CONSOLIDATE SCIENCES, INC.
QUALITY ASSURANCE/QUALITY CONTROL
Prepared By: Michael A. Sommer, Ph.D.

 

Organization and Responsibility
Performance And Systems Audits
Corrective Action
QA/QC Reporting To Management And Client
Quality Control Program For The Analysis Of RCRA Samples
Other Quality Control Programs At Consolidated Sciences
Definitions
QUALITY CONTROL
Analytical Quality Control
Spikes, Blanks and Duplicates
Field Duplicate Samples
Blanks
Surrogate Compounds
Quality Control Reference Sample
Check standard
Clean-Ups
Column Check Sample
Column Check Blank
Determinations of Instrument Adjustment, Tuning, and Alignment
Calibration
Additional QC Requirements for Inorganic Analysis
Additions Quality Control Requirements for Organic Analysis
Identification of Compounds
Quantification of Compounds
Method Detection Limit
Data Reporting
Quality Control Documentation
Analytical Results
Calibration
Column Check
Extraction/Digestion
Surrogates
Matrix-Spiked Samples
Check Standard
Blank
Chromatograms
Quantitative Chromatogram Report
Mass Spectrum
Metal Interference Check Sample Results and Detection Limit
QUALITY CONTROL REQUIREMENT FOR EPA VOLATILE ORGANIC ANALYSIS METHODS AND REPORTING REQUIREMENTS
DEFINITIONS AND CALCULATIONS


GENERAL ASPECTS OF QUALITY ASSURANCE AND QUALITY CONTROL

The terms quality assurance and quality control are frequently used interchangeably. In our context, quality control is used specifically to refer to the routine laboratory application of statistically based procedures to evaluate and control the accuracy of results from analytical measurements. Quality assurance refers to those activities necessary to generate confidence in the results of sampling and measurement. In general, this implies good laboratory practice. The implantation of the quality assurance plan ensures the validity of the data, which provides a reliable basis for decision-making.

A comprehensive laboratory quality assurance program must be based on careful attention to sample preservation techniques, sample chain of custody, use and care of instruments, glassware, chemicals data management, and laboratory personnel. Consolidated Sciences follows the strict QA/QC guidelines discussed in Test Methods for Evaluating Solid Waste Physical/Chemical Methods, (proposed update) 1987, third edition, EPA, PB89-148076, Washington, DC 20460 (SW 846) ; Methods for Chemical Analysis of Water and Wastes, 1983, Environmental Monitoring and Support Laboratory, Office of Research and Development, U.S. EPA, Cincinnati, Ohio 45268 and referenced in:

  1. Guidelines and Specification for Preparing Quality Assurance Program Plans, September 20, 1980, Office of Monitoring Systems and Quality Assurance, ORD, U.S. EPA, QAMS-004/80, Washington, DC 20460.
  2. Interim Guidelines and Specification for Preparing Quality Assurance Project Plans, December 29, 1980, Office of Monitoring Systems and Quality Assurance, ORD, U.S. EPA, QAMS-005/80, Washington, DC 20460.

Organization and Responsibility

As part of the analytical program at Consolidated Sciences, activities for the data generators data reviewers/approvers, and data user/requesters must be clearly defined. The data generator is typically the individual who carries out the analyses at the direction of the data user/requestor or a designate within or outside the laboratory. The reviewer/approver is responsible for ensuring that the data produced by the data generator meet agreed-upon specifications.

Responsibility for data review is assigned to the Consolidated Sciences Quality Assurance Officer or QA Manager. This individual has broad authority has broad authority to approve or disapprove project palns, specific analyses and final reports. The QA officer is responsible for reviewing and advising on all aspects of QA/QC, including:

Assisting the data requester in specifying the QA/QC procedure to be used during the program;

Making laboratory evaluations and submitting audit samples to assist in reviewing QA/QC procedures; and if problems are detected taking corrective action. Consolidated Sciences primary mission is laboratory analysis, however when large and complex amounts of data are generated from both field and laboratory activities, it is helpful to designate sampling monitors, analysis monitors, and quality control/data monitors to assist in carrying out the program or project: Consolidated Sciences can assist and designate the sampling monitor who is responsible for field activities. These duties include:

  • Determining (with the analysis monitor) appropriate sampling equipment and sample containers to minimize contamination
  • Ensuring that sample are collected, preserved, and transported as specified in the work plan
  • Checking that all sample documentation (labels, field notebooks, chain-of-custody records, packing lists) is correct and transmitting that information, along with the samples, to the analytical laboratory.

