Some Mass Spectrometry Consultant 5354 Thunderbird Court very good examples were provided, but they often lacked clear explanation of fragmentation mechanisms. *II, *III Unusual problems found with the data that have been described in Section II, "Sample Management," or Section III, "Method Analyses." The . the performance mix, a solution of DFTPP, endrin, and 4,4'-DDT at 5 g/mL in iso-octane (Thermo Scientic PN 60181-311). A mass spectrometer and a technique for operating it involve setting an operating parameter that influences a rate of flow of electrons from an electron source into an ion volume so that ions produced from a material in the ion volume in response to electrons satisfy an ion production target, performing a plurality of analytical runs using the mass spectrometer with the electron source while . If M/Z 51 is below 30%, turn up Resolution Low. Site is running on IP address 213.244.86.35, host name 213.244.86.35 ( Palestine ) ping response time 4ms Excellent ping. Performance criteria are verified with a single click. Each NPS was analyzed 100 times per instrument; 10 replicates per tune repeated under 10 different tunes. Results showed that passing a DFTPP tune check was not correlated with reduced RA variation. Correct mass assignments. I think something was unchecked or checked but I can't find it. Antioch, California, USA ods@compuserve . It does this by direct thermal transfer of heat from the transfer line tip to the MSD source and source supporting housing. This option sends the DFTPP target tune report directly to the printer (see Appendix 2). The system must . Refer to the Agilent 5977B Series MSD Operating Manual. Figure 7 - Spectral Tilt evaluation (m/z = 51 and m/z = 442) at 3.1 Hz Refer to specific cleaning procedures in your MSD Hardware Manual or MSD Maintenance and Troubleshooting Manual. Relative. Hi Dave, What instrument model are you using? Use a temperature above the boiling point of the solvent but below the limit of the column. T Presumed contamination from trip blank. The automatic DFTPP target tune, as required by some government methods, can also be used. DFTPP every 12-hour period (reference ASP for tune values) ICAL %RSD is variable (< 20 and 40%); depends on analyte ICV RRF is variable (< 25 and 40%); depends on analyte CCV %D is variable (< 25 and 40%); depends on analyte [4 allowed failures or approximately 6% of analyte list] MB is < RL or Not detected If M/Z 365 is over 2.5% it would be a good idea to lower the Electrometer zero somewhat. toxicology laboratories performing common drug detection might include 69, 131, 219, 264, 414, and 501 when using PFTBA tune gas. Troubleshooting and Maintenance Manual 3 Contents 1 Introduction Abbreviations Used 8 The 7200 Accurate-Mass Quadrupole Time-of-Flight GC/MS . Scan 1rate Up to 20,000 u/s (Extraction tune only), 12,500u/sec SIM 60 ions 100 groups Pumping system (Helium) 65 L/s Diffusion Pump and 255 L/s Turbo Pump with 2.5 m 3/hr mechanical pump Maximum recommended analytical gas flow 1.5 mL/ i n(D f us o P p) 4 mL/ in (T urbo P p) Recommended max imum sustained column flow to MS 2 3 mL/ n(D f us o . M-525.2-TS-A. Step 1: Power on the PC. 3.2. The auto tuning algorithm sets the parameters to maximize the mid-range and high-end sensitivity (i.e., high abundances of ions 219 and 502). This requires the operator to tune the mass spectrometer using PFTBA (the tuning fluid internal to the MSD) as a reference compound to adjust the voltages of the source to We suggest doing it for both filaments. The best source to fix your HP/Agilent and Thermo Finnigan GC/LC/MS/MS problems by the next day. The diversity of the analytes in this method, along with specific DFTPP tune requirements, presents particular chal- . Figure 1 displays ENVIRONMENTAL application note SEMI-VOLATILE ORGANICS IN DRINKING WATER DFTPP is an active compound and reacts with the injector, the column, etc. c) Pass the eluates through the Na 2 SO 4 bed. The 8270D tune evaluation criteria are NOT the default DFTPP tune evaluation criteria in EnviroQuant. Sample extracts are now ready for analysis. Venting the MSD 57 To View MSD Temperature and Vacuum in Manual Tune 58 To Set Monitors for MSD Temperature and Vacuum Status 59 To Set Analyzer Temperatures from the Instrument Control View 61 To Set the GC/MSD Interface Temperature from MassHunter 63 To Monitor High Vacuum Pressure 64 After explaining the fundamentals, it discusses optimizing, tuning, using, and maintaining GC/MS equipment; explores advances in miniaturized and field-portable GC/MS systems and microfluidic components; and more. sample preparation and GC troubleshooting, method development tips and tricks, and an overview of popular environmental, forensics, food safety and POP's applications. 4. As a result the transfer line is normally kept at between 250C and 290C in order to maintain a source temperature of 180C. The Method 8270C tune criteria are: m/z criterion. If you are having trouble passing BFB/DFTPP and your system does not pass Autotune with flying colors, you should take corrective action as soon as possible. Alternatively, sonicate for 15 minutes in a water bath sonicator. The extent of matrix interferences will vary considerably from source to source, depending upon the nature and diversity of the industrial complex or Method 525.2 - Tuning Standard Mix. Troubleshooting the MSD is included to help you diagnose problems. Tune checks include verification of mass assignments and mass resolution, which are important considerations for quantitative analysis under all of these conditions. less than 2% of m/z 69. . The slopes are very different. + False positive - reported compound was . Note: This needs to be run and pass every 12 hours before sample runs. No. DFTPP Tune (DFTPP.U) BFB Tune (BFB.U) Tune Wizard. must pass using a specific"Tune Mix." This mix contains a mass spectrometer tuning compound (DFTPP) and a collection of active compounds: PCP (an acid), benzidine (a base), and DDT (a reactive pesticide). Does it work now? Troubleshooting DFTPP Tuning Issues DFTPP is the compound specified by the EPA to be used to verify that mass spectrometer voltages are set correctly. Fax (510) 477-8938. The tune report generated is invaluable because it indicates how well the instrument is operating, and is an essential tool when troubleshooting is required. A B Figure 1. eWorkflows for environmental GC-MS analysis Figure 2. problems. The tune of the MS is a check of the MS system only. Dftp.gov.ps Dftp.gov.ps . 