ASTM D5788-95

NOTICE: This standard has either been superseded and replaced by a new version or
withdrawn. Contact ASTM International (www.astm.org) for the latest information.
Designation: D 5788 – 95
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Guide for
1
Spiking Organics into Aqueous Samples
This standard is issued under the fixed designation D 5788; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope a homogeneous solution of analyte and sample. Meaningful
recovery data cannot be obtained if an aqueous solution or
1.1 This guide covers the general technique of “spiking”
homogeneous suspension of the analyte of interest in the
aqueous samples with organic analytes or components. It is
sample cannot be attained.
intended to be applicable to a broad range of organic materials
1.5 Matrix spiking may be performed in the field or in the
in aqueous media. Although the specific details and handling
laboratory, depending on which part of the analytical process is
procedures required for all types of compounds are not
to be tested. Field spiking tests the recovery of the overall
described, this general approach is given to serve as a guideline
process, including preservation and shipping of the sample.
to the analyst in accurately preparing spiked samples for
Laboratory spiking tests the laboratory process only. Spiking of
subsequent analysis or comparison. Guidance is also provided
sample extracts, concentrates, or dilutions will test only that
to aid the analyst in calculating recoveries and interpreting
portion of the process subsequent to the addition of the spike.
results. It is the responsibility of the analyst to determine
1.6 The values stated in SI units are to be regarded as the
whether the methods and materials cited here are compatible
standard. The values given in parentheses are for information
with the analytes of interest.
only.
1.2 The procedures in this guide are focused on “matrix
1.7 This standard does not purport to address all of the
spike” preparation, analysis, results, and interpretation. The
safety concerns, if any, associated with its use. It is the
applicability of these procedures to the preparation of calibra-
responsibility of the user of this standard to establish appro-
tion standards, calibration check standards, laboratory control
priate safety and health practices and determine the applica-
standards, reference materials, and other quality control mate-
bility of regulatory limitations prior to use.
rials by spiking is incidental. A sample (the matrix) is fortified
2. Referenced Documents
(spiked) with the analyte of interest for a variety of analytical
and quality control purposes. While the spiking of multiple
2.1 ASTM Standards:
2
sample test portions is discussed, the method of standard
D 1129 Terminology Relating to Water
2
additions is not covered.
D 1193 Specification for Reagent Water
1.3 This guide is intended for use in conjunction with the D 3694 Practices for Preparation of Sample Containers and
3
individual analytical test method that provides procedures for for Preservation of Organic Constituents
analysis of the analyte or component of interest. The test D 3856 Guide for Good Laboratory Practices in Laborato-
2
method is used to determine an analyte or component’s ries Engaged in Sampling and Analysis of Water
background level and, again after spiking, its now elevated D 4375 Terminology for Basic Statistics in Committee
2
level. Each test method typically provides procedures not only
D-19 on Water
for samples, but also for calibration standards or analytical E 200 Practice for Preparation, Standardization, and Stor-
control solutions, or both. These procedures include prepara-
age of Standard and Reagent Solutions for Chemical
2
tion, handling, storage, preservation, and analysis techniques. Analysis
These procedures are applicable by extension, using the
3. Terminology
analyst’s judgement on a case-by-case basis, to spiking solu-
3.1 Definitions—For definitions of terms used in this guide,
tions, and are not reiterated in this guide. See also Practice
refer to Terminology D 1129.
E 200 for preparation and storage information.
3.2 Definitions of Terms Specific to This Standard:
1.4 These procedures apply only to analytes that are soluble
3.2.1 matrix spike, n—the quantity (mass) of a component
in water at the concentration of the spike plus any background
(analyte) of interest which is added to a sample (matrix) in
material, or to analytes soluble in a solvent that is itself
order to test bias as measured by recovery (of that component
water-soluble. The system used in the later case must result in
under spe
...