Table of Contents

Section Page

Title Page 1 

Table of Contents 2 

1 Project Management 3 

 1.1 Project Description 3 

 1.2 Distribution List 3 

 1.3 Project Organization 4 

 1.4 Problem Definition/Background 4 

 1.4.1 Constituents for which EPA Listing is based 4 

 1.4.2 Waste Generation Process/Treatment Process 5 

 1.4.3 Constituents of Concern and Quantification Methods 6 

 1.4.4 Information on Waste Variability over Time 6 

 1.4.4.1 Chemical Authorization Process 6 

 1.4.4.2 Environmental Impact Assessment Process 7 

 1.4.5 Proposed Waste Disposal Location, if Delisted: 7 

 1.5 Project Description and Schedule 7 

 1.6 Quality Objectives and Criteria for Measurement Data 7 

 1.6.1 Objectives and Project Decisions 7 

 1.6.2 Action Limits/Levels 8 

 1.6.3 Measurement Performance Criteria/Acceptance Criteria 8 

 1.7 Special Training Requirements/Certification 8 

1.8 Documents and Records 8 

2 Data Generation and Acquisition 9 

 2.1 Sampling Design 9 

2.2 Sampling Methods 9 

 2.3 Sample Handling and Custody 10 

 2.4 Analytical Methods 10 

 2.5 Quality Control Requirements 10 

 2.6 Instrument/Equipment Testing, Inspection, and Maintenance 10 

 2.7 Data Management 10 

3 Assessment and Oversight 12 

 3.1 Assessment/Oversight and Response Actions 12 

 3.2 Reports to Management 12 

4 Data Review and Usability 12 

 4.1 Data Review, Verification, and Validation Requirements 12 

 4.2 Verification and Validation Methods 12

Attachments 

 1 Wastewater Treatment Process Overviews 

 2 Table 1 - IBM Essex Junction, VT Sludge Delisting Constituents of Concern 

 3 Chemical Management Process Overview 

 4 Laboratory (Endyne) Quality Systems Manual 

 5 Laboratory (Endyne) Method SOPs (9) and associated QC tables (3) 

 1311, 6010, 8260, 8270, 3060A, 7196A, 7471A, 9012A 

 6 Endyne QA/QC Elemental Analysis of Water and Sludge Samples
1 PROJECT MANAGEMENT 

1.1 Project Description

The waste consists of industrial wastewater treatment sludge generated from the treatment of 

wastewaters from semiconductor manufacturing operations. The applicable RCRA waste code for this 

waste is F006 (wastewater treatment sludges from electroplating operations). However, the sludge is a 

functionally nonhazardous waste stream and as generated meets the treatment standards outlined in 40 

CFR Part 268 Subpart D for F006 nonwastewaters. It is proposed to collect representative samples of 

sludge for laboratory analysis, and provide new sludge characterization data that will lead to delisting 

the sludge to a nonhazardous classification. 

1.2 Distribution List

Name: David Kost 

Title: Chief Industrial Wastewater Treatment Operator 

Organization: IBM Corporation 

Contact Information: 1000 River Street Mailstop 966A Essex Junction, VT 05452 

(802) 769-2761 dlkost@us.ibm.com 

Name: Candice Callahan 

Title: Hazardous Waste Program Manager 

Organization: IBM Corporation 

Contact Information: 1000 River Street Mailstop 966A Essex Junction, VT 05452 

(802) 769-0579 ccallaha@us.ibm.com 

Name: Tim Baechle 

Title: Manager of Energy, Environmental and Chemical Programs 

Organization: IBM Corporation 

Contact Information: 1000 River Street Mailstop 966A Essex Junction, VT 05452 

(802) 769-4153 tbaechle@us.ibm.com 

Name: Roland Luxenberg, P.E. 

Title: Consulting Engineer, Field Sampling 

Organization: Aquaterra 

Contact Information: 255 Flynn Avenue Burlington, VT 05401 

(802) 238-0071 roland@luxenberg.us 

Name: Harry Locker 

Title: Chemist 

Organization: Endyne, Inc. 

Contact Information 160 James Brown Drive Williston, VT 05445 

(802) 879-4333 hlocker@endyne.com 
Name: Sharon Leitch 

Title: EPA Project Manager 

Organization: EPA New England Region 1 

Contact Information: 5 Post Office Square Suite 100 (OSRR07-1) Boston, MA 02109-3912 

(617) 918-1647 leitch.sharon@epa.gov 

1.3 Project Organization

Project Manager David Kost (IBM, Chief Industrial Wastewater Treatment Operator) will be the 

responsible official for this project overseeing the overall project and budget, as well as tasking 

contractors with work required to complete this project. He will communicate project needs to the 

contractor’s project managers. 

QA Manager Candice Callahan (IBM, Hazardous Waste Program Manager) will be responsible for 

reviewing and approving the QA Project Plan. She may provide technical input on proposed sampling 

design, analytical methodologies, and data review. She may assist with coordinating laboratory 

services. 

Contractor Project Manager Roland Luxenberg (Aquaterra, Field Sampling) and Mark Fausel

(Endyne, Laboratory Analysis) will have overall responsibility for assigning appropriate personnel to 

complete the tasks included in this plan. They will ensure that the project budget is adhered to. They 

will communicate with the Project Manager on work accomplished in this plan and any problems or 

deviations that need to be resolved. Roland will be responsible for collecting sludge samples in 

accordance with this document. Mark will be responsible for assigning appropriate laboratory staff to 

perform the analyses specified in this plan. 

EPA Project Manager Sharon Leitch (EPA, Project Manager) will have the responsibility to see that the 

final report is reviewed, to inform IBM of any reporting deficiencies and assist in their resolution, and 

will inform IBM if sludge is delisted (or if not, reason(s) why not). 

1.4 Problem Definition/Background

The waste proposed for delisting consists of industrial wastewater treatment sludge generated from the 

treatment of wastewaters from semiconductor manufacturing operations. The sludge is primarily made 

up of lime added during the wastewater treatment process. The sludge is typically 40% solids (ranging 

from 20 to 55%), with a pH of 12 (range of 5 to just under 12.5). The applicable RCRA waste code for 

this waste is F006 (wastewater treatment sludges from electroplating operations). 

 1.4.1 Constituents for which EPA Listing is based 

The hazardous constituents that were the basis for the F006 listing are found in 40 CFR 261, Appendix 

VII (cadmium, hexavalent chromium, nickel, and complexed cyanide). These constituents are not 

present in the sludge at concentrations that would impact human health or the environment. The sludge 

is a functionally nonhazardous waste stream and as generated meets the treatment standards outlined in 

40 CFR Part 268 Subpart D for F006 nonwastewaters. The sludge is not regulated for any hazardous 

characteristics, such as a toxicity characteristic metal (40 CFR 261.24). 
 1.4.2 Waste Generation Process/Treatment Process 

The sludge is generated from the combination of three separate wastewater treatment processes. The 

sludge from each process is combined, thickened/conditioned, and pressed to generate this waste stream. 

The majority of sludge mass is from the industrial wastewater treatment plant (IWTP) process. The 

smaller contributors are the biological wastewater treatment (BWTP) process and the chemical 

mechanical polishing (CMP) microfiltration process. 

Sludge is generated on a continual basis, as the IBM Essex Junction manufacturing facility operates 365 

days per year 24 hours per day. Approximate average waste generation annually (over previous 5 years) 

is 7 million pounds per year, with an approximate maximum waste generation rate (over previous 5 

years) of 10 million pounds per year (these values include sludge generated from periodic cleaning and 

maintenance of the two 7.5 million gallon IWTP process water storage tanks). 

Chemical Mechanical Polishing (CMP) Pretreatment Waste

The CMP process is used to smooth the surface of the wafer using a combination of chemical etching 

and mechanical polishing. The CMP waste treatment system receives wastewater from 

chemical/mechanical polishing tools (CMP) used in semiconductor manufacturing. This system filters 

ferric nitrate solids, copper particles, silica solids, copper sulfate plating bath solutions (30-50 gallons 

per day), and tungsten solids. The CMP treatment system also filters some organics present in the 

polishing slurries (polyacrylic acid, sodium octylsulfate, benzotriazole, and tetramethylammonium 

hydroxide). The filters are backflushed after each approximately 20 minute cycle, producing sludge 

with a pH of 7.5 to 8. Periodic cleaning of the filters with sulfuric acid may temporarily drop the pH of 

the sludge in the CMP thickener to around 5. The CMP process treats approximately 100,000 gallons of 

water per day. 

Biological Wastewater Treatment Plant (BWTP)

The three major waste streams treated at the BWTP are concentrated waste (CW), dilute organic waste 

(DOW), and sanitary waste. All three wastes are mixed and equalized prior to treatment in Sequential 

Batch Reactors (SBR). The BWTP process treats approximately 120,000 gallons of water per day. 

Concentrated Waste (CW) 

The concentrated waste stream consists of waste from semiconductor and mask manufacturing 

photolithography develop steps, chemical wafer cleaning, etching, and stripping operations, and parts 

decontamination. The major chemical constituents in the waste stream are tetramethylammonium 

hydroxide (TMAH), hydrofluoric acid, phosphoric acid, glacial acetic acid, ammonium hydroxide, and 

hydrogen peroxide. The fluoride in the CW waste is treated by flash mixing with lime slurry to produce 

calcium fluoride, a solid which precipitates in the treatment system and is accumulated in the sludge. 

These inorganic wastes are biodegradable and treated by the microorganisms in the BWTP process. The 

CW process contributes approximately 40,000 gallons of water per day to the BWTP process. 

Dilute Organic Waste (DOW) 

The DOW waste stream receives discharges from chemical wafer cleaning and stripping, Deep UltraViolet (DUV) photolithography waste, air abatement adsorber decant waters, and facility chilled water 
and boiler maintenance operations. The major chemical constituents in the DOW waste stream are 

isopropyl alcohol (IPA), propylene glycol monomethyl ether acetate (PGMEA), gamma-butyrolactone 

(GBL), n-butyl acetate (NBA), and propylene and ethylene glycols. These organic wastes are 

biodegradable and treated and consumed by the microorganisms in the BWTP process. The DOW 

process contributes approximately 5,000 gallons of water per day to the BWTP process. 

Sanitary Waste 

The sanitary waste stream consists of discharges from the site cafeterias and restrooms. These typical 

sanitary wastes are biodegradable and treated by the microorganisms in the BWTP process. 

Industrial Wastewater Treatment Plant (IWTP)

The IWTP waste stream receives discharges from chemical wafer and mask manufacturing cleaning, 

etching, and stripping, photolithography waste, chemical etching and mechanical polishing, air 

abatement scrubbers, effluent from the CMP and BWTP treatment systems, wafer rinse, and facility 

maintenance operations. The major chemical constituents in the IWTP waste stream are acids, bases, 

deionized water rinses, metals (Cu, Fe, Pt, etc.), and deionized water system reject water. The 

wastewaters also include rinse waters from copper electroplating manufacturing operations (1000 

gallons per day) and wastewaters from acid etching of a thin platinum film and the subsequent rinse step 

(800 gallons per day). The IWTP treatment process consists of a sodium bisulfite pretreatment step to 

reduce hydrogen peroxide and chlorine. This is followed by acid and base neutralization, solids 

precipitation, and a final pH adjustment step. The IWTP process treats approximately 3 million gallons 

of water per day. 

See Attachment 1 for the wastewater treatment process overviews. 

1.4.3 Constituents of Concern and Quantification Methods 

The constituents of concern are listed in Table 1 (Attachment 2). Also included in this table is the 

selection basis for each constituent. 

 1.4.4 Information on Waste Variability over Time 

Potential variability is identified and managed through the following review processes. 

 1.4.4.1 Chemical Authorization Process 

Before any chemical is brought onto the IBM campus for use by IBM personnel, contractors, or tenants, 

the chemical is identified and authorized through the company’s on-line chemical information and 

authorization management system. This review process identifies hazards and environmental issues 

associated with the use of a particular chemical. In addition, the expanded use of any existing chemical 

in a new process at the facility is also reviewed. 

This system also provides access to supplier Material Safety Data Sheets (MSDS), which contain 

information about the chemical’s health and safety hazards, storage compatibility, and handling 

characteristics. The authorization review process includes consideration of how any waste to be 

generated will be managed. Additional information may be obtained from the requester or the chemical 
supplier when necessary to properly characterize the waste expected to be generated. 

 1.4.4.2 Environmental Impact Assessment Process 

The objectives of conducting a process environmental impact assessment are to identify potential 

significant impacts to the environment from IBM processes; to consider feasible alternatives for 

avoiding potential impacts; and to ensure compliance with applicable legal and regulatory requirements. 

Installation, modification, or relocation of chemical-using equipment proposed to discharge waste to any 

drains leading to the wastewater treatment facility is managed via an on-line environmental impact 

assessment system. The hazardous waste engineer or coordinator must review and approve all such 

waste discharges. These reviews are conducted on an ongoing, real-time basis to insure that 

compatibility and impacts are assessed. 

See Attachment 3 for the chemical management process overview. 

 1.4.5 Proposed Waste Disposal Location, if Delisted: 

The existing disposal locations (Stablex Canada in Blainville, Quebec or Chemical Waste Management 

in Model City, NY) could continue to be used, in addition to potential new opportunities. The preferred 

future use for the delisted sludge would be as a raw material in a cement kiln. 

1.5 Project Description and Schedule

Field sampling will commence within 2 weeks of QAPP approval. Four (4) sampling events will be 

equally spaced out over a 4 week period. Each sampling event will be completed within two days, with 

samples delivered to the laboratory within the sampling week. Analysis for each sample event will be 

completed within 3 weeks. A summary table and brief narrative, along with laboratory reports, will be 

submitted within 4 weeks following receipt of the final laboratory results. 

The following is a timetable summary, with elapsed time from QAPP approval: 

Field sampling commences: 2 weeks 

Field sampling completed: 6 weeks 

Lab analysis commences: 3 weeks 

Lab analysis completed: 9 weeks 

Report submittal: 13 weeks 

1.6 Quality Objectives and Criteria for Measurement Data

1.6.1 Objectives and Project Decisions 

The objective of this study is to demonstrate that the industrial wastewater treatment sludge currently 

regulated as hazardous can be delisted to a nonhazardous waste. Samples will be collected and results 

compared to target levels to be determined by EPA from an EPA model, in addition to already stated 

toxicity characteristic concentrations. If all sludge concentrations are below target levels and toxicity 

characteristic concentrations, then enough information will exist to allow for delisting of the sludge. 
 1.6.2 Action Limits/Levels 

The EPA will determine target levels through the use of their internal model. 

 1.6.3 Measurement Performance Criteria/Acceptance Criteria 

The constituents of concern are identified in Table 1 (Attachment 2). Table 1 shows each constituent, 

holding times, extraction and analysis methods, the expected method reporting limit, and quality control 

(QC) criteria. In their reporting, the laboratory will identify which QC criteria, if any, were not initially 

satisfied, and what steps were taken to insure that overall accuracy was maintained. 

1.7 Special Training Requirements/Certification

Field sampling and laboratory analysis will follow standard techniques, so no special training or 

laboratory certifications are required. The laboratories will have National Environmental Laboratory 

Accreditation Conference (NELAC) certification (if applicable) for all analysis. 

1.8 Documents and Records

The approved QAPP will be distributed to key personnel by email. Field sampling documentation will 

be contained on the chain-of-custody, which will be included in the laboratory data package. The data 

package will consist of the results, along with appropriate QC data. This will be transmitted as a pdf file 

to the IBM project manager. The final report, with appropriate narrative, summary table, and laboratory 

data package, will be emailed to EPA New England Region 1. 

All files (both electronic and hardcopy) will be part of IBM Corporation Records Retention Program. A 

hardcopy of the QAPP and final report will be kept in on-site files for a minimum of 3 years.
 

2 DATA GENERATION AND ACQUISITION 

2.1 Sampling Design

Wastewater has at least one day hydraulic residence time before and during treatment (3 million gallons 

per day (MGD) passing through one or two 7.5 million gallon (MG) process water storage tanks and a 1 

MG equalization basin prior to treatment in a 0.3 MG clarifier). There is estimated to be just over four 

days of solids residence time within the process tanks, based on 3000 mg/l total suspended solids (TSS) 

in the 0.3 MG clarifier, 30,000 mg/l TSS in the 0.109 MG gravity thickeners, and eight thousand pounds 

of sludge solids (dry weight) generated per day. Sludge is generated in stirred (biological, sequential 

batch reactor) or raked (industrial, clarifiers and thickeners) tanks, so sludge resulting from a filter press 

cycle is expected to be uniform. Pressed sludge drops into a wheeled trailer, with about five to six filter 

press cycles required to fill a trailer over the course of three to four days. 

It is relatively easy to obtain a systematic random grid sample of the pressed sludge in a trailer by 

collecting samples of pressed sludge at the end of a filter press cycle before it drops into the trailer. In 

addition, the primary contaminants of concern are stable, so multiple filter press cycles can be 

composited over time. It is proposed that during each filter press cycle, samples be obtained from a 

random filter press plate towards each end, and in the middle of a filter press (three samples). During 

the next filter press cycle, another three random filter press plates would be sampled, and again for a 

third filter press cycle, for a total of nine samples to make one composite sample. This sample 

technique will be repeated every week, so that four composite samples are collected over a four week 

period. 

2.2 Sampling Methods

Prior to sampling, a glass bottle will be labeled with a filter press location, date, and time. Each sample 

from a random filter press plate will be collected by pressing a thin walled plastic cylinder into the 

pressed sludge, then removing the cylinder. A total of three (3) locations at one filter plate will be 

sampled, so that the 12 grams of sludge per sample tube (using a 2.5 cm diameter sample tube pressed 5 

cm into the sludge, and using a sludge density of 0.5 grams per cubic centimeter) will accumulate the 

300 grams of required sludge (3 plates/cycle x 3 sample tubes per plate x 3 cycles x 12 grams per 

sample tube). The retained sludge will be extruded into the sample bottle with a plastic ram. After 

sampling is completed for a filter press cycle, the sampling equipment will be placed in another glass 

bottle, and all bottles (samples, sampling device) will be stored in a refrigerator, with a partially 

completed chain-of-custody. The chain-of-custody form will be used to document the filter plates 

sampled, along with date and time, for each filter press cycle. 

Additional bottles will be filled for the second and third filter press cycle. The sample bottles will then 

be placed in the sample refrigerator along with the completed chain-of-custody prior to laboratory 

courier pick-up. Prior to the next sample collection, the sampling equipment will be cleaned with soap 

and tap water. 
2.3 Sample Handling and Custody

Once picked up by the laboratory their general sample handling procedures will be followed. These 

procedures can be found in their Quality Systems Manual (Attachment 4). For TCLP VOC and SVOC 

analysis, one sample core from each sample bottle will be used (1 core/bottles x 9 bottles x 12 

grams/core). For VOC/SVOC analysis, a 1/4 section from a sample core will be collected from each 

sample bottles (taking one core, cutting it in half, then cutting it in half again). All remaining sample 

core material from all bottles will be placed together, manually disaggregated using plastic tools until all 

sample fragments are less than 1 cm, then placed into a glass bottle and manually agitated for 1 minute 

to insure complete mixing prior to aliquots removed for all other sample analyses. 

2.4 Analytical Methods

Each sample will be analyzed for a variety of metals (TCLP and total), cyanide (total and amenable to 

chlorination), semi-volatile organic compounds (TCLP and total), and volatile organic compounds 

(TCLP and total); see Table 1 (Attachment 2). Analytical procedures will follow general analysis 

guidelines found in the laboratory's Quality Systems Manual (Attachment 4), and those found in the 

method Standard Operating Procedures (SOPs) (Attachment 5). 

The sub-contracted laboratory (VHG Labs, Inc of Manchester, NH) that will analyze for total content of 

two metals (platinum and tin) will use the same extraction and analysis methods (listed in Attachment 2) 

as Endyne for total metals analysis, and will meet or exceed Endyne's quality control criteria for total 

metals analysis. Endyne is the contracted lab (by IBM) and will be ultimately responsible for the 

QA/QC of any sub-contracted analysis. Attachment 6 (Endyne QA/QC Elemental Analysis of Water 

and Sludge Samples) describes Endyne's method associated with the analysis of the sub-contracted 

metals. 

2.5 Quality Control Requirements

Quality Control requirements are found in the method SOPs and associated QC criteria tables 

(Attachment 5). These include laboratory reagent blanks, laboratory fortified blanks, calibration 

check/verification, calibration blank, interelement check standard, matrix spike, matrix spike duplicate, 

duplicate analysis, internal standards, and surrogate standards. The acceptance criteria are summarized 

in Table 1 (Attachment 2). In addition, a field duplicate will be collected during the first sampling 

event. Sampling will involve collecting an additional three (3) sample tubes at the same filter press 

plate used for the regular sample.

2.6 Instrument/Equipment Testing, Inspection, and Maintenance

Laboratory equipment testing, inspection, and maintenance will follow those contained in the 

laboratory's Quality Systems Manual and method SOPs (Attachments 4 and 5).

2.7 Data Management

The IBM Project Manager will receive the laboratory data package. The IBM Project Manager will 

review the package with assistance from IBM's Hazardous Waste Program Manager. The IBM Project 

Manager will enter the data into a summary spreadsheet, stored on both an office computer and on a 
company-wide accessible electronic data storage area. The IBM Project Manager’s data entry will be 

checked by the Hazardous Waste Program Manager. The IBM Project Manager will communicate with 

the laboratory if any deviation from the QC criteria is found that has not already been addressed by the 

laboratory. 