4.2.3 DFTPP Tune Check. For example, decafluorotriphenyl phosphine (referred to as "DFTPP") is a common internal tuning standard used to validate appropriate instrument tuning. And what revision of software are you using for Acquisition. For such problems, the stationary phase is coated on polytetrafluoroethylene or polychloro-trifluoroethylene support material. Chromeleon CDS solves these problems using built-in eWorkflows, a set of rules capturing all the unique aspects of a chromatography workflow, guiding the users through a minimum number of choices needed to create a . III. Figure 1: Example autotune report. This method outlines the analysis of volatile organic compounds in a variety of solid waste matrices including vari- ous air sampling trapping media, ground and . Keep the report in the binder for the instrument performance. This tune uses the target relative abundances provided in the macro file DFTPP.TGT: PFTBA ion DFTPP ion Rel. Lastly, daily maintenance should include evaluation of the chromatographic and . The mass spectrometer was tuned automatically using Autotune Tuning software to meet DFTPP tuning criteria. For a one-day course, too much time was spent on discussion of the ionization tech- Reviewed by O. David Sparkman niques and the different types of m/z analyzers. Make sure your audio driver is up to date and update it if needed. 4.0 INTERFERENCES AND POTENTIAL PROBLEMS 5.0 EQUIPMENT/APPARATUS 6.0 REAGENTS 7.0 PROCEDURES 7.1 Sample Preparation 7.2 GC/MS Chromatographic Conditions 7.3 DFTPP Tune 7.4 PCB Congener Retention Time Windows 7.5 Initial Calibration 7.6 Continuing Calibration 7.7 Sample Analysis 8.0 CALCULATIONS 9.0 QUALITY ASSURANCE/QUALITY CONTROL 10.0 DATA . This stand-alone capillary detector was specifically designed to be used with the HP 6890 Gas Chromatograph series. 2 General Troubleshooting. 4 The foreline pump may be located on the floor, on the lab bench next to or behind the MSD, or under the analyzer chamber at the back of the MSD. We have special price for dealers. The TIC for the mid-level standard is shown in Figure 1. b) Insert the collection rack with 40-60 mL glass vials into the manifold to collect the dried eluates. . Accuracy DFTPP Tune 1 every 12 hours CAS SOP SOC8270CPAH Table 4 or 4A tune criteria, depending on instrument used for analysis Performinstrumentmaintenance; reanalyze until acceptable Analyst Accuracy Initial Calibration (ICAL) Initially and when CCV fails Lowest-level standard in calibration must be at or below the PQL; minimum 5-level . Under DFTPP tuning, the fluctuations in the abundance of m / z = 69, 219, and 502 were 6.5%, 8.2%, and 11.0%, respectively. T Presumed contamination as indicated by the trip blank results. Attn: our new addres. Air and Water Check Tune Evaluation Execute MS ON MS OFF Profile scan Repeat profile Detailed profile Ramp Lenses Matrix. 3. To perform this tilt evaluation for the 3.1 Hz scan rate, we created an X,Y scatter plot, with the responses for m/z = 51 and m/z = 442 entered for each of the three scans used for the DFTPP evaluation (Figure 7). Apply R to all results for all samples associated with the calibration. DFTPP tuning was performed to obtain uniform mass spectra using a DTFPP tune . The HP 5973 MSD system gives operators full control through a data system that features MSD compatible data analysis . E.g. The first step is to make sure that your software is configured to automatically switch between alternate base peaks ( Figure 2 - Edit DFTPP tune evaluation criteria interface). Increasing the zero will increase system noise and increase the 365. The ultra-large aperture drawout lens was used to maintain linearity across the wide calibration range of .01-10. ppm. We are pleased to offer you more choices for your lab analysis with the addition of some of the most popular solvents and reagents. The reviewer determined that these chromatographic problems did not affect identification of pesticides in . There are several parameters that need to be examined in this autotune report: 1. UJ (all non-detects) P II. The HP 5973 MSD system gives operators full control through a data system that features Hewlett-Packard MSD . M Tuning (BFB or DFTPP) was noncompliant. A tuning standard ensures that ion ratios (relative ion abundances) across a range of masses are detected accurately by the mass spectrometer 10. Step 3: On your computer, go to the Bluetooth settings and select "Add Bluetooth" or other devices. The HP Agilent 5973 is a high performing mass selective detector that offers unmatched reliability for every use. Dry all cleaned metal parts in the GC oven before reassembling and reinstalling them. Data was acquired using Xcalibur instrument control The Pest/PCB analyses met instrument performance guidelines although several pesticides had overlapping retention time windows on one or both columns. Seven points are being used for initial calibration before dropping lower and/or higher end standard (s). Let window open and save it. Initial Calibration and Initial Calibration Verification An initial calibration was performed as required by the method. In order for the system to work, you must have a calibration flashed to your . A zero that is too high will cause too much disk space to be used. Each NPS was analyzed 100 times per instrument; 10 replicates per tune repeated under 10 different tunes.