The analysis monitor is responsible for laboratory activities. These include:

  • Training and qualifying personnel in specified laboratory QC and analytical procedures, prior to receiving samples
  • Receiving samples from the field and verifying that incoming samples correspond to the packing list or chain-of-custody sheet; and verifying that laboratory QC and analytical procedures are being followed as specified in the work plan, reviewing sample and QC data during the course of analyses and, if questionable data exist, determining which repeat samples or analyses are needed.

The quality control and data monitor is responsible for QC activities and data management. These include:
Maintaining records of all incoming samples, tracking those samples through subsequent processing and analysis, and ultimately, appropriately disposing of those samples at the conclusion of the program;

Preparing quality control samples for analysis prior to and during program;

Preparing QC and sample data for review by the analysis coordinator and the program manager; and,

Preparing QC and sample data for transmission and entry into a computer database, if appropriate.

Performance And Systems Audits

The Consolidated Sciences QA/QC officer may carry out performance and/or systems audits to ensure that data of known defensible quality are produced.

Systems audits are qualitative evaluations of all components of field and laboratory quality control measurement system, and they determine if the measurement systems are being used appropriately. The audits may be carried out before all systems are operational, during the program, or after the completion of the program. Such audits typically involve a comparison of the activities given in the QA/QC plan with those actually scheduled or performed. A special type of systems audit is the data management audit. This audit addresses only data collection and management activities.

The performance audit is a quantitative evaluation of the measurement systems of a program. It requires testing the measurement systems of a program. It requires testing the measurement systems with samples of known composition or behavior to evaluate precision and accuracy. The performance audit is carried out by or under the auspices of the QA office without the knowledge of the analyst. Since this is seldom achievable, many variations are used that increase the awareness of the analyst as to the nature of the audit material.

Corrective Action

Corrective action procedures should be addressed in the program plan project. These should include the following elements:

The EPA predetermined limits for data acceptability beyond which corrective action is required;

Procedures for corrective action; and,

For each measurement system, identification of the individual responsible for approving the corrective action, if necessary.

The need for corrective action may be identified by system or performance audits or by standard QC procedures. The essential steps in the corrective action system are:

  • Identification and definition of the problem
  • Assignment of responsibility for investigating the problem
  • Investigation and determination of the cause of the problem
  • Determination of the corrective action to eliminate the problem
  • Assigning and accepting responsibility for implementing the corrective action
  • Implementing the corrective action and evaluating its effectiveness
  • Verifying that the corrective action has eliminated the problem

The QA officer should ensure that these steps are taken and that the problem that led to the corrective action has been resolved.

QA/QC Reporting To Management And Client

QA project program or plans should provide a mechanism for periodic reporting to management (or to the data user) on the performance of the measurement system and the data quality. Minimally, these reports include:

  • Periodic assessment of measurement quality indicators, i.e., data accuracy, precision and completeness
  • Results of performance audits
  • Results of system audits
  • Significant QA problems and recommended solutions

The final report for each project or data set includes a separate QA section which summarize data quality information.

Quality Control Program For The Analysis Of RCRA Samples

A RCRA required analytical quality control program at Consolidated Sciences supplies additional information that can be used to:

  • Evaluate the accuracy and precision of analytical data in order to establish the quality of the data
  • Provide an indication of the need for corrections to the analytical system, when comparison with existing regulatory of program criteria or data trends shows that activities must be changed or monitored to a different degree
  • To determine the effect of corrections to the analytical system

Other Quality Control Programs At Consolidated Sciences

Other guidance on Quality Assurance management and organization is available from the Agency and professional organizations such as ASTM, AOAC, APHA and FDA.

Definitions

ACCURACY: Accuracy is the nearness of a measurement or the mean (x) of a set of measurements to the true value. Accuracy is assessed by means of reference samples and percent recoveries.

