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# INTRODUCTION

## Cyanide Analysis Description

Cyanide will be analyzed according to the CLP SOW ILM03.0 for water and
soil samples. Soil samples must be prepared per Attachment A. This
method uses spectrophotometry. The required detection limits for cyanide
are 10μg/L for water and 2 mg/kg for soil.

## References

DOE 1995. "Remedial Investigation/Feasibility Study Operable Unit 9,
Site-Wide Quality Assurance Project Plan," Final Revision 4, U.S.
Department of Energy, April 1995.

EPA. 1996. "U.S. EPA Contract Laboratory Program, Statement of Work for
Inorganic Analysis, Multi-media, Multi-Concentration." Document No.
ILM03.0. U.S. Environmental Protection Agency, March 1990.

# PRESERVATION

Cyanide Analysis\
Sample Containers, Volumes, Preservation, and Holding Times

  -------- --------------- ------------ -------------- --------- ---------------- ----------
  Matrix   Parameters^1^   Analytical   Container      Minimum   Preservation     Holding\
                           Method                      Volume                     Time

  Water    Cyanide         CLP SOW      Polyethylene   1500 mL   NaOH to pH ≥ 12  14 days
                                        bottle                   Cool 4°C         

  Soil     Cyanide         CLP SOW      Wide-mouth     100 grams Cool 4°C         14 days
                                        polyethylene                              
                                        bottle                                    
  -------- --------------- ------------ -------------- --------- ---------------- ----------

^1^ the analyses have been listed to ensure field personnel know which
analyses can be taken from the same container.

# CALIBRATION

Cyanide will be analyzed according to the procedures presented in the
CLP SOW for inorganic analyses. The spectrophotometer is calibrated
daily, or once every 24 hours, and each time the instrument is set up.
The minimum correlation coefficient for cyanide calibration is 0.996.

A initial calibration verification (ICV) is performed to assess the
accuracy of the initial calibration using a standard of a certified
concentration from an external source. When the measurement exceeds the
CLP-established control limits, the problem is corrected, the instrument
is re-calibrated and the ICV is run again. The initial calibration is
verified by analysis of a continuing calibration verification (CCV)
standard every two hours during an analysis run or at a frequency of
10%, whichever is more frequent. This standard is also analyzed for at
the beginning and end of each sample run. The concentration and source
of the CCV and acceptance criteria are specified in the CLP SOW.

# QC CRITERIA

Table 4.1 - Cyanide Analysis\
Field QC Sample Frequency

+-----------+-----------+--------------+------------+-----------------+
| Parameter | Quality   | Frequency    | Acceptance | Corrective      |
|           | Control   |              | Criteria   | Action          |
|           | Check     |              |            |                 |
+-----------+-----------+--------------+------------+-----------------+
| Cyanide,  | Duplicate | 1 every 10   | ≤ 25% RPD  | Evaluate data   |
| CLP SOW   |           | or fewer     |            | for usability.  |
| ILM03.0   |           | field        | Not        |                 |
|           |           | samples      | applicable | Evaluate        |
|           |           | (**water**)  |            | variability.    |
|           |           |              |            |                 |
|           |           | 1 every 10   |            |                 |
|           |           | or fewer     |            |                 |
|           |           | field        |            |                 |
|           |           | samples      |            |                 |
|           |           | (**soil**)   |            |                 |
+-----------+-----------+--------------+------------+-----------------+
|           | Equipment | 1 every 10   | ≤ 10 ×     | Evaluate        |
|           | (rinsate) | or fewer     | level in   | potential       |
|           | blank     | field        | associated | sources;        |
|           |           | samples      | samples    | Evaluate        |
|           |           | (**water**)  |            | associated data |
|           |           |              |            | for usability.  |
+-----------+-----------+--------------+------------+-----------------+

