10
ME-1902-01 Determination of Dicamba in Polyurethane Foam (PUF) Air Sampling Traps by LC-MS/MS Chemicals & Reagents Chemical/Reagent Number/Specification Appendix A Reagent/Solution Preparation Solution Preparation Monsanto Report Number: MSL0027191 Page 110 of 315

Monsanto Report Number: MSL0027191 Page 110 of 315 · PDF fileMonsanto Report Number: ... Concentration Factor 25% methanol in water, mL Monsanto Report Number: ... Ex. 26C .pdf Author:

  • Upload
    lenhi

  • View
    213

  • Download
    1

Embed Size (px)

Citation preview

Page 1: Monsanto Report Number: MSL0027191 Page 110 of 315 · PDF fileMonsanto Report Number: ... Concentration Factor 25% methanol in water, mL Monsanto Report Number: ... Ex. 26C .pdf Author:

ME-1902-01Determination of Dicamba in Polyurethane Foam (PUF) Air Sampling Traps by LC-MS/MS

Chemicals &Reagents

Chemical/Reagent Number/Specification

Appendix A

Reagent/Solution Preparation

Solution Preparation

Monsanto Report Number: MSL0027191 Page 110 of 315

Page 2: Monsanto Report Number: MSL0027191 Page 110 of 315 · PDF fileMonsanto Report Number: ... Concentration Factor 25% methanol in water, mL Monsanto Report Number: ... Ex. 26C .pdf Author:

ME-1902-01Determination of Dicamba in Polyurethane Foam (PUF) Air Sampling Traps by LC-MS/MS

Standard Calibration and QC Solution Preparation

Overview

Stability

SolutionComponents

SolutionType

Concentrationor Range1,2 Solvent

Approx.Storage

( C)

DemonstratedStability(Days)

DicambaCalibrationStock Solution(0.10 mg/mL)

Monsanto Report Number: MSL0027191 Page 111 of 315

Page 3: Monsanto Report Number: MSL0027191 Page 110 of 315 · PDF fileMonsanto Report Number: ... Concentration Factor 25% methanol in water, mL Monsanto Report Number: ... Ex. 26C .pdf Author:

ME-1902-01Determination of Dicamba in Polyurethane Foam (PUF) Air Sampling Traps by LC-MS/MS

Dicamba QCStock Solution(0.48 mg/mL)

IntermediateCalibrationSolutions

Intermediate CalibrationSolution (µg/mL) Aliquot Solution ID

AliquotVolume

(mL)

DiluentVolume

(mL)

Monsanto Report Number: MSL0027191 Page 112 of 315

Page 4: Monsanto Report Number: MSL0027191 Page 110 of 315 · PDF fileMonsanto Report Number: ... Concentration Factor 25% methanol in water, mL Monsanto Report Number: ... Ex. 26C .pdf Author:

ME-1902-01Determination of Dicamba in Polyurethane Foam (PUF) Air Sampling Traps by LC-MS/MS

WorkingCalibrationStandardSolutions

Dicamba Working Calibration Solutions

WorkingCalibration

Solution(µg/mL)

AliquotSolutionConcn

(µg/mL)

AliquotVolume

(mL)

DiluentVolume

(mL)Equivalent Concn1

(ng/PUF)

This concentration represents 0.100 mL of Working Calibration Solution diluted bythe extraction solvent (30 fold). For example, 0.100 mL of the 0.015 µg/mL WorkingCalibration Solution diluted to 30 mL results in an equivalent concentration of 1.5 ngdicamba/PUF.

Monsanto Report Number: MSL0027191 Page 113 of 315

Page 5: Monsanto Report Number: MSL0027191 Page 110 of 315 · PDF fileMonsanto Report Number: ... Concentration Factor 25% methanol in water, mL Monsanto Report Number: ... Ex. 26C .pdf Author:

ME-1902-01Determination of Dicamba in Polyurethane Foam (PUF) Air Sampling Traps by LC-MS/MS

QCFortificationSolutions

Dicamba QC Fortification Solutions

QC SolutionConcn

(µg/mL) Aliquot Solution ID

AliquotVolume

(mL)

DiluentVolume

(mL)

FortificationConcn

(ng/PUF)

1 Concentration represents 0.100 mL of QC Fortification Solution diluted by theextraction solvent. For example, 0.100 mL of the 0.030 µg/mL QC Solution diluted to30 mL resulted in an equivalent concentration of 3.0 ng dicamba/PUF.

(13C6)DicambaIS StockSolution(0.10 mg/mL)

Monsanto Report Number: MSL0027191 Page 114 of 315

Page 6: Monsanto Report Number: MSL0027191 Page 110 of 315 · PDF fileMonsanto Report Number: ... Concentration Factor 25% methanol in water, mL Monsanto Report Number: ... Ex. 26C .pdf Author:

ME-1902-01Determination of Dicamba in Polyurethane Foam (PUF) Air Sampling Traps by LC-MS/MS

IS WorkingSolution(0.0225 µg/mL)

IS SolutionConcn (µg/mL) Aliquot Solution ID

Aliquot Volume(mL)

ACN Volume(mL)

Sample Preparation Procedure

Sample Storage

SampleProcessing

Step Action

QC Sample Fortification Level (ng/PUF)

Monsanto Report Number: MSL0027191 Page 115 of 315

Page 7: Monsanto Report Number: MSL0027191 Page 110 of 315 · PDF fileMonsanto Report Number: ... Concentration Factor 25% methanol in water, mL Monsanto Report Number: ... Ex. 26C .pdf Author:

ME-1902-01Determination of Dicamba in Polyurethane Foam (PUF) Air Sampling Traps by LC-MS/MS

Note:

Concentration Factor 25% methanol in water, mL

Monsanto Report Number: MSL0027191 Page 116 of 315

Page 8: Monsanto Report Number: MSL0027191 Page 110 of 315 · PDF fileMonsanto Report Number: ... Concentration Factor 25% methanol in water, mL Monsanto Report Number: ... Ex. 26C .pdf Author:

ME-1902-01Determination of Dicamba in Polyurethane Foam (PUF) Air Sampling Traps by LC-MS/MS

Injection VolumeAdjustment

Instrumental Analysis

SampleAnalysisGuidance andAcceptanceCriteria

Calibration Curve:

Quality Control Samples:

Monsanto Report Number: MSL0027191 Page 117 of 315

Page 9: Monsanto Report Number: MSL0027191 Page 110 of 315 · PDF fileMonsanto Report Number: ... Concentration Factor 25% methanol in water, mL Monsanto Report Number: ... Ex. 26C .pdf Author:

ME-1902-01Determination of Dicamba in Polyurethane Foam (PUF) Air Sampling Traps by LC-MS/MS

Injection Carryover:

InstrumentSetup

SystemConditions forAnalysis

LC-MS/MS System Conditions

Monsanto Report Number: MSL0027191 Page 118 of 315

Page 10: Monsanto Report Number: MSL0027191 Page 110 of 315 · PDF fileMonsanto Report Number: ... Concentration Factor 25% methanol in water, mL Monsanto Report Number: ... Ex. 26C .pdf Author:

ME-1902-01Determination of Dicamba in Polyurethane Foam (PUF) Air Sampling Traps by LC-MS/MS

DataProcessing

Calculations

Overview

Monsanto Report Number: MSL0027191 Page 119 of 315