ANALYTICAL BATCH: The basic unit for analytical quality control is the analytical batch is defined as samples that are analyzed together with the same method sequence and the same lots of reagents and with the manipulations common to each sample within the same time period or in continuous sequential time periods. Samples in each batch should be of similar composition (e.g. ground waste, sludge, ash, etc.)

BLANKS:

  1. CALIBRATION BLANK: Usually an organic or aqueous solution that is as free of the analyte as possible and prepared with the same volume of chemical reagents used in the preparation of the calibration standards and diluted to the appropriate volume with the same solvent (water or organic) used in the preparation of the calibration standard. The calibration blank is used to give the null reading for the instrument response versus concentration calibration curve. One calibration blank should be analyzed with each analytical batch, or every 20 samples, whichever is greater.
  2. EQUIPMENT BLANK: usually an organic or aqueous solution that is as free of analyte as possible and is transported to the site, opened in the field, and poured over or through the sample collection device, collected in a sample container, and returned to the laboratory. This serves as a check on sampling device cleanliness. One equipment blank should be analyzed with each analytical batch, or every 20 samples, whichever is greater.
  3. FIELD BLANK: Usually an organic or aqueous solution that is as free or analyte as possible and is transferred from one vessel to another at the sampling site and preserved with the appropriate reagents. This serves as a check on reagent and environmental contamination. One field blank should be analyzed with each analytical batch, or every 20 samples, whichever is greater.
  4. REAGENT BLANK: Usually an organic or aqueous solution that is as free of as possible and contains all the reagents in the same volume as used in the processing of the samples. The reagent blank must be carried through the complete sample preparation procedure and contains the same reagent concentrations in the final solution as in the sample solution used for analysis. The reagent blank is used to correct for possible contamination resulting from the preparation or processing of the sample. One reagent blank should be prepared for every analytical batch, or for every 20 samples, whichever is greater.
  5. TRIP BLANK: Usually an organic or aqueous solution that is as free of analyte as possible and is transported to the sampling site and returned to the laboratory without being opened. This serves as a check on sample contamination originating from sample transport, shipping, and from the site conditions. One trip blank should be analyzed with each analytical batch, or every 20 samples, whichever is greater.
  6. CHECK STANDARD: A material of known composition that is analyzed concurrently with test samples to evaluate a measurement process. An analytical standard that is analyzed to verify a standard should be analyzed with each analytical batch, or every 20 samples, whichever is greater.

MATRIX SPIKE: A Matrix Spike is employed to provide a measure of accuracy for the method used in a given matrix. A matrix spike analysis is performed by adding a predetermined quantity of stock solutions of certain analytes to a sample matrix prior to sample extraction/digestion and analysis. The concentration of the spike should be at the regulatory standard level or the PQL for the method. When the concentration of the analyte in the sample is greater than 0.1%, no spike of the analyte is necessary.

MDL: The method detection limit (MDL) is defined as the minimum concentrating of a substance that can be measured and reported with 99% confidence that the analyte concentration is greater than zero and is determined from analysis of a sample in a given matrix containing the analyte.

PRECISION: Precision is the agreement between a set of replicate measurements with out assumption or knowledge of the true value. Precision is assessed by means of duplicate/replicate sample analysis.

RCRA: The Resource Conservation And Recovery Act.

REAGENT GRADE: Analytical reagent (AR) grade, ACS reagent grade, and reagent grade are synonymous terms for reagents that conform to the current specifications of the Committee on Analytical Reagents of the American Chemical Society.

SAMPLES: The following diagram illustrates the difference between duplicate and replicate samples.

DUPLICATE SAMPLES: Duplicate samples are two separate samples taken from the same source (i.e. in separate containers and analyzed independently).

ENVIRONMENTAL SAMPLES: An environmental sample of field sample is a representative sample of any material collected from any source of which determination of composition or contamination is requested or required.
Drinking Water: Delivered water (treated or untreated) designated as potable water.
Water/Waste water: Raw source waters for public drinking water supplies, ground waters, municipal influents/effluents, and industrial influents/effluents.

