We recently stocked custom EPA Method 541 standards made specifically for labs participating in Unregulated Contaminant Monitoring Rule 4 (UCMR4). Quantitative Certificates of Analysis with Data Packs are available for each item. Contact Customer Service to place your order (items are not available at Restek.com).
Cat# 572263 – Method 541 UCMR4 Standard (in P&T Methanol)
Contaminant | CAS Registry Number | Minimum Reporting Level | Standard Concentration |
---|---|---|---|
1-Butanol | 71-36-3 | 2.0 µg/L | 2000 µg/mL |
2-Methoxyethanol | 109-86-4 | 0.40 µg/L | 400 µg/mL |
2-Propen-1-ol | 107-18-6 | 0.50 µg/L | 500 µg/mL |
Cat# 572267 – Method 541 UCMR4 Surrogate Standard (in P&T Methanol)
Contaminant | CAS Registry Number | Standard Concentration |
---|---|---|
1-Butanol-D10 | 34193-38-9 | 50 µg/mL |
Cat# 572268 – Method 541 UCMR4 Internal Standard (in P&T Methanol)
Contaminant | CAS Registry Number | Standard Concentration |
---|---|---|
Chlorobenzene-D5 | 3114-55-4 | 50 µg/mL |
The analyte concentrations make it easy to prepare calibration levels based on the minimum reporting level (MRL) required by the UCMR4 program. I’ve included example chromatograms collected at the MRL and 10x the MRL using the GC conditions taken from EPA Method 541. The SIM conditions were generated using the AutoSIM feature of MSD Chemstation version D.03.
SIM Analysis of EPA 541 UCMR4 Standard Run at Method Reporting Limit (MRL) on the Stabilwax
SIM Analysis of EPA 541 UCMR4 Standard Run at 10x the Method Reporting Limit (MRL) on the Stabilwax
Peaks | tR (min) | MRL Conc. (µg/mL) | 10x MRL Conc. (µg/mL) | |
---|---|---|---|---|
1. | 2-Propen-1-ol | 6.94 | 0.013 | 0.13 |
2. | 1-Butanol-D10 (SUR) | 7.25 | 0.25 | 0.25 |
3. | 1-Butanol | 7.38 | 0.050 | 0.50 |
4. | 2-Methoxyethanol | 7.97 | 0.010 | 0.10 |
5. | Chlorobenzene-d5 | 8.66 | 0.25 | 0.25 |
Column | Stabilwax, 30 m, 0.25 mm ID, 0.50 µm (cat.# 10638) | ||||||||||||||||||||
Sample | Method 541 UCMR4 Standard (cat.# 572263) | ||||||||||||||||||||
Method 541 UCMR4 Internal Standard (cat.# 572268) | |||||||||||||||||||||
Method 541 UCMR4 Surrogate Standard (cat.# 572267) | |||||||||||||||||||||
Diluent: | Dichloromethane | ||||||||||||||||||||
Injection | |||||||||||||||||||||
Inj. Vol.: | 1 µL pulsed splitless (hold 0.50 min) | ||||||||||||||||||||
Liner: | 4 mm Single Taper w/Wool (cat.# 23303) | ||||||||||||||||||||
Inj. Temp.: | 200 °C | ||||||||||||||||||||
Pulse Pressure: | 10 psi (68.9kPa) | ||||||||||||||||||||
Pulse Time: | 0.55 min | ||||||||||||||||||||
Purge Flow: | 100 mL/min | ||||||||||||||||||||
Oven | |||||||||||||||||||||
Oven Temp.: | 30 °C (hold 0.5 min) to 110 °C at 10 °C/min (hold 0 min) to 200 °C at 25 °C/min (hold 6 min) | ||||||||||||||||||||
Carrier Gas | He, constant flow | ||||||||||||||||||||
Flow Rate: | 0.9 mL/min | ||||||||||||||||||||
Detector | MS | ||||||||||||||||||||
Mode: | SIM | ||||||||||||||||||||
SIM Program: |
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Transfer Line Temp.: | 200 °C | ||||||||||||||||||||
Analyzer Type: | Quadrupole | ||||||||||||||||||||
Source Type: | Stainless Steel | ||||||||||||||||||||
Drawout Plate: | 6 mm ID | ||||||||||||||||||||
Source Temp.: | 230 °C | ||||||||||||||||||||
Quad Temp.: | 150 °C | ||||||||||||||||||||
Solvent Delay Time: | 6.0 min | ||||||||||||||||||||
Tune Type: | BFB | ||||||||||||||||||||
Ionization Mode: | EI | ||||||||||||||||||||
Instrument | HP6890 GC & 5973 MSD |
Will Restek be including the second surrogate compound 2-propen-1-ol-d6 (CAS# 1173018-56-8) required by the method?
Our CRM department wasn’t able to source the compound.
CIL has a c13 labeled allyl alcohol, which should also work, but unlike the deuterated analog, it will coelute with the target compound
http://shop.isotope.com/productdetails.aspx?itemno=CLM-2043-0.1
Sigma sells a d5 analog, which does not have a deuterated hydroxy group. Since the hydrogen in the hydroxy group is acidic, it really shouldn’t be deuterated when used to spike aqueous samples. It will exchange with the hydrogens in water at different rates depending on pH, causing inconsistent recovery.
http://www.sigmaaldrich.com/catalog/product/aldrich/452491?lang=en®ion=US&cm_sp=Insite-_-prodRecCold_xorders-_-prodRecCold2-1