New Custom UCMR4 Standards for EPA Method 541

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. Email csreps@restek.com or phone 800-356-1688 ext. 3 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:
Group Start Time (min) Ion(s) (m/z) Dwell (ms)
1 6.000 39, 55, 57, 58 25
2 7.153 41, 43, 46, 50, 55, 56, 63, 64 25
3 7.685 45, 47, 58, 76 25
4 8.292 76, 117, 119 25
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

 

2 Responses to “New Custom UCMR4 Standards for EPA Method 541”

  1. James Ball says:

    Will Restek be including the second surrogate compound 2-propen-1-ol-d6 (CAS# 1173018-56-8) required by the method?

  2. 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&region=US&cm_sp=Insite-_-prodRecCold_xorders-_-prodRecCold2-1

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