Table 4.2 - Cyanide Analysis CLP SOW ILM03.0\
Laboratory QC Sample Frequency

+---------+-----------+----------------+-----------+------------------+
| Pa      | Quality   | Frequency      | A         | Corrective       |
| rameter | Control   |                | cceptance | Action           |
|         | Check     |                | Criteria  |                  |
+---------+-----------+----------------+-----------+------------------+
| C       | Initial   | After every    | ≤ CRDL    | Correct problem; |
| yanide, | and       | ICV and CCV or |           | recalibrate;     |
| CLP SOW | c         | 10% or every 2 |           | reanalyze        |
| ILM03.0 | ontinuing | hours,         |           | preceding 10     |
|         | ca        | whichever is   |           | samples or all   |
|         | libration | more frequent. |           | since last good  |
|         | blanks    |                |           | blank.           |
|         | (ICB,CCB) |                |           |                  |
+---------+-----------+----------------+-----------+------------------+
|         | Spike     | 1 per group of | 75-125%   | Evaluate data    |
|         | sample    | samples of a   | Recovery  | for usability.   |
|         | (S)       | given matrix,  |           |                  |
|         |           | concentration, |           |                  |
|         |           | or sample      |           |                  |
|         |           | delivery       |           |                  |
|         |           | group,         |           |                  |
|         |           | whichever is   |           |                  |
|         |           | more frequent. |           |                  |
+---------+-----------+----------------+-----------+------------------+
|         | Sample    | 1 per group of | If result | Evaluate data    |
|         | duplicate | samples of a   | ≥ 5 ×     | for usability.   |
|         | (D)       | given matrix,  | CRDL: ±   |                  |
|         |           | concentration, | 20% RPD   |                  |
|         |           | or sample      |           |                  |
|         |           | delivery       | If result |                  |
|         |           | group,         | ≤ 5 ×     |                  |
|         |           | whichever is   | CRDL: ±   |                  |
|         |           | more frequent. | CRDL      |                  |
+---------+-----------+----------------+-----------+------------------+
|         | L         | One per        | 85-115    | Evaluate data    |
|         | aboratory | laboratory     |           | for usability.   |
|         | Control   | batch.         |           |                  |
|         | Sample    |                |           |                  |
|         | (LCS)     |                |           |                  |
+---------+-----------+----------------+-----------+------------------+

# ANALYTE LIST AND REPORTING LIMITS

These are expected quantitation limits based on reagent grade water or a
purified solid matrix. Actual quantitation limits may be higher
depending upon the nature of the sample matrix. The limit reported on
final laboratory reports will take into account the actual sample volume
or weight, percent moisture (where applicable), and the dilution factor,
if any.

  ------------------------------------------------------------------------
  Table 5.1 Cyanide - CLP                           
  SOW ILM03.0\                                      
  Target Analyte List                               
  -------------------------- ---------------------- ----------------------
  Analyte                    Water (μg/L)           Soil (mg/kg)

  Cyanide                    10                     2
  ------------------------------------------------------------------------

attachment a for\
method a-006

Attachment A for Method A-006

Statement of Work for Soil Preparation for Common Organic, Inorganic,
and\
Selected Radiological Analyses

1.0 Scope and Application

This procedure describes how to aliquot Mound soil and soil-like samples
for laboratory preparation and analysis. This procedure applies to soil
analysis for metals, semi-volatiles, pesticide/PCBs, cyanide, anions,
explosives, and radiological analyses which do not have a prescribed
soil preparation procedure. This procedure should not be used for
volatile organic analysis. Soils for volatile organic analysis will be
prepared and homogenized as described in the method of analysis.

2.0 Summary

A representative aliquot of a sample is taken in the laboratory by
either visually examining and taking a representative portion from each
layer in a sample or taking a core of the sample.

3.0 Interferences

Soil samples are heterogeneous by nature. Because of this nature, target
analytes are often channeled and concentrated in the soil in specific
layers or locations. This heterogeneity may affect both how
representative the sample is of the field location and how
representative the laboratory aliquot is of the sample.

Heterogeneous nature of soils can sometimes be eliminated in laboratory
aliquoting by visually inspecting the sample for layering and selecting
a representative aliquot or by taking a core of the sample.

4.0 Equipment

4.1 Spatula or Scoop

4.2 Glass tray, plastic tray, or other material for containing spilled
soil

4.3 Large container, i.e. 1000 mL Pyrex beaker

5.0 Reagents/Supplies

5.1 Disposable gloves

6.0 Sample Collection/Holding Time/Preservation

6.1 See Section 2.0 of Method A-006.

7.0 Procedure

7.1 Place a glass tray, plastic tray, or disposable paper beneath the
sample container. The tray or paper will be used to contain any soil
which accidentally falls off the bottle lip when the cap is opened or
falls out while the sample is taken.

7.2 Visually examine the contents of the sample container. If obvious
layering is present, then representative portions of each layer must be
taken for the aliquot.

1.  If the sample is obviously a core sample (cylindrical soil mass),
    then use the spatula to core from the top of the sample to the
    bottom of the sample. This procedure should be representative of the
    entire core.

2.  If the sample cannot be easily cored, it may be necessary to
    transfer the sample to a large container and thoroughly and
    carefully mix the sample with a spatula or scoop. Mixing will not be
    performed on soil samples for volatile and semi-volatile analyses.

3.  If the sample is neither layered nor a core sample, then use a
    spatula to core through the middle of the sample. The core should be
    representative of the entire sample.

7.3 Process the sample as specified in the applicable method.

8.0 Quality Control

8.1 Each analytical method has specific types of quality control samples
introduced to evaluate laboratory precision and reproducibility of
sample results. Typically, these quality control samples are laboratory
duplicates or matrix spike duplicates. These quality control samples
permit the laboratory to calculate the relative percent difference and
evaluate the soil aliquoting procedure and the precision of the method.

9.0 References and Associated Standard Operating Procedures

None