Studies on the analysis of hydrogen in high strength steels

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D. B. McDONNELLis Coordinator, QualityAssurance, Environmental Technology Centre, Ottawa, ON K1A tC8. Canada. V.S. SASTRI, Research Scientist, C. TJAN, SummerStudent, and J. BEDNAR, Technologist, are with Physical MetallurgyResearchLaboratories. CANMET. Department of Energy, Mines, and Resources, 552 Booth Street, Ottawa, ON, Canada. Manuscript submitted February 27, 1984. 1694--VOLUME16A,SEPTEMBER1985

Table I.

Analysis of Steels (Percent)

Type of AISI Steel Constituent C Mn P (Max) S (Max) Si Mo Fe

1062 0.64 1.03 0.02 0.02 --98.29

4037 0.40 0.76 0.02 0.02 0.31 0.26 98.23

Each steel pin was cut into three pieces which were cleaned in methanol with ultrasonic agitation for five seconds, dried in a stream of air, and weighed. One piece was analyzed directly to yield a value for the inital hydrogen content. The remaining two pieces were washed with distilled water and immersed in the acid mixture (NAP) for thirty minutes or until the evolution of gas bubbles had stopped. They were then washed again in distilled water and methanol, dried, and analyzed for hydrogen. The certificate of analysis for the steel ball obtained from Alpha Resources stated that the samples contained 1.9 +0.3 weight ppm of hydrogen. Twenty standards were analyzed over a period of a few weeks and an average value of 1.80 -+ 0.13 weight ppm obtained (one sigma limits). Analysis of type AISI 4037 steel samples before and after treatment with the NAP solution gave the results presented in Table II. Initial hydrogen content of the cut samples varied from 1.64 to 0.48 weight ppm and the residual hydrogen content of the samples after treatment with NAP solution gave a range of values between 0.14 to 0.54 weight ppm with an average residual/hydrogen content of 0.30 +- 0.11 weight ppm. Analysis of AISI 1062 steel samples for hydrogen content before and after treatment with the NAP solution yielded the results presented in Table III. Initial hydrogen content

Table II.

Analysis of Type 4037 Steel for Hydrogen

Weight (ppm Hydrogen) Weight (g)

Before Treatment

After Treatment

3.04 3.21 3.44 3.33 3.34 3.38 3.16 3.22 3.16 3.34 3.21 3.00 2.84 3.22 3.23 3.51 3.31 3.35 3.24 _+0.16 Average

0.64 0.60 0.48 0.91 0.83 0.78 1.35 0.76 1.64 0.87 1.23 0.89 0.59 0.95 1.30 1.16 1.12 0.98 0.949 +0.304

0.17 0.14 0.19 0.29 0.38 0.19 0.44 0.38 0.37 0.30 0.22 0.27 0.20 0.36 0.38 0.32 0.33 0.54 0.304 +0.106

METALLURGICALTRANSACTIONSA

Table III.

Analysis of Type 1062 Steel for Hydrogen

Weight (g) 2.48 2.15 2.13 2.41 2.12 2.22 2.70 2.57 3.03 2.49 2.49 2.59 2.69 3.00 2.56 2.80 2.54 2.72 2.79 2.67 2.60 Average 2.56 +0.26

Weight (ppm Hydrogen) Before Treatment After Treatment 0.46 0.44 0.40 0.47 0.43 0.70 0.91 0.79 1.26 0.80 0.65 1.14 0.89 0.69 0.64 0.76 0.80 1.03 1.55 0.79 0.64 0.773 -+0.291

0.32 0.34 0.40 0.47 0.29 0.40 0.45 0.43 0.59 0.29 0.47 0.47 0.38 0.45 0.32 0.59 0.40 0.57 0.64 0.59 0.54 0.442 -+0.105

average residual hydrogen value was found to be 0.45 -+ 0.11 weight ppm NAP solution treatment of 4037 and 1062 steel samples resulted in removal of 70 and 4