土壤/岩石中有机碳含量分析检测方案(红外水份测定)

LECO Corporation |3000 Lakeview Avenue| St. Joseph， MI 49085|800-292-6141| Phone： 269-985-5496info@leco.com·www.leco.com| ISO-9001：2008 HQ-Q-994| LECO is a registered trademark of LECO Corporation.LCRM = LECO Certified Reference Material， LRM = LECO Reference Material and are registered trademarks of LECO Corporation.Form No.203-821-5431/18—REV1C 2018 LECO Corporation LECO Corporation； Saint Joseph， Michigan USA Instrument： RC612 Series Introduction Total Organic Carbon (TOC) in soil， rock， and shale is acommon analysis used for determining locations ofnatural hydrocarbon fossil fuel deposits， quality controlof raw building materials， and assessment of soilquality in agriculture. Direct measurement of TOC isdifficult due to the unique properties of soil， rock andshale and must be performed using either an aciddigestion or temperature dependent differentiationmethod. The acid digestion method utilizes aninorganic non-oxidizing acid like hydrochloric acid，which is not strong enough to effect the organiccarbon， to digest the carbonates present in the sampleto carbon dioxide gas， leaving the TOC intact. Thedetermination is then calculated by difference (TOC =Total Carbon-TIC). The temperature-dependentmethod requires no sample pretreatment and noadditional sample preparation， removing hazardouschemicals and time consuming acid digestions from theprocess. With the assumption that organic speciesdecompose to CO， between 150 ℃ to 450℃， and inorganic species below 1000 C， heating to thesespecific temperatures in an oxidizing environmentallows differentiation of the TOC from the TotalInorganic Carbon (TIC). The LECO RC612， with its variable ramp furnace， widerange carbon detection range and simultaneous carbonand moisture determination， is optimized for thetemperature differentiation analysis of forms of carbonin soil， rock and shale. The following application noteoutlines the instrument parameters and procedure fortemperature dependent carbon determination with theRC612. Accessories 781-335 Quartz Crucibles or 625-505-430 NickelBoats. Method Parameters： TOC Analysis Analysis Parameters Carrier Gas： Oxygen Purge Flow： 3.00 Ipm Analysis Flow： 0.75 Ipm Catalyst Heater Temp： 850 °C Afterburner Temp： 850℃ Temperature-Dependent Determinationof Total Organic Carbon (TOC) inSoil， Rock， and Shale Element Parameters Carbon Water Analyze： Yes Conversion Factor： 1.00 No1.00 Significant Digits： 5 5 Carbon Range： Auto Switch Level to High Cell： 37500 Switch Level to Low Cell： 35000 IR Baseline Time： 2 seconds Endline Time： 2 seconds Procedure 1. Prepare the instrument as outlined in the operator'sinstruction manual. 2.CDetermine Blank.Note： 781-335 Quartz Crucibles and 625-505-430 NickelCrucibles， should be pre-baked at 1100℃， to remove anyresidual carbon， and cooled in a desiccator until time ofanalysis. Handle the crucibles with clean tongs only. a. Enter 1.0000 g mass into Sample Login (F3) usingBlank as the sample name， select the number ofreplicates， "TOC Analysis" as the Method， and"Synthetic Carbon Calibration" as the FurnaceStep Method (parameters noted above). b. Place a "clean" crucible on the shelf directly infront of the closed combustion tube door， or intothe appropriate autoloader location， and initiatethe analysis sequence (F5). c. When the load sample message appears， select"Ok" in the message box，open the door， loadthe crucible into the combustion tube until itreaches the sample stop， remove the samplepuller， and close the door. d. When analysis is complete， remove the crucibleand close the combustion tube door. e. RFepeat steps 2a through 2d a minimum ofthree times. f.Set the blank following the procedure outlinedin the operator's instruction manual. 3.Calibration. a. Weigh selected reference material into a "clean"crucible. b.EEnter mass and sample identification intoSample Login (F3)， select "TOC Analysis" as theMethod， and "Synthetic Carbon Calibration" asthe Furnace Step Method (parameters notedabove). c. Place the crucible， containing the sample， onthe shelf directly in front of the closedcombustion tube door， or into the appropriateautoloader location， and initiate the analysissequence (F5). d. When the load sample message appears， select"Ok" in the message box， open the door， loadthe crucible into the combustion tube until itreaches the sample stop， remove the samplepuller， and close the door. Method Equation Parameters Equation Name Equation Formula Organic Carbon % @PeakCO2("Organic") Inorganic Carbon %@PeakCO2("Inorganic") e. When analysis is complete， remove the crucible andclose the combustion tube door. f. Repeat steps 3a through 3e a minimum of three timesfor each reference material used. g.Calibrate the instrument using single standard curvefollowing the procedure outlined in the operator’sinstruction manual. h. Verify the calibration by analyzing a referencematerial， different than the material used forcalibration， following steps 3a through 3e. 4.DDetermine Sample Blank. a. Enter 1.0000 g mass into Sample Login (F3) usingBlank as the sample name， select the number ofreplicates，"TOC Analysis" as the Method， and "TOCSample Analysis" as the Furnace Step Method(parameters noted above). b. Analyze Blank following steps 2b through 2da minimum of three times. c. Set the blank following the procedure outlined in theoperator's instruction manual. 5. AAnalyze Samples. a. Weigh sample into a "clean" crucible. b. Enter mass and sample identification into SampleLogin (F3)， select "TOC Analysis" as the Method， and"TOC Sample Analysis" as the Furnace Step Method(parameters noted above). c. Analyze the sample following steps 3c through 3eoutlined above. Typical Results )Organic Carbon (%) Inorganic Carbon (%) *Results reported on a dry basis. Low carbon calibration was performed utilizing a single standard force through origincalibration using LECO 502-696 1% Synthetic Carbon. High carbon calibration was performed utilizing a linear， full regressioncalibration using LECO 502-905 5% Synthetic Carbon and LECO 502-902 Calcium Carbonate. coo 力可RC612多相碳水分析仪，可以直接检测土壤和岩石中有机碳和无机碳含量，水分含量，表面碳水含量等。利用程序升温电阻炉和释放峰型可区分有机碳无机碳，具体方法见附件：