Sludge: Municipal sludges and industrial sludges.
Waste: Aqueous and non-aqueous liquid wastes, chemical solids, contaminated soils, and industrial liquid and solid wastes.

REFERENCE SAMPLE: A Sample prepared from an independent standard at a concentration other than that used for calibration, but within the calibration range. An independent standard is defined as a standard composed of the analyte (s) of interest from a different source than that used in the preparation of standards for use in the standard curve. A quality control reference sample is intended as a independent check of technique, methodology, and standards and should be run with every analytical batch or every 20 samples, whichever is greater. This is applicable to all organic and inorganic analyses.

REPLICATE SAMPLES: Replicate samples are two aliquots taken from the same sample container and analyzed independently. In cases where aliquoting is impossible, as in the case of volatiles, duplicate samples must be taken for the replicate analysis.

STANDARD CURVE: A standard curve is a curve that plots concentrations of known analyte standards versus the instrument response to the analyte. Calibration standards are prepared by diluting the stock analyte solution in graduated amounts that cover the expected range of the sample being analyzed. Standards should be prepared at the frequency specified in the appropriate section. The calibration solvent must be prepared using the same type of acid or solvent and at the same concentration as will result in the samples following sample preparation. This is applicable to organic and inorganic chemical analyses.

SURROGATE: Surrogates are organic compounds that are similar to analytes of intereset in chemical composition, extraction, and chromatography, but which are not normally found in environmental samples. These compounds are spiked into all blanks, calibration and check standard, samples (including duplicates and QC reference samples) and spiked samples prior to analysis. Percent recoveries are calculated for each surrogate.

WATER: Any reference to water in a Chapter or Method refers to ASTM Type II reagent water (unless otherwise specified) which is free of contaminants that may interfere with the analytical test in question.

QUALITY CONTROL

The procedures indicated below are to be performed for all analyses. Specific instructions relevant to particular analyses are given in the pertinent analytical procedures in SW846.
Field Quality Control (When requested of Consolidated Sciences or to guide clients).
The sampling component of the Quality Assurance Program Plan (QAPP) shall include as appropriate:

  • Reference to or incorporation of accepted sampling techniques in the sampling plan
  • Procedures for documenting and justifying and field actions contrary to the accepted techniques
  • Documentation of all pre-field activities such as equipment check-out, calibrations, and container storage and preparation
  • Documentation of field measurement quality control data (quality control procedures for such measurements shall be equivalent or corresponding laboratory QC procedures)
  • Documentation of field activities
  • Documentation of post-field activities including sample shipment and receipt, field team de-briefing and equipment check-in
  • Generation of quality control samples including field duplicate samples, gield blanks, equipment blanks and trip blanks
  • The use of these samples in the context of data evaluation, with details of the methods employed (including statistical methods) and of the criteria upon which the information generated will be judged

Analytical Quality Control

A quality control operation or component is only useful if it can be measured or documented. The following components of analytical quality control are related to the analytical batch. The procedures described are intended to be applied to chemical analytical procedures.

Consolidated Sciences shall retain all quality control data and records required by these sections for three years from the time the results are reported. The data is available to the client or enforcement officials upon request.

Spikes, Blanks and Duplicates

General Requirements: These procedures shall be performed at least once with each analytical batch with a minimum of once per twenty samples.

Matrix-Spiked Samples: A matrix-spiked sample shall be analyzed with every analytical batch, or every 20 samples, whichever is more frequent. The sample shall be spiked with the analyte (s) of interest (see the appropriate SW 846 method). The sample to be spiked should be typical or representative of the batch. Ideally, it should be an intermediate between the cleanest and the most contaminated sample based on the best information available. It is recommended that the spike be made in a replicate of one of the field duplicate samples. The procedure is applicable to all organic or inorganic chemical analytes.

Field Duplicate Samples

Field Duplicate samples shall be analyzed with every analytical batch, or every 20 samples, whichever is greater. This procedure is applicable to all organic or inorganic chemical analytes.

Blanks

Each batch shall be accompanied by the reagent blank. The reagent blank shall be carried through the entire analytical procedure.