Once the laboratory data is considered complete, the IBM Project Manager will prepare the summary 

narrative, and then distribute the draft summary narrative, results summary spreadsheet, and laboratory 

data package for IBM internal review. Once all reviewers have responded with comments or concerns, 

the IBM Project Manager will resolve these issues as needed. The IBM Project Manager will send out 

final documents to EPA New England Region 1.
3 ASSESSMENT AND OVERSIGHT 

3.1 Assessment/Oversight and Response Actions

The IBM Project Manager will oversee sampling procedures on one or more of the four sample 

collection efforts. He will inform field sampling personnel of deviations from proposed sampling 

methods, and with assistance from Aquaterra will determine if these deviations are significant. After 

review of the first laboratory data package, the IBM Project Manager will contact Endyne if reporting 

times are not met, if insufficient documentation is received, or if quality control deviations are not 

adequately explained in the reporting narrative. If QC criteria are not met or adequately explained, the 

IBM Project Manager will delay further field sampling or stop additional laboratory analysis until QC 

deviations are resolved. The IBM Project Manager will contact the IBM Environmental Programs and 

Operations Manager and the EPA Project Manager if the timetable will be exceeded by more than one 

month, or if changes need to be made in the QC criteria as the result of matrix peculiarities. 

3.2 Reports to Management

The IBM Project Manager will prepare an interim memorandum if there are quality control issues in 

field sampling or laboratory analysis, with assistance from IBM's Hazardous Waste Program Manager. 

This will be sent to the IBM Environmental Programs and Operations Manager and discussed with the 

relevant Contractor Project Manager. 

4 DATA REVIEW AND USABILITY 

4.1 Data Review, Verification, and Validation Requirements

The field inspection of sampling events and comparison of the laboratory data package to QC criteria in 

Table 1 (Attachment 2) will be used to determine the validity of the final results. 

4.2 Verification and Validation Methods

In their results narrative, the laboratory will identify analyses not meeting QC criteria, and corrective 

steps they used to try and resolve QC issues. The IBM Project Manager will review the laboratory data 

package to insure that no other QC criteria were not met, and will identify these unmet QC criteria, 

and/or those identified in the narrative, in the summary report. The IBM Project Manager will consult 

with EPA to determine if these QC deficiencies are significant when compared to target levels.
ATTACHMENT 1 
WASTE TREATMENT FACILITY

Process Overview

LIME PRETREATMENT

CHEMICAL PROCESSCALCIUM HYDROXIDE + FLUORIDES = CALCIUM FLUORIDE PRECIPITATE

CONCENTRATED WASTE (CW)

- AMMONIA- FLUORIDE- PHOSPHORUS- PEROXIDE

BIOLOGICAL WASTE TREATMENT

BIOLOGICAL PROCESS- SEQUENTIAL BATCH REACTORS (SBRs)- TREATS: ORGANICS, PHOSPHORUS, AMMONIA, PEROXIDE

SANITARYWASTE

DILUTE ORGANICWASTE (DOW)

- ADSORBER DECANT WATER- IPA < 24%- NBA/GBL- GLYCOL SOLUTIONS - DUV PGMEA WASTE

INDUSTRIAL WASTE TREATMENT

- CHEMICAL PROCESS- SOLIDS CONTACT AND REACTOR TYPE CLARIFIERS- TREATS: ACIDS, BASES, METALS,  PHOSPHORUS, pH - DOES NOT TREAT: ORGANICS, AMMONIA

INDUSTRIALWASTE (IW)

- ACIDS/ BASES- RINSEWATERS- REJECT WATER- METALS

CMP PRETREATMENT

CHEMICAL PROCESSPRECIPITATION, COAGULATION, FLOCCULATION, FILTRATION, METAL AND PARTICULATE REMOVAL

CMP WASTES

WINOOSKI RIVER

- POLISHING SLURRIES- SURFACTANTS, DISPERSANTS, SOAPS- METALS (Cu, Fe, Al)- SOLIDS

Chemical Mechanical Polishing (CMP)

Photolithography DevelopClean, Etch, & StripParts Decontamination

Wafer Cleaning and StrippingPhotolithographyAir AbatementFacilities Maintenance 

Wafer and Mask Manufacturing Cleaning, Etching, and StrippingPhotolithographyChemical PolishingRinsewatersAir Abatement ScrubbersPre-treated Waste (CMP & BWTP)DI Water System

Drain Key Contributors Wastes

CafateriaBathrooms

- TYPICAL SANITARY WASTE
INDUSTRIAL WASTE TREATMENT SYSTE

PROCESS FLOW SCHEMATIC

SLUDGE

CONDITIONING

TANK

9'DX7'SWD

CLAR 4

MAX CAP

5.0 MGD

65'DX12'D

1 MGAL

EQUALIZATION

BASIN

70'LX95'WX25'D

FORWARDING

PUMPS

RECIRCULATION/

WASTING PUMPS 21'DX10'SWD

25KGAL

THICK.

2

THICK.

3

30'DX16'SWD

84KGAL

3.3

KGAL

PROCESS WATE

FORWARDING

PUMPS

RECIRCULATION/

WASTING PUMPS

PROCESS 

WATER 

STORAGE 

TANK #2

7.5 MG

PROCESS 

WATER

STORAGE 

TANK #1

7.5 MG

CLAR 2

MAX CAP

2.0 MGD

46'DX12'D

CLAR 3

MAX CAP

2.3 MGD

46'DX14.5'D

- RO REJECT- TREATED GROUNDWATER- GROUNDWATER FIRE 

TRAINING AREA
INDUSTRIAL WASTE TREATMENT S

Process Flow

EQUALIZATION CLARIFICATION

NaHSO3

H2SO4

pH ADJUST TO 2.5 to 3

REDUCTION OF H2O2

REDUCTION OF Cr6+ TO Cr 3+

KILLS ORGANISMS FROM BWTP

LIME

POLYMER

FINAL p

H2SO4

pH ADJU

pH ADJUST TO 9 TO 10

LIME HYDROXIDE PRECIPITATION

OF METALS

INFLUENT

TO IWTP 

FILTER PRESS OF SLUDGE

SLUDGE TO OFF SITE 
BIOLOGICAL WASTEWATER TREATMENT P

PROCESS FLOW SCHEMATIC

DILUTE ORGANIC

WASTE 10 KGD

AMMONIA-FLUORIDE

WASTE50 KGD

HIGH BOD ORGANIC

FROM CDC

(Intermittent to 0.5 KGD)

SANITARY

WASTE:

WILLISTON, 

900, 963, 964, 965, 966, 986, 

& 974, CMP

SBR #1

SBR #2

SBR #3

WET 

WELLS

1993

SEWAGE

PUMPS

RECIRCULATION/

FEED PUMPS

LIME

BLEND

TANK

A

BLEND

TANK

B

AIR 

BLOWERS

SEWAGE

GRINDERS

FLASH

MIX

TANK

60 

GAL

LIME 

25 

KGal

WASTED

SOLIDS

TO IWTP

THICKENE

HIGH STRENGTH 

ORGANIC

FEED/RECIRC PUMPS

SITE SANITARY

BACKBONE

FORCEMAIN

SANITARY 

LOAD 

100K GPD

25 

KGal
CMP WASTE TREATMENT SYSTE

PROCESS FLOW SCHEMATIC

FILTER PR

Process Water 

Storage & 

Equalization

Microbar EnChe

Treatment

FILTER PRESS

CMP DRAIN SYSTEM

BWTP

ORGANICS/AMMONIA

EQUALIZATION

CLARIFICATION

PROCESS 

WATER

STORAGE

SITE IW FLOWS

IWTP

SOLIDS/METALS

CMP

SOLIDS/METALS

EQUALIZATION

SEQUENTIAL BATCH 

REACTORS

SANITARY

DOW

CMP stream conditioning(pH, polymer, coagulant)

AF

Thickener 2 & 3
Acid, 

Caustic,

Metclear

Acid, 

Caustic, 

Metclear, 

Coagulant, 

Polymer

Acid, 

Caustic,

Coagulant, 

Polymer

Backflush

CMP FILTRATION PROCESS FLOW SCHEM

Design Capacity 310 KGD

Chemical 

addition 

capabilities:

Processes

pH 

adjustment

flocculation coagulation Mixing
ATTACHMENT 2 
Table 1 IBM Essex Junction, VT Industrial Wastewater Treatment Sludge De-Listing Constituents of Conce

 Selection Basis Hold time US EPA Method Detection Limit Analysis Quality Contro

Constituent CAS No. EM HC LDR PC TC Ext/An., d Extraction Analysis ug/l ug/Kg LRB LFB CCV Aluminu

m 7429-90-5

Y 180/180 3050B 6010 na 2500 <RL 70% R 10% 

Arsenic 7440-38-2

Y 180/180 1311 3050B 6010 2 2000 <RL 70% R 10% 

Bariu

m 7440-39-3

Y 180/180 1311 3050B 6010 20 500 <RL 70% R 10% 

Cadmiu

m 7440-43-9

Y

Y

Y

Y 180/180 1311 3050B 6010 3 500 <RL 70% R 10% 

Chromiu

m 7440-47-3

Y

Y

Y 180/180 1311 3050B 6010 20 1000 <RL 70% R 10% 

Chromium, hexavalen 18540-29-9

Y 30/2 3060A 7196A na 5000 <RL 80% R 20% 

Copper 7440-50-8

Y

Y 180/180 3050B 6010 na 1000 <RL 70% R 10% 

Iron 7439-89-6

Y 180/180 3050B 6010 20 5000 <RL 70% R 10% 

Lead 7439-92-1

Y

Y

Y 180/180 1311 3050B 6010 2 2000 <RL 70% R 10% 

Mercury 7439-97-6

Y 28/28 1311 7471A 7471A 1 600 <10% 90% R 10% 

Nickel 7440-02-0

Y

Y

Y 180/180 1311 3050B 6010 20 1500 <RL 70% R 10% 

Platinu

m 7440-06-4

Y

Y 180/180 3050B 6010 na 5000 <RL 70% R 10% 

Seleniu

m 7782-49-2

Y 180/180 1311 3050B 7010 5 3000 <10% 85% R 10% 

Silver 7440-22-4

Y

Y

Y 180/180 1311 3050B 6010 20 2000 <RL 70% R 10% 

Tin 7440-31-5

Y 180/180 3050B 6010 na 5000 <RL 70% R 10% 

Zinc 7440-66-6

Y 180/180 3050B 6010 na 1500 <RL 70% R 10% 

Cyanides - Tota 57-12-5

Y

Y 14 9010B 9012A na 710 <RL 80% R 10% 

Cyanides - Amenable 57-12-5

Y 14 9010B 9012A na 710 <RL 80% R 10% 

Cresols, Tota N/A

Y 14/7/40 14/40 1311 3550B 8270C 5 100 <RL 20% 

2,4-Dinitrotoluene 121-14-2

Y 14/7/40 14/40 1311 3550B 8270C 5 100 <RL 48-106%R 20% 

Hexachlorobenzene 118-74-1

Y 14/7/40 14/40 1311 3550B 8270C 5 100 <RL 20% 

Hexachlorobutadiene 87-68-3

Y 14/7/40 14/40 1311 3550B 8270C 5 100 <RL 20% 

Hexachloroethane 67-72-1

Y 14/7/40 14/40 1311 3550B 8270C 5 100 <RL 20% 

Nitrobenzene 98-95-3

Y 14/7/40 14/40 1311 3550B 8270C 2 40 <RL 20% 

Pentachloropheno 87-86-5

Y 14/7/40 14/40 1311 3550B 8270C 15 300 <RL 32-120%R 20% 

Pyridine 110-86-1

Y 14/7/40 14/40 1311 3550B 8270C 10 200 <RL 20% 

2,4,5-Trichloropheno 95-95-4

Y 14/7/40 14/40 1311 3550B 8270C 10 200 <RL 20% 

2,4,6-Trichloropheno 88-06-2

Y 14/7/40 14/40 1311 3550B 8270C 10 200 <RL 20% 

Benzene 71-43-2

Y 14/14 14 1311 5035 8260B 1 10 <RL 70% R 25% 

Carbon Tetrachloride 56-23-5

Y 14/14 14 1311 5035 8260B 1 10 <RL 70% R 25% 

Chlorobenzene 108-90-7

Y 14/14 14 1311 5035 8260B 1 10 <RL 70% R 25% 

Chlorofor

m 67-66-3

Y 14/14 14 1311 5035 8260B 1 10 <RL 70% R 20% 

1,4-Dichlorobenzene 106-46-7

Y 14/14 14 1311 5035 8260B 1 10 <RL 70% R 25% 

1,2-Dichloroethane 107-06-2

Y 14/14 14 1311 5035 8260B 1 10 <RL 70% R 25% 

1,1-Dichloroethylene 75-35-4

Y 14/14 14 1311 5035 8260B 1 10 <RL 70% R 20% 

Methyl Ethyl Ketone 78-93-3

Y 14/14 14 1311 5035 8260B 10 100 <RL 70% R 25% 

Tetrachloroethene 127-18-4

Y 14/14 14 1311 5035 8260B 1 10 <RL 70% R 25% 

Trichloroethene 79-01-6

Y 14/14 14 1311 5035 8260B 1 10 <RL 70% R 25% 

Vinyl Chloride 75-01-4

Y 14/14 14 1311 5035 8260B 2 20 <RL 70% R 20% 

Notes: 

EM = Identified by the EPA as either a precious or common metal used in electroplating (http://www.epa.gov/guide/electroplating/#guidance)HC = Listed in 40 CFR Part 261 Appendix VII as a Hazardous Constituent that is the Basis for the F006 ListingLDR = Regulated Hazardous Constituent in Land Disposal Restrictions for F006PC = Used in Process Contributing to F006 ClassificationTC = Toxicity Characteristic Metal or CompoundHold time with / = to extraction/to analysis after extraction; with / / = to solid extraction/to liquid extraction/to analysis Two extraction methods = TCLP and total; one = totalLRB = Laboratory Reagent Blank LFB = Laboratory Fortified Blank CCV = Continuing Calibration Verification Dup = Duplicate LFM = LF Matrix IS = Internal Standards RL = Rep. LRB criteria for 6010 analysis is greater of <RL or <10% of sample concentration; for 8270/8260 is greater of <RL or <5% of sample concentration%R = percent recovery, with acceptable range both below and above 100% (e.g. 70% means 70% to 130% is acceptable)Surrogate recoveries for 8270 are found in Method QC tables; surrogate recoveries for 8260 are 70%-130%A total of ~ 300 grams of sludge are required for all analyses: 100 for TCLP SVOC, 100 for TCLP metals, 25 for TCLP VOCs, 30 for SVOCs, 20 for VOCs, and ~ 10 for other
ATTACHMENT 3 
Environmental Program Managers

Regulatory 

Interactions

Reporting R

Pollu

Operational Control

Capital 

Programs

New 

Chemicals Tool 

Designs

Process 

Changes

Chemical 

Authorizations 

/Chemical Info

Environmental 

Impact 

Assessments

Review and Approvals

1. Wastewater Discharge Monitoring2. Hazardous Waste / Chemical Waste Disposal Authorizations3. Air Emissions Control4. Boiler Emissions5. Excavation Permits6. Inspections / Commissioning7. Treatability Studies

1. Regulatory Review 2. Modify Permits as Required3. Set Requirementts for Waste Generators4. Initiate new Treatment as needed5. Generate Facility Change Notes as Required

1. Ene2. Poll3. Too4. Com

1. NPDES2. Air Emissions3. TRI4. RCRA5. SARA6. Act 1007. Regulatory Required

 Chemical Management Databases

Funding Approval

Chemical Management Inputs and Control

Approval Loop
ATTACHMENT 4 
Document Control Copy on Buff colored paper. Any other color is not official version 

Endyne, Inc. 

160 James Brown Dr. 

Williston, VT 05495 

Phone: (802) 879-4333 

Fax: (802) 879-7103 

QUALITY SYSTEMS 

MANUAL

REVISED: October 6, 2009 

Revision #: 11 

Technical Director: Date : 

Harry B. Locker Ph.D. 

QA Officer: Date : 

Mark L. Fausel 
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Williston, VT 05495 Page 2 of 42 

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Table of Contents 

1.0 Quality Policy Statement 3 

2.0 Organization Structure/Personnel 4 

2.1 Personnel Responsibilities 5 

2.2 Personnel Qualifications 6 

2.3 Personnel Training 7 

3.0 Laboratory Environment 7 

4.0 Document Control 8 

5.0 Sample Management 8 

 5.1 Review of All New Work 8 

 5.2 Sampling Protocol 9 

 5.3 Sample receipt Protocol 10 

 5.4 Chain-of-Custody 11 

 5.5 Sample Preservation 11 

 5.6 Analytical Holding Times 11 

 5.7 Minimum Required Volumes 12 

6.0 Instrumentation and Equipment 12 

 6.1 De-Ionized Water 11 

 6.2 Balances, Thermometers and Pipettors 12 

 6.3 Glassware 12 

 6.4 Instrumentation 12 

7.0 Internal Quality Control of Test Procedures 12 

 7.1 Method and Analyst Capability Demonstrations 13 

 7.2 Quality Control Protocols 14 

 7.3 Analytical Standards 15 

 7.4 Data Storage and Archival 15 

7.5 Internal Audit and Data Review 15 

8.0 Testing Discrepancies and Corrective Action 16 

9.0 Exceptionally Permitted Departures 16 

10.0 Proficiency Testing and Certification 16 

11.0 Complaints and corrective Action 17 

12.0 Reporting of Results 17 

13.0 Revision History 18 

14.0 References 18 

Figure 1 Chain-of-Custody 19 

Table 1 Sampling Preservation and Volumes 20 

Table 2 Laboratory Equipment and Instrumentation 35 

Appendix A Demonstration of Capability Form 38 

Appendix B Client Confidentiality Policy 39 

Appendix C Analyst Signature 40 

Addendum State of Vermont & New York NELAC Certification 

 Most current documents provided by Certifying Agency 
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1.0 Quality Policy Statement 

Endyne, Inc. is committed to providing consistent, high quality data in a timely 

manner. It is our belief that each individual analytical result generated by Endyne is 

of critical importance to our client. It is thus imperative that Endyne be able to 

generate and report data of known quality. 

To that end, we have outlined our thorough Quality Systems Protocols with the intent 

of clarifying for our clients all the procedures and precautions that insure the highest 

level of quality data. Demonstration of Endyne’s commitment to maintain our quality 

objective is evidenced in the following. 

- An expertly staffed and fully equipped Laboratory facility. 

- Successful participation in multiple EPA/NELAC approved proficiency 

testing programs. 

- Successful implementation of a NELAC compliant quality system. 

- Annual internal audits with management review. 

- Timely reporting of analytical results. 

- Laboratory test results that are supported by quality control data and 

documented testing procedures. 

This quality policy is communicated to all new employees. It is understood, 

implemented, and maintained by employees at all levels. This is documented by 

management through the employee evaluation process, the training procedure, the 

internal audit process, and the document control process. 
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2.0 Organization Structure/Personnel 

The laboratory is comprised of 3 major analytical divisions; Organic, Inorganic and 

Microbiological. Analysts in each division are trained to perform a variety of analyses 

and each analysis has at least two analysts trained and qualified to perform the 

procedure. Laboratory management is comprised of four positions; Laboratory 

Director, Laboratory Manager and QA Officer and Department Managers. There are 

two auxiliary divisions which assist in the overall sample flow within the laboratory; 

Sample Preparation and Office Staff. 

Board of Directors

Laboratory 

Manager 

Sample Preparation

Office Organic Inorganic Microbiology

Laboratory Director

Quality Assurance 

Officer 

Endyne, Inc. 

Randolph Vermont 

Endyne, Inc. 

Plattsburgh New York 

Department 

Manager 

Department 

Manager 
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2.1 Position Responsibilities 

Although Endyne uses a hierarchy structure in managing employee workload, Endyne 

has an open-door management policy.. All employees have full access to the highest 

levels of management and ownership and are instructed in how to contact them for any 

reason. 

2.1.1 Organic and Inorganic and Microbiological analysts are responsible for 

maintaining their own method workloads. Analysts record data and individual 

QA/QC results in the appropriate databases. Analysts trained in a method may 

perform the initial data quality review of another analysts’ work. This data review is 

approved by managerial review before data is accepted in the LIMS database. 

Analysts report to their Department Supervisor or Laboratory Manager. 

2.1.2 The Chief Microbiologist is responsible for all microbiology and related 

abilities. The Chief Microbiologist receives training and education necessary to meet 

certification requirements. The Chief Microbiologist reports to the Inorganic-MicroMetals Department Manager. 

2.1.3 The Sample Preparation department is responsible for all sample preservation 

and storage at the laboratory. This includes dispersing sample aliquots to the different 

divisions of the laboratory and ensuring there is sufficient sample volume to perform 

all requested analyses. Sample technician prepares all sample containers for shipment, 

including preservation and sampling instructions. The sample tech is also responsible 

for assigning every sample its unique sample identification number. 

2.1.4 Office Staff are responsible for the initial receipt of samples at the laboratory, 

the proper completion of the C-of-C, and the entry of analytical requests into the 

Laboratory Information Management System (LIMS). Office staff is also responsible 

for the generation of the final report and ensuring the proper delivery of all analytical 

results to the client. 

2.1.5 Department Managers are responsible for the immediate supervision of 

analysts within their department and adherence to quality control policies. They coordinate the work load and assist in technical and analytical responsibilities when 

necessary. Department Supervisors report to the Laboratory Manager and QA Officer. 

2.1.5 The Laboratory Manager coordinates with clients and analysts to develop work 

schedules to meet analytical demands. The Laboratory Manager is available to 

analysts to assist in analytical troubleshooting. The Laboratory Manager reports 

directly to the Laboratory Director. 
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2.1.6 The Quality Assurance Officer reviews the QA/QC results of individual 

analyses, compiles the data, and reviews the data with the Laboratory Director. The 

Q.A. Officer is also responsible for ensuring that the overall laboratory operations 

comply with the Laboratory QA/QC Plan. The Q.A. Officer reports to the Laboratory 

Director, but has access to the Board of Directors 

2.1.7 The Laboratory Director has overall responsibility for the technical operation 

of the laboratory. The Director is responsible for arranging and overseeing the 

maintenance of all equipment and instrumentation, as well as the physical 

maintenance of the laboratory. The Director provides supervision to all laboratory 

personnel to ensure adherence to all lab-documented procedures including the Quality 

Manual. 

