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. Contact Customer Service to place your order (items are not available at Restek.com).
EPA Method 530, the Determination of Select Semivolatile Organic Chemicals in Drinking Water by Solid Phase Extraction and Gas Chromatography / Mass Spectrometry was developed on the Rtx-1701, but section 6.12.1 of the method states that "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; the 4th target analyte, dimethipin, was included in UCMR4 as part of EPA 525.3. It isn't really clear to me why a new method was made for these compounds instead of relying on EPA Method 525.3. Method 530 uses a 6mL divinyl benzene or polystyrene/divinyl benzene cartridge for extracting 1L where 525.3 has multiple cartridge and disk SPE options. The analysis is a couple minutes faster on the Rxi-5Sil MS under the 525.3 conditions. The selectivity of the two columns are similar, the primary difference being that butylated hydroxyanisole (BHA) is less retained relative to acenaphthene-D10 on the Rxi-5Sil MS. If your lab has limited resources, you should be able to perform both method 530 and 525.3 on one instrument set up for method 525.3.
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 |
I've collected example chromatograms on the Rxi-5sil MS using the same GC conditions that were used for the EPA Method 525.3 UCMR4 standard (Section 10.2.3.1), but with a new SIM program generated using the AutoSIM feature of MSD Chemstation. This was mainly to demonstrate the the two methods can be run on the same GC-MS with the same analytical column.
SIM Analysis of EPA 530 UCMR4 Standard Run at Method Reporting Limit (MRL) on the Rxi-5Sil MS
SIM Analysis of EPA 530 UCMR4 Standard Run at 10x the Method Reporting Limit (MRL) on the Rxi-5Sil MS
| Peaks | tR (min) | MRL Conc. (µg/mL) | 10x MRL Conc. (µg/mL) | |
|---|---|---|---|---|
| 1. | o-Toluidine-D9 (SUR) | 5.64 | 1.0 | 1.0 |
| 2. | o-Toluidine | 5.70 | 0.070 | 0.070 |
| 3. | Quinoline-D7 (SUR) | 8.22 | 1.0 | 1.0 |
| 4. | Quinoline | 8.26 | 0.20 | 0.20 |
| 5. | Butylated hydroxyanisole (BHA) | 11.50 | 0.30 | 0.30 |
| 6. | Acenaphthene-D10 (IS) | 11.54 | 1.0 | 1.0 |
| 7. | Phenanthrene-D10 (IS) | 15.05 | 1.0 | 1.0 |
| Column | Rxi-5Sil MS, 30 m, 0.25 mm ID, 0.25 µm (cat.# 13623) | ||||||||||||||||||||
| 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: | 30 psi (206.8kPa) | ||||||||||||||||||||
| Pulse Time: | 1.05 min | ||||||||||||||||||||
| Purge Flow: | 60 mL/min | ||||||||||||||||||||
| Oven | |||||||||||||||||||||
| Oven Temp.: | 70 °C (hold 1.5 min) to 200 °C at 10 °C/min (hold 0 min) to 320 °C at 7 °C/min (hold 3 min) | ||||||||||||||||||||
| Carrier Gas | He, constant flow | ||||||||||||||||||||
| Flow Rate: | 1.2 mL/min | ||||||||||||||||||||
| Detector | MS | ||||||||||||||||||||
| Mode: | SIM | ||||||||||||||||||||
| SIM Program: |
|
||||||||||||||||||||
| 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: | 1.45 min | ||||||||||||||||||||
| Tune Type: | DFTPP | ||||||||||||||||||||
| Ionization Mode: | EI | ||||||||||||||||||||
| Instrument | HP6890 GC & 5973 MSD |