Surrogate Compounds

Every blank, standard, and environmental sample (including duplicates, QC reference samples, and check standards) shall be spiked with surrogate compounds prior to purging or extraction. Surrogates shall be spiked into samples according to the appropriate analytical methods. Surrogate spike recoveries shall fall within the control limits set by the laboratory (in accordance with procedures specified in the method or within + 20%) for samples falling within the quantification limits without dilution. Dilution of samples to bring the analyte concentration into the linear range of calibration may dilute the surrogates bellow the quantification limit; evaluation of analytical quality then will rely on the quality control embodied in the check, spiked and duplicate spiked samples. This is applicable only to organic analyses.

Quality Control Reference Sample

A quality control reference sample is a sample prepared from an independent standard at a concentration other than that used for calibration, but within the calibration range. An independent standard is defined as a standard composed of the analytes of interest from a different source than that used in the preparation of standards for use in the standard curve. A quality control reference sample is intended as an independent check of technique, methodology, and standards and should be run with every analytical batch or every 20 samples, whichever is greater. This is applicable to all organic and inorganic analyses.

Check standard

A standard of known concentration prepared by the analyst to monitor and verify instrument performance on a daily basis.

Clean-Ups

Quality control procedures described here are intended for absorbent chromatography and back extractions applied to organic extracts. All batches of adsorbents (Florisil, Alumina, Silica gel, etc.)

Column Check Sample

The elution pattern shall be reconfirmed with a column check of standard compounds after activation or deactivating a batch of absorbent. These compounds after activating or deactivating a batch of adsorbent. These compounds shall be representative of each elution fraction. Recovery as specified in the methods is considered an acceptable column check. A result lower than specified indicates that the procedure is not acceptable or has been misapplied. This is applicable to organic analyses only.

Column Check Blank

The column check blank shall be run after activation or deactivating a batch of adsorbent. This is applicable only to organic analyses.

Determinations of Instrument Adjustment, Tuning, and Alignment

Requirements and procedures are instrument and method specific. Analytical instrumentation shall be tuned and aligned in accordance with requirements specific to the instrumentation procedures employed. Individual determinative procedures shall be consulted. Criteria for initial conditions and for continuing confirmation conditions for methods within this manual are found in the appropriate procedures. This is applicable to all organic and inorganic analyses.

Calibration

Analytical instrumentation shall be calibrated in accordance with requirements specific to the instrumentation and procedures employed. Methods 6010, 7000 and 8000 as well as the appropriate analytical procedures shall be consulted for criteria for initial and continuing calibration.

Additional QC Requirements for Inorganic Analysis

Standard curves used in the determination of inorganic analytes shall be prepared as follows:

Standard curves derived from data consisting of one calibration blank and three concentrations shall be prepared for each analyte. The response for each prepared standard shall be based upon the average of three replicate readings of each standard. The standard curve shall be used with each subsequent analysis provided that the standard curve is verified by using at least one reagent blank and one standard at a level normally encountered or expected in such samples. The response for each standard shall be based upon the average of three replicate readings of the standard. If the results of the verification are not within + 10% of the original standard curve, a reference standard should be employed to determine if the discrepancy is with the standard or with the instrument. New standards should also be prepared on a quarterly basis at a minimum. All data used in drawing or describing the curve shall be so indicated on the curve or its description. A record shall be made of the verification. Standard deviations and relative standard deviations shall be calculated for the percent recovery of analytes from the spiked sample duplicates and from the check samples. These values shall be established for the twenty most recent determinations in each category.

Additions Quality Control Requirements for Organic Analysis

The following requirements shall be applied to the analysis of samples by gas chromatography, liquid chromatography and gas chromatography/mass spectrometry. The calibration of each instrument shall be verified at frequencies specified in the methods. A new standard curve must be prepared as specified in the methods.

The tune of each GC/MS System used for the determination of organic analytes shall be checked with 4-Bromofluorobenzene (BFB) for determination of volitiles and with decafluorotriphenylphosphine (DFTPP) for determinations of any analytes. If the system does not meet the required specification for one or more of the required ions, the instrument must be returned and rechecked before proceeding with sample analysis. The tune performance check criteria must be achieved daily or for each 12 hour operating period, whichever is more frequent.