2.2 Personnel Qualifications 

Endyne, Inc. will hire only the most qualified and capable applicants for any position 

to be filled. Each new employee must have a combination of education and 

experience to adequately demonstrate the specific knowledge necessary to perform 

their assigned duties as well as a general knowledge of the mathematics and good 

laboratory techniques, which would be required. Endyne sets several conditions to 

ensure this minimum level of qualification. All individuals hired for analytical 

positions will have at least two years of course work towards a four-year college 

degree in a related science discipline or have completed a post-high school laboratory 

analyst program at a recognized technical school. Any individual without a college 

level education would require two years of on the job training in a laboratory 

environment prior to performing independent analytical work. 

2.3 General Procedural and Ethical Personnel Training 

Once hired a new employee will undergo a thorough training regimen to ensure they 

are capable of performing their tasks to the defined level of acceptance. Proper 

training consists of an initial training at the start of employment and continued training 

through-out their career. This training includes Safe Laboratory Practices, Chemical 

Hygiene, Ethical, Data Integrity and Technical education. Endyne tries to use various 

forms of training tools to instill sound learning practices. Most analytical procedures 

have specific requirements to demonstrate analytical capability. Those requirements 

are adhered to as well as our general guidelines for training. Documented training 

activities are stored in employee’s personnel files. 
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2.3.1 Analytical Training 

- The trainee reviews literature associated with the published methods. This includes 

all related internal SOPs such as the method SOP, equipment SOPs such as balance, 

glassware or pipettor SOPs and, if pertinent, the chromatography integration SOP. 

- The trainee also reviews all MSDSs for chemicals used during the procedure. . 

Analysts must read and become familiar with all elements of each chemical’s MSDS, 

making special awareness of the symptoms of exposure and potential routes of entry. 

- If it’s a new procedure and there is no internal method SOP, then the analyst reads 

the original method, writes a summary and reviews the procedure with the Laboratory 

Manager. 

- The trainee works several days under the direct supervision of an analyst who is 

experienced with the method. This training includes any specific laboratory 

techniques such as pipetting, syringe use, titration. Equipment maintenance and use 

such as probes, scales, meters or chromatograph operation. 

- The trainee may assist in the generation of data in a trainee mode. However, the 

trainee may not work independently until certification is fully documented. 

- The trainee performs a Demonstration of Capability (DOC). This is an analysis of 

four replicate quality control samples. The average of the results must be within 20% 

of the industry-standard expected mean value and the standard deviation must be less 

than 20%, unless the method specifically indicates otherwise. 

- The new analyst completes a DOC Certificate (see Appendix A) which documents 

his training and proficiency in a method. 

- The Laboratory Manager will authorize an analyst to perform a method only after 

successful completion of the DOC and upon conference with the primary trainer. 

Documentation of this authorization will be kept in the employee’s personnel file in 

the form of an “Analyst Certification Form”. 

2.3.2 Initial Training 

- An overall review of sample flow through the laboratory is provided, so that they 

may better understand their relationship within the laboratory. 

- A review of safety protocols and emergency response procedures is performed. A 

copy of Endyne Safety Handbook is provided and reviewed. 

- A review of general laboratory procedures, including balance, pipetting, etc. 

techniques is performed.

- Ethical and legal responsibilities are thoroughly reviewed, including potential 

punishments and penalties for improper, unethical or illegal actions. The analyst is 

given a copy of the “Laboratory Ethics and Data Integrity” SOP, as well as 

participates in detailed training of Endyne’s ethics policies. New employee signs an 

attestation agreeing to abide by Endyne’s ethics policies.- A review of Endyne’s 

client confidentiality policy is performed, including the privacy of general client 

information as well as the delivery of analytical data via phone or electronic means. 

Refer to Appendix B. 
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2.3.3 Continued Training 

- Regular Inorganic and Organic department meetings are held to discuss safety and 

quality control issues that arise during the course of the previous week. 

- Laboratory wide staff meetings occur as needs dictate. Topics range from employee 

benefits and staffing changes to analytical issues and ethical/legal responsibilities. 

- Employees attend off-site training seminars as well as internet based on-site 

seminars, which are deemed valuable by management. These have included office 

skills, hazardous waste handling, safety training, and analytical instrumentation 

courses. 

- Employees on an annual basis demonstrate continued proficiency in an analytical 

method by participation in blind proficiency testing of the method or submitting a 

continuing DOC form summarizing the last four LFB samples as defined in the initial 

Demonstration of Capability in Section 2.3.1. 

- Employees on an annual basis undergo documented refresher training on Laboratory 

Ethics, Data Integrity and Client Confidentiality. 

3.0 Laboratory Environment 

Endyne, Inc. consists of three levels covering approximately 3,500 square feet of work 

area. The top floor consists of meeting rooms and organic prep/extraction lab on one 

side of the building, on the other side of the building is the microbiology lab and 

Semi-volatile GC laboratory. The middle floor consists of office space and the 

Volatile Organics instrumentation lab. The bottom floor consists of the Metals and 

Inorganics work areas. 

Endyne has no equipment requiring extremely tight environmental conditions. Each 

floor contains its own heating and cooling systems designed to keep temperatures 

around 70°0 F and humidity around 40%. Electronic scales are mounted on vibration 

inhibiting platforms. Exhaust hoods are located on each floor. They are inspected and 

calibrated on an annual basis 

Biological work areas are sterilized between uses. Test areas of incompatible 

activities are separated to eliminate contamination. Work areas are wiped down at the 

end of each day and good housekeeping practices in general are followed to minimize 

contamination and health risks. 

4.0 Document Control 

The Document Control System is designed so that documents, which are generated by 

the laboratory and deemed critical to proper laboratory operation, are tracked and 

access is limited to responsible parties. This system ensures that only the most recent 

revisions are available to the appropriate personnel, and all documents in use have the 

proper authorization. Documents covered by this system are listed in the Master 

Document Control List, which lists all the records, their location, and revision history. 

Records covered in the Document Control List include the following; 
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 -The Master Document Control List 

 -This Quality Assurance Manual 

 -All Analytical SOPs 

 -Equipment Maintenance SOPs, i.e. Analytical Balance and Pipette SOPs 

 -Externally produced literature used in method Development and Troubleshooting. 

 -Sampling Procedures, i.e. Coliform Bacteria 

 -Employee Qualification Summaries 

The Quality Assurance Officer is responsible for maintaining the Document Control 

System. Master List Controlled Documents are indicated by the paper color indicated 

in the footer. Uncontrolled copies are determined by being printed on any other 

colored paper. The Q.A. Officer has control over the supply of the specified colored 

paper. The Laboratory Director approves all newly released control documents. The 

Q.A. Officer is responsible for archiving the obsolete documents. 

5.0 Sample Management 

Endyne has policies and personnel to manage the sample load generated from its 

clients. In the event that there is a surplus of work so that Endyne could not process 

all samples within stated hold times, Endyne would follow the protocols as outlined in 

the Sample Custody SOP for sub-contracting the excess work. 

5.1 Review of all New Work 

All new work is defined as analytical procedures for which Endyne does not already 

have an internal documented procedure with established quality control objectives. A 

list of established analyses is provided in Table 1. All new work is accepted by the 

Laboratory Director or Laboratory Manager, after ensuring the laboratory has the 

proper facilities and equipment to perform the analyses. Staff, involved in the new 

work, meets to discuss any pertinent issues regarding quality assurance considerations. 

The plan for any new testing must be reviewed and approved by the Laboratory 

Director. The designated employee(s) shall write a SOP for the procedure, which will 

be included in the document control. A DOC will be kept in the employees personnel 

file. 

5.2 Sampling Protocol 

 In general, samples received by Endyne are collected by representatives of firms 

contracting with the laboratory to perform the analysis. These firms are responsible for 

insuring that proper sampling procedures are followed. Endyne’s responsibility is limited 

to providing written sampling procedures for sample collection, preservation, field 

filtration and transport for specific analysis when requested. Upon request, Endyne can 

provide expert sampling services for air, water, and solid media. Endyne makes no 

guarantee, assumed or otherwise, as to the validity of documentation or sample integrity 

outside the direct control of its personnel.
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5.3 Sample Receipt Protocol 

Upon arrival at the laboratory, samples and associated Chain-of-Custody (C-of-C) are 

reviewed for accuracy and sample integrity. In summary, the C-of-C should contain the 

following information: (For a more detailed review, refer to the Sample Custody SOP) 

1. Client and contact person. 

2. Project Name 

3. Client sample identification (station location or number). 

4. Name of sample collector, date and time of collection. 

5. Analyses requested. 

6. Container type and volume. 

7. Type of preservation performed in the field. 

8. Special requests or instructions (e.g. rush analyses). 

9. Signature of Endyne personnel who received samples. 

10. Date and time of receipt. 

Samples are then inspected for general condition, which includes the following: 

1. If seals are present on containers, an inspection of each seal is made to insure that 

each seal is intact. Documentation as to the integrity of the seals is made on the 

Chain-of-Custody. 

2. Proper sampling containers have been utilized for the requested analyses, and 

adequate sample volume is available. 

3. For volatile organic compounds (VOC), any air bubbles will be noted on the C.O.C. 

4. Proper temperature and preservation guidelines have been followed. 

5. Comparison of notations on sample containers with those on the Chain-of-Custody 

(sample location, date, time) are made to insure that all samples which were collected 

have arrived at the laboratory, and are properly labeled. 

If discrepancies or omissions exist in any of these areas, the Laboratory Director and 

client are notified. If the client cannot be reached, the samples are placed in cold storage 

(4°C) and no further action is taken until the problem is resolved. 

In conjunction with the C-of-C, Endyne documents pertinent sample preservation 

information and sample condition on the Log-In report. The person receiving the sample 

records the condition of the samples, the temperature, the accuracy of the C-of-C and the 

means of delivery to the laboratory. The person prepping the sample records any 

preservation or sample preparation procedures necessary for sample storage until the time 

of analysis. 

Once logged in, the samples are delivered to the appropriate department, preserved, as 

appropriate, and/or refrigerated at 4°C. 

For further information refer to the Sample Custody SOP. 
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5.4 Chain-of-Custody 

The purpose of the Chain-of-Custody form is to provide a written record, which traces 

the collection, possession, and handling of samples from the moment of collection to 

arrival at the laboratory. An example of our Chain-of-Custody Record is provided in 

Figure 1. The Chain-of-Custody form is signed by the sample collector, by those 

responsible for the transportation of the sample, and finally, by laboratory personnel. 

Any breach in the Chain-of-Custody is reported to the Laboratory Director, the sampler, 

and the client. In most instances, the Chain-of-Custody form will also be used by the 

client as an order form to specify the requested analyses, and as a reporting sheet for field 

results. Upon receipt at the laboratory, a carbon copy of the Chain-of-Custody form is 

returned to the sampler. All original forms become property of the laboratory. 

5.5 Sample Preservation 

Sample preservation is divided into two areas. They are the following: 

 1. Field preservation by sampler. 

 2. Preservation by Endyne personnel.

Endyne, Inc. takes no responsibility for preservation procedures or materials used in the 

field. As stated in Section 5.2, we will provide methods, bottles and chemicals 

appropriate for proper field preservation. Any observed deviation of field preservation 

from these recommended methods will be reported to the client and noted on the Chain of 

Custody. 

If the sample is received without preservation, Endyne personnel will preserve the sample 

following Table 1, as long as handling the sample will not affect data integrity. Any nonstandard preservation requested by the sampler will be reported to the client and noted on 

the Chain-of-Custody. 

5.6 Analytical Holding Times 

Also listed on Table 1 are recommended holding times for all analyses. As discussed in 

Section 5.3, notification will be made to the Laboratory Director of any samples received 

by Endyne, which have exceeded the specified holding time limit. At Endyne, all 

samples will be processed within the recommended holding time. If, due to equipment 

malfunction or other circumstances beyond the control of the laboratory, an analysis 

cannot be performed at Endyne, a subcontracting laboratory will be assigned to perform 

the analysis. The client will be informed in writing of Endyne’s intention to sub-contract 

the analysis. Once permission from the client has been granted, a Chain-of-Custody 

record will be forwarded with all samples sent to the subcontracting laboratory. 
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5.7 Minimum Required Volumes 

Table 1 indicates the minimum required volumes to perform all analyses. During 

laboratory preservation procedures (see Section 5.5), the sample will be split, if 

necessary, such that appropriate volumes are preserved for all requested analyses. The 

notification procedure set forth in Section 5.3 will be implemented for samples with 

inadequate volume. In these cases, it will be the client’s responsibility to decide which 

analyses to perform. 

6.0 Instrumentation and Equipment 

The proper operation of the analytical instrumentation, all measuring devices, the deionized water supply, as well as the cleanliness of the glassware must be insured to meet 

the quality control requirements of the laboratory. Individual Standard Operating 

Procedures are maintained and adhered to for each type of Equipment. The following 

sections are summaries of those SOPs. A listing of all major pieces of equipment is 

provided in Table 2. 

6.1 De-Ionized Water 

A continuous resistivity meter is mounted on the de-ionized water unit. De-ionized water 

has an acceptable quality when the resistance value ranges from 14 to 18 μohms. If the 

resistance falls below this value, new filter elements are installed. De-ionized water from 

the conditioned device is not used until it can pass the 14 to 18 μohms standard. Grab 

samples are also analyzed using a separate electronic conductivity meter on at least a 

monthly basis, to verify the accuracy of the continuous recording device. This 

conductivity measurement must be < 2.0μmhos. Individual methods have their own 

requirements for reagent water that are defined in the method specific SOPs. For 

additional information refer to the De-Ionized water SOP. 

6.2 Balances, Thermometers and Pipettors 

All weights and calibration thermometers are calibrated against NIST traceable standards 

at an offsite certified facility. In-house use thermometers are calibrated against the offsite calibrated thermometer on an annual basis. Balances are inspected by a certified 

specialist on an annual basis and an internal calibration is performed daily. Balances are 

checked using NIST traceable weights on a daily basis. A variety of pipettors capable of 

measuring from 10ul to 10ml are calibrated on a monthly basis and spot checked by 

analysts on a more frequent basis. A record of all calibrations and checks is maintained 

in instrument logs. A notation of when re-calibration of each instrument is posted on the 

instrument for easy reference. For additional information refer to the individual 

equipment SOPs. 
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6.3 Glassware 

All glassware used for measurement is Class A certified. Glassware is cleaned 

thoroughly with soap and water. Tap water is used for the preliminary wash followed by 

rinses with de-ionized water. For trace metal analysis, the glassware is also subjected to 

an acid wash. All glassware used for organic extraction is rinsed with appropriate solvent 

prior to analysis. . For additional information refer to the Glkassware SOP. 

6.4 Instrumentation 

Each major piece of instrumentation is assigned to an individual analyst, for which they 

are responsible. A separate bound notebook or excel spreadsheet is maintained at each 

instrument station. In this notebook, the daily operation status of the instrument is noted 

as well as its complete maintenance history. All changes and servicing to the original 

factory equipment are noted, dated, and signed by the analyst responsible for the 

instrument. The Laboratory Director is notified of any problems with the equipment. 

Routine checks of the instrument log notebooks are made by the Laboratory Director to 

insure proper reporting. 

Regular site visits are made to Endyne by manufacturer’s service staff for equipment 

servicing. Some major instruments are covered by service contracts, which provide for 

rapid response by the manufacturer in the event of an equipment malfunction. 

7.0 Internal Quality Control of Test Procedures 

All method-referenced analyses performed at Endyne adhere to the quality control 

standards outlined in the published literature. Methods, which do not specifically 

reference quality control parameters, as well as in-house developed methods, adhere to, at 

the minimum, the QA/QC protocols outlined here. In some cases however, some of the 

following protocols are not possible to perform. Individual method SOPs have the 

appropriate QA/QC protocols referenced within them. 

Endyne’s internal QA/QC plan consists of method and analyst capability demonstrations, 

as well as a suite of quality control protocol steps during the analysis of samples. 

7.1 Method and Analyst Capability Demonstrations 

All records include references to the raw data files or dates analyzed, so that calculations 

can be regenerated from the original data. 

Demonstration of Capability (DOC)- Every new analyst performs a set of four mid-range 

concentration LFBs. The LFBs should be prepared as one sample, then split into four 

aliquots. The percent standard deviation and average percent recovery are determined 

for each analyte. Each must be less than 20% to ensure proper capability of the analyst 

for that method. Documentation of the DOC is kept in the analyst’s personnel file. 
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Continuing Demonstration of Capability (CDOC)- On an annual basis, every analyst 

must demonstrate continued proficiency in the analytical method. This may be 

evidenced by a statistical calculation of the last 4 concurrent LFBs as defined in the 

initial DOC or by successful completion of blind proficiency test samples. 

Documentation of the CDOC is kept in the analyst’s personnel file. 

Method Detection Limit Study (MDL)- The analyst performs a set of seven LFBs at a 

concentration of 2 to 5 times the expected MDL value. The standard deviation is 

multiplied by 3.14 to determine the laboratories MDL. The MDL should be less than 

half the laboratory’s reporting limit. MDLs are performed on an annual basis at the 

beginning of each year. Copies of the MDL are stored with the QA/QC data for the 

method. 

7.2 Quality Control Protocols 

Endyne generates control limits for the quality control samples using method-defined 

limits. Typically, those limits are +/- three standard deviations of the average recovery. 

In the event there is no accrued history of QC data an absolute acceptance limit of 70%-

130% is employed. Duplicate precision limits are based on 3.27 multiplied by the mean 

relative percent differences. In the event, there is no accrued history of duplicate data an 

absolute acceptance limit of 20% relative percent difference is applied. 

Analytical Calibration Line- A minimum of a 3-point calibration line not including “0”, 

which must have a linear correlation of 0.995 or better. The lowest point in the line must 

be less than the reporting limit or regulatory level. 

Continuing Calibration Check (CCC)- A calibration line standard is analyzed if a 

calibration line already exists. A CCC is analyzed at the start of each analytical day. 

Laboratory Reagent Blank (LRB)- A reagent water sample which is treated as a normal 

sample and must be shown to be free of all target analytes at reportable levels. An LRB 

is run with every 20 samples or each analytical batch, whichever is more frequent. 

Laboratory Fortified Blank (LFB)- An independent source standard containing all the 

target compounds is analyzed like a normal sample. A LFB is run with every 20 samples 

or each analytical batch, whichever is more frequent. 

Matrix Duplicate (MD)- Aliquots of the same sample which are analyzed identically. A 

MD is run with every 20 samples or each analytical batch, whichever is more frequent 

Matrix Spike (MS)- A sample aliquot to which a known amount of analyte(s) is added. 

A MS is run with every 20 samples or each analytical batch, whichever is more frequent. 

Matrix Spike/Duplicate (MS/D)- This quality control parameter may be employed in 

place of the Sample Duplicate and Matrix Spike. Two sample aliquots are spiked with 

known amounts of analyte and the percent recovery and percent difference is determined 

for the samples. 
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7.3 Analytical Standards and Chemicals 

Endyne takes special care to ensure the accuracy of all analytical standards. Standards 

are made in-house from neat materials or purchased from suppliers with at least an ISO 

9001 certification. Whenever possible standards are purchased from independent 

suppliers. All Certificates of Analysis from suppliers are kept on file. In-house standards 

are made using Class A glassware and a NIST traceable balance. All working standards 

are documented in individual method logbooks that insure traceability to the original 

manufacturer. 

All chemicals and standards have manufacturer defined expiration dates assigned to 

them. Chemicals which do not have an expiration date assigned by the manufacturer are 

given an expiration date by the laboratory; liquid chemicals and acids are assigned 10 

years and dry chemicals are assigned 20 years. The quality of chemicals and standards is 

dictated by the analyst and the quality assurance officer. The purchasing agent has no 

control over the purchase of less expensive materials. 

7.4 Data Storage and Archival 

All raw data and calculations, sufficient to completely reconstruct the data packet, are 

kept on file by the laboratory for a period of at least 7 years. New York drinking water 

analyses are kept on file for 10 years. Data storage during the course of the year is 

outlined in individual SOPs. At the start of each calendar year all data and paperwork is 

archived in banker boxes. These boxes for the two previous years are kept on site. Data 

older than two years is kept off-site in a secured location. In case of transfer of 

ownership or closure of business, the owners of Endyne will continue storage of required 

documents for the required time or ensure transfer of documents to new ownership. 

7.5 Internal Audit and Data Review 

-Raw Data - Each analyst must keep detailed information of the raw data in a bound 

notebook or on the computer printout. Entries must include the analyst initials, date and 

time of analysis, sample identification number, parameter tested and analytical method, 

documentation of all readings, and results of all weightings and dilutions. All 

calculations documenting the final concentration of the constituent as well as 

determinations of all quality control samples must be recorded with the data. 

-Data Checking – Data checking is initially performed by an independent analyst trained 

in the analytical methodology or Department Manager. After the analyst has processed 

all the associated data and recorded the results of an analysis, the data reviewer reviews 

the sample and associated quality control data. The reviewer then signs off on the Data 

packet and submits to the Department Manager or other laboratory officer with QC 

approval authority in the database. The independent analyst is held equally accountable 

for certifying all quality control aspects of the methodology. The completed report is 

submitted to the Laboratory Director for final review and approval before being released 

to the client. 
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-System Audits – The QA Officer or Department Manager with oversight by the QA 

Officer will review individual methods on an annual basis with the primary analyst. 

Procedures will be compared to the SOP, the original referenced method and Quality 

Systems Manual to confirm adherence. Review of records and logs is performed to 

ensure proper documentation and traceability. Any corrective actions will be 

documented. A component of the Audit includes an in-depth review of a random data 

set focussing on data integrity issues. Where audit findings cast doubt on the validity of 

results, clients will be contacted immediately in writing. 

-Managerial Review – On an annual basis, the Laboratory Director will review the 

quality system and its testing and calibration activities. The review will be based on 

feedback from the QA Officer, the results of proficiency tests, as well as audits from 

external certification officers. Any necessary changes will be implemented at this time 

and documented in the Quality Systems Manual. 

-Internal Audit – On an annual basis, the Quality Control Officer will present to the 

management staff a summary of the Internal Audit. This will include the findings of the 

systems audits as well as the managerial review, proficiency testing results and customer 

complaints. For additional information on the topics covered in Section 7.5 refer to the 

Managerial Review SOP. 

