View Actual EPA Method 332 (PDF File) - Columbia Analytical ...

More documents

Recommendations

Info

TABLE 2. METROHM-PEAK IC-MS OPERATING CONDITIONS* Ion Chromatograph Metrohm-Peak, Houston, TX Mobile Phase 30 mM NaOH/30% Methanol Guard and Separator Columns Metrohm ASUPP4/5 + ASUPP5-100, 100 mm X 4 mm Flow Rate 0.7 mL/min Suppressor Regenerant 60 mM nitric acid/10% Methanol, Rinse 10% Methanol Column Temperature 30 O C Injection Volume 100 µL Mass Spectrometer 1100 Series MSD Quad SL, Agilent Technologies, Wilmington, DE Low Mass Resolution 0.65 Capillary Voltage -2 kV Nitrogen Pressure 80 psi Fragmentor Voltage 150 V Drying Gas Temperature 320 o C Drying Gas Flow Rate 9 - 10 L/min Selected Ion Monitoring m/z 99, 101, 107 Mass Scan Range 0.1 amu Dwell Time Per Mass 0.25 sec *Instrumentation, when specified, does not constitute endorsement. Brand names are included for illustration only. <strong>332</strong>.0-34
TABLE 3. SAMPLE ANALYSIS BATCH Injection # Sample Description Acceptance Criteria Remedial Action 1 Mid-Level CCC 80 - 120 % recovery using Initial Calibration Instrument maintenance and recalibration. 2 MRL CCC 50 - 150% recovery Instrument maintenance to recover sensitivity and recalibration. 3 LRB MRL to highest CAL std 50 - 150% recovery 80 - 120% recovery Identify and correct source of problem. 5 . . 14 Field Samples 1 - 10 Pass RT, m/z 99/101 area count ratio, and IS area count QC criteria at concentrations >MRL concentration. If problem is due to sulfate, clean up sample using Ba form cartridge, otherwise report. 15 CCC (rotating concentrations) 16 LFSM of a field sample previously analyzed 17 Laboratory Duplicate or a LFSMD of field sample previously analyzed. Choose LFSMD if samples are low in perchlorate. 80 - 120% recovery using Initial Calibration for concentrations > MRL 50-150% recovery for concentrations < MRL At fortification concentrations > MRL concentration, 80- 120% recovery. At fortification concentrations < MRL, 50-150% of true value. RPD 2 X MRL RPD MRL Instrument maintenance and recalibration. <strong>332</strong>.0-35
Page 1 and 2: EPA Document #: EPA/600/R-05/049 ME
Page 3 and 4: atio and relative retention time ar
Page 5 and 6: and processed like a field sample (
Page 7 and 8: eluent strength or modifying the el
Page 9 and 10: 5.2 Pure ClO 4 - salts are classifi
Page 11 and 12: ate (>15 L/min), liquid nitrogen or
Page 13 and 14: 7.1.2 ACETONITRILE - ACN, CASRN 75-
Page 15 and 16: 7.2.3 CALIBRATION STANDARDS (CAL) -
Page 17 and 18: 9.1.1 METHOD MODIFICATIONS - The an
Page 19 and 20: 9.2.4.3 The target MRL is validated
Page 21 and 22: more than ±30 percent from the are
Page 23 and 24: 9.3.8 LABORATORY DUPLICATE OR LABOR
Page 25 and 26: counts for ClO 4 - at m/z 99 while
Page 27 and 28: 11. PROCEDURE 10.4.3 After every te
Page 29 and 30: 11.5 COMPOUND IDENTIFICATION - Iden
Page 31 and 32: 12.4.1 Calculations must utilize al
Page 33: 17. TABLES, DIAGRAMS, FLOWCHARTS AN
Page 37 and 38: TABLE 5. DETECTION LIMIT AND LCMRL
Page 39 and 40: TABLE 8. ON-GOING QUALITY CONTROL R
Page 41 and 42: FIGURE 1. IC-ESI/MS Configuration U
Page 43 and 44: FIGURE 4. MASS CHROMATOGRAM OF AN L
Page 45 and 46: Procedure 1. Prepare and inject, in
Page 47 and 48: APPENDIX A TABLE A1. SAMPLE DATA CO

View Actual EPA Method 332 (PDF File) - Columbia Analytical ...

You also want an ePaper? Increase the reach of your titles

Delete template?

Save as template?