Background subtraction should be straightforward and designed only to eliminate column bleed or instrument background ions. Background subtraction actions resulting in spectral distortions for the sole purpose of meeting special requirements are contrary to the objectives of Qual;ity Assurance and are unacceptable.

For determinations by HPLC or GC, the instrument calibration shall be verified as specified in the methods.

Identification of Compounds

Identification of all analytes must be accomplished with authentic standard of the analyte. When authentic standards are not available, identification is tentative.

For gas chromatographic determinations of specific analytes, the relative retention time of the unknown must be compared with that of an authentic standard. For compound confirmation, a sample and standard shall be re-analyzed on a column of different selectivity to obtain a second characteristic relative retention time. Peaks must elute within daily retention time windows to be declared a tentative or confirmed identification.

For gas chromatographic/mass spectrometric determinations of specific analytes, the spectrum of the analyte should conform to a literature representation of the spectrum or to a spectrum of the authentic standards.

Quantification of Compounds

The procedures for quantification of analytes are discussed in the appropriate general procedures (7000, 8000) and the specific analytical methods.

In some situation in the course of determining metal analytes, matrix-matched calibration standards may be required. These standards shall be composed of the pure reagent, approximation of the matrix, and reagent addition of major interference in the samples. This will be stipulated in the procedures.

Estimation of the concentration of an organic compound not contained within the calibration standard may be accomplished by comparing mass spectral response of the compound with that of an internal standard. The procedure is specified in the methods.

Method Detection Limit

For operational purposes, when it is necessary to determine the method detection limit in the sample matrix, the MDL defined shall be determined by multiplying by 7 the standard deviation obtained from the triplicate analyses of a matrix spike containing the analyte of interest at a concentration three to five times the estimated MDL.

Determine the estimated MDL as follows:

Obtain the concentration value that corresponds to:

  1. An instrument signal/noise ration within the range of 2.5 to 5.0, or
  2. The region of the standard curve where there is a significant change is sensitivity, i.e., a break in the slope of the standard curve

Determine the variance (S2) for each analyte as follows:

Determine the standard deviation (S) for each analyte as follows:

S = (S2) ½

Determine the MDL for each analyte as follows:

MDL = t(n-1, 1-a = 0.99) (S)

where MDL = t(n-1, 1-a = 0.99) = 6.965 for three replicates as determined from the table of student’s values at the 99% level.

Data Reporting

The requirement of reporting analytical results on a wet-weight or a dry weight basis is dictated by factors such as: sample matrix; program or regulatory requirement; and objectives of the analysis.

Analytical results shall be reported with the percent moisture or percent solid content of the sample.

Quality Control Documentation

The following sections list the QC documentation that comprises the complete analytical package; this package can be obtained from Consolidated Sciences upon request.

Analytical Results:

  • Analyte concentration
  • Sample weight
  • Percent water (for non-aqueous samples when specified)
  • Final volume of extract or diluted sample
  • Holding times

Calibration:

  • Calibration curve or coefficients of the linear equation that describes the calibration curve
  • Correlation coefficients of the linear equation which describes the calibration curve
  • Concentration/response data (or relative response data) of the calibration check standards, along with dates on which they were analytically determined

Column Check:

Results of column chromatography check, with the chromatogram

Extraction/Digestion:

Date of the extraction for each sample

Surrogates:

Amount of surrogate spiked, and percent recovery of each surrogate

Matrix-Spiked Samples:

Amount spiked, percent recovery, and relative percent difference for each compound in the spiked samples for the analytical batch

Check Standard:

Amount spiked, and percent recovery of each compound spiked

Blank:

Identity and amount of each constituent

Chromatograms:

All chromatograms for reported results, properly labeled with:

  • Sample Identification
  • Method Identification
  • Identification of retention time of analyte on the chromatograms

Quantitative Chromatogram Report:

Retention time on analyte
Amount injected
Area of appropriate calculation of detection response
Amount of analyte found
Date and time of injection

Mass Spectrum:

Spectra of standards generated from authentic standards (one for each report for each compound detected)
Spectra of analytes from actual analyses
Spectrometer identifier

Metal Interference Check Sample Results and Detection Limit:

Analyte detection limits with methods of estimation
Results of standard additions
Results of serial dilutions
Instrument detection limits