8.0 Testing Discrepancies and Corrective Action 

Occasionally analytical data fails the quality control protocols outlined in each method 

SOP. Procedures for determining the source of these failures are outlined in the SOP. In 

general, the primary analyst immediately reviews the work and assesses where the error 

occurred, corrects the deficiency and reanalyzes the associated samples. No further 

sample analysis is performed until the source of the error is determined and corrected. 

The laboratory manager and director are available for immediate consultation if 

necessary. In some instances, due to the sample volume submitted or the expiration of 

the analytical holding time, it is impossible to reanalyze the sample within QA/QC 

protocols. In that event the client is notified of the violation by telephone or in writing. 

No data, which is outside method specified quality control parameters, will be reported 

without the appropriate notation informing the client of the transgression. 

9.0 Exceptionally Permitted Departures from Documented Policies 

The Laboratory Director is responsible for ensuring adherence to the documented 

policies of the laboratory. However, in some instances departure from documented 

procedure may be necessary. In this instance, digression from the procedure is allowed 

as long as the changes are fully documented as well as the reason why the deviation 

occurred and the Laboratory Director approves all the departures. 

10.0 Proficiency Testing and Certification 
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Endyne participates in several proficiency-testing programs for drinking water, 

wastewater and solid waste. Endyne participates in a Potable Water testing program on a 

semi-annual basis. The testing encompasses all available parameters for which Endyne 

receives certification for from the State of Vermont and New York State Environmental 

Laboratory Accreditation Program (ELAP)/NELAC program. Endyne participates in 

semi-annual wastewater and solid waste/material proficiency testing administered by the 

New York State ELAP. Both sets of proficiency testing are approved by the National 

Environmental Laboratory Accreditation Council (NELAC). Endyne also participates 

annually in the DMR proficiency testing program administered by the EPA for 

wastewater/NPDES testing. 

Endyne Inc., maintains accreditation for a broad suite of parameters in several states. 

Endyne maintains potable water certification in the State of Vermont as granted by the 

Vermont Department of Health.. Endyne also maintains accreditation with the National 

Environmental Laboratory Accreditation Program in the areas of Potable Water, NonPotable Water and Solid Waste/Material for a broad variety of parameters. Our primary 

NELAC certification is administered through the New York ELAP. Endyne maintains 

secondary NELAC certification in Potable water and Non-Potable water for the state of 

New Hampshire. Currently New Hampshire does not offer accreditation in solid 

waste/material. The State of Vermont does not offer certification in wastewater or solid 

waste. However Endyne does maintain a level of wastewater certification in Vermont 

through our participation in the EPA/NPDES DMR proficiency testing, the results of 

which are reported to the State of Vermont Wastewater Division which implements the 

NPDES program in Vermont. 

An addendum to this manual is a current listing of State of Vermont and NELAC 

certified methods from our primary accrediting authority. Endyne frequently receives 

updates to our certification. As copies of our QSM are requested we append the most 

recent versions of our NELAC certification for distribution. This is done without 

revising the QSM manual itself. Therefore, for the laboratory’s most current version of 

NELAC certifications for the multiple states Endyne is certified in refer to our website 

www.endynelabs.com. 

11.0Complaints and Corrective Action Procedures 

Endyne continually strives to improve data quality and customer satisfaction. In an 

effort to track complaints and quality control problems, Endyne maintains a file where 

complaints, from clients or other parties, and their corrective actions are recorded. A 

five-step plan is implemented to correct the deficiencies. 

Endyne documents Corrective Actions using a standardized investigative Report 

Template (Corrective Action Report). Initially the complaint, whether from a client or 

discovered in any of the internal QA review processes, is documented. Assessment of 

the route cause of the problem is performed. A program to address the cause is 

implemented. Initial assessment to determine if the problem/complaint is corrected. 

Finally the system is reevaluated at a later date to ensure the proposed solution is still 

effective. 
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12.0Reporting of Results 

Endyne policy is to report results solely to the client listed on the Chain-of-Custody. 

Delivery of results is accomplished in four ways. The only authoritative results reported 

by Endyne are in the form of a hard copy report with the original signature of the 

Laboratory Director or appointed signer. The other forms of data deliverables are by fax 

,e–mail or verbal. Clients who request a verbal transmission of results must concretely 

establish themselves as the proper client, This is accomplished by referencing the C-of-C 

number in the upper right hand corner. Clients who request a fax must indicate on the Cof-C whom will receive results or if the request is made by phone proof must be made 

that they are the stated client. This is usually accomplished by referencing the distinctive 

C-of-C sequence number. Deliverables in the form of e-mails are only provided to 

established customers, whom have made formal arrangements for receipt of results. All 

electronic transmissions are accompanied with a disclaimer stating that the material is 

confidential information intended solely for the recipient and to notify Endyne 

immediately upon incorrect receipt. Refer to Appendix C. 

13.0 Revision History

Revision 1: July 18, 2000: Complete Draft 

Revision 2: March 15, 2001: Minor Revision 

Revision 3: March 15, 2002: Minor Revision 

Revision 4: January 28, 2003: Minor Revision 

Revision 5: February 28, 2003: Added Certification Addendum 

Revision 6: March 2, 2004: 2.2 Personnel Qualifications 

 2.3.1 Analytical Training 

 7.5 Internal Audit and Data Review 

Revision 7: September 20, 2005 2.0 Added reference to Scitest, Inc. in corporate 

Structure. 

3.0 Laboratory Environment- Noted reconstruction 

& location of departments. 

 4.0 Add instrument manuals to Document Control 

 11.0 Multi-point Corrective Action Report 

Revision 8 October 12, 2007 2.0 Added Endyne-Plattsburgh and Department 

Managers to corporate structure. 

7.3 Analytical Standards and Chemicals 

7.5 Data Checking 

10.0 Eliminated reference to AIHA. Clarified 

proficiency testing participation and defined the 

Addendum referencing current certifications. 

Table 1. Update laboratory method container, 

preservation and holding time information divided 

into matrix. 

Table 2. Update laboratory equipment and 

instrumentation table. 
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Revision 9 February 19, 2008 2.3 Revised Employee Training. Included 

reference to Data Integrity SOP 

5.2 Sampling Protocol 

6.0-6.4 Equipment 

7.1 Analyst Capability Demonstration 

7.5 Internal Audit & Data Review 

Table 1 - Temperature Requirements 

Revision 10 October 1, 2009 Figure 1. New Chain-of Custody Form 

Table 1. Updated Sample Preservation Table 

Appendix A. Included DOC tracking procedures 

within LIMS 

Revision 10 October 6, 2009 Table 2-Laboratory Instrumentationges 

14.0 References 

Standard Methods for the Examination of Water and Wastewater. 17th Edition. 

APHA, AWWA, WPCF. Denver Colorado (1989) 

Test Methods for Evaluating Solid Watse, Physical/Chemical Methods (SW-846 Version 

2) on CD-ROM. NTIS U.S. DOC. Springfield, VA (1997). 

EPA Methods and Guidance for Analysis of Water (Version 2) on CD-ROM. Office of 

Science and Technology, U.S. EPA. Washington DC (1999) 

Environmental Laboratory Approval Program Certification Manual. New York 

Department of Health. Albany, NY (1999) 

1999 Annual New York and Pennsylvania Environmental Laboratory Conference & 

Exposition. August 8th-10th, 1999. 

NELAC Quality Systems Checklist Rev. 6. National Environmental Laboratory 

Accreditation Conference. 1997. 
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TABLE 1. 

POTABLE WATER

Parameters Analytical 

Methods 1

Volume 

Required 

(mls) 

Container 

Type2

Preservative3,4 Holding 

Time5

Escherichia 

coli 

enumeration 

SM18 9223B 100 ml 125 ml 

Sterile 

> 10°C 0.008% 

Na2S203

6 hrs 

Fecal 

Coliform 

SM18 9222D 100 ml 125 ml 

Sterile 

> 10°C 0.008% 

Na2S203

6 hrs 

Heterotrophic 

Plate Count 

SM18 9215B 100 ml 125 ml 

Sterile 

> 10°C 0.008% 

Na2S203

8 hours 

Total Coliform 

Present/Absent 

SM18 9223B 100 ml 125 ml 

Sterile 

> 10°C 0.008% 

Na2S203

30 hrs 

Acidity EPA 305.1 200ml P,G 0-6°C 14 days 

Alkalinity EPA 310.1 200ml P,G 0-6 °C 14 days 

Bromide EPA 300.0 50 ml P.G None Required 28 days 

Chloride EPA 300.0 50 ml P,G None Required 28 days 

Chlorine EPA 330.5 200 ml P,G None Analyze 

Immediat

ely 

Color EPA 110.2 200 ml P,G 0-6 °C 48 hrs. 

Conductance EPA 120.1 100 ml P,G 0-6 °C Filter,0-

6 °C 

24 hours 

28days 

Cyanide9 EPA 335.1 250 ml P,G 0-6°C NaOH of 

pH >12 

0.6 g ascorbic 

acid7

14 days 

Fluoride EPA 300.0 50 ml P,G None Required 28 days 
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TABLE 1 continued 

POTABLE WATER

Parameters Analytical 

Methods 1

Volume 

Required 

(mls) 

Container 

Type2

Preservative3,4 Holding 

Time5

Hardness EPA 200.7 100 ml P,G HNO3 to pH 6 mos. 

Nitrogen, 

Nitrate

EPA 300.0 50 ml P,G 0-6 °C 48 hours 

Nitrogen, 

Nitrite 

EPA 300.0 50 ml P,G 0-6 °C 48 hours 

Odor EPA 140.1 1000 ml G only 0-6 °C 48 hrs. 

pH EPA 150.1 100 ml P,G None Analyze 

ASAP 

Phenolics9 EPA 420.1 1000 ml G only 0-6 °C H2SO4

to pH <2 

28 days 

Phosphorus, 

orthoPhosphate, 

EPA 

300.0/365.1 

50 ml G 0-6 °C 48 hours 

Solids, 

Filterable 

EPA 160.1 500 ml P,G 0-6 °C 7 days 

Solids, Total EPA 160.3 500 ml P,G 0-6 °C 7 days 

Sulfate EPA 300.0 50 ml P,G Cool, 4°C 28 days 

Sulfide, 

Hydrogen 

EPA 376.1 1000 ml P,G 0-6 °C, 2ml 

Zinc Acetate 

NaOH to pH >9 

7 days 

Sulfite EPA 377.1 50 ml P,G None Analyze 

Immediat

ely 
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TABLE 1 continued 

POTABLE WATER

Parameters Analytical 

Methods 1

Volume 

Required 

(mls) 

Container 

Type2

Preservative3,4 Holding 

Time5

Total Organic 

Carbon9

EPA 415.1 2 40ml v 

mlials 

Amber G 

No Air 

Bubbles 

0-6 °C 

H2SO4 or HCl 

 to pH <2 

28 days 

Turbidity EPA 180.1 100 ml P,G 0-6°C 48 hrs. 

UV 

Transmittance 

SM20 5910B 100ml ml Glass 0-6°C 48 hours 

Chromium+6 EPA 7196A 200 ml P,G 0-6°C 24 hrs. 

Metals, Total SM18 3113B 

EPA 200.7, 

200.9, 245.1, 

500 ml P,G HNO3 to pH <2 6 mos. 

Hg 28 

days 

Carbamates9 EPA 531 2-40ml 

vials 

G only Na2S2O3

Pot. Hydrogen 

Citrate 

28 days 

Haloacetic 

Acids 

EPA 552 3-60ml 

vials 

Amber G Ammonium 

Chloridee 

14 days/ 

14 days 

Herbicides EPA 515.4 2-40ml 

 vials 

Amber G 0-6 °C, 

3mg Na2SO3

7

14 days/ 

21 days 

MBAS EPA 425.1 500 ml P,G 0-6 °C 48 hrs 
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TABLE 1 continued 

POTABLE WATER

Parameters Analytical 

Methods 1

Volume 

Required 

(mls) 

Container 

Type2

Preservative3,4 Holding 

Time5

Microextractables EPA 504 2 40-ml 

vials 

G only 

No Air 

Bubbles 

0-6 °C 

10 mg 

Na2S2O3

7

14days/ 

1 day 

Pesticides/ 

PCB 

EPA 505 2 40-ml 

vials 

G only 0-6 °C 

5 mg Na2S2O3

7

7 days/ 

1day 

Synthetic 

Organic 

Contaminants 

EPA 525.2 2 1000-ml Amber G 0-6 °C 1:1 HCl 

,50mg Na2SO3

7

14 days/ 

14 days 

TriHaloMethanes 

VOCs 

EPA 524.2 2 40ml 

vials 

G only 

No Air 

Bubbles 

0-6 °C 

5 mg Na2S2O3

14 days 

Volatile 

Organic 

Contaminants 

EPA 524.2 2 40ml 

vials 

G only 

No Air 

Bubbles 

0-6 °C 

1:1 HCl 

 Ascorbic Acid7

14 days 

Gross Alpha9 EPA 900.0 1000 ml P None 24 hours/ 

28days 

Radium 

226,2289

EPA 903.1 2000 ml P None 28 days 

Uranium9 EPA 200.8 1000 ml P None 28days 
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TABLE 1 continued 

NON-POTABLE WATER

Parameters Analytical 

Methods 1

Volume 

Required 

(mls) 

Container 

Type2

Preservative3,4 Holding 

Time5

Escherichia 

coli 

SM18 9223B 100 ml 

Sterile 

125 ml > 10°C 0.008% 

Na2S203

6 hrs 

Fecal 

Coliform 

SM18 9222D 100 ml 

Sterile 

125 ml > 10°C 0.008% 

Na2S203

6 hrs 

Heterotrophic 

Plate Count 

SM18 9215B 100 ml 

Sterile 

125 ml > 10°C 0.008% 

Na2S203

8 hours 

Total 

Coliform 

SM18 9223B 

enumeration 

100 ml 

Sterile 

125 ml > 10°C 0.008% 

Na2S203

6 hrs 

Acidity EPA 305.1 200 ml P,G 0-6 °C 14 days 

Alkalinity EPA 310.1 200 ml P,G 0-6 °C 14 days 

BOD EPA 405.1 1000 ml P,G 0-6 °C 48 hrs. 

BOD, Soluble EPA 405.1 1000 ml P,G 0-6 °C 48 hrs 

Bromide EPA 300.0 50 ml P.G None Required 28 days 

Chloride EPA 300.0 50 ml P,G None Required 28 days 

Chlorine EPA 330.5 200 ml P,G Dark, 0-6 °C 15 min. 

COD EPA 410.1 50 ml P,G 0-6 °C H2SO4 

to pH <2 

28 days 

Color EPA 110.2 200 ml P,G 0-6 °C 48 hrs. 

Conductance EPA 120.1 100 ml P,G 0-6 °C 

Filter, 4°C 

24 hours 

28days 
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TABLE 1 continued 

NON-POTABLE WATER

Parameters Analytical 

Methods 1

Volume 

Required 

(mls) 

Container 

Type2

Preservative3,4 Holding 

Time5

Cyanide9 EPA 335.1 250 ml P,G 0-6 °C 

NaOH pH >10 

14 days 

Fluoride EPA 300.0 50 ml P,G None Required 28 days 

Hardness EPA 200.7 100 ml P,G HNO3 to pH 6 mos. 

Nitrogen, 

Ammonia 

EPA 350.3 100 ml P,G 0-6 °C 

H2SO4 to pH 

<2 

28 days 

Nitrogen, 

Nitrate 

EPA 300.0 50 ml P,G 0-6 °C 48 hours 

Nitrogen, 

Nitrite 

EPA 300.0 50 ml P,G 0-6 °C 48 hours 

Nitrogen, 

Total Kjeldahl 

EPA 351.4 100 ml P,G 0-6 °C H2SO4 

to pH <2 

28 days 

Odor EPA 140.1 1000 ml G only 0-6 °C 48 hrs. 

pH EPA 150.1 100 ml P,G None 15 min. 

Phenolics9 EPA 420.1 1000 ml G only 0-6 °C H2SO4 

to pH <2 

28 days 
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TABLE 1 continued 

NON-POTABLE WATER

Parameters Analytical 

Methods 1

Volume 

Required 

(mls) 

Container 

Type2

Preservative3,4 Holding 

Time5

Phosphorus, 

orthoPhosphate, 

EPA 

300.0/365.2 

50 ml G 0-6 °C 48 hours 

Phosphorus, 

Total 

EPA 365.2 200 ml G 0-6 °C H2SO4 

to pH <2 

28 days 

Phosphorus, 

Total 

Dissolved 

EPA 365.2 200 ml G Filter on-site 0-

6 °C H2SO4 to 

pH <2 

28 days 

Solids, 

Filterable 

EPA 160.1 500 ml P,G 0-6 °C 7 days 

Solids, Nonfilterable EPA 160.2 500 ml P,G 0-6 °C 7 days 

Solids, 

Settleable 

Matter 

EPA 160.5 1000 ml P,G 0-6 °C 48 hrs. 

Solids, Total EPA 160.3 500 ml P,G 0-6 °C 7 days 

Solids, Total 

Volatile 

EPA 160.4 500 ml P,G 0-6 °C 7 days 

Sulfate EPA 300.0 50 ml P,G 0-6 °C 28 days 

Sulfide, 

Hydrogen 

EPA 376.1 1000 ml P,G 0-6 °C 2ml 

Zinc Acetate 

NaOH to pH 

>9 

7 days 
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TABLE 1 continued 

NON-POTABLE WATER

Parameters Analytical 

Methods 1

Volume 

Required 

(mls) 

Container 

Type2

Preservative3,4 Holding 

Time5

Sulfite EPA 377.1 50 ml P,G None 15 min. 

Total Organic 

Carbon9 

EPA 415.1 2 40ml 

vials 

Amber G 

No Air 

Bubbles 

0-6 °C H2SO4 

or HCl to pH 

<2 

28 days 

Turbidity EPA 180.1 100 P,G 0-6 °C 48 hrs. 

UV 

Transmittance 

SM20 5910B 100ml Glass 0-6 °C 48 hours 

Chromium+6 EPA 7196A 200 P,G 0-6 °C 24 hrs. 

Metals, 

Dissolved 

SM18 3113B 

EPA 200.7, 

245.1, 6010B, 

7471A 

25 P,G Filter on-site 

Then 

HNO3 to pH 

<2 

6 mos. 

Hg 28 

days 

Metals, Acid 

Soluble 

SM18 3113B 

EPA 200.7, 

245.1, 6010B, 

7471A 

25 P,G HNO3 to pH 

<2 THEN 

Filter on-site 

6 mos. 

Hg 28 

days 

Metals, 

Suspended 

SM-18 3113B 

EPA 200.7, 

245.1, 6010B, 

7471A 

25 P,G Filter on-site 6 mos. 

Hg 28 

days 

Metals, Total SM-18 3113B 

EPA 200.7, 

245.1, 6010B, 

7471A 

25 P,G HNO3 to pH 

<2 

6 mos. 

Hg 28 

days 
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TABLE 1 continued 

NON-POTABLE WATER

Parameters Analytical 

Methods 1

Volume 

Required 

(mls) 

Container 

Type2

Preservative3,4 Holding 

Time5

Fats, Oil & 

Grease 

EPA 1664 2-1000 G only 0-6 °C H2SO4 

to pH <2 

28 days 

MBAS EPA 425.1 500 P,G 0-6 °C 48 hrs 

PCBs EPA 

608/8082 

2 1000ml Amber G 0-6 °C pH 

between 5-9 

7 days/ 

40 days 

Pesticides EPA 

608/8081A 

2 1000-ml Amber G 

pH 

between 5-

9 

0-6 °C pH 

between 5-9 

7 days/ 

40 days 

S.V.O.C. 

BN/A 

EPA 

625/8270C 

2 1000-ml Amber G 0-6 °C pH 

between 5-9 

7 days/ 

40 days 

TPH DRO EPA 8015B 2 40-ml G only 0-6 °C HCl to 

pH <2 

7 days/ 

40days 

Gross Alpha9 EPA900.0 1000 P None 28days 

Radium 

226,2289 

EPA 903.1 2000 P None 28 days 

Uranium9 EPA 200.8 1000 P None 28days 

TPH GRO EPA 8015B 2 40-ml VOA G 

only 

No bubbles 0-6 

°C HCl to pH 

<2 

14 days 

Volatiles EPA 624 2 40-ml 

vials 

G only No bubbles 0-6 

°C 

7 days 

Volatiles EPA , 8260B, 

8021B 

2 40-ml 

vials 

G only No bubbles 0-6 

°C HCl to pH 

<2 

14 days 
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TABLE 1 continued 

SOIL/SOLID WASTE

Parameters Analytical 

Methods 1

Volume 

Required 

(mls) 

Container 

Type2

Preservative3,4 Holding 

Time5

Fecal 

Coliform 

SM18 

9222D 

20g 125 ml 

Sterile 

 0-10 °C 24 hrs 

Bromide EPA 9056 50g P.G None Required 28 days 

Chloride EPA 9056 50g P,G None Required 28 days 

Conductance EPA 120.1 50g P,G 0-6 °C 28days 

Corrosivity as 

pH 

EPA 9045D 50g P,G 0-6 °C 28 days 

Reactive 

Cyanide & 

Sulfide9

EPA Chapter 

7.3 

50g P,G 0-6 °C 14 days 

Fluoride EPA 9056 50g P,G None Required 28 days 

Fraction 

Organic 

Matter 

ASTM 

D2974-87 

25g P.G 4°C 28 days 

Ignitability/ 

Flashpoint 

EPA Ch 7.1 

 EPA 1010A 

100g G 4°C 28 days 

Nitrogen, 

Ammonia 

EPA 350.3 100 P,G 0-6 °C 28 days 

Nitrogen, 

Nitrate 

EPA 9056 10g P,G 0-6 °C 28 days 

Nitrogen, 

Nitrite 

EPA 9056 10g P,G 0-6 °C 28 days 
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TABLE 1 continued 

SOIL/SOLID WASTE

Parameters Analytical 

Methods 1

Volume 

Required 

(mls) 

Container 

Type2

Preservative3,4 Holding 

Time5

Nitrogen, 

Total Kjeldahl 

EPA 351.4 25g P,G 0-6 °C 28 days 

Paint Filter 

Test 

EPA 9095B 100g P,G 0-6 °C 28 days 

pH EPA 9045C 25g P,G 0-6 °C 14 days 

Phosphorus, 

Total, 

Reserve, 

Available 

EPA 365.2 25g G 0-6 ° 28 days 

Solids, Total EPA 160.3 50g P,G 0-6 °C 7 days 

Solids, Total 

Volatile 

EPA 160.4 100g P,G 0-6 °C 7 days 

Sulfate EPA 9056 10g P,G 0-6 °C 28 days 

Chromium+6 EPA 7196A 200 P,G 0-6 °C 24 hrs. 

