820 TOC分析仪器标准操作规程.pdf

Standard Operating ProcedureTitle:Operation and Calibration of Sievers 820 TOC Analyser_C.All rights reservedUnauthorized copying,publishing,transmission and distribution of any part of the content by electronicmeans are strictly prohibited.Page 2 of 17Table of Contents1.25 ppm IC as Sodium Carbonate-standard preparation procedure22.25 ppm TOC as KHP standard preparation procedure33.Calibration Procedure44.Performing Calibration-Prepare the following Calibration Protocol file using the Sievers program65.System Suitability Procedure86.Preparation of 500 ppb Benzoquinone standard97.System Suitability Analysis Procedure108.Routine Analysis119.Routine Maintenance1210.Summary of Changes12Preparation of Calibration Standards1.25 ppm IC as Sodium Carbonate-standard preparation procedureMaterials and Equipment:Materials:Sodium Carbonate anhydrous,Na2CO3 Analytical Reagent Grade(Mol wt.105.99 g/mol)Para filmEquipment:Milli-Q water100mL volumetric flask,Class A50mL volumetric pipette,Class A1 L volumetric flask,Class AProcedure:1.1.Obtain required glassware and thoroughly rinse 5 times with Milli-Q water.Note:For Calibration solutions dedicated glassware must be used,therefore use onlyglassware identified for the standard being prepared.Ensure all pipettes are cleaned andthoroughly rinsed with Milli-Q water.1.2.Obtain an“Inorganic Carbon Standard Worksheet”(Form 615).1.2.1.Record the current date and name of preparer in line 1.1.2.2.Record the lot number of the Na2CO3 in line 2.1.3.Dry approximately 1-2 grams Na2CO3 in an oven.1.3.1.Place the Na2CO3 into a clean beaker and place in a 110C oven for not less than 2hours.1.3.2.Transfer the Na2CO3 into a desiccator and allow the material to cool to roomtemperature.1.4.Weigh dried Na2CO3 for preparation of standard.1.4.1.Record the weight of the weigh boat in line 4 of the“Inorganic Carbon StandardWorksheet”(Form 615).1.4.2.Accurately weigh out approximately 0.441+0.0001g Na2CO3 in the weigh boat,andrecord the value in line 3 of the“Inorganic Carbon Standard Worksheet”.1.4.3.Calculate the difference in line 5 of the“Inorganic Carbon Standard Worksheet”.1.5.Transfer to 100mL volumetric flask.1.5.1.Dilute solid with Milli-Q water while it is in the weigh boat.1.5.2.Verify the water used in preparation contains less than 100 ppb TC and IC.Standard Operating ProcedureTitle:Operation and Calibration of Sievers 820 TOC Analyser_C.All rights reservedUnauthorized copying,publishing,transmission and distribution of any part of the content by electronicmeans are strictly prohibited.Page 4 of 172.3.1.Place the KHP into a clean beaker and place in a 110C oven for not less than 2hours.2.3.2.Transfer the KHP into a desiccator and allow the material to cool to roomtemperature.2.4.Weigh dried KHP for preparation of standard.2.4.1.Record the weight of the weigh boat in line 4 of the“Organic Carbon StandardWorksheet”.2.4.2.Weigh out approximately 0.425+0.0001g KHP in the weigh boat,and record thevalue in line 3 of the“Organic Carbon Standard Worksheet”.2.4.3.Calculate the difference in line 5 of the“Organic Carbon Standard Worksheet”.2.5.Transfer to 100mL volumetric flask2.5.1.Dilute solid with Milli-Q water while it is in the weigh boat2.5.2.Verify the water used in preparation contains less than 100 ppb TC and IC.2.5.3.Transfer the contents of the weigh boat into the 100mL volumetric flask.2.5.4.Using Milli-Q water,wash down the weigh boat,flask neck,and ground glass jointand allow the rinse water to flow into the 100mL volumetric flask.2.5.5.Add Milli-Q water until the 100mL volumetric flask is approximately 50%full.2.5.6.Ensure that the KHP is fully dissolved.2.6.Dilute the solution to 100mL.2.6.1.Add Milli-Q water to the 100mL volumetric flask to bring the total volume to 100mL2.6.2.Cover the flask with volumetric lid and than with the clean side of a 4 x 4 square ofPara film.2.6.3.Invert the flask not less than 3 times and mix well.2.7.Calculate the carbon concentration of the stock solutionconc.of stock TC std(ppm)=Weight of KHP(g)x 8 mol C/mol KHP x 12.01g C/mol x 1000 (0.1L)x(204.22 g/mol KHP)2.7.1.Record the result in line 6,Table 1 of the“Organic Carbon Standard Worksheet”.2.8.Prepare the dilute TC standard2.8.1.Rinse a 25mL pipette with approximately 20mL of stock solution and discard.2.8.2.Pipette 25mL of stock solution into a 2L volumetric flask.2.8.3.Dilute to 2L with Milli-Q water,washing down the neck and ground glass joint of the2L volumetric flask.2.8.4.Cover the flask with volumetric lid and than with a 4 x 4square of Para film.2.8.5.Invert the flask not less than three times and mix well.2.8.6.Calculate the final carbon content of the dilute solution.Conc.of dilute TC standard(ppm)=Conc.of