 

QUALITY CONTROL REQUIREMENT FOR EPA VOLATILE ORGANIC ANALYSIS METHODS AND REPORTING REQUIREMENTS

 
Procedure Method 624 Method 8240
Holding Time 14 Days 14 Days

Tuning

  • Requirement
  • Frequency
  • Criteria
50 ppb BFB
Daily
Table 1
50 ppb BFB
12 Hours
Table 1

Initial Calibration (IC)

  • Requirement
  • Levels
  • Criteria: RRF
All Analytes
3:10, 20, 40 ppb
4 SPCC > 0.300
All Analytes
5:10, 20, 30, 40 ppb
4 SPCC > 0.300
Bromoform > 0.250
6 CCC < 30%
% RSD All < 35% 6 CCC < 30%

Continuing Calibration (CC)Requirement

  • Includes
  • Frequency
  • Criteria: RRF

    %D
    IS
    IS RT

20 ppb QC check
All Analytes
Daily
4 SPCC > 0.300
Bromoform > 0.250
6CCC +/- 25%
redue
or new IC
-50% to +100% of
area of last CC
+/-30 sec of last CC
20 ppb QC check
All Analytes
12 Hours
4 SPCC > 0.300
Bromoform > 0.250
6CCC +/- 25%
redue
or new IC
-50% to +100% of
area of last CC
+/-30 sec of last CC

Method Blank

  • Frequency
  • Criteria
Daily Interference free 12 Hours Interference free

Spike

  • Frequency
  • Concentration
  • Criteria
Daily 20 ppb or 1-5x MDL 80-120% recovery 12 Hours 20 ppb or 1-5x MDL 80-120% recovery

Duplicate

  • Frequency
  • Criteria
5% samples or 1 per batch (whichever is greater)%Rec 80-120%;RSD < 20% 5% samples or 1 per batch (whichever is greater)%Rec 80-120%;RSD < 20%

Sample Analysis

  • Qualitative ID
  • IS area
  • IS RRT
  • Surrogate Criteria
  • Quantitative

RT within +/-30
Sec of standard RT
3 characteristic ions in sample within +/-20% relative intensity
ns
ns
80-120% within cal. range

RRT within +/-0.06
RRT units of
standard RRT
Ions > 10% in std. present with +/-20% of ions in std
ns
ns
80-120%
within cal. range

QC Check Sample

  • Frequency
  • Criteria
20 ppb
5% samples
Method QC limits
20 ppb
Each sample batch
Specified QC limits

Initial Demonstration of Competency

  • Requirement
  • Frequency
  • Criteria
4 replicate spikes
at 20 ppb
initial, one time
% Rec and SD limits
4 replicate spikes
at 20 ppb
initial, one time
% Rec and SD limits
Method Detection Limit Determination Required May be required for specific matrices
Other QC
% Moisture
Field Duplicates Equipment blanks,
trip blanks, field cups
required for all solids

DEFINITIONS AND CALCULATIONS

CC Calibration check
ns Not specified
SPCC System performance check compounds
CCC Calibration check compounds
DL Detection limit
RRF Relative response factor
BBF 4-bromofluorobenzene
RRT Relative retention time
MDL Method detection limit
PQL Practical quantification limit
%RSD (Standard deviation of 5 CCC/average 5 CCC) x 100
CCC 1,1-dichloroethane, chloroform, 1,2-dichloropropane, toluene, ethylbenzene, vinyl chloride
SPCC chloromethane, 1,1-dichloroethane, bromoform, 1,1,2,2-tetrachloroethane, chlorobenzene
%D 100 x (average RFi – RFc)/average RFi
average RFi average initial calibration
RFc Current verification
RF (Ax x Cis) (Ais x Cx)
RF Response factor
Ax Area of characteristic ion being measures
Ais Area of internal standard for comparison
Cis Concentration (ppv) of the internal standard
Cx Concentration of ion being measures
IS Internal standard
IS RT Internal standard retention time
RSD Standard deviation of set of values/average of the values
 
 

 

Copyright © 1998-2008 Last modified: July 2008
This web site is maintained by Consolidated Sciences
webmaster@conscicorp.com