Metals, Total SM18 3113B 

EPA 6010B, 

7471A 

5g P,G None Required 6 mos. 

Hg 28 

days 

Metals, TCLP EPA 6010B, 

7471A 

25g P,G None Required 6 mos. 

Hg 28 

days 
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TABLE 1 continued 

SOIL/SOLID WASTE

Parameters Analytical 

Methods 1

Volume 

Required 

(mls) 

Container 

Type2

Preservative3,4 Holding 

Time5

Fats, Oil & 

Grease 

EPA 1664 50g G only 0-6 °C 28 days 

PCBs EPA 8082 100 g G only 0-6 °C 14 

days/40 

days 

Pesticides EPA 8081A 100 g G only 0-6 °C 14 

days/40 

days 

Herbicides EPA 8151A 100 g G only 0-6 °C 14 

days/40 

days 

S.V.O.C. 

BN/A 

EPA 8270C 100 g G only 0-6 °C 14 

days/40 

days 
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TABLE 1 continued 

SOIL/SOLID WASTE

Parameters Analytical 

Methods 1

Volume 

Required 

(mls) 

Container 

Type2

Preservative3,4 Holding 

Time5

TCLP SVOC 

BN/A 

EPA 1311/ 

8270C 

100 g G only 0-6 °C 14 days 

14 

days/40 

days 

TCLP 

Pesticides 

EPA 1311/ 

8081A 

100 g G only 0-6 °C 14 days 

14 

days/40 

days 

TCLP 

Herbicides 

EPA 1311/ 

8151A 

100 g G only 0-6 °C 14 Days 

14 

days/40 

days 

TPH DRO EPA 8015B 20-g G only 0-6 °C 14 

days/40 

days 

TPH GRO EPA 8015B 20g G-VOA 0-6 °C , No 

Head Space 

14 days 

Volatile 

Organics 

EPA 8021B, 

8260B 

20 g G-VOA 0-6 °C No 

Head Space 

14 days 

TCLP VOC EPA 1311/ 

8260B 

100 g G only 0-6 °C No 

Head Space 

14 Days 

14 days 
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TABLE 1 FOOTNOTES 

1. Referenced Methods are from approved publications. “EPA” indicates 

Environmental Protection Agency. “SM” indicates “Standard Methods for the 

Examination of Water and Wastewater”. ASTM indicates “American Society for 

Testing and Materials”. 

2. A general discussion on sampling water and industrial wastewater may be found in ASTM, 

Part 31, pgs. 72-82 (1976) Method D-3370. 

3. Plastic (P) or Glass (G). For metals, polyethylene with a polypropylene cap with teflon liner 

is preferred. 

4. Sample preservation should be performed immediately upon sample collection. For 

composite samples each aliquot should be preserved at the time of collection. When use of 

an automated sampler makes it impossible to preserve each aliquot, then samples may be 

preserved by maintaining at 4°C until compositing and sample splitting is completed. 

5. When any sample is to be shipped by common carrier or sent through the United States Mail, 

it must comply with the Department of Transportation Hazardous Materials Regulations (49 

CFS Part 172). The person offering such material for transportation is responsible for 

ensuring such compliance. For the preservation requirements of Table 1, the Office of 

Hazardous Materials, Materials Transportation Bureau, Department of Transportation has 

determined that the Hazardous Materials Regulations do not apply to the following materials: 

Hydrochloric acid (HCl) in water solutions at concentrations of 0.04% by weight or less (pH 

about 1.96 or greater); Nitric acid (HNO3) in water solutions at concentrations of 0.15% by 

weight or less (pH about 1.15 or greater); Sulfuric acid (H2SO4) in water solutions at 

concentrations of 0.35% by weight or less (pH about 1.15 or greater); Sodium hydroxide 

(NaOH) in water solutions at concentrations or 0.080% by weight or less (pH about 12.3 or 

less). 

6. Samples should be analyzed as soon as possible after collection. The times listed are the 

maximum times that samples may be held before analysis and still considered valid. Samples 

may be held for longer periods only if the permittee , or monitoring laboratories, has data on 

file to show that the specific types of sample under study are stable for the longer time, and 

has received a variance from the Regional Administrator. Some samples may not be stable 

for the maximum time period given in the table. A permittee, or monitoring laboratory, is 

obligated to hold the sample for a shorter time if knowledge exists to show this is necessary 

to maintain sample stability. 

7. Should only be used if residual chlorine is present in the sample. 

8. For samples from non-chlorinated drinking water supplies, concentrated H2SO4 should be 

added to lower sample pH to less than 2. The sample should be analyzed before 14 days.

9. Indicates the analysis is subcontracted to a NELAC certified laboratory.
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Table 2 Laboratory Instrumentation 

Item # of 

Units 

Manufacturer Model 

Air Pump 5 SKC 224-PCXR8 

Atomic Absorption, 1 Perkin-Elmer 600 

Autoclave 1 NAPCO 8000-DSE 

Autoclave 1 Castle BB 

Balance, Analytical 0.01g sensitivity 1 Acculab VI-200 

Balance, Analytical 0.1mg sensitivity 1 Mettler AE100 

Balance, Analytical Class S calibration 

weights 

2 Rick Lake Weighing 

Systems 

Centrifuge Centrific 225 

Chromatograph, Gas 

with Mass Selective detector 

with Purge & Trap sample introduction

1 

1 

1 

Agilent 

Agilent 

OI 

5890 II w/EPC 

5971 

DPM-16/4560 

Chromatograph, Gas 

with Mass Selective detector 

with Purge & Trap sample introduction

1 

1 

1 

Agilent 

Agilent 

OI 

5890 II w/EPC 

5971 

DPM-16/4560 

Chromatograph, Gas 

with Mass Selective detector 

with auto-sample introduction 

1 

1 

1 

Agilent 

Agilent 

Agilent 

5890 Seies II 

5970 

7673 

Chromatograph, Gas 

with PID/FID detector 

with Purge & Trap sample introduction

1 

1 

1 

Agilent 

OI 

Tekmar 

5890 Seies II 

4430 

ALS 2016/LSC2000 

Chromatograph, Gas 

with Mass Selective detector 

with Purge & Trap sample introduction

1 

1 

1 

Agilent 

Agilent 

OI 

5890 SeiesII w/EPC 

5971 

MPM-16/4560 

Chromatograph, Gas 

with Mass Selective detector 

with auto-sample introduction 

1 

1 

1 

Agilent 

Agilent 

Agilent 

6890 Plus 

5973 

7683B 

Chromatograph, Gas 

with FID detector 

with auto-sample introduction 

1 

1 

1 

Agilent 

Agilent 

Agilent 

5890 SeiesII 

7673B 

Chromatograph, Gas 

with FID detector 

with auto-sample introduction 

1 

1 

1 

Agilent 

Agilent 

Agilent 

5890 SeiesII 

7673B 

Chromatograph, Gas 

with ECD detector 

with auto-sample introduction 

1 

1 

1 

Agilent 

Agilent 

Agilent 

5890 SeiesII w/EPC 

19233 

7673B 

Chromatograph, Gas 

with ECD detector 

with auto-sample introduction 

1 

1 

1 

Agilent 

Agilent 

Agilent 

5890 SeiesII 

19233 

7673B 

Chromatograph, High Performance 

Liquid With Conductivity Detector 

1 Dionex DX-120 

Chromatograph, High Performance 

Liquid with UV and Conductivity 

Detectors 

1 Waters 712/486 

Concentrator, Solvent sample 1 TurboVap II 

Dessicators 4 Fisher 
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Digestor, 36-Place (metals) 1 Environmental 

Express 

ETR-3020 

Digestor, 54-Place (metals) 1 Environmental 

Express 

SC-154 

Digestor, Block Nutrient 1 Lachat BD-46 

Digestor, COD 2 HACH 45600 

Falsh Tester, Closed Cup 1 Pensky-Martin 74637 

Flourimeter 1 Turner Designs 10-005R 

Glassware, Class A Volumetric Multi-Supplier 

Hot Plate 10 Multi-Supplier 

ICP 1 Leeman Prodigy 

Incubator, BOD 1 Fisher 307C 

Incubator, BOD 1 Fisher 307 

Incubator-Air Jacketed 1 Chicago Surgical & 

Electrical 

200 

Incubator-Water bath 1 GCA Precision 

Incubator-Water Jacketed 1 Forma-Scientific 3187 

Incubator-Water Jacketed 1 NAPCO 5100 

Mercury Analyzer 1 Perkin-Elmer FIMS 100 

Meter, Conductivity 1 YSI 35 

Meter, Conductivity 1 Fisher 95081372 

Meter, Expandable Ion Analyzer 2 Orion EA940 

Meter, Oxygen, Dissolved 2 YSI 58 

Meter, pH 1 Accumet 

Meter, pH & Ion specific probes 2 Orion 940 

Micro, Quanti-tray Sealer 1 IDEXX 2X 

Oven, Drying 2 VWR 1305U 

Oven, Drying 1 Despatch LDB 

Oven, Drying 1 Agilent 5890 

Oven, Muffle Furnace 1 Thermolyne 1500 

Pipettors, 10ul up to 10ml Multiple Suppliers 

Probe, Oxygen, Dissolved 3 YSI 5905 

Probe, Redox Combination 1 Orion 9678BN 

Refrigerator, Sample Double wide 3 United USF 

Refrigerator, Sample Single Wide 3 Multi-Supplier 

Refrigerator, Standards Single Wide 4 Multi-Supplie 

Sonicator 1 Tekmar TM 375 

Spectrophotometer 1 Sequoia-Turner 340 

Spectrophotometer Thermo Genesys 10UV 

Scanning 

Spectrophotometer-Colorimeter 1 HACH DR 890 

Sterilizer, UV Light Crosslinker 1 UVP CL-1000 

Stirrer, Magnetic Variable Speed 3 Corning PC 351 

TCLP Rotator 1 Associated Design 4A 

TCLP, ZHE Extractor 3 Associated Design 

Thermal Tube Desorber 1 Dynatherm 890 

Thermometer, Digital NIST certified 

(0.0°C to 105°C) 

1 Control Company 4000 

Thermometer, Digital NIST certified 1 Control Company 4015 
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(160°C- 450°C) 

Thermometer, glass working 

thermometers 

~15 Multi-Supplier 

Trap, Refridge-Condensation 1 Savant RT400 

Turbidimeter 1 HF Scientific Micro100 

Turbo-Vap 2 Caliper Model 500 

Vortex 2 Fisher Genie 2 

Water Bath 1 Fisher 

Water Purification System 

Reverse Osmosis 

1 AquaSolutions RO2002 

Water Purification, Polisher System 1 Millipore Milli-Q 

Wet Chemistry, Flow Injection 

Analyzer, 

1 Lachat Quikchem 8000 
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Appendix A Endyne, Inc.-QSM Manual Rev10 

160 James Brown Dr. 

Williston, VT 05495 

Demonstration of Capability 

Certification Statement 

Analyst Name: 

Parameter: Method #: (Pesticides, BOD, Arsenic, etc.) (EPA #, SM #, etc.) 

Matrix: Data Summary Table Attached: (Y / N ) (Solid, Potable and/or Non Potable) 

Summary of Training: 

 

 

 

I, the analyst, agree to use only the most current version of the applicable SOP. 

Analyst Signature: Date: 

We, the undersigned, certify that: 

1. The analyst(s) identified above, using the cited test methods, which is in use at this facility for 

the analyses of samples under the National Environmental Laboratory Accreditation Program 

(NELAP), have met the Demonstration of Capability (DOC). 

 2. The analyst identified on this certification performed the test method 

 3. A copy of the test method and the laboratory-specific SOPs are available for personnel on-site. 

 4. The data associated with the DOC are true accurate complete and self-explanatory. 

5. All raw data necessary to reconstruct and validate these analyses have been retrained at the 

facility, and that the associated information is well organized and available for review by 

authorized assessors. 

 Harry Locker Ph.D. Technical Director Signature Date 

Mark Fausel Q.A Officer Signature Date 
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DOC Submittal Protocol 

Introduction: 

A Demostration of Capability (DOC) is required for every Analyst-Parameter-Matrix 

combination on an annual basis. To track the completion of these DOCs, at the 

beginning of the year, a WorkOrder is generated in LabTask and assigned the project 

name Demonstration of Capability. Each analyst is assigned a sample number and all of 

the tests they perform are logged in under that sample number. When an analyst creates a 

Workload Management Report, the DOC Sample ID shows up like any other test. This 

tells the analyst they need to create their DOC and submit it to the QA Officer. Once the 

DOC has been reviewed and signed off on by the Technical Director and the QA Officer, 

the associated DOC sample is “QC Accepted” in LIMS and is removed from the analyst’s 

Workload Management Report. This provides an easy way of monitoring an analyst’s 

suitability to perform a certain test. 

The DOC will be either an Initial DOC (IDOC)or a continuing DOC (CDOC). An IDOC 

is a summary of training and a Statistical calculation of 4 QC samples presented in a Data 

Summary Table. A CDOC is a summary of on-going training with either a statement of 

successful participation in blind PT testing or a statistical calculation of 4 QC samples 

presented in a Data Summary Table. 

Procedure: 

1. Every DOC submitted for authorization should have a Q-list # associated with it. 

a. The Q-list will only be for one sample: the DOC WO-Analyst Sample Number 

b. The Test-code of the analysis specific to the DOC. 

c. The entered result can be “Complete” or the default value. 

d. The Analysis Date is the essential parameter. Which will be used as the guide to 

track the annual performance of the DOC. 

2. The Data Summary Table is not mandatory for the DOC and form indicates whether a 

Data Summary Table is attached or not. 

3. Whenever possible, there should be no raw data associated with the DOC Q-List. 

4. The raw data should have already gone through full QA review as a component of 

data sets associated to other Q-lists. 

5. If a Data Summary Table is attached, the data must have a reference to the Q-lists 

with which the QCs were originally analyzed. 

6. If the DOC QA samples were not analyzed with lab samples and incorporated into a 

standard Q-list data packet then, the entire data packet must be submitted for review. 

a. The data packet would consist of a typical data packet including all calibration, 

blanks, etc. 
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b. The primary QA Reviewer reviews the entire data packet, signs-off on and 

forwards to the QA officer WITHOUT QC Accepting in LIMS. 

c. The Data Summary Table must list the Q-list number for each data point. 

7. If there is no raw data packet requiring review, then the LIMS DOC Q-list with DOC 

form, with or without the Data Summary Table, can be submitted directly to the QA 

Officer. 

8. Once the QA Officer receives the Q-List, it will be signed by the QA Officer and the 

Laboratory Technical Director. 

9. After signing, the Q-list is approved in LabTask and the DOC form with or without 

the Data Summary Table, is filed in the analyst’s Training Folder. 

a. The Data Summary Table reference to the Q-list numbers is what provides 

traceability to the raw data. 

10. If there is a data packet associated with the Q-list it is filed with the other Q-lists. If 

there is no data then the Q-list page is discarded. 
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Appendix B 

Client Confidentiality and Privacy 

Policy 

1. I understand that it is Endyne’s policy that our clients have a right to the privacy 

of their information, in all of its manifestations, and that they are free from the 

risk of disclosure of this information from any current or past employee of 

Endyne. 

2. I understand item 1. includes any discussions in which the name or identity of a 

client is revealed to any individual not currently employed by Endyne. The 

disclosure of this identity includes any reference in which the identity of the client 

is implicit and that the revelation of this information in any way could demean the 

standing of that client in the community. 

3. I understand that this policy applies not only to our customers but to any projects 

or work performed by our customers for which the identity of their clients has 

been made known to us. 

4. I have been apprised of Endyne’s procedures for the release of all data, be it 

verbal, electronic or written. I understand the only authoritative results reported 

by Endyne are in the form of a hard copy report with the original signature of the 

Laboratory Director or appointed signer. 

a. Clients who request a verbal notification of results must establish proof of 

identity as the proper client. This is accomplished by referencing the C-of-C 

number in the upper right hand corner. 

b. Clients who request a fax must indicate on the C-of-C whom will receive 

results or if the request is made by phone, the individual must prove they are 

the stated client. This is usually accomplished by referencing the distinctive 

C-of-C sequence number. 

c. Deliverables in the form of e-mails are only provided to established 

customers, whom have made formal arrangements for receipt of results. 

d. All electronic transmissions are accompanied with a disclaimer stating that the 

material is confidential information intended solely for the recipient and to 

notify Endyne immediately upon incorrect receipt 

Employee’s Signature: ____________________________ Date: _________________ 

Trainer’s Signature: ______________________________ Date: _________________ 
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I acknowledge that I have read this Quality Systems Manual and agree 

 to adhere to the policies outlined within. 

 Name Date 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 
ATTACHMENT 5 
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Endyne, Inc.

160 James Brown Dr.

Williston, VT 05495

Phone: (802) 879-4333

Fax: (802) 879-7103

TOXICITY CHARACTERISTIC

LEACHING PROCEDURE (TCLP)

Method EPA 1311

Standard Operating Procedure

REVISED: January 21, 2008

Revision #: 9

Technical Director: Date : 

Harry B. Locker Ph.D.

QA Officer: Date : 

Mark L. Fausel
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TABLE OF CONTENTS

Section Page

I – Overview 3

II – Storage 3

III – Waste Disposal 3

IV – Sample Collection, Preservation & Storage 3-4

V – Equipment & Supplies 4

VI – Reagents 5

VII – Interferences 5

VIII – Quality Control

5

IX – Extraction Procedure 6-8

X – Calibration and Standardization 9

XI – Data Reduction 9

XII – Data Recording 9-10

XIII – Instrument Maintenance 10

XIV – Trouble Shooting 10

XV – References 10

XVI - Definitions and Acronyms 10-11

XVII - Revision History 11

Analyst Review Sign Off Sheet 12
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I. Overview:

TCLP is used to evaluate the mobility of analytes in wastes. It is designed to

mimic the leaching which occurs in landfills over 20 years. Sample aliquots are

spun in a buffered solution for 18 hours. The sample is filtered and the filtrate is

analyzed for target compounds that have migrated into the solution.

II. Safety:

A. This method involves the handling of the chemicals outlined below. Each of

these chemicals may have specific associated hazards. Analysts must read and

become familiar with all elements of each chemical’s MSDS. Make special

awareness of the symptoms of exposure and potential routes of entry. Analysts

must notify the Safety Officer immediately if any symptoms of exposure are

suspected.

B. Personal protective equipment (i.e. gloves, goggles, and lab coats) must be worn

at all times in designated work areas. All applicable engineering controls, such as

fume hoods or splash shields, must be used when performing analyses. To ensure

the safety of all laboratory personnel, work areas must be kept neat and

organized. Equipment and bench-tops must be cleaned and sterilized at the

completion of each task. All containers must be properly labeled as to contents

and hazard ratings. Spills must cleaned promptly and completely.

III. Waste Disposal:

A. Sample extracts should be treated and disposed of in the same manner as the

original sample.

B. Contact the laboratory’s Hazardous Waste Manager for samples that have

high levels of contamination for proper disposal.

C. Only personnel that have been trained to properly dispose of hazardous waste

may do so in the hazardous waste room in the proper waste drums.

IV. Sample Collection, Preservation & Storage:

A. Samples should be collected and stored in the same manner as if the TCLP

procedure were not being performed except there is no chemical preservation

until after the samples have been TCLP prepared.

1. Metals should be collected in glass or plastic containers.

2. Organics should be collected in glass containers.

3. Volatiles should be collected in glass containers with minimal headspace.

B. Samples must not be preserved until after the TCLP extraction has been

performed. Extracts should be preserved in the same manner as typical liquid

samples for each method.

1. Metals pH <2.0 with HNO3.

2. Semi-volatiles are refrigerated.
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3. Volatiles pH <2.0 with HCl.

Sample Maximum Holding Times

Parameter to TCLP Extraction Preparative Extraction Extraction to Analysis

Volatiles 14 days NA 14 days 

Semi-Volatiles 14 days 7 days 40 days 

Mercury 28 days NA 28 days 

Metals, except Hg 180 days NA 180 days

V. Equipment & Supplies:

• Rotator/Tumbler

• Zero-headspace Extraction Vessel (ZHE)

• Bottle Extraction Vessel

• Filter Pump

• pH Probe (+/- 0.05 accuracy)

• Analytical Balance

• Low metal acid treated filters

• Buchner funnel

• Side arm flask

• Gas tight syringe

• HCl preserved 40 mL VOA vials

• glass jars (for tumbling and final sample storage)- new, borosilicate

• plastic containers

• Nitrogen gas tank for pressuring ZHE

• stirring hot plate and stir bar

• beakers or flasks

• Pressure filtration apparatus

• Magnetic Stirrer and Hot Plate

• Min./Max. Thermometer
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VI. Reagents: (ACS Reagent grade or better)

1. Extraction Fluid #1

22.8ml Glacial Acetic Acid and 257.2mls 1N NaOH made up to 4.0 Liters.

Target pH : 4.93 +/- 0.05

2. Extraction Fluid #2

22.8ml Glacial Acetic Acid to 4.0 Liters DI

Target pH: 2.88+/- 0.05

3. 1N NaOH:

40.0g NaOH in 1L DI Water

4. 1N HCl:

10mls concentrated HCL brought up to 120ml with DI Water

VII. Interferences:

A. Sample carry-over from contaminated extraction vessels. Be sure to clean

vessels well after each use.

