钢中扩散氢和残余氢检测方案(氧氮分析仪)

LECO Corporation3000 Lakeview Avenue·St. Joseph， MI 49085·Phone： 800-292-6141·Fax： 269-982-8977info@leco.com·www.leco.com·ISO-9001：2000·No. FM 24045· LECO is a registered trademark of LECO Corporation.Form No. 203-821-37610/09—REV0C 2009 LECO Corporation Hydrogen in Steel Samples LBCo LECO Corporation； Saint Joseph， Michigan USA Instrument： DH603 Introduction The determination of hydrogen in steel is a time-testedquality control parameter. Excess amounts of hydrogenpresent during the solidification and cooling process hasan adverse effect on both physical and mechanicalparameters including embrittlement， porosity， cracking，and flaking. This application poses a unique challenge due to therapid diffusion of hydrogen from steel during sampling.To accommodate this， a vacuum pin tube sampler isemployed that traps the diffusible hydrogen in an outerenclosure and retains the solidified sample (pin) forresidual hydrogen analysis and correlation. The DH603 allows the analyst to determine the amountof hydrogen present in its molten form and aftersolidification and cooling by incorporating an optionalvacuum pin tube sample piercer for diffusible hydrogendetermination and a hot extraction furnace for residualhydrogen determination. AccessoriesTweezersSample SizeNominal 5 g Furnace Temp500℃ standby and 1100℃ Analyze System Parameters Conservation Timeout (minutes) 180Pre-Analysis Purge Time (seconds)Nominal Mass for BlanksAuto Increment Sample Name DisableStandby Flow 0.12 IpmFurnace Standby Temperature 500℃Ambient Temperature DisableFurnace Start Up Temperature 1000COven Temperature 50Enable Piercer Unit Enable(requires software restart when changed)Diffusible Purge Time (seconds) 15 Furnace Step Method Gas Dose Hold Gas DoseDiffusible Hydrogen Temperature 1100℃Diffusible Hydrogen Hold DiffusibleResidual Hydrogen Furnace StepsName 7Target RampHold Estimated TimeStart 1100 N/A Residual300-1000 Procedure 1. Prepare instrument for operation as outlined in theoperator's instruction manual. 2Determine Sample Blank. a. Enter 5.0 g mass into Sample Login (F3) using Blankas the sample name， select Residual as type ofanalysis. b. Start analysis by initiating Analyze (F5) (Reactiontube door closed). c. When User Loading Sample message appears in the lower left part of the screen and LoadSample display box appears on center of screen，click OK or press the enter key. Openreaction tube door and slide push rod into tubeuntil it reaches the boat stop； remove push rod，close door. d. When analysis is complete， repeat steps 2athrough 2c a minimum of three times. e. Set the blank following the procedure outlinedin the operator's instruction manual. c.The diffusible analysis will begin automatically whenthe piercing unit senses a sample. The hydrogenconcentration will be displayed in the diffusiblewindow. 3.).Calibrate/Drift Correct. d. When finished， the piercing unit will release thesampler. a. Weigh ~5.0 g of the 502-060 calibrationsample； enter mass and sample identificationinto Sample Login (F3)， select Residual as typeof analysis. e. Extract the pin sample from the metal sampler tubeby cutting the outer tubing 3/8 inch from the collarwith a tube cutter or other suitable device. Removeand discard the outer tube. b. Start analysis by initiating Analyze (F5) (Reactiontube door closed). C.When User Loading Sample message appearsin the lower left part of the screen and LoadSample display box appears on center of screen，click OK or press the enter key.Openreaction tube door and load sample intofurnace， using push rod to slide sample intotube until it reaches the boat stop； remove pushrod， close door. f.Cut the pin as close to the base collar as possibleusing a hacksaw or bolt cutter. Avoid contaminatingthe sample； the device used for cutting should befree from foreign material such as paint. Do notheat the sample while cutting； this can drivehydrogen from the sample. d. When analysis is complete， remove sampleusing the push rod and close door. e. Repeat steps 3a through 3d a minimum ofthree times. g.When User Loading Sample message appears in thelower left part of the screen and Load Sampledisplay box appears on center of screen， clickOK or press the Enter key. Open reaction tube doorand load sample into furnace， using push rod toslide sample into tube until it reaches the boat stop；remove push rod， close door. f.Calibrate or Drift Correct the instrumentfollowing the procedure outlined in theoperator's instruction manual (Single StandardCalibration Recommended). h. When analysis is complete， remove sample usingthe push rod and close door. 5. Analyze Residual (only) Samples. 4.Analyze Diffusible/Residual Samples. a. Weigh~5.0 g of the sample； enter mass andsample identification into Sample Login (F3)， selectResidual type of analysis. a. Enter 5.0 g mass and sample identification intoSample Login (F3) as the sample name， selectBoth as type of analysis. b. Proceed as directed in steps 3b through 3d. b. Push the steel sampler tube firmly into the piercerunit and hold it until the piercer seals clamp the tube. Typical Results Sample Mass g Diffusible H ppm Residual H ppm Total H ppm Steel Sampler 5.000 7.31 3.05 10.36 LECO 903-9A3-184 5.000 7.79 3.13 10.92 ±0.3 4.9981 6.01 6.01 5.0034 6.14 6.14 4.9960 6.04 6.04 X= 5.96 5.96 S= 0.16 0.16 502-061 4.9925 2.15 2.15 @ 2.19 ppm H 5.0062 2.08 2.08 ±0.35 4.9891 2.14 2.14 4.9966 2.20 2.20 5.0269 2.18 2.18 X= 2.15 2.15 S= 0.05 0.05 8 利用力可LECO DH603氢分析仪分析钢中扩散氢和残余氢含量，具体获得的结果如下：详细方法见附件：