of
oil (Houghto- evaluated for
data used
Quench G) attributes

Production Laboratory
User Data
data set integrity check

50 Lots of One lot of Multiple

Single operator 131 Curves 38 Customers
material material operators
Maximum Cooling Rate
120

100

80
Population

60

40

20

0
60 65 70 75 80 85 90 95 100 105 110 115 120
Maxium Cooling Rate, °C/s

Production Data Laboratory Data User Data

Temp. at Maximum Cooling Rate
50

45

40

35

30
Population

25

20

15

10

0
552 560 568 576 584 592 600 608 616 624 632 640 648
Temperature at Maxium Cooling Rate, °C

Production Data Laboratory Data User Data

Start of Boiling
80

70

60

50
Population

40

30

20

10

0
667 675 683 691 699 707 715 723 731 739 747 755 763
Temperature at the Start of Boiling, °C

Production Data Laboratory Data User Data

Start of Convection
40

35

30

25
Population

20

15

10

0
320 325 330 335 340 345 350 355 360 365 370 375 380
Temperature at the Start of Convection, °C

Production Data Laboratory Data User Data

Cooling Rate 300°C
45

40

35

30
Population

25

20

15

10

0
4.7 5.0 5.3 5.6 5.9 6.2 6.5 6.8 7.1 7.4 7.7 8.0 8.3
Cooling Rate at 300°C, °C/s

Production Data Laboratory Data User Data

Time to 600°C
70

60

50
Population

40

30

20

10

0
5.6 6.0 6.4 6.8 7.2 7.6 8.0 8.4 8.8 9.2 9.6 10.0 10.4
Time to 600°C, seconds

Production Data Laboratory Data User Data

Time to 400°C
80

70

60

50
Population

40

30

20

10

0
8.5 9.0 9.5 10.0 10.5 11.0 11.5 12.0 12.5 13.0 13.5 14.0 14.5
Time to 400°C, seconds

Production Data Laboratory Data User Data

Time to 200°C
60

50

40
Population

30

20

10

0
32.5 35.0 37.5 40.0 42.5 45.0 47.5 50.0 52.5 55.0 57.5 60.0 62.5
Time to 200°C, seconds

Production Data Laboratory Data User Data

Summary Data
Laboratory Data
Maximum Temp. at Max. Temp at Start of Temp at Start of Cooling Rate at
Property Time to 600°C Time to 400°C Time to 200°C
Cooling Rate Cooling Rate Boiling Convection 300°C
Average 97.3 619.2 724.8 365.8 6.1 6.6 10.9 45.0
Std Deviation 2.0 8.4 6.0 7.9 0.4 0.3 0.3 2.3
2σ 4.0 16.9 12.0 15.7 0.8 0.6 0.5 4.6
Minimum 93.3 602.3 712.8 350.0 5.4 6.0 10.4 40.4
Maximum 101.3 636.0 736.8 381.5 6.9 7.2 11.4 49.6
Production Data
Maximum Temp. at Max. Temp at Start of Temp at Start of Cooling Rate at
Property Time to 600°C Time to 400°C Time to 200°C
Cooling Rate Cooling Rate Boiling Convection 300°C
Average 101.0 614.5 721.8 344.1 6.3 7.2 10.9 41.7
Std Deviation 2.1 4.8 11.5 7.8 0.5 0.4 0.3 0.9
2σ 4.1 9.6 23.0 15.6 0.9 0.7 0.7 1.8
Minimum 96.9 604.9 698.8 328.6 5.4 6.5 10.2 39.8
Maximum 105.2 624.2 744.7 359.7 7.2 7.9 11.6 43.5
User Data
Maximum Temp. at Max. Temp at Start of Temp at Start of Cooling Rate at
Property Time to 600°C Time to 400°C Time to 200°C
Cooling Rate Cooling Rate Boiling Convection 300°C
Average 90.4 604.2 714.8 350.1 5.9 7.6 11.6 46.0
Std Deviation 8.1 18.5 18.5 11.9 0.3 0.7 0.9 1.7
2σ 16.2 36.9 37.0 23.9 0.6 1.5 1.8 3.3
Minimum 74.3 567.2 677.9 326.3 5.3 6.2 9.8 42.7
Maximum 106.6 641.1 751.8 374.0 6.6 9.1 13.4 49.4

ASTM D6200
Average 97.3 619.2 6.1 6.6 10.9 45.0
Variation (2σ) 8.6 25.3 1.5 1.4 2.1 10.1
Minimum 88.7 593.89 N/A N/A 4.59 5.21 8.79 34.93
Maximum 105.9 644.49 N/A N/A 7.65 8.01 12.99 55.13
Summary Data
800

700

600

500
Temperature, °C

400

300

200

100

0
Maximum Cooling Rate Temp. at Max. Cooling Rate Temp at Start of Boiling Temp at Start of Convection
Laboratory Data Production Data User Data ASTM D6200
Summary Data
60

50

40
Time, Seconds

30

20

10

0
Cooling Rate at 300°C Time to 600°C Time to 400°C Time to 200°C
Laboratory Data Production Data User Data ASTM D6200
View publication stats

Conclusions
• ASTM Specification
evaluated

Found to be adequate for
new oils

Not adequate for used oils
• Specification is too tight
to make good/bad
decisions on used single
oil
• Will result in excessive
audit bait