B. Bleed from Filters. Be sure to use proper low metal, TCLP filters.

C. Method specific interference’s are outlined in the analytical SOPs.

VIII. Quality Control:

A. Tumbled Reagent Blanks should be performed for all analyses for every 20

samples spun in each extraction vessel used. Reagent Blanks shall be tumbled

with new batches of extraction fluid. Volatile blanks should be spun in ZHE

vessel. Sufficient volume should be provided for LRB and LFB analyses.

B. Matrix spikes shall be performed at the appropriate frequency for each

analytical technique. Sample extract volumes should be sufficient to perform

these analyses. The analyst shall perform metal and semi-volatile spikes at

the time of digestion or extraction. Volatile samples shall be spiked following

the TCLP tumble at the time of sample extract preservation.

C. Duplicates shall be performed at the appropriate frequency for each analytical

technique. Sample extract volumes should be sufficient to perform these

analyses.

D. MDLs, DOCs and quality control analysis are tracked under the individual

analytical method QA protocols.
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IX. Extraction Procedure:

A. Sample Evaluation

1. Determination of percent solids (non-filterable). Use only 1 filter per

sample. Any sample left behind on the filter (even liquid) is considered

non-filterable. Note: aliquots may be allowed to settle or be centrifuged

prior to filtering to facilitate more complete filtering prior to filterclogging.

a. If the waste will obviously yield no liquid when subjected to filtration

the sample is determined to be 100% solids. Proceed to section IX.A.2

b. If the sample is determined to be liquid or multiphasic, weigh >100g

of sample and record the weight.

c. Pre-weigh a filter and the container that will receive the filtrate and

filter the sample under gradual pressure increase.

i. Apply pressure starting at approximately 10psi and increase

incrementally up to a maximum of 50psi.

ii. If no filtrate is collected, the percent solid is determined to be

100%. Proceed to section IX.A.2.

d. Determine weight of filtrate and that of the solid material.

e. Determine the % solid (% solid = solid mass/total sample mass*100)

i. If the % solid is < 0.5%, the collected filtrate is the TCLP extract

for metal and semi-volatile analysis. Filter additional sample as

needed for analytical requirements.

ii. If the % solid is < 0.5% and volatile analysis is required, charge a

ZHE vessel with a fresh portion of waste sample, the collected

filtrate is the volatile TCLP extract.

f. If the % solid is determined to be > or equal to 0.5% and it is noticed

that a small amount of filtrate is entrained in wetting of the filter,

determine the percent dry solids.

i. Dry the solid phase and filter at 100o

C (+/-20oC) until two

successive weighing yield the same value within +/- 1%.

ii. Calculate the % Dry solids.

 % Dry = (Dried filter mass – Tare Wt. of filter)/Initial mass*100

g. If the % dry solid is determined to be < 0.5%, follow the procedure

outlined in section A.1.e.i for metals and semi-volatile analysis.

Follow the procedure outlines in section A.1.e.ii. for volatile analysis.

2. Determination of Extraction Fluid

a. All ZHE extractions use Extraction Fluid #1.

b. Metal and Semi-Volatile Extraction fluid determination.

i. Transfer a 5.0g portion of the solid phase of the sample to a 250ml

Beaker.

ii. Add 96.5mls of DI water and stir for five minutes.

iii. Measure pH, if <5.0 use Extraction fluid #1.

iv. If pH >5.0, add 3.5mls of 1N HCl heat to 50°C and hold for 10

minutes.
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v. Allow solution to cool and measure pH. If pH < 5.0, use

extraction fluid #1 otherwise use extraction fluid #2.

3. Determination of Particle Size – Particle size must be sufficiently small so

as to provide satisfactory surface area contact with the extraction fluid. (>

3.1cm2/gram or less than 0.95cm at its narrowest dimension).

a. Solid phase of sample must be capable of passing through a 9.5mm

(0.375 inch) standard sieve, unless material would provide adequate

surface area contact.

b. If sample is not able to pass through the sieve, the solid portion of

sample must be prepared by crushing, cutting or grinding. If the

sample is being prepared for volatile analysis, the waste and reduction

material should be kept at 4o

C with minimal exposure to the

atmosphere.

B. Extraction Procedure - Semi-Volatiles, Metals

1. Liquid samples with <0.5% Solids

a. Filter sample, filtrate is used as extract. Filter is discarded

2. Solid samples with 100% solid determination

a. Transfer a minimum of 100g of waste sample to an extraction vessel.

b. Add 20x the weight of the sample of proper extraction fluid to the

vessel.

c. Spin for 18 hours ±2 hours.

d. Filter sample, filtrate is the TCLP sample to be analyzed.

3. Multi-Phase samples with >0.5% Solids

a. Filter a minimum of 100g sample and collect filtrate. Store filtrate in

fridge for later use.

b. Determine the weight of the solid phase. Transfer solid phase of

sample to Extraction Vessel.

c. Add 20x the weight of the solid phase of proper Extraction fluid to the

vessel.

d. Spin for 18 hours ±2 hours.

e. Filter sample and collect tumbled filtrate. Combine the tumbled

filtrate with the filtrate from step B. 3. a. Sample aliquots for analysis

must maintain the appropriate ratio of pre and post extraction filtrates.

f. Combined filtrate is the TCLP extract to be analyzed.

4. Multi-Phase samples with >0.5% Solids where the liquid fraction is not

miscible with the TCLP Extraction Fluid.

a. Filter a minimum of 100g sample and collect filtrate. Store filtrate in

fridge for later use.

b. Transfer solid phase to extraction vessel.

c. Add 20x the weight of the sample of proper Extraction Fluid to the

vessel.

d. Spin for 18 hours ±2 hours.

e. Filter sample and collect all of the extract.
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f. Separate phases and determine volume of each phase.

i. If extracted filtrate contains additional non-aqueous fraction. The

non-aqueous fraction should be combined with the pre-extraction,

non-aqueous fraction.

ii. If the Pre-extraction filtrate contains aqueous fraction. The

aqueous fraction should be combined with the TCLP buffer

extract.

iii. Once all like-phase extract and filtrates have been combined the

volume of each phase should be determined for use in the

weighted-average quantitation equation.

g. Analyze sample aliquots separately mathematically combine values to

determine final concentration.

(V1) (C1) + (V2) (C2)

Final Analyte Concentration = V1 + V2

where:

V1 = The volume of the first phase (L).

C1 = The concentration of the analyte of concern in the first phase (mg/L).

V2 = The volume of the second phase (L).

C2 = The concentration of the analyte of concern in the second phase

(mg/L).

C. Extraction Procedure – Volatiles

1. Liquid samples with < 0.5% solids.

a. Filter samples through a clean ZHS extractor as per Section IXC2 and

analyze as a filtrate sample.

2. Solid samples with 100% solid determination.

a. Transfer an aliquot of sample (minimum of 25g) to a Zero Headspace

Extraction Vessel (ZHE).

b. Add 20x the weight of sample of Extraction Fluid #1.

c. Compress the cylinder piston with 30psi Nitrogen and remove any

headspace.

d. Spin for 18 hours ±2 hours.

e. Pull off sample from Extractor using a gas-tight syringe.

f. Transfer to 40ml VOA vial with no air bubbles, preserve and analyze

as soon as possible.

3. Multi-Phase samples with > 0.5% Solids

a. Based on the % solid, determine how much of the sample combined

with 20x the fraction of the solid material is needed to total 500mls.

b. Add the unadulterated sample to the ZHE.

c. Gradually charge the ZHE and collect filterable fraction of the sample

in a gas tight syringe. Mass of the filtrate is determined and filtrate is

stored with zero headspace (in Tedlar bag or VOA vials) at 4o

C until

reconstitution with solid extract or analysis.

d. Vent the ZHE pressure charge and leave vent valve open.
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e. Add 20x the weight of the solid fraction of Extraction Fluid #1 to the

ZHE with a gas tight syringe through the sample collection valve.

f. Close the ZHE vent valve and the sample collection valve.

g. Charge the ZHE vessel to +/- 30psi and check to ensure there is no

headspace

h. Spin for 18 hours ±2 hours.

i. Pull off extract from vessel using a gas-tight syringe.

j. Combine initial sample filtrate with filtrate from solid phase ZHE

extraction. The combined filtrates are the TCLP extract. Sample

aliquots for analysis must maintain the appropriate ratio of pre and

post extraction filtrates. Preserve to a pH<2 with HCl and store for

analysis at 4o

C with zero headspace

k. If the two filtrates are not miscible, each filtrate will be analyzed

separately and the final analyte concentration will be determined as

outlined in section IX.B.4.f.

X. Calibration & Standardization:

Calibration and standardization is based on individual analytical methods. Refer

to individual analytical SOPs.

XI. Data Reduction:

A. Percent Solids Determination

( A - B) x 100 = C

A

Where:

A = Total weight of sample before filtration

B = Weight of filtrate

C = % Weight of solid portion

B. Analyte Concentration Determination of Biphasic Extracts

FAC = (V1 x C1) + (V2 + C2)

V1 + V2

V1 = Volume of the 1st phase

C1 = Concentration of Analyte in 1st phase

V2 = Volume of the 2nd phase

C2 = Concentration of Analyte in 2nd phase

FAC = Final Analyte Concentration
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XII. Data Recording:

.

A. All TCLP extraction parameters are recorded in the TCLP log book binder.

This would include the preparation date, manufacturer, lot #, date of receipt

and expiration date of all the chemicals required to make the fluid. Once the

fluid is prepared it is given an expiration date of one year from the preparation

date. It is discarded if held past longer than the expiration date.

B. Before using a batch of extraction fluid the pH must be checked and recorded

in the TCLP reagent log located in the log book binder and on the bottle.

Calibration of the pH meter is documented in its own maintenance log.

C. Descriptions of samples (appearance and form), their preparation (crushing,

cutting, grinding) and all details of the extractions (for example: mass of

sample. percent solid, extraction fluid used, date and time of start and finish of

extraction, etc.) are recorded by sample number in the TCLP log binder.

D. Start and stop pressure of the ZHE extraction vessels is documented on the

sample extraction sheet in the TCLP log binder. If the ZHE stop pressure is

zero upon tumble completion, the extracted sample is invalid. The ZHE

vessel must be repaired for leaks and the sample re-extracted.

E. The tumble area Min./Max. Thermometer is reset at the start of each

extraction tumble. The high and low tumble time temperatures are

documented in the sample extraction sheet in the TCLP log binder. If the

temperature extremes fall outside 23o

C +/- 2oC the extracted sample is invalid.

The tumble area atmosphere will be corrected to maintain stable temperature,

and the sample re-extracted.

F. The TCLP tumbler is calibrated monthly and documented in the tumbler log

of the TCLP log binder. Acceptance is 30RPM +/- 2RPM. Instrument

maintenance is required prior to sample extraction if the tumble rate falls

outside method acceptance limits.

XIII. Instrument Maintenance:

A. TCLP Tumbler needs regular cleaning. Contact Associated Designs if RPM

fall outside acceptance. Contact information is posted on front of the tumbler.

B. Balance Maintenance is performed as the Balance SOP dictates.

C. pH Meter maintenance is performed as the pH SOP dictates

D. Submerge charged ZHE in sink of water for convenient leak check. Do not

submerge pressure gauge above glass PSI display.

E. Min./Max. Thermometer is NIST traceable. Refer to thermometer section of

TCLP log binder for calibration due date.

XIV. Trouble Shooting:

A. Be sure that all vessels are either brand new or cleaned properly with hot

soapy water and rinsed with DI prior to analysis.
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B. ZHE gaskets are a likely source of volatiles contamination. If the Volatiles

analyst detects high levels of solvents the extractionist should be notified

promptly so all gaskets can be replaced with new.

C. Be sure that there is no headspace in the ZHS vessels and that it is airtight. If

liquid leaks out of the vessel, check and replace gaskets as necessary.

XV. References:

A. EPA Method 1311 Toxicity Characteristic Leaching Procedure. Rev. 0, EPA

Methods and Guidance for Analysis of Water CD version 2.0. July, 1992.

XVI. Definitions and Acronyms:

A. TCLP-Toxicity Characteristic Leaching Procedure

B. ACS Reagent Grade Chemicals-A Chemical grade of highest purity which

meets or exceeds purity standards set by the American Chemical Society.

C. Multi-phase sample-a sample with multiple phases which are not miscible

with one another. (Solid/Liquid or Liquid/Solvent or multiple combinations)

D. ZHE-Zero Headspace Extraction Vessel - For use with the preparation of

samples to be analyzed for volatile organic contaminants

E. Percent Solid-Method specific definition of percent solid as determined by

TCLP sample evaluation procedure. More of an assessment of the portion of

sample unable to pass through a TCLP filter than a determination of solid

material. (Not to be confused with EPA 160.3 percent solid determination)

F. Percent Dry Solid-Method specific definition of percent dry solid as

determined by TCLP sample evaluation procedure (Not to be confused with

EPA 160.3 percent solid determination)

G. DI/DIW-De-ionized filter polished laboratory grade water

H. HNO3-Nitric Acid

I. HCl-Hydrochloric Acid

J. NaOH-Sodium Hydroxide

K. MSDS-Material Safety Data Sheet

L. 1N-A One Normal Solution

XVII. Revision History:

Revision 5. - April 2004. General review for edits and added References section.

Revision 6. - April 2005. General Review for edits and added Revision History

Revision 7. - January 2006. General Review for edits.

Revision 8 - October, 2007 General review and edits.

Revision 9 - January 21, 2008 -Edit typos in section IV.

-Added Misc. Equipment and supplies to section V.

-Added 1N NaOH and 1N HCl to VI Reagents.

-Edit of typos and procedural steps in VIII Quality Control

-Modifications to IX Extraction Procedures clarifying method specified extraction

requirements and procedures
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-Added tumbler requirements, temperature requirements and ZHE pressure

requirements to XII Data recording.

-Added thermometer, tumbler and ZHE leak check information to XIII

Maintenance.

-Added section XVI Definitions and Acronyms section to SOP
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I acknowledge that I have read this Standard Operating Procedure and agree

 to adhere to the Safety and Quality Control policies outlined within.

Name Date

 
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Endyne, Inc. 

160 James Brown Dr. 

Williston, VT 05495 

Phone: (802) 879-4333 

Fax: (802) 879-7103 

ICP 

Standard Operating Procedure

EPA Method 6010B 

REVISED: October 1, 2009 

Revision #: 5 

Technical Director: Date: 

Harry B. Locker Ph.D. 

QA Officer: Date: 

Mark L. Fausel 
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TABLE OF CONTENTS

Section Page

I – Overview 3 

II – Safety 3 

III – Waste Disposal 3 

IV – Sample Collection, Preservation and Storage 4 

V – Equipment & Supplies 4 

VI – Reagents & Standards 4 

VII – Interferences 5 

VIII – Quality Control 5 

IX – Analytical Procedure 6 

X – Calibration and Standardization 14 

XI – Data Reduction 15 

XII – Data Recording 15 

XIII – Troubleshooting 15 

XIV – Revision History 16 

XV – References 16 

XVI – Method Modifications 16 

Appendix 1 – Digestions 17 

XVII – SOP Attestation 18 
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I. Overview: 

- Inductively coupled plasma-atomic emission spectrometry (ICP-AES) may be used for 

the determination of dissolved, suspended, or total elements in drinking water, surface 

water, and domestic and industrial wastewater. This SOP is based upon EPA Method 

200.7 and 6010B. The analysis described in this method involves multielemental 

determinations by ICP-AES using either a sequential or simultaneous instrument. The 

instruments measure characteristic atomic-line emission spectra by optical spectrometry. 

Samples are nebulized and the resulting aerosol is transported to the plasma torch. 

Radio-frequency inductively coupled plasma produces element specific emission spectra. 

The spectra are dispersed by a grating spectrometer, and the intensities of the line spectra 

are monitored at specific wavelengths by a photosensitive device. Photocurrents from 

the photosensitive device are processed and controlled by a computer system. A 

background correction technique is required to compensate for variable background 

contribution to the determination of the analytes. 

II. Safety: 

 - Gloves, goggles, and lab coat should be worn when handling all samples, 

reagents, and standards. Acids and uncovered digesting samples should be handled in the 

fume hoods. An exhaust fan is installed above the ICP to remove emissions. The 

toxicity or carcinogenicity of each reagent used in this method has not been fully 

established. Each chemical should be regarded as a potential health hazard and exposure 

to these compounds should be as low as reasonably achievable. A reference file of 

Material Safety Data Sheets (MSDS) is available to all personnel involved in the 

chemical analysis. Specifically, concentrated nitric and hydrochloric acids present 

various hazards and are moderately toxic and extremely irritating to skin and mucous 

membranes. Use these reagents in a fume hood whenever possible and if eye or skin 

contact occurs flush with large volumes of water. Always wear safety glasses or a shield 

for eye protection, 

protective clothing and observe proper mixing when working with these reagents. 

The acidification of samples containing reactive materials may result in the release of 

toxic gases, such as cyanides or sulfides. Acidification of samples should be done in a 

fume hood. The inductively coupled plasma should only be viewed with proper eye 

protection from the ultraviolet emissions. It is the responsibility of the user of this 

method to comply with relevant disposal and waste regulations. 

III. Waste Disposal: 

- Liquid waste from the drain lines of the ICP is collected in a plastic container with a 

cap. When this container fills it is removed and taken to the hazardous waste disposal 

area and combined with the aqueous acidic metals wastestream. 
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IV Sample Collection Labeling, Preservation, and Storage: 

A. Collection: 

Samples are collected in plastic and glass containers of various sizes. 

B. Labeling: 

All samples are assigned a number, plus a unique identifier to indicate preservative 

and bottle type. 

C. Preservation: 

Upon arrival at the lab, soil samples are refrigerated for preservation. 

D. Storage: 

Soils and sludge samples are stored in the fridge on the first floor. 

V. Equipment and Supplies:

 - Volumetric flasks for making standards and diluting samples. 

 - Pipettes for digestions 

 - Leeman Labs Inc. ICP Prodigy Dual View System with Auto-sampler. 

 - Water recirculator, exhaust fan, Argon gas 

 - Leeman Labs Salsa computer software 

 - A variable-speed peristaltic pump which is required to deliver both standard and 

 sample solutions to the nebulizer is integral to the instrument. 

 - Analytical balance, with capability to measure to 0.1 mg, for use in weighing 

 solids, for preparing standards, and for determining solids in digests 

 or extracts. 

 - Block digester capable of maintaining 950

C 

- 50 ml plastic containers for the block digester, plastic watchglasses, caps, and 

associated plunger-type filters. 

- Timer for turning block digester on and off 

- Mixed Cellulose Ester Air Filters 

- Smear Tabs 

VI. Reagents and Standards: 

- Concentrated Nitric acid 

- Concentrated Hydrochloric Acid 

 - 30% Hydrogen Peroxide 

 - Multielement and single element standards 

- Concentrated Perchloric Acid 

NOTE: All incoming standards, reagents, dry chemicals, and acids shall be marked with 

date of receipt, date of expiration, and date of opening. Dry chemicals and concentrated 

acids shall be used within 20 years and 10 years respectively of the date of receipt or 

before the manufacture’s specified expiration date. 
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VII. Interferences: 

A. Spectral Interferences are caused by background emission from continuous or 

recombination phenomena, stray light from the line emission of high concentration 

elements, overlap of a spectral line from another element, or unresolved overlap of 

molecular band spectra. 

B. High concentrations of Iron may interfere with other elements. 

C. Aluminum used in sludges can interfere when analyzing Arsenic by ICP 

D. An Interelement Correction Std. is run annually. Relatively high concentrations of 

the single element standards listed in Table 3 of Method 200.7 are analyzed and the 

Apparent concentrations of all elements in the method are measured to ascertain 

which elements each element may interfere with. 

E. To perform an Inter-element Correction: 

1. The method is calibrated with the IEC function turned off. 

2. The single element standards are run at relatively high concentrations. 

3. A CSV file is generated. 

4. The apparent concentration of each observed element is divided by the measured 

concentration of the IEC standard. This coefficient may be positive or negative. 

5. These coefficients, for any reading greater than the associated MDL, are entered 

into the IEC tables on the element pages in the method. 

6. The instrument is calibrated with the IEC function turned on. 

7. An IEC Check Standard as described in the method should be run to confirm an 

IEC coefficient accuracy of +/- 20%. 

F. The ICP is very temperature sensitive. A temperature change of a few degrees an 

hour will interfere with results, especially for Ba and Al. 

VIII. Quality Control:

1. Demonstration of Capability (DOC). Each new analyst performs a set of four 

mid-range LFBs. The percent standard deviation and average percent recovery 

are determined for each analyte. Each must be less than 20% to ensure proper 

capability of the analyst for that method. This process is repeated annually for 

each metals analyst. 

2. Method Detection Limit (MDL). 

a. An MDL is run annually for each element. The final calculated MDL value 

must be at least 1⁄2 the reported value and the MCL. MDL’s should be digested 

and also non-digested. 

b. A QC is made with a concentration 1-10 times higher than the expected MDL. 

c. This sample is analyzed 7 times. The calculation should only use sequentially 

acquired results. 
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3. The MDL is calculated by taking the standard deviation of the values and 

multiplying by the appropriate number from the chart from the Code of Federal 

Regulations Appendix B to part 136 of chapter 1(7 is 3.143 

4. Quality Control Standard (QCS) is from an independent source. It shall be run 

quarterly with acceptance limits of +/- 5%. This is based upon the average of 3 

replicates. 

5. Laboratory Reagent Blank (LRB) is run every batch, or 20 samples, and be +/- the 

reporting limit or less than 1/10 of the measured sample concentration.. 

6. Laboratory Fortified Blank (LFB ) is from an independent source. It is run every 

batch, or 20 samples, with acceptance limits determined by a control chart for 

digested matrix. When digested it will have a prefix of TM and a suffix of S when 

digested as a soil. 

7. Calibration Check/Verification, CCV (or Instrument Performance Check – IPC) is 

analyzed before samples are analyzed. The percent recovery of the CCV should 

be +10%. The CCV shall be run every 10 samples. There is a CCV for each the 

axial and radial lines and are labeled CCVA and CCVR respectively 

8. A Calibration Blank (BLK) is analyzed before samples are analyzed and after 

every ten samples. The BLK should have concentration below that of the 

reporting limit or less than 1/10th of the measured sample concentration 

9. An IEC check standard should be run daily with a percent recovery of +/- 20%. 

10. Duplicate samples are run every 10 samples with a percent difference of no more 

than 20%. 

11. LFM (spike) samples are run every 10 samples or when results are questionable. 

Percent recovery for LFM’s must be +/-30%. 

12. LFM’s are not acceptable as Independent QC’s. 

13. If data does not meet the criteria outlined above, it may be used, but MUST be 

noted on the final client report. 

IX. Analytical Procedure:

A. Sample Preparation 

1. Drinking water sample preparation is dependent on the turbidity. If the turbidity 

is < 1.0 the samples are preserved, allowed to sit for at least 18 hours, and 

analyzed “as is”. If the turbidity is > 1.0 the samples are digested and analyzed as 

“total”. 

2. For dissolved metals analysis see Appendix 1 

3. For Total metals see Appendix 1 

4. For metals analysis in air samples see Appendix 1 

B. Data Acquisition 

1. Data acquisition is done using Leeman Lab Salsa software.

2. Overview: 

a. The Leeman Labs Software is "Command Central" of ICP operations. So in 

order to operate the ICP, the Leeman Software must be currently running. There 

is a shortcut icon on the Desktop to access Salsa (It looks like a chili pepper). 
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b. All data is stored in an Access database file located in the Salsa folder on the C: 

drive. 

3. The Lay of the Land 

a. The Salsa software is accompanied by a tutorial disk, which takes the operator 

through all of the major functions of the software. The software also has a very 

comprehensive manual, which is stored in the cabinet below the instrument. 

b. The instrument, argon supply, and software must remain on at all times. This 

will ensure that the camera is purged with argon so that no moisture is allowed to 

collect on the camera. If moisture were to collect on the camera and the coolers 

are turned on, then the camera will freeze and the instrument will be inoperable. 

c. The Instrument Control Page allows the operator to control all parts of the 

instrument manually: spectrometer, autosampler, torch gas, plasma, and 

pump. The values for each of these can be entered and saved as part of the 

method. 

C. Igniting the Plasma 

1. The plasma should run for 20 minutes prior to use in order to reach thermal 

equilibrium. There are a number of interlocks as indicated in the interlock drop 

down box of the Salsa software. These interlocks include Power, Plasma Door, 

Argon, Water, and ICP Covers. If any one of these interlocks is lit, the plasma will 

not ignite. Argon supply must be 90 psi. If the Argon pressure falls below 75 psi, 

the Argon interlocks will begin to flash. If the pressure falls below 60 psi, the 

plasma will self-extinguish. The Argon pressure should never go above 120 psi. 

After installing a new tank allow the instrument to purge for fifteen minutes to 

remove any moisture from the camera. If the argon supply is interrupted for any 

reason (if the tank runs out over night) it is imperative that the camera be purged with 

the camera cooler off to ensure that there is no moisture on the camera or it will 

freeze and render the instrument inoperable. 

a. Automatic Ignition 

i. Software, instrument and argon should already be on; if not then they need to 

be. Allow five minutes after turning on the instrument for the camera to 

stabilize. 

ii. Make sure all guards and covers are in place. 

iii. Turn on exhaust fan by flipping the single light switch behind the liquid 

argon tank and be sure that the baffle is in the open position. 

iv. Turn on Water recirculator. 

v. Check pump tubing integrity. 

vi. Clamp down pump tubing. 

vii. From the Instrument Control Screen select Autostart. 

b. Manual Ignition - only to be used by experienced operators! 

Leeman Tech support can guide the operator through this process. It is 

usually only used for diagnostic purposes. 
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D. Open Method 

1. A Method is a Leeman data file that contains information concerning analytical lines, 

integration parameters, calibration and check standards, and other related data. A 

Method must be created and opened before any analysis can begin. Once a Method 

has been created, it can be saved and opened at a later date. 

2. In order to create a Method 

a. From Method tab in the lower left corner of the screen, select Method from the 

tool bar and enter a Method name. Any name can be used, but for month to 

month general analysis, a Method indicating the month the Method is used may 

be a good idea. For example, Method name 02032007 would refer to a Method 

that was created in Feb. 2003. 

b. Proceed to Instrument Control panel and modify any necessary settings for 

spectrometer, autosampler, torch gas, plasma, and pump. 

c. If you are creating a completely new Method, choose Element Selection. If not, 

proceed to E. 

d. Select the atomic symbol for the first element of the list for which you will want 

to analyze. For example, enter Ba for Barium. 

i. After you enter the symbol, a list of available lines for the selected element 

will appear. Each available line will be indicated by the atomic symbol 

combined with a number. 

ii. The second major column contains the wavelength, in nm, of the line. The 

third column contains either a “I” or “II”; “I” indicates that emission for that 

lines originates from an excited atom; “II” from an excited ion. The fourth 

column contains the relative intensities of each line. The fifth column 

indicates whether or not that line has been aligned. This screen also lists 

those elements known to interfere with each selected line and pressing the 

add line button. 

3. Generally, you will want to choose the preferred line as indicated by the asterisk. If 

more than one line has an asterisk, choose the line with an asterisk and the highest 

relative intensity. A line is selected double-clicking on that line. 

4. If your chosen line has not been aligned, you must perform a Peak Wavelength on 

that line before using it. Peak Wavelength tells the ICP where to find that line in the 

Optics Box. 

5. Continue entering lines until you have entered all the desired elements. 

E. Analytical Parameters. 

Analytical Parameters contains integration parameters, sample uptake time, peaking 

line information, and computation options. 

1. Choose 3 Integrations. 

2. Uptake time choose a time of 15 seconds and check the ‘fast uptake’ option. The 

ICP will draw up sample for 15 seconds with the pump running faster before the 

pump slows and it begins analyzing it. 

3. Axial integration should be set for 30 seconds and radial should be 15 seconds. 

4. If you will be using Weight and Dilution factors, check the box for each option. 

More information on these options will appear in the Sample Analysis Section. 
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5. The Peaking Line is a line that is scanned to find the optimum viewing position in 

the plasma. The line Mn 257.610 is a good line to use because it is centrally located 

within all other lines. Therefore, the line Mn 257.610 should be included in Element 

Selection regardless of whether you will be testing for Mn. The Position Plasma 

Routine will be discussed in Section IX. M. 

F. Customizing Lines 

Under element selection when a particular line is selected from the list on the left 

side of the screen four option tabs appear: general, calibration, alignment, and IEC. 

1. General: This is where the torch view can be selected for each line, a line can be 

activated, and minimum or maximum values can be defined. 

2. Calibration: This is where the calibration curve can be viewed, type of calibration 

can be selected, and the calibration concentrations with their associated emission 

values are displayed. 

3. Alignment: This is where scans can be viewed to manually align peaks and 

background points can be set. 

4. IEC: This is where IEC coefficients are entered to compile the IEC tables. 

G. Internal Standards compensates for a group of elements that shift together. However, 

this option is not used currently. 

H. Standards/MSA is where line standards are entered. Each standard is assigned a 

name, checking the box next to their symbol can turn on elements, values are entered 

and units are assigned. Once a standard is entered the software assigns a location in 

the autosampler. 

I. Quality Control Checks is the screen where the QCS, CCV, BLK, Duplicates, and 

Spikes are defined. This is accomplished in a very similar manner to the Standards 

entry. 

J. QC Automation is where the operator indicates which standards should be run with 

each run. Standards can be run before, during, or after a sequence. Once items have 

been selected on this screen they can be viewed on the Sequence screen. 

K. Summaries Screen is where one can look to find the table form of Calibration 

information, Standards, and QC Checks. 

L. General stores the date and times that a method was created and modified and any 

additional notes that have been entered. 
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M. Position Plasma 

1. Prepare a standard that includes Mn at a concentration equal to the mid-point of 

the line. 

2. Put this Mn standard in a cup and send the sampler there by using the instrument 

control page. Allow 45 seconds for the standard to reach the torch. 

3. In the Spectrometer box of the Instrument Control page press the position plasma 

button. 

4. Press the Peak Plasma button in the window that comes up. 

5. Watch the peaks that come off. There should be two sets of symmetrical and 

matching peaks. This may require a second Peak Plasma to achieve. 

6. Once the each set of peaks are symmetrical and matching send the tip to rinse. 

N. Aligning Peak Wavelengths 

1. Once the lines are entered and the plasma is positioned each wavelength will need to 

be aligned. This can be done using the mid-point of the line. Single-element 

standards are best but multi-element standards will work for most elements. 

2. This can be done Automatically or Manually. 

a. Automatic Peak Alignment 

i. Select Tools from the toolbar and Auto Align 

ii. Select the Hg line and Auto Align. This will align the Hg lamp. 

iii. Accept the Hg alignment. 

iv. Send the autosampler to the standard and select those elements to be 

aligned by checking the box next to their symbol. 

v. Once the standard has reached the torch hit the Auto align button. 

vi. Accept the peaked lines. 

vii. Send auto sampler to rinse. 

b. Manual Peak Alignment 

i. From the instrument control page send the autosampler to the standard 

containing the target analyte. 

ii. In the tool bar select the Echelle Image Icon(black box with stars) 

iii. Enter a name for the Echelle Image such as Mn 2ppm 

iv. Enter a time for exposure such as 10, 1, 0.1, or 0.1 seconds.(When using 

multi-element standards, running multiple images with different exposure 

times will help as each element has a specific time that works best) 

v. Press OK 

vi. Once the image is acquired (icons will return on tool bar) send sampler to 

rinse. 

vii. Open the Element list of the Method and select one of the elements that 

needs to be manually aligned. 

viii. Select the Align Wavelength tab. 

ix. Select one of the recently acquired images by clicking on one of the 

images listed on the left side of the alignment window. 

x. The ideal image will have a small ball of bright pixels no larger than the 

height of the target box. 
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xi. If the image is an appropriate intensity move the box using the arrows on 

the screen to obtain the greatest intensity number in the lower right 

corner of the screen. Click accept to save the alignment if it has changed. 

xii. If the image is too bright try an image with a shorter exposure time. 

xiii. If the image is too dim to be seen hit the contrast button and see if that 

helps. If it does not then use an image with a longer exposure time. 

O. Selecting Background Points 

1. This can be accomplished concurrently with the manual peak alignment. 

2. Capture Echelle Images as described above. 

3. Open each element and look at the image with the most appropriate intensity (should 

already be aligned). 

4. Look at the graph on the lower portion of the window. The background points are in 

green. The ones that are of import here are the left and right background points. 

They should be located where the peak meets the baseline, or before the beginning of 

the next peak if there is another metal close by. 

5. Background points can be moved by clicking and dragging them. 

6. The other place that background points can be viewed is in the plot screen of the 

analysis page. 

P. Choose Sequence Tab 

1. Sequence screen is where the working sequence is entered and displayed. The left 

side of the screen displays graphically the standards and samples that are in the 

sequence. 

2. The Sample ID column of the table should include all pertinent information for the 

sample: identification number with suffix, duplicate or spike notation, and dilution 

ratio if applicable. 

3. The Extended ID column is not a working field. Any information entered in this 

field will not appear on the report. 

4. The Weight and Volume columns can be used if these computation options were 

turned on in the Analytical Parameters screen. 

5. The Macro (5th) column is for the entry of specific codes: D = Duplicate, S1= Spike, 

and the complete list can be found in the manual on page 158. 

6. In order for these changes to take effect the Update button must be pressed. 

7. The run sequence button will run the sequence as displayed on the left side of the 

screen. 

8. The Graphics on the lower part of the right side indicate which cups in the 

autosampler are active. 

Q. Calibrating the ICP 

1. Select Standards on QC Automation Page (i.e.: S1-S4) 

2. Calibration standards should be run before any other samples are run. 

3. Go to the Sequence page to be sure that the standards are set to go. 

4. UI should be 0 for all lines since an acid blank will be used as the Update Intercept. 

5. US should be equivalent to the highest standard. 

6. S1 is, again, the acid blank and should be 0 for all lines. 
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7. S2-S8 are the line standards as defined in the Standards page and in the positions 

seen on the sequence page. 

8. Immediately following the calibration standards should be the following standards 

CCV, BLK, and an Interference Check. 

9. The instrument is ready to be calibrated. 

10. Press the test tube rack icon on the tool bar or the Run Sequence button on the 

Sequence page to calibrate the ICP. 

11. The results of the CCV, and INT CHK samples will give a picture of how the 

instrument is performing. 

12. Individual line calibrations can be viewed from the list of elements on the Method 

page. 

13. The software automatically accepts lines. 

14. A calibration summary can be printed from the Summary page. 

R. Load Samples into Autosampler 

1. Turn off any unnecessary standards in the QC Automation page. 

2. Open the Sequence page.4 

3. Enter the Sample Identifications and macros in the appropriate columns. 

4. Update the Sequence page. 

5. Load the samples into the corresponding racks of the autosampler. 

6. Run Samples. 

S. Printing from the Results Page 

1. Open the Results page. 

2. Every analysis day should have an associated Analysis folder. 

3. To create a new Analysis folder click on Analysis, New and a box will pop up for a 

name. Use the date (i.e.: 01092006). 

4. As samples run they can be viewed on the Analysis Results page. A Detailed view 

shows each exposure’s value while the Statistics view shows a mean value. The 

detailed values may be helpful for diagnostics, but the statistical value is generally 

the one that is reported. 

5. The Single and All choices allow the operator to view a single sample or all of the 

samples in the open Analysis folder. 

6. Results can be printed from here by pressing the Print button. This will print out the 

measured value for every element in the method. 

T. Viewing Results from the Scan Page. 

1. From the Analysis page select the Scan tab. 

2. The Scan screen displays the peak and background correction points for selected 

samples. 

2 Select samples by checking the box to the left of the sample ID. 

3 Select the line by choosing from the list in the Line drop-down-box. 
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U. Viewing Samples from the Profile Page 

1. From the Analysis page select the Profile tab 

2. The Profile screen displays the peak shape of selected samples. This is a good way to 

view “scan” samples. 

3. Select samples by checking the box to the left of the sample ID. 

V. Viewing Samples on the Calculation Validation Page 

1. From the Analysis page select the Calc Validation tab. 

2. The Calculation Validation page displays the peak shape with background points as 

well as the raw numbers and IEC corrections. 

3. Select a sample by clicking on the Sample ID. 

W. Viewing a sample on the Image Page 

1. From the Analysis page select the Image tab. 

2. Select an Echelle image from the list of samples that have been run. 

3. The Image viewer displays the camera’s exposure. Each point of light is a 

quantifiable wavelength. 

4. The Zoom button allows the viewer to look more closely at a particular region. 

5. Clicking on any point in the image will re-center the image on that point. 

6. Spectral +/- buttons provide for the option of compounding images. Icons for these 

images will appear at the bottom of the analyzed sample list. 

X. Viewing sample data on the Control Chart Page 

1. From the Analysis page select the Control Chart tab. 

2. Select a series of samples or standards that you would like to chart. 

3. Control limits and markers can be added to the chart. 

Y. Viewing Samples on the Report Page 

1. From the Analysis page select the Report tab. 

2. Select those standards and samples that should appear on the report. 

3. Select Detailed (shows data for all three exposures) or Statistical (shows the mean). 

4. Choose the elements that should appear on the report. 

5. Choose the Report fields or Load a saved template. 

6. Press the Report button to generate a report. 

7. For a CSV file press the CSV file button and it will ask where to save it. 

8. Print a hard copy by pressing the print button. 

Z. Using the Recalculate page. 

1. To recalculate a sample with new calibration data. 

a. After recalibrating select the desired samples 

b. Press the recalculate button 

c. The recalculated data will appear at the bottom of the sample list. 

2. To Print a Summary of Calibration Data 

a. Select a sample or standard from the batch of concern. 

b. Press the Print button. 

AA. Shutting Down the Instrument 
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1. Pour 25% HNO3 into standard cup 14 and send the sampler there. 

2. Allow to flush for 2-3 minutes. 

3. Send the Sampler to rinse. 

4. Pour DI into standard cup 14 and send the sampler there. 

5. Allow to rinse for 2-3 minutes. 

6. Send the sampler to rinse and immediately to air. 

7. Once all of the tubing is dry press either the extinguish button on the tool bar or the 

Instrument Control page. 

8. Unclamp and release the tension from the tubing. 

9. Turn off the Exhaust Fan. 

10. Turn off the recirculator. 

11. Close the baffle on the Fan Duct. 

12. Pour any remaining standards into their appropriate containers. 

13. Instrument main power should remain on, with argon flowing, and the software 

open. 

BB. Method of Standard Additions 

The Method of Standard Additions allows for compensation of chemical interference 

by using the sample as the diluent for samples. The sample and two spikes of the 

sample are used as the standards of the calibration curve. The sample is used as S1. 

The first spike should contain twice the expected concentration while the second will 

contain four times the expected sample concentration. 

Build a new method for this using the sample number as the name of the method 

followed by SA. The line must be calibrated as linear. 

To retrieve results go to the calibration screen for each element of interest. The 

negative of the C value is the concentration of the sample in the same units as the 

line. 

X. Calibration and Standardization 

A. Each method is calibrated on a daily basis before use. 

1. Each line must have a correlation of ≥ 0.995. 

2. Analyst should verify correlation values and look at the calculated values for 

each line in the method. 

B. A CCV and BLK must be run before samples are run, every ten samples and after 

the last sample. 

1. All CCV must fall within +/-10% of the target concentration. 

2. Blank should be less than 1/10 of the MCL or 1/10 of the lowest reported value. 

C. An interference check standard must be run daily 

D. The interference check standard verifies the effectiveness of the interferal element 

correction. 

1. Recovery for the interference check must be +/-20%. 
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E. Any data that does not meet the above criteria must be appropriately qualified in the 

database and on the final report. 

XI. Data Reduction: 

All data is generated as mg/L (ppm) and can be reported in LIMS as such unless the 

client requests another unit of measure. If another unit of measure was requested the 

appropriate conversion should be applied before entering the value into LIMS. 

-Soil/sludge values are reported as mg/Kg dry weight. These values are calculated using 

the following equation: 

 

Conc. From Instrument (mg/L) x Digestion Volume (L) = Sample Conc. Mg/Kg dry wt. 

(Mass Digested (Kg) x Percent Solid (as a decimal) 

XII. Data Recording/Archival: 

Workload management report is generated from LIMS which indicates any metals 

analysis that are in house includes information such as Work Order Nos, Client, Due 

Date, if it’s a RUSH, the type of digestion or the metals requested. 

- Data is entered into Queue List and a copy of the data set is attached . 

- Queue with data is submitted for QC Review. 

- A metals digestion log is kept in Excel to record when and how samples are digested 

- A standards log is kept in Excel to record when new stocks are made up. 

-An instrument maintenance log is kept in Excel to record any maintenance or routine 

cleaning that may be done, such as when the water in the recirculator is changed or the 

pump lines are changed. 

-Data and spreadsheets are backed up and stored on the Inorg Central computer and a 

copy is burned onto cd. 

-Hard copy raw data is kept with Queue list in hanging folders in the in the filing cabinets 

on the second floor. 

-All raw data is archived annually in banker boxes and kept for a minimum of 5 years. 

XIII. Troubleshooting: 

• If the torch sputters and goes out immediately after ignition make sure that the lines 

are clamped down and the lines are dry form the pump to the torch. 

• If the torch sputters and goes out while running a sample, and the argon supply is 

sufficient, then the sample most likely has too many salts in it and should be run at a 

dilution. 

• If the CCV fails twice then try recalibrating, or position plasma. 

• If intensities drop off try the position plasma routine. If they are still low try a 

different nebulizer. 
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• If you have blanks failing for some metals (i.e. Na, Al) look at the scans to confirm a 

measurable peak on the blank. The sample uptake or torch may be contaminated. 

• If the intensities for all the standards of a given line are about the same and the scans 

confirm, then the instrument is probably peaked on an argon line for that element. 

Peak the line. 

XIV. Revision History 

February 2003 

April 2004 

October 2004 

January 2005 

April 2006 

 New ICP 

Revision 4, September 2009, Changes to QA section, minor revisions 

XV. References 

Method 6010B Inductively Coupled Plasma-AtomicEmission Spectrometry. EPA Test 

Methods for Evaluating Solid Waste Physical/ Chemical Methods, Version 2. EPA SW 

846, December 1997 United States Environmental Protection Agency. 

Electronic Code of Federal Regulations, 40 CFR – Chapter 1 – Part 136 – Appendix B. 

Definition and Procedure for the Determination of the Method Detection Limit - 

Revision 1.11. 

XVI. Method Modifications:

 
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Appendix 1: Digestions/Sample Preparation 

Metals in Soil/Sludge (EPA Method 3050B):

Soils: 1-30 grams (depending on how solid the sample is) of the sample is placed in the 

digestion cups. Teflon chips are added to the QC’s and Blanks. 2.5 mls of 50% Nitric Acid is 

added. Sample is digested at 95o

C for 15 minutes. An additional 2.5 mls of Conc. Nitric 

Acid is added to each sample 

These samples only require 1hr in the block digester at 950

C. However, if they are being 

digested with other Total metals, they can be left in for 4-6hrs. If this is 

 the case, add 30-40mls of DI to the samples so they won’t dry up. 

1 ml of DI and 1.5 mls of 30% Hydrogen Peroxide is then added and the samples are returned 

to the block digester at 950

C until they begin to effervesce. They are allowed to cool and an 

additional 1 ml of 30% Hydrogen Peroxide is added. They are warmed again until they begin 

to effervesce and removed to cool. Then they are digested for an hour at 95o

C. 

5mls of conc. HCl is added and digested for 1 hour. The samples are then brought back up to 

50mls with DI. A 2.0 um Teflon fiber filter is then used to be sure no large particulate matter 

is present that would block the lines of the ICP (Allowing to settle before filtering works 

well). 

Sludges: Sludges are digested just like Soils, except that an initial weight of 20-30 grams of 

sample is used. 

Metals in Air (NIOSH 7300):

Make ashing acid IN HOOD WITH ALL PPE - In 200ml Volumetric Flask add 40mls 

Conc. Perchloric Acid (HClO4) bring to the mark with Conc. Nitric Acid (HNO3) 

Make Dilution Acid - 50mls Ashing Acid to 600mls DI, dilute to 1L 

Place Cellulose filters (samples, QC’s, Blanks etc.) in 50ml Digestion cups. 

1. Add 5mls Ashing acid, cover with watchglass and let sit for 30min at room temperature. 

2. Heat in digestion block at 95o

C until 0.5ml remains. 

3. Add 2mls Ashing Acid and repeat step 2 until solution is clear. 

4. Remove watchglass and rinse residue into digestion cup with DI. Let heat until 0.5mls or 

less remains. Digest 3-4 hours max. 

5. Bring to 50mls with dilution acid. 

6. Separate calibration lines are run using the dilution acid matrix.
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XVI. SOP Attestation 

I acknowledge that I have read this Standard Operating Procedure and agree 

 to adhere to the Safety and Quality Control policies outlined within. 

 Name Date 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 
Element Method MDL mg/L

 Reporting 

Limit mg/L

Independent 

LFB 

Accuracy 

Limit %

Precision 

Limit % Element Method

MDL 

mg/Kg 

Reportin

Limit 

mg/kg

Aluminum EPA 200.7 0.01995 0.050 +/- 10.0 20.0 Aluminum EPA 6010B 0.617 2.5 

Antimony SM 3113B 0.00044 0.002 +/- 10.0 20.0 Antimony EPA 6010B 0.296 1.00 Arsenic SM 3113B 0.00014 0.002 +/- 10.0 20.0 Arsenic EPA 6010B 0.007 1.00 Barium EPA 200.7 0.00036 0.020 +/- 10.0 20.0 Barium EPA 6010B 0.0084 1.00 Beryllium EPA 200.7 0.00022 0.001 +/- 10.0 20.0 Beryllium EPA 6010B 0.0059 0.50 Boron EPA 200.7 0.01162 0.05 +/- 10.0 20.0 Boron EPA 6010B 1.09 2.50 Cadmium EPA 200.7 0.00042 0.002 +/- 10.0 20.0 Cadmium EPA 6010B 0.022 0.50 Calcium EPA 200.7 0.00523 0.100 +/- 10.0 20.0 Calcium EPA 6010B 1.620 5.00 Chromium EPA 200.7 0.00044 0.005 +/- 10.0 20.0 Chromium EPA 6010B 0.033 0.50 Chromium +6 EPA 7196A 0.01100 0.05 +/- 20 20.0 Chromium +6 EPA 7196A 1.083 5.00 Cobalt EPA 200.7 0.00083 0.020 +/- 10.0 20.0 Cobalt EPA 6010B 0.035 1.00 Copper EPA 200.7 0.0002 0.020 +/- 10.0 20.0 Copper EPA 6010B 0.484 1.00 Iron EPA 200.7 0.00504 0.020 +/- 10.0 20.0 Iron EPA 6010B 1.31 5.00 Lead SM 3113B 0.00037 0.001 +/- 10.0 20.0 Lead EPA 6010B 0.151 1.00 Magnesium EPA 200.7 0.0341 0.050 +/- 10.0 20.0 Magnesium EPA 6010B 0.162 2.50 Manganese EPA 200.7 0.000888 0.020 +/- 10.0 20.0 Manganese EPA 6010B 0.023 1.00 Mercury EPA 245.1 0.00003 0.001 +/- 10.0 20.0 Mercury EPA 7471A 0.0004 0.050 Nickel EPA 200.7 0.00054 0.005 +/- 10.0 20.0 Nickel EPA 6010B 0.037 1.00 Potassium EPA 200.7 0.00256 0.100 +/- 10.0 20.0 Potassium EPA 6010B 4.98 10.0 Selenium SM 3113B 0.00033 0.005 +/- 10.0 20.0 Selenium EPA 7740 0.0168 0.250 Silver EPA 200.7 0.0028 0.020 +/- 10.0 20.0 Silver EPA 6010B 0.053 1.00 Sodium EPA 200.7 0.0427 0.050 +/- 10.0 20.0 Sodium EPA 6010B 1.250 5.00 Thallium SM 3113B 0.00023 0.001 +/- 10.0 20.0 Thallium EPA 6010B 0.249 2.50 Vanadium EPA 200.7 0.000639 0.020 +/- 10.0 20.0 Vanadium EPA 6010B 0.0216 1.00 Zinc EPA 200.7 0.0032 0.005 +/- 10.0 20.0 Zinc EPA 6010B 0.060 1.00 Calculated values are based on a standard digestion mass and a 100% dry sample.

2010 Quality Control RCRA 8/ PRIORITY 

POLLUTANT 13 METALS in Water

2010 Quality Control for RCR

POLLUTANT 13 META

Endyne, Inc.

160 James Brown Drive

Williston, Vermont

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Endyne, Inc.

160 James Brown Dr.

Williston, VT 05495

Phone: (802) 879-4333

Fax: (802) 879-7103

VOLATILE ORGANIC COMPOUNDS

Method EPA 8260/8260B

Standard Operating Procedure

REVISED: September 26, 2007

Revision #: 10

Technical Director: Date : 

Harry B. Locker Ph.D.

QA Officer: Date : 

Mark L. Fausel
Endyne, Inc. VOC Method EPA 8260/8260B SOP

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TABLE OF CONTENTS

Section Page

I – Overview 3

II – Safety 4

III – Waste Disposal 4

IV – Sample Collection, Preservation & Storage 4

V – Equipment & Supplies 5

VI – Reagents 5

VII – Interferences 5-6

VIII – Quality Control 6-9

IX – Procedure 9-11

X – Calibration and Standardization 11-12

XI – Data Reduction 12-13

XII – Data Recording 14-15

XIII – Instrument Maintenance/Trouble Shooting 16

XIV – Method Modifications 16

XV – Bibliography/Reference 17

XVI – Revision History 17

Table 1-BFB Mass Intensity Criteria 18

Appendix A-Soil Sample Preservation with Methanol 19

Table 2 - Reporting limits 20

I. Overview:
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-Method 8260B is used to determine volatile organic compounds (VOCs) in a variety of

waste matrices, including waters, soils, sludges, waste solvents and petroleum wastes.

Samples are purged with an inert gas (N2). Analytes are captured on a packed sorbent

trap, then back flushed with a stream of Helium into a capillary GC Column interfaced to

a mass spectrometer.

-The following compounds are determined by this method:

Dichlorodifluoromethane

Chloromethane 2-Hexanone

Vinyl Chloride 1,3-Dichloropropane

Bromomethane Tetrachloroethene

Chloroethane Dibromochloromethane

Trichlorofluoromethane 1,2-Dibromoethane

Diethyl Ether Chlorobenzene

Acetone 1,1,1,2-Tetrachloroethane

1,1-Dichloroethene Ethylbenzene

Methylene Chloride m/p-Xylene

Carbon Disulfide o-Xylene

Methyl-t-butylether (MTBE) Styrene

trans-1,2-Dichloroethene Bromoform

1,1-Dichloroethane Isopropylbenzene

2-Butanone 1,1,2,2-Tetrachloroethane

2,2-Dichloropropane 1,2,3-Trichloropropane

cis-1,2-Dichloroethene n-Propylbenzene

Chloroform Bromobenzene

Bromochloromethane 1,3,5-Trimethylbenzene

Tetrahydrofuran (THF) 2-Chlorotoluene

1,1,1-Trichloroethane 4-Chlorotoluene

1,1-Dichloropropene tert-Butylbenzene

Carbon Tetrachloride 1,2,4-Trimethylbenzene

1,2-Dichloroethane sec-Butylbenzene

Benzene p-Isopropyltoluene

Trichloroethene 1,3-Dichlorobenzene

1,2-Dichloropropane 1,4-Dichlorobenzene

Dichlorobromomethane n-Butylbenzene

Dibromomethane 1,2-Dichlorobenzene

4-Methyl-2-pentanone 1,2-Dibromo-3-chloropropane

cis-1,3-Dichloropropene 1,2,4-Trichlorobenzene

Toluene Hexachlorobutadiene

trans-1,3-Dichloropropene Naphthalene

1,1,2-Trichloroethane 1,2,3-Trichlorobenzene

Isopropyl Alcohol Methyl isothiocyanate (MITC)

ETBE Isopropyl ether

TAME t-Butanol

Acrylonitrile Acrolein
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II. Safety:

This method involves the handling of the chemicals outlined below. Each of

these chemicals may have specific associated hazards. Analysts must read and

become familiar with all elements of each chemical’s MSDS. Make special

awareness of the symptoms of exposure and potential routes of entry. Analysts

must notify the Safety Officer immediately if any symptoms of exposure are

suspected.

PPE must be worn at all times in designated work areas. All applicable

engineering controls, such as fume hoods or splash shields, must be used when

performing analyses. To ensure the safety of all laboratory personnel; work areas

must be kept neat and organized, equipment and bench-tops must be cleaned and

sterilized, if necessary, at the completion of each task, all containers must be

properly labeled as to contents and hazard ratings and spills cleaned immediately

and completely.

A. Lab coats, nitrile gloves and protective eyeglasses are to be worn at all times during

analysis by this method and when handling any laboratory sample.

B. A thorough MSDS review of Hydrochloric Acid, Methanol, Ascorbic Acid, Sodium

Thiosulfate and all laboratory calibration standards should be performed prior to

analysis by this method.

C. All standards should be made in a fume hood away from heat sources.

D. Several analytes tested by this method have been classified as human carcinogens.

Stock standards of these materials should be handled in fume hoods with appropriate

personal protective equipment.

III. Waste Disposal:

A. Expired standards, QCs and misc. solvents are disposed of in the flammable liquids

drum in the hazardous waste room.

B. Non-contaminated (“non-hot”) samples can be dumped down the drain with a stream

of running water.

C. Contaminated (“Hot”) samples are disposed of in the corrosive liquids drum in the

hazardous waste room.

D. Soil samples are disposed of in the soil waste drum in the hazardous waste room.

IV. Sample Collection, Preservation and Storage:

A. Sample holding time is 14 days from the sample time.

B. All liquid samples should be sampled in duplicate, pH adjusted to < 2 with HCl and

stored at 4°C with no headspace.

C. All soil samples should be sampled in duplicate and stored at 4°C with no headspace.

D. Refer to Appendix A for MeOH preservation sample collection (if samples are

methanol preserved in the field).

E. Air Samples collected in tedlar bags should be analyzed within 8 hours of sampling

V. Equipment and Supplies:
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-GC: Hewlett Packard 5890 Split/Splitless option with EPC

-MS: Hewlett Packard 5971 Series

-Miscellaneous Syringes & Vials

-Analytical Balance

-OI Analytical 4560 sample concentrator with MPM 16

-OI Analytical 4560 sample concentrator with DMP 16

-Injection port liners, 2mm (Supelco P/N 2-0513,01 or equivalent)

-Purge Trap (Supelco P/N 2-4938 or equivalent)

-Capillary column-60m, 0.32mm ID, 1.8um df (Restek P/N 10972 or equivalent)

-Glass vials, 20ml and 40ml with PFTE lined screw cap

VI. Reagents:

-Reagent Grade DI Water (Organic-free)

-Methanol (Purge & Trap Grade or Better)

-Volatile Mix Standard (NSI Q2479 Custom Volatiles Mix - 200 ppm)

-Volatile Mix Standards (AccuStandard #’s M-502A-r, M-8260-ADD-10x, M-502B, 

S-457S-10X, S-078-10X)

-Internal Standard Mix (AccuStandard M-8260-IS 200 ppm)

-Surrogate Standard Mix (AccuStandard M-8260-SS 200ppm)

-Hydrochloric Acid diluted to 1:1 v/v with DI water.

-Ultra high purity Helium

-Ultra High purity Nitrogen

-2-Chloroethylvinylether Standard (AccuStandard M-601C-10X 2000ppm)

-Oxygenated Gas Additive Standard (AccuStandard OGAD-001 2000ppm)

-Priority Pollutant Standards (Acrylonitrile APP-9-008; Acrolein APP-9-007 100ppm)

-Misc. neat standards (Isopropanol – Fisher Sci; MITC – Sigma Aldrich)

Note: Standards in Italic font are referenced as a convenience for analysts reordering

analytical standards. The use of these standards is subject to change based on several

variables including manufacture pricing and various analytical needs. All standards used

by this method shall be referenced in the Volatile Standards Log, including manufacture

information, lot numbers, expiration dates and date of use. These standards shall be

traceable back to the manufacture certificate of analysis. Calibration and independent

source standards should be from different lot numbers and when possible different

manufactures.

VII. Interferences:

A. Special precaution must by taken to isolate samples from all atmosphere Methylene

Chloride contamination. MeCl2 will permeate through PTFE tubing. It is readily

carried on clothing exposed to fumes during common liquid/liquid extractions

creating random background levels.

B. Interfering contamination may occur when a sample containing low concentration of

VOCs is analyzed immediately after samples containing high concentrations of

VOCs. Late eluting analytes tend to “carry over” in greater abundance than early

eluting analytes.
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C. Trace levels of Ketones, Methylene Chloride, Chloroform and other organic solvents

can be present in high purity methanol. Analysis of each new lot of methanol should

be performed prior to use.

D. Impurities from purge and carrier gas can be minimized with gas traps.

E. Trihalomethanes may occur in blanks as traps from the DI water system age.

Replace traps as needed.

VIII. Quality Control:

A. Initial demonstration of capability (DOC) is performed by analysts training under the

supervision of individuals familiar with interpreting GC/MS data. DOCs will be

updated annually thereafter and at any time there is a change in instrument type,

personnel or test method. Continuing DOC studies are stored in analyst personnel

files and filed with the VOC QA/QC data. Electronic copies of current DOCs are

located at the VOC workstation.

1. Four replicate aliquots of mid-calibration reference standards are analyzed by the

procedure outlines in section IX

2. Calculate the average recovery, the standard deviation and the % standard

deviation of the recoveries for each analyte of interest.

3. Results of DOC are compared to laboratory control charts to see if acceptance

criteria are met. In the absence of laboratory acceptance criteria recoveries of 70-

130% can be used as guidance in evaluating the results.

4. If any % standard deviation fails precision limits of 20% or any mean fails

accuracy limits (+/-30% or control limit value, whichever is lower), the source of

the problem must be found and corrected. Analytes that failed must be

reanalyzed and acceptance criteria must be met.

B. Method detection limits (MDL) study is performed annually on each operating

system to determine acceptable detection limits. Current MDL studies are stored with

the VOC QA/QC data. Electronic copies of current MDLs are located at the VOC

workstation.

1. Seven reference standards at 2.5 times the minimum reporting limit are analyzed

according to the procedure outlines in section IX

2. Determine the standard deviation of each compound. Multiply the standard

deviation by 3.14 to determine the MDL value.

3. The calculated MDL value must be 2.5 – 5 times less than the target of the

reference standards or the MDL is reanalyzed.

4. The calculated MDL value must be lower than reporting limits outlined in Tbl.2

C. Method Reporting Limit (quantitation limit) determination

1. Laboratory quantitation limit is established by the concentration of the lowest

standard analyzed during the initial calibration, which exceeds the calculated

MDL value for that analyte.

2. Reporting limits can be increased for analytes with poor purge efficiencies,

analytes frequently present in the laboratory atmosphere, or analytes which tend

to carry over from one run to the next. The increased reporting limits must be in

compliance with regulatory limits, action limits, client permit requirements,

NELAC and the State of Vermont.
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D. 4-Bromofluorobenzene analysis (BFB)- 50ng of BFB is introduced to the MSD at the

beginning of each data set by direct injection or standard purge and every 12 hours of

sample analytical time. The mass intensities are then compared to the tune criteria

listed in Table 1.

1. If all tune criteria is not met, system maintenance and reanalysis of the BFB are

required until system performance is acceptable.

2. A maximum of 50ng of BFB is analyzed at the start of each data set.

3. Continuous monitoring of BFB tune criteria may be observed with each sample

analyzed as BFB is use as a method surrogate.

E. A Line check (calibration) standard is analyzed, following the BFB analysis, and

with every 12-hour analytical batch.

1. Analyte recovery from the line check standard must be within +/- 25% of the

target. System maintenance and reanalysis of standards is required prior to

sample analysis if recovery criteria are not met. All data is qualified if recoveries

are outside acceptance range.

2. System performance check compounds (SPCC) are calculated daily from the line

check standard. Minimum acceptable average RFs should be > 0.100 for

chloromethane, 1,1-dichloroethane and Bromoform. Minimum acceptable

average RF should be > 0.300 for Chlorobenzene and 1,1,1,2-Tetrachloroethane.

See calibration and standardization section for RF calculation

3. Calibration check compounds (CCC) are calculated daily from the line check

standard. The RF % difference for 1,1 Dichloroethene, Chloroform, 1,2-

Dichloropropane, Toluene, Ethylbenzene and Vinylchloride should be < 20% of

the initial calibration.

 % Difference = (RF of Initial Cal-RF of Current Check std) x 100

 RF of Initial Cal

F. An Independent fortified blank is analyzed, following the continuing calibration

analysis, and with every 12-hour analytical batch.

1. Independent fortified standards are tabulated prior to sample analysis. Percent

recoveries should fall within acceptable limits tabulated in the method control

charts. System maintenance and reanalysis of standards is required prior to

sample analysis if recovery criteria are not met. All data is qualified if recoveries

are outside-tabulated acceptance ranges.

2. Control charts are tabulated annually from the percent recoveries of the

independent fortified standards. Upper and lower warning limits are ± 2 standard

deviations of the mean. Upper and lower control limits are ± 3 standard

deviations of the mean. Control limits are posted and stored electronically at the

VOC workstation.

3. Analysts should periodically review recovery trends with graphic printouts of

compound recoveries to avoid instrument bias.

G. A method blank is analyzed, following the Independent fortified blank, and with

every 12-hour analytical batch.

1. Additionally, a blank should be used to check for contamination by carryover

from a high-concentration sample into subsequent samples when practical.

2. Blank results should be less than 5% of the regulatory limit associated with an

analyte or less than 5% of the sample result for the same analyte, whichever is

greater.
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3. If blank criteria are not met, corrective action to locate and reduce the source of

contamination is taken and reanalysis of samples associated with the

contaminated blank is required. Data is qualified if blank criteria are not met.

H. Calibration line quality control

1. The relative standard deviation (RSD) of the initial calibration should be less

than 15% for each analyte. Reanalysis of calibration standards and acceptable

RSD levels must attained prior to sample analysis.

2. As an alternative to calculating mean response and applying the RSD test to the

initial calibration, a linear or second order regression calibration curve is

acceptable. Correlation coefficient (r) acceptance of > 0.990 is required. All

changes to the calibration are documented and control standard requirements

must be met. It should not be the intention of the analyst to use alternate line

calculation equations to supercede good instrument performance and

maintenance practices.

I. Instrument and software performance

1. Good column and GC performance should produce symmetrical peaks.

2. Software should recognize and integrate 99% of compounds analyzed or

instrument maintenance is required.

3. Entire symmetrical peak for each analyte must elute in the retention time window

established in the initial calibration. Instrument maintenance is require if

analytes fall outside retention time windows

J. Matrix spike and matrix spike duplicate (MS/MSD) samples are analyzed every 20

samples.

1. Percent recoveries should fall within acceptable limits tabulated annually in the

method control charts. Data is qualified if recoveries are outside tabulated

acceptance ranges.

2. MS/MSD Precision is measured from the relative percent difference (RPD) of the

concentrations measured for MS/MSD pairs. Acceptance limits are tabulated

annually in the method control charts. The RPD upper control limit,

recommended by NELAC, is defined as 3.27 times the average RPD of minimum

30 data points.

K. Internal Standards (IS) are Chlorobenzene-d5, 1,4-Dichlorobenzene-d4,

Pentafluorobenzene, and 1,4-Difluorobenzene. 10uL of a 25 ppm (target=50ppb) IS

solution is added to each 5ml sample and standard analyzed.

1. IS area counts of the continuing calibration standard, analyzed with each

analytical batch, are compared to the initial calibration IS area counts with an

acceptance range of a factor of 2 (-50 to +100% recovery).

2. IS area counts of the samples and standards analyzed in each analytical batch are

compared to the IS area counts of the continuing calibration of that batch with an

acceptance range of a factor of 2(-50 to +100%).

L. Surrogates are 4-Bromofluorobenzene, Dibromofluoromethane, and Toluene-d8.

10uL of a 25 ppm (target=50ppb) surrogate solution is added to each 5ml sample and

standard analyzed.
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1. Surrogate percent recoveries should fall within acceptable limits tabulated

annually in the method control charts. Data is qualified if recoveries are outside

tabulated acceptance range.

M. If the above mentioned quality control elements are outside laboratory acceptance

limits, corrective action must be taken. Refer to the SOP troubleshooting section,

instrument maintenance logs and manufacturer operating manuals. If corrective

action is not possible due to hold times or limited sample volume, the data must be

qualified in the final report as not acceptable.

IX Procedure

A. Instrument Operating Conditions

1. 5971 GC/MS suggested operating parameters could be modified as instrument

conditions change over time. Purge time of 11 min. and desorb time of 4 ins. are

defined by the method and must remain constant. MS tune parameters used to

acquire the BFB tune at time of initial calibration must be carried forward on all

subsequent standards and sample analysis.

a. Trap: VOCARB 3000 or 4000 Supelco

b. Column: 60m; 0.32mm ID; 1.8um dF Restek (RTX-624)

c. Constant flow inlet B ON 9.0 PSI (He)

d. Purge Flow (N2); 20-25mls/min

e. Source vacuum; 5.3 x 10-5 Torr. (Approximate)

f. Purge time 11 min; desorb time 4 min; bake time 12 min

g. Acquisition parameters save in method aq-8260.m are as follows:

-Sample Inlet: B 200C – Detector B: 280C

-Pressure 7.00 – Velocity 29.0ml/min

-Tune file “BFB.U”-

-Mass Scan 42-260AMU

-Split Ratio 10:1

-Initial Set points – valves 3and 4 are on, all others valves and relays off

-Initