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State of Connecticut Department of Environmental Protection Recommended Reasonable Confidence Protocols


State of Connecticut

Department of Environmental Protection

Recommended Reasonable Confidence Protocols

Quality Assurance and Quality Control Requirements

Synthetic Precipitation Leaching Procedure

By SW-846 Method 1312

Version 2.0

December 2006











Written by the Connecticut DEP QA/QC Workgroup







Revision
Comments
Date
1.0
First Version for Publication
03/30/2006
2.0
Final version based upon public comments
December 2006












Connecticut DEP RCPs

Version 2.0
QA/QC Requirements

December 2006
SPLP by Method 1312

Page 2 of 18


TABLE OF CONTENTS

Item

Page

1.0 Overview of Method 1312
1

2.0 Summary of Method 1312
1

3.0 Interferences
1

4.0 Apparatus and Materials
1

5.0 Reagents
4

6.0 Sample Collection, Preservation and Handling
5

7.0 Procedure
5

8.0 Quality Control
15

9.0 Report Deliverables
16





List of Tables
Table 1.0 Report Deliverables
16

Table 1A Specific QA/QC Requirements and performance Standards
17

Table 2A Sample Containers, Preservation, and Holding Times
18













ii

1.0 Overview of Method 1312

1.1 Method 1312 is designed to determine the mobility of both organic and inorganic analytes
present in liquids, soils, and wastes. Samples are leached (or extracted) with a dilute acid solution
and filtered. The resulting extract can be analyzed by a variety of methods to determine the
pollutant mobility of various analytes.

All method references are to the latest promulgated version of the method found in Test Methods
for Evaluating Solid Waste, SW-846.

2.0 Summary of Method

2.1 For liquid samples (i.e., those containing less than 0.5 % dry solid material), the sample, after
filtration through a 0.6 to 0.8 µm glass fiber filter is defined as the SPLP extract.

2.2 For samples containing greater than 0.5 % solids, the liquid phase, if any, is separated from
the solid phase and stored for later analysis; the particle size of the solid phase is reduced, if
necessary. The solid phase is extracted with an amount of extraction fluid equal to 20 times the
weight of the solid phase. The extraction fluid employed is a function of the region of the country
where the sample site is located if the sample is a soil. If the sample is a waste or wastewater, the
extraction fluid employed is a pH 4.2 solution. A special extractor vessel is used when testing for
volatile analytes. Following extraction, the liquid extract is separated from the solid phase by
filtration through a 0.6 to 0.8-µm glass fiber filter.

2.3 If compatible (i.e., multiple phases will not form on combination), the initial liquid phase of
the waste is added to the liquid extract, and these are analyzed together. If incompatible, the
liquids are analyzed separately and the results are mathematically combined to yield a volume-
weighted average concentration.

3.0 Interferences

3.1 Potential interferences that may be encountered during analysis are discussed in the individual
analytical methods.

3.2 Significant losses of volatile organics may be encountered due to improper sample handling,
both in the field and in the laboratory. Samples for SPLP volatiles should be collected and stored
in core and store type sampling devices in accordance with the Connecticut Department of
Environmental Protections Guidance on Collecting and Preserving of Soil and Sediment
Samples for Laboratory Determination of Volatile Organic Compounds.

3.3 Upon receipt in the laboratory the sample container for volatiles must be stored frozen (-12º C
± 3º C). When preparing the sample for extraction, the laboratory must transfer the sample for
extraction from the storage container to the zero headspace extractor (ZHE) as quickly as possible
after the container is opened. The ZHE must be sealed as soon as the sample is added.

4.0 Apparatus and Materials

4.1 Agitation apparatus: The agitation apparatus must be capable of rotating the extraction vessel
in an end-over-end fashion at 30 ± 2 rpm. Suitable devices are identified in Table 2 of SW-846
Method 1312. Connecticut DEP RCPs

Version 2.0
QA/QC Requirements

December 2006
SPLP by Method 1312

Page 2 of 18

4.2 Extraction Vessels

4.2.1 Zero Headspace Extraction Vessel (ZHE). This device is for use only when the sample is
being tested for the mobility of volatile analytes. The ZHE (depicted in Figure 2) allows for
liquid/solid separation within the device and effectively precludes headspace. This type of vessel
allows for initial liquid/solid separation, extraction, and final extract filtration without opening the
vessel (see Step 4.3.1). These vessels shall have an internal volume of 500-600 mL and be
equipped to accommodate a 90-110 mm filter. The devices contain VITON® O-rings which
should be replaced frequently. Suitable ZHE devices known to EPA are identified in Table 3 of
SW-846 Method 1312.

For the ZHE to be acceptable for use, the piston within the ZHE should be able to be moved with
approximately 15 psig or less. If it takes more pressure to move the piston, the O-rings in the
device should be replaced. If this does not solve the problem, the ZHE is unacceptable for 1312
analyses and the manufacturer should be contacted. The ZHE should be checked for leaks after
every extraction. If the device contains a built-in pressure gauge, pressurize the device to 50 psig,
allow it to stand unattended for 1 hour, and recheck the pressure. If the device does not have a
built-in pressure gauge, pressurize the device to 50 psig, submerge it in water, and check for the
presence of air bubbles escaping from any of the fittings. If pressure is lost, check all fittings and
inspect and replace O-rings, if necessary. Retest the device. If leakage problems cannot be solved,
the manufacturer should be contacted.

Some ZHEs use gas pressure to actuate the ZHE piston, while others use mechanical pressure
(see Table 3 of SW-846 Method 1312). Whereas the volatiles procedure (see Step 7.3) refers to
pounds-per-square-inch (psig), for the mechanically actuated piston, the pressure applied is
measured in torque inch- pounds. Refer to the manufacturer's instructions as to the proper
conversion.

4.2.2 Bottle Extraction Vessel. When the sample is being evaluated using the nonvolatile
extraction, a jar with sufficient capacity to hold the sample and the extraction fluid is needed.
Headspace is allowed in this vessel. The extraction bottles may be constructed from various
materials, depending on the analytes to be analyzed and the nature of the waste (see Step 4.3.3). It
is recommended that borosilicate glass bottles be used instead of other types of glass, especially
when inorganics are of concern. Plastic bottles, other than polytetrafluoroethylene, shall not be
used if organics are to be investigated. Bottles are available from a number of laboratory
suppliers. When this type of extraction vessel is used, the filtration device discussed in Step 4.3.2
is used for initial liquid/solid separation and final extract filtration.

4.3 Filtration Devices: It is recommended that all filtrations be performed in a hood.

4.3.1 Zero-Headspace Extraction Vessel (ZHE): When the sample is evaluated for volatiles, the
zero-headspace extraction vessel described in Step 4.2.1 is used for filtration. The device shall be
capable of supporting and keeping in place the glass fiber filter and be able to withstand the
pressure needed to accomplish separation (50 psig).
NOTE: When it is suspected that the glass fiber filter has been ruptured, an in-line glass fiber
filter may be used to filter the material within the ZHE.

4.3.2 Filter Holder: When the sample is evaluated for other than volatile analytes, a filter holder
capable of supporting a glass fiber filter and able to withstand the pressure needed to accomplish
separation may be used. Suitable filter holders range from simple vacuum units to relatively
Connecticut DEP RCPs

Version 2.0
QA/QC Requirements

December 2006
SPLP by Method 1312

Page 3 of 18
complex systems capable of exerting pressures of up to 50 psig or more. The type of filter holder
used depends on the properties of the material to be filtered (see Step 4.3.3). These devices shall
have a minimum