New Custom UCMR4 Standard for EPA Method 530 on the Rtx-1701

We recently stocked custom EPA Method 530 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# 572262 – Method 530 UCMR4 Standard (in Methanol)

Contaminant CAS Registry Number Minimum Reporting Level Standard Concentration
butylated hydroxyanisole (BHA) 25013-16-5 0.03 µg/L 150 µg/mL
o-Toluidine 95-53-4 0.007 µg/L 35 µg/mL
Quinoline 91-22-5 0.02 µg/L 100 µg/mL

 

Cat# 572265 – Method 530 UCMR4 Surrogate Standard (in Methanol)

Contaminant CAS Registry Number Standard Concentration
Quinoline-D7 34071-94-8 500 µg/mL
o-Toluidine-D9 194423-47-7 500 µg/mL

 

Cat# 572266 – Method 530 UCMR4 Internal Standard (in Acetone)

Contaminant CAS Registry Number Standard Concentration
Acenaphthene-D10 15067-26-2 500 µg/mL
Phenanthrene-D10 1517-22-2 500 µg/mL

 

The suggested analytical column for EPA Method 530, the Determination of Select Semivolatile Organic Chemicals in Drinking Water by Solid Phase Extraction and Gas Chromatography / Mass Spectrometry, is the Rtx-1701, though “any capillary column that provides adequate capacity, resolution, accuracy, and precision may be used.” 3 of the 4 Method 530 target analytes, butylated hydroxyanisole, o-toluidine, and quinoline have been included in UCMR4; dimethipin, the 4th target analyte, was included in UCMR4 as part of EPA 525.3. I’ve included example chromatograms collected at the method reporting limit (MRL) and at 10x the MRL below. The GC inlet, oven and detector settings were taken directly from the method, and the AutoSIM function in MSD Chemstation version D.03 was used to generate the SIM analysis windows.

SIM Analysis of EPA 530 UCMR4 Standard Run at Method Reporting Limit (MRL) on the Rtx-1701

SIM Analysis of EPA 530 UCMR4 Standard Run at 10x the Method Reporting Limit (MRL) on the Rtx-1701

Peaks tR (min) MRL Conc. (µg/mL) 10x MRL Conc. (µg/mL)
1. o-Toluidine-D9 (SUR) 8.426 1.0 1.0
2. o-Toluidine 8.481 0.070 0.70
3. Quinoline-D7 (SUR) 10.622 1.0 1.0
4. Quinoline 10.641 0.20 2.0
5. Acenaphthene-D10 (IS) 13.45 1.0 1.0
6. Butylated hydroxyanisole (BHA) 14.25 0.30 3.0
7. Phenanthrene-D10 (IS) 17.318 1.0 1.0

 

Column Rtx-1701, 30 m, 0.25 mm ID, 0.25 µm (cat.# 12023)
Sample Method 530 UCMR4 Standard (cat.# 572262)
Method 530 UCMR4 Surrogate Standard (cat.# 572265)
Method 530 UCMR4 Internal Standard (cat.# 572266)
Diluent: Dichloromethane
Injection
Inj. Vol.: 1 µL pulsed splitless (hold 1.0 min)
Liner: 4 mm Single Taper w/Wool (cat.# 23303)
Inj. Temp.: 275 °C
Pulse Pressure: 20 psi (206.8kPa)
Pulse Time: 1.05 min
Purge Flow: 60 mL/min
Oven
Oven Temp.: 60 °C (hold 1.0 min) to 290 °C at 10 °C/min (hold 1 min)
Carrier Gas He, constant flow
Flow Rate: 1.0 mL/min
Detector MS
Mode: SIM
SIM Program:
Group Start Time (min) Ion(s) (m/z) Dwell (ms)
1 3.50 106, 107, 112, 114 25
2 9.55 102, 108, 129, 136 25
3 12.08 162, 164 25
4 14.02 137, 180 25
4 15.92 160, 188 25
Transfer Line Temp.: 280 °C
Analyzer Type: Quadrupole
Source Type: Stainless Steel
Drawout Plate: 6 mm ID
Source Temp.: 280 °C
Quad Temp.: 180 °C
Solvent Delay Time: 3.5 min
Tune Type: DFTPP
Ionization Mode: EI
Instrument HP6890 GC & 5973 MSD
Notes The EPA Method 530 UCMR4 Standard analyte concentrations vary to simplify preparing ICAL levels based on the minimum method reporting levels.

Leave a Reply