Teledyne Leeman Labs

This application note describes the capability of the Teledyne Leeman Lab's Prodigy7 High-Dispersion ICP for performing analysis according to SW-846 Method 6010C. This method is applicable to groundwaters, Toxicity Characteristic Leaching Procedure (TCLP) and Extraction Procedure (EP), industrial organic wastes, soils, sludge, and sediments. 

As with other US EPA mandated methods, Method 6010C requires adherence to specific procedures to ensure analytical quality control. 

A Prodigy7 inductively coupled plasma (ICP) spectrometer equipped with a radial view torch and a 240-position CETAC ASX-520 autosampler was used to generate the data.  

The Prodigy7 is a compact benchtop simultaneous ICP-OES system featuring a 500 mm focal length Echelle Optical System coupled with a megapixel CMOS Detector. At 28 × 28 mm, the active area of the CMOS Detector is significantly larger than any other solid-state detector currently used for ICP-OES. This combination allows Prodigy7 to achieve higher optical resolution than other solid-state detector based ICP systems. The detector also provides continuous wavelength coverage from 165 to 1100 nm permitting measurement over the entire ICP spectrum in a single reading without sacrificing wavelength range or resolution. This detector design is inherently anti-blooming and is capable of random access, nondestructive readout that results in a dynamic range of more than six orders of magnitude. 

The sample introduction system consists of: 					

The volume of cyclonic spray chamber is low to allow for fast washout between samples, while its knockout tube or baffle, efficiently reduces the amount of sample aerosol reaching the torch.  

The torch and sample introduction system are uniquely integrated into the optical system through Prodigy7's innovative Image Stabilization System, which treats the torch as an optical component by rigidly attaching it to the spectrometer. 

The initial performance parameters measured for this application note were determined as specified in Method 6010C. All samples were analyzed using the Prodigy7 equipped with a radially viewed torch. 

Method 6010C requires that the upper limit of the linear dynamic range (LDR) be established. This is accomplished by analyzing increasingly higher concentration analyte standards. The LDR is considered exceeded when the measured concentration is more than 10% below the true concentration. The upper limit of the LDR must be established for each wavelength utilized by determining the signal responses from a minimum of three different concentration standards across the range. The ranges that may be used for the analysis of samples should be judged by the analyst from the resulting data. A standard at the upper limit must be prepared, analyzed, and quantitated against the normal calibration curve. The calculated value must be within 10% (±10%) of the true value.  

The types of samples analyzed under the scope of Method 6010C may exhibit considerable spectral complexity. As a result, interferences due to spectral overlaps may be observed. When present and uncorrected, these interferences will produce biased determinations. For this study, checks are performed for the major matrix elements, Al, Ca, Fe, Mg, Si, and P on the other analyte elements. This is done using single element solutions. Once the interferences are identified, the Prodigy7 will automatically calculate the interfering element correction factors. 

A certified water sample, ERA WatR™  Pollution Trace Metals, Lot P213-500, and four certified soil samples were prepared and analyzed: ERA Metals in SewageSludG™ , Lot. D078-160 (Environmental Resource Associates, Arvada, Colorado) and Standard Reference Materials (SRM) 2709, 2710, 2710 (NIST, Gaithersburg, Maryland).  

The Prodigy7 ICP readily accommodated all of the soil samples for analysis. Examination of the data indicates the results for all elements lie well within the performance acceptance limits (PAL) for the ERA soil or the range specified for the NIST SRM soils. The results demonstrate excellent precision, as indicated by the low relative standard deviation (RSD) data, indicating the Prodigy7 is operating well above the detection limit (DL) and limit of quantitation (LOQ) for the elements determined. 

http://web.teledyneleemanlabs.com/spectroscopyAN1305

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This application note describes the capability of the Teledyne Leeman Lab's Prodigy7 High-Dispersion ICP for performing analysis according to SW-846 Method 6010C.

US EPA SW-846 Method 6010C Using the Prodigy7 High-Dispersion ICP Introduction

Mercury is a toxic, persistent pollutant found in many native ores rich in copper, silver and gold. As such ores are processed mercury can be released to the environment. This can be either during the "stamping" process (crushing rocks to "sand") where mercury rich tailings can enter the local watershed or during smelting where volatile mercury can be released into the atmosphere. It is for these reasons and their potential impact on the environment that it is important to be able to reliably measure mercury.  

Four samples of copper concentrates were acquired and analyzed using a direct analysis technique. The technique involves thermal decomposition of mercury compounds present in the sample through combustion followed by pre-concentration via gold amalgamation and subsequent detection using cold vapor atomic absorption (Figure 1). 

Figure 1: Cold vapor atomic absorption illustration.			

Oxygen was used as the carrier gas at a flow rate of 350 ml/min. Signal integration was set at 100 s. 

 provides two optical paths of differing lengths to extend its dynamic range, producing both low and high calibration curves. These calibration curves were generated using weighed deposits of aqueous standards in concentrations of 0.1, 1.0, and 10.0 ppm (w/w) mercury. All samples and standards were analyzed using nickel boats. 

The low range calibration extended to 40 ng and the high range calibration to 520 ng. Both calibrations delivered linear correlation coefficients better than 0.997; however, a quadratic curve provided a slightly more precise fit for the standards. 

Each of the submitted samples was introduced five times. Carryover was determined to be less than 1% by remeasuring the same sample boat with sample residue untouched. A 250 ng standard was run between sample replicates to ensure that no shift in sensitivity had occurred. 

 provides a 70-position autosampler and has on-the-fly loading capability for virtually unlimited capacity. Additionally, a conversion kit is available which employs chemical reduction to satisfy the monitoring of drinking water in accordance with US EPA Method 245.1 and European Standards EN1483 and EN13806. 

For more information on this application or on Teledyne Leeman Lab Mercury family of products, please visit our website at 

			tel. (603) 886-8400, fax (603) 886-9141 

Mercury is a toxic, persistent pollutant found in many native ores rich in copper, silver and gold. As such ores are processed mercury can be released to the environment.

Teledyne Leeman Labs

Articles

US EPA SW-846 Method 6010C Using the Prodigy7 High-Dispersion ICP Introduction

The Determination of Mercury in Copper Concentrates by Thermal Decomposition, Amalgamation and Cold Vapor Atomic Absorption