1 / /12/16 Perkin Elmer 2400II CHN Analyzer He, 1.4 kgf; O2, 1.0 kgf; Air, 4.0 kgf 2 AIR He He O2 1) TIME ENTER (9:10:00 ) 2) DATE
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1 1 / 1 Perkin Elmer 2400II CHN Analyzer He, 1.4 kgf; O2, 1.0 kgf; Air, 4.0 kgf 2 AIR He HeO2 1) TIME ENTER (9:10:00 ) 2) DATE ENTER ( ) 3) OPERATOR ID XXX ENTER ( 4) Fill Pressure ENTER ( 5) REDC COUNTER 175 ENTER ( 6) COMB COUNTER 968 ENTER ( Blank 7) VRCPT COUNTER 175 ENTER ( 8) COMBUST TEMP 950 ENTER ( ) REDC TEMP 640 ENTER ( 10) P. XXX TIME XXXXXX Check Pressure He 1.4 kgf Monitor1 & Monitor 2 Diagnostics[1 HARDWARE 2 Gas]2[1 LEAK TESTS 2 VALVE]1 [ENTER CODE ]2 ENTER LEAK TEST PASSED PASS mmhg 45 ENTER CODE 2 1= ; 2= ; 3= 11) [HELIUM? Y/N]Yes120 ENTER[OXYGEN? Y/N]Yes60 ENTER [Purge Gas] 12) [Parameters]12 ENTER1[Parameters] 13) [Parameters]24[ACCESS NO.?]2400 ENTER[PRINT LIST Y/N?]YES 14) [Parameters]91 CONSTANT1 OXYFIL2 (sec) ENTER ([Parameters]) p.7 15) ([Parameters]91 CONSTANT ) 2 COMB10 (sec) ENTER[Parameters] p.7 KFACTOR mg [Monitor]N5TCD
2 Blank Runs without O2, x35? Blank Runs with O2, x35? Single Run Mode Auto Run Mode CHN KFACTOR Run & Blank Run, x35? KFACTOR Runs, x3 Sample Runs, x10 KFACTOR Run, x1 Sample Runs, x10 KFACTOR Run, x1 Sample Runs, x10 KFACTOR Run, x1 Sample Runs, x10 KFACTOR Run, x / 2
3 Blank RunsKFACTOR RunsSample Runs 3 / 3
4 1. [Purge Gas][HELIUM? Y/N]Yes120 ENTER[OXYGEN? Y/N]Yes60 ENTER STANDBY ( ) 2. [Parmeters]202 OFF[Parameters] 3. [Single Run]1 BK[NUMBER OF RUNS?]3 ENTER[Single Run][Start] 4. Blank C30, H100, N [Single Run]1 BK[NUMBER OF RUNS?]1 ENTER[Single Run][Start] 7. [Parmeters]201 ON [Parameters] 8. [Single Run]1 BK[NUMBER OF RUNS?]3 ENTER[Single Run][Start] 9. Blank C30, H100, N [Single Run]1 BKNUMBER OF RUNS?1 ENTER[Single Run][Start] [Auto Run]4 RP1 RESET[RESET ALL? Y/N]Y 15. [AUTO RUN NO.1 1B 2K 3S]2[STANDARD S1 S2 S3 S4]1 16. [AUTO RUN NO.1 K1 WEIGHT _]2.123 ENTER 17. [Auto Run]START ( )[Auto Run] Auto Run 18. [AUTO RUN NO.2 1B 2K 3S]1 19. [AUTO RUN NO.3 1B 2K 3S]2[STANDARD S1 S2 S3 S4]1 20. [AUTO RUN NO.3 K1 WEIGHT _]1.976 ENTER 21. [AUTO RUN NO.4 1B 2K 3S]1 22. [AUTO RUN NO.5 1B 2K 3S]2[STANDARD S1 S2 S3 S4]1 23. [AUTO RUN NO.5 K1 WEIGHT _]2.043 ENTER 24. [AUTO RUN NO.6 1B 2K 3S]1[Auto Run] 25. No.1, No.3, No.5 No.X KC/KH/KN KC= ; KH= ; KN= KC0.15; KH3.75; HN No.5 No.X ( )[Auto Run] 28. [AUTO RUN NO.X 1B 2K 3S]2[STANDARD S1 S2 S3 S4]1 29. [AUTO RUN NO.X K1 WEIGHT _]1.976 ENTER X 30. [AUTO RUN NO. 1B 2K 3S]1[Auto Run] 31. [Auto Run] 32. [AUTO RUN NO.1B 2K 3S]2[STANDARD S1 S2 S3 S4]1 4 / 4
5 33. [AUTO RUN NO.K1 WEIGHT _]1.998 ENTER 34. [AUTO RUN NO. 1B 2K 3S]2[STANDARD S1 S2 S3 S4]1 35. [AUTO RUN NO. K1 WEIGHT _]1.958 ENTER 36. [AUTO RUN NO. 1B 2K 3S]2[STANDARD S1 S2 S3 S4]1 37. [AUTO RUN NO. K1 WEIGHT _]1.937 ENTER ============== Sample Runs =============== =================== Samples Kfactor Run 1 ================== [Auto Run][AUTO RUN NO.1B 2K 3S]3 40. [ID _ W]ID SA1 ENTER 41. [AUTO RUN NO.SA1 WEIGHT _]2.113 ENTER KFactor 44. KFactor Run 45. [Auto Run] STANDBY 48. [Auto Run][AUTO RUN NO. _90]( 89 ) [ ]11ENTER[11 ID SA1, WEIGHT 2.113]Parameters RUN [1 RESET 2 PR INFO, 3 PR RESULTS 4 RECALC]4 [1 BLANK 2 KFACTORS, 3 SAMPLE WEIGHT]2 [AUTO RUN, CARBON xx.xxx] KC xx.xxx ENTER KH KN KFactor ENTER [NUMBER OF RUNS? _] ENTER KFACTOR RUN Parameters+14 default 0.5 K 0.5 Paramters+2 K AVERAGE RESULTS AVERAGE RESULTS 49. KC, KH, KN 5 / 5
6 50. Found1, Found2, Found3 [Purge Gas]HELIUM? Y/NYes200 ENTEROXYGEN? Y/NNo200 [Parameters]7 ENTER[COMBUST TEMP 950]100 ENTER8 ENTER [REDUC TEMP 640]100 ENTER[Parameters] [Monitor]1 OFF () () () () [Monitor] [Monitor]NO1 [Monitor]NO2 [Monitor]NO3 [Monitor]NO4 mmhg [Monitor]NO5 ( 2.5 h ) ( ) [Monitor]YES6 [Monitor] TANDBY Parameters [Parameters]2 KFACTOR [Parameters]3S1-S4 C, 29.99; H, 11.66; N, % [Parameters]7 [Parameters]8 [Parameters]9 1 OXYFIL2 sec2 COMB10 sec 3 OXB1 4 OXB2 p.7 [Parameters]13 Default: 100 counts for C/H/N [Parameters]14KFACTOR Default: 0.5 % for KC/KH/KN 6 / 6
7 [Parameters]17 [Parameters]18 [Parameters]20 [Parameters]22 [Parameters]23 Parameters 2, 3 ( ) C=71.09, H=6.71, N=10.36 % ROM [Parameters]24 Parameters-9 Security Area OXYFIL= 2 sec OXB1 = 0 sec COMB = 30 sec OXB2 = 0 sec Parameters-9 Parameters-9 6 Oxygen ON [Oxygen ON]+[OXYFIL]= 4.5 sec extended from 10 sec into 30 sec on in order to enhance the complete combustion of compounds involving P atoms COMBUST+COMB=0.1+30=30.1 sec Extended Combustion COMB 30 sec 7 / 7
8 10.1 sec 30.1 p.10 Monitor [Parameters]27Monitor/Parameters/Diagnostics AUTO RUN Auto Run STANDBY Auto Run START AUTO RUN [Auto Run][AUTO RUN NO. _XX]XX Run ENTER[Parameters] [1 BK 2KF 3S 4RP] [Auto Run] [Diagnostics]1 ENTER 1 ROM [Diagnostics]Yes CE 2.5 h 2030 Blank Run, KFACTOR Run, Sample Run 8 / 8
9 Start Auto Run [Start] Auto Run [Start] Single Run Single Run Parameters+19 [INSTRUMENT UNSTABLE, START Y/N?] Yes No [Start] Standby [Auto Run] [Single Run] [Standby] [STANDBY? Y/N] [Yes] Auto Run [Start] Auto Run [Standby] [Start] p.1 (3)-10 NO2, CO2, H2O NO2 N2 N2, CO2, H2O 9 / 9
10 N2, CO2, H2O TCD Counts HR CR N 2 + CO 2 N 2 + CO 2 + H 2 O HR-CR CR-NR NR ZR Baseline T1 (s) T2 (s) N 2 NR-ZR T3 (s) T4 (s) 0 time (s) Presumably, this time corresponds to GSV (line 13th in Security Area Codes) Security Area p.7 (NR-ZR)(CR-N)(NH-ZC) KN, KC, KH, N, C, H KN= KC= (NR-ZR) KF-RUN - (NR-ZR) Blank-RUN 10.36x(Sample Weight mg)x10 (CR-NR) KF-RUN - (CR-NR) Blank-RUN 71.09x(Sample Weight mg)x10 KH= (HR-CR) KF-RUN - (HR-CR) Blank-RUN 6.71x(Sample Weight mg)x10 N (%)= (NR-ZR) KF-RUN - (NR-ZR) Blank-RUN KNx(Sample Weight mg)x10 C (%)= (CR-NR) KF-RUN - (CR-NR) Blank-RUN KCx(Sample Weight mg)x10 H (%)= (HR-CR) KF-RUN - (HR-CR) Blank-RUN KHx(Sample Weight mg)x10 (NR-ZR)Blank-RUN, (CR-NR)Blank-RUN, (NH-ZC)Blank-RUN NB, CB, HB 10 / 10
11 Fax: / 11
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