stock(ppm)x 0.01252.8.7.Record the final concentration of the dilute standard in line 7,Table 2 of the“OrganicCarbon Standard Worksheet”.3.Calibration ProcedureMaterials and Equipment:25 ppm Inorganic Carbon standard(Sodium Carbonate Anhydrous)25 ppm Total Carbon standard(Potassium Acid Phthalate)“Calibration Worksheet for Autosampler Calibration”(Form 615).Powder-free glovesStandard Operating ProcedureTitle:Operation and Calibration of Sievers 820 TOC Analyser_C.All rights reservedUnauthorized copying,publishing,transmission and distribution of any part of the content by electronicmeans are strictly prohibited.Page 6 of 174.Performing Calibration-Prepare the following Calibration Protocol file usingthe Sievers programThe sampling schedule is as follows:SampleSampleNo.Acid Flow Rate No.Oxidiser Flow Rate(L/min)No.of Replicates/Sample(L/min)DI blank1,2,30.750.00425 ppm TC(KHP)4,5,60.752.50425 ppm IC(Na2CO3)7,8,90.750.004Cleanup(DI)10-.-.-Select Create New Protocol from the Files menu.Enter the protocol file name without an extension at the prompt.An empty protocol file will be displayed for editing.Highlight the protocol file window then use the button to zoom the window to full screen.Edit the protocol by typing in the following:No.Group NameSamp./groupRep./SampleAcid RateOxid.Rate1DI water blank140.750.00225 ppm TC(KHP)140.752.50325 ppm IC(Na2CO3)140.750.00The software will automatically add the cleanup vial to the Table when you save the protocol.Type over any defaults in the columns for each group.Check the table in the protocol program to ensure it is correct.Select Save Displayed Protocol from the Files menu.Use Save and return to menu to save the protocol.Use Save As _ and return to menu to select a new name or path.Use the button to zoom the windows to normal size.4.1.Prepare a water blank flaskFill 3 x 40mL vials with the same water used to prepare the 25 ppm standards.Label as“DIBlank”.4.2.Fill the sample vials and load in Autosampler4.2.1.Always use clean sample vials,caps,and septa and rinse the solution to beanalysed 3 times into the vial.4.2.2.Label each vial with the standard name,including the blanks and the cleanup vial.4.2.3.Obtain a standard or blank to be measured in the protocol.4.2.4.Fill three vials directly from the standard flask.4.2.5.Re-seal the standard flask.4.2.6.Repeat for each remaining standard.4.2.7.Fill one cleanup vial with Milli-Q water.4.2.8.Load the vials sequentially into the Autosampler according to the sampling schedule.4.2.9.Ensure that the cleanup vial is the last vial in the sequence.4.2.10.Using the index button on the left rear of the Autosampler,index the vials until thefirst blank vial is directly under the sampling needle.4.3.Run the protocol file from the Autosampler software4.3.1.Select the Run Current Protocol from the Start menu.Standard Operating ProcedureTitle:Operation and Calibration of Sievers 820 TOC Analyser_C.All rights reservedUnauthorized copying,publishing,transmission and distribution of any part of the content by electronicmeans are strictly prohibited.Page 9 of 17Para filmMilli-Q water1L volumetric flask,Class A500mL volumetric flask,Class A10.0mL volumetric pipette,Class AProcedure:5.1.1.Obtain required glassware and ensure it has been cleaned in the Laboratorydishwasher and thoroughly rinsed 5 times with Milli-Q Water.Note:For Calibration solutions dedicated glassware must be used,therefore useonly glassware identified for the standard being prepared.Ensure all pipettes arecleaned and thoroughly rinsed with Milli-Q water.5.1.2.Record relevant Sucrose information in the“500 ppb Sucrose Standard Worksheet”(Form 615)for Sucrose preparation.5.1.3.Prepare nominal 25,000 ppb stock standard solution.1.Dry the sucrose at 105C for 4 hours.Let it cool in a desiccator.2.Accurately weigh approximately 0.059 0.0001g sucrose for preparation of stockstandard solution and record in“500 ppb Sucrose Standard Worksheet”.3.Transfer to 1L volumetric flask and make up to volume using Milli-Q waterwashing down weigh boat and flask to ensure 100%transfer.Verify that waterused is low TOC i.e.less than 100ppb and prepare a blank sample of this water.5.1.4.Calculate the concentration of the stock as follows:conc.of stock(ppb C)=weight of sucrose(g)x carbon content x 1065.1.5.Prepare the dilute standard.1.Use standards as soon after preparation as possible.2.Using a 500mL volumetric flask,partially fill it with Milli-Q water.3.Using a 10mL volumetric pipette,pipette the stock solution into the partially filled500mL volumetric flask,mix and make up to 500mL.5.1.6.Calculate the dilute standard concentration:conc.of dilute standard(ppb C)=conc.of stock(ppb C)505.1.7.Record the calculated concentration on line 8 of the“500 ppb Sucrose StandardWorksheet”.6.Preparation of 500 ppb Benzoquinone standardMaterials and Equipment1,4-Benzoquinone(Mol wt.108.10g/mol)Para filmMilli-Q waterTwo x 1L volumetric flasks,Class A10.0mL volumetric pipette,Class AProcedure6.1.Obtain required glassware and ensure it has been cleaned in the Laboratory dishwasher andthoroughly rinsed 5 times with Milli-Q Water.Note:For Calibration solutions dedicated glassware must be used therefore use onlyglassware identified for the standard being prepared.Ensure all pipettes are cleaned andthoroughly rinsed with Milli-Q Water.6.2.Record the relevant Benzoquinone information in the“500 ppb Benzoquinone StandardWorksheet”(Form 615)for 500 ppb Benzoquinone preparation.6.3.Prepare nominal 50,000 ppb stock standard solution.Standard Operating ProcedureTitle:Operation and Calibration of Sievers 820 TOC Analyser_C.All rights reservedUnauthorized copying,publishing,transmission and distribution of any part of the content by electronicmeans are strictly prohibited.Page 12 of 179.Routine MaintenanceItemPartNo.ReplacementScheduleNotes60 m filterelementMRF94401Every 3months or asrequiredIn-line filter applies only to on-line measurement.The filterelement replacement schedule depends on the level ofparticulates in the water being sampled.A clogged filtermay be detected by decreasing pressure on the sampleinlet pressure gauge,or by a decrease in flow from thesample bypass waste line.At a minimum,the filter statusshould be checked every 3 months on the same scheduleas replacement of the oxidiser reagent reservoir.Continued15%AmmoniumPersulfateReagentreservoirAPF80020Every 3monthsBecause of loss of activity of the oxidiser over time,the 3-month replacement schedule is independent of whether theinstrument is used for measurements,or is idle.Thelifetime of the oxidiser reagent is tracked by the instrumentwith date/time information in non-volatile RAM,and Error 14is reported when the lifetime has been exceeded.Error 13is reported when the amount of oxidiser available is lessthan 10 percent of the full reservoir value.6MPhosphoricAcid ReagentreservoirAPF80010as requiredReplacement schedule of the acid reservoir,sample pumptubing,and ultraviolet lamp depends on the total time theinstrument is on and/or making measurements.Lifetime ofthese items is tracked by the instrument with date/timeinformation in non-volatile RAM,and specific errors arereported when the lifetime has been exceeded for any item.Error 12 is reported when the amount of acid available isless than 10 percent of the full reservoir value.SamplePump TubingassemblyATU00644Every 12monthsError 16 is reported when the age of the sample pumptubing has exceeded the planned life expectancy.UltravioletLampassemblyEMI00800Every 6monthsError 15 is reported when the age of the UV lamp hasexceeded the planned life expectancy.Refill DIWaterreservoirn/aEvery 2-12weeks asrequiredSmall amounts of DI water can be lost from the DI reservoirover time.The level of water in the DI reservoir should beperiodically checked and the reservoir refilled if necessary.The procedure for checking and filling the reservoir isdetailed in the Operation and Service Manual.The requiredinspection schedule depends on the mode of measurement.For on-line use,check the reservoir every 3 months,on thesame schedule as replacement of the oxidiser reagentreservoir.For container sampling or Autosampler use,check the reservoir every 2 weeks.Detailed procedures to replace all maintenance items and perform other maintenance procedures are givenin Chapter 11 of the Operation and Service Manual.10.Summary of ChangesVersion#Revision HistoryMICLAB 115NewEnd of ProcedureForm 615Issue date:Toc Analyser Calibration Worksheets(Ref.MICLAB 115)_C.All rights reservedUnauthorized copying,publishing,transmission and distribution of any part of the content by electronicmeans are strictly prohibited.Page 15 of 17Calculation of Calibration ConstantsCurrent TC calibration constant=TCcal,oldNew TC calibration constant=TCcal,old TCadj,TC=TCcal,newTCave,TCCurrent IC calibration constant=ICcal,oldNew IC calibration constant=ICcal,old TCadj,TC TCave,IC=ICcal,newTCave,TCICave,ICVerification of CalibrationAverage TC of 3rd TC(KHP)standard=TCave,chk,TCAverage TC of 3rd IC(Na2CO3)standard=TCave,chk,ICAverage IC of 3rd IC(Na2CO3)standard=ICave,chk,ICNew TCadj,TC=TC(KHP)std+average TC 3rd DI Blank=TC Std%difference=(New TCadj,TC-TCave,chk,TC)x 100 =New TCadj,TC(NMT 3%)IC Std%difference=(TCave,chk,IC-ICave,chk,IC)x 100=TCave,chk,IC(NMT 3%)500 ppb Sucrose Standard WorksheetDate,Name of Preparerline 1Lot No.of Sucrose usedline 2Carbon Assay(%value/100)line 3nominal 0.421Gross Weight(Sucrose+Boat)line 4Tare Weight of Weigh Boatline 5