Shimadzu TOC-VCSN and SSM-5000A标准操作程序.pdf

California Department of Pesticide Regulation Environmental Monitoring Branch 1001 I Street,Sacramento CA 95814-2828 P.O.Box 4015,Sacramento CA 95812-4015 SOP Number:METH013.00 Previous SOP:NONE Page 1 of 14 STANDARD OPERATING PROCEDURE Sediment TOC analysis using Shimadzu TOC-VCSN and SSM-5000A KEY WORDS KEY WORDS Sediment,total organic carbon,inorganic carbon,acid,ceramic boat APPROVALSAPPROVALS APPROVED BY:Original signed by DATE:3/4/2016 _ _ Kean S.Goh,Ph.D.Environmental Monitoring Branch Manager I APPROVED BY:Original signed by DATE:2/29/2016 _ _ Michael P.Ensminger,Ph.D.Senior Environmental Scientist(Specialist)APPROVED BY:Original signed by DATE:3/4/2016 _ _ Chang-Sook Lee Peoples Environmental Monitoring Branch Quality Assurance Officer PREPARED BY:Original signed by DATE:2/29/2016 _ _ Korena L.Goodell Scientific Aide Environmental Monitoring Branch organization and personnel,such as management,senior scientist,quality assurance officer,project leader,etc.,are defined and discussed in SOP ADMN002.California Department of Pesticide Regulation SOP Number:METH013.00 Environmental Monitoring Branch Previous SOP:NONE 1001 I Street,Sacramento CA 95814-2828 Page 2 of 14 P.O.Box 4015,Sacramento CA 95812-4015 STANDARD OPERATING PROCEDURE Sediment TOC analysis using Shimadzu TOC-VCSN and SSM-5000A 1.0 INTRODUCTION 1.1 Purpose The Shimadzu TOC-V analyzer and the SSM-5000A(solid sample combustion unit)are used to measure total organic carbon in solid samples.1.2 Definitions Total Organic Carbon(TOC)is a measure of the amount of organic carbon after inorganic carbon has been removed.2.0 MATERIALS 2.1 TOC-VCSN analyzer 2.2 SSM-5000A solid combustion unit 2.3 Plastic weigh boats Medium size with spout recommended 2.4 Ceramic sediment boats Shimadzu part number 630-02679-00 2.5 Sediment sample(s)2.6 Fructose,a certified sediment standard,and sodium bicarbonate 2.7 Ceramic fiber Shimadzu part number 638-60074-00 2.8 TOC Certified water 25%.5.0 TESTING SAMPLES 5.1 As described in Section 4.1,weigh out sediment sample.Measure 50-150 mg of sediment per ceramic boat,dependent on expected carbon content.5.2 For QC,it is recommended to run three reps,with a CV of 10%.After the first ceramic boat has been removed from the injection port,refer back to the screen and press add injection(F1)to measure multiple reps of the same sample.5.3 Both TC and IC analysis can be selected for one sample.5.4 If necessary,the result of a rep can be removed by pressing the EXC(exclude)key.5.5 After TC analysis has been completed,refer back to the screen and press go to next analysis(F6)to change analysis type to IC.5.6 When TC and IC analysis are completed,press exit analysis(F6)to end the analysis.6.0 POWERING OFF TOC-VCSN AND SSM-5000A 6.1 On initial display California Department of Pesticide Regulation SOP Number:METH013.00 Environmental Monitoring Branch Previous SOP:NONE 1001 I Street,Sacramento CA 95814-2828 Page 13 of 14 P.O.Box 4015,Sacramento CA 95812-4015 STANDARD OPERATING PROCEDURE Sediment TOC analysis using Shimadzu TOC-VCSN and SSM-5000A 6.1.1 Press the F1(stand by option)key 6.1.2 Press F5(power off)key 6.1.3 Press F6(execute)key to turn off the TOC-VCSN machine.For automatic shutdown press yes(F6),this is a termination.6.1.4 After 30 minutes the TOC-VCSN automatically turns off.6.1.5 After the SSM-5000A machine has reached ambient temperature,turn off by pressing the switch on the side.6.1.6 Lastly,shut off the oxygen tank.7.0 CLEAN UP 7.1 Cleaning ceramic boats 7.1.1 When cool,dispose of dry materials in the trash bin and wet materials in the sink.7.1.2 Rinse the ceramic boats with tap water and brush off any debris.Scrub out inside of boat with a brush(as a toothbrush).Rinse boats with low TOC certified water.7.1.3 Carefully submerge the ceramic boats into a 3N HCl solution for 15min.7.1.4 Remove boats from HCl solution with long tweezers and rinse with TOC certified water.7.1.5 Invert boats on metal slotted tray to dry.7.1.6 When dry,briefly heat boats over the gas flame generated by a Bunsen burner.Heat with long tweezers to avoid burns.7.1.7 Place boats in TOC free container.7.2 Cleaning Tweezers and Spatulas 7.2.1 Rinse tools with tap water and scrub off any debris,then rinse with TOC certified water.California Department of Pesticide Regulation SOP Number:METH013.00 Environmental Monitoring Branch Previous SOP:NONE 1001 I Street,Sacramento CA 95814-2828 Page 14 of 14 P.O.Box 4015,Sacramento CA 95812-4015 STANDARD OPERATING PROCEDURE Sediment TOC analysis using Shimadzu TOC-VCSN and SSM-5000A 7.2.2 Let tools dry then heat the tips using the Bunsen burner.Heat with long tweezers to avoid burns.7.2.3.Place tools in a TOC free container.8.0 REMEDIAL ACTION IN CASE OF MALFUNCTION For minor problems,visit Shimadzus TOC Advisor at https:/ additional help contact a Shimadzu sales rep at http:/ SAFETY 9.1 Wear gloves for personal protection and to prevent sample contamination.9.2 Wear closed toe shoes when conducting TOC analysis.9.3 Wear safety glasses with side shields or goggles for eye protection when using phosphoric or hydrochloric acid.9.4 Ensure the oxygen tanks are secured to the wall.9.5 Do not touch hot components or open housing when unit is in use.10.0 REFERENCES DPR SOP METH011.00.Water TOC Analysis Using the Shimadzu TOC-VCSN and ASI-V Autosampler at http:/cdpr.ca.gov/docs/emon/pubs/sops/meth01100.pdf TOC Operating Conditions.2016.ProjectZZ at http:/ Total Organic Carbon Analysis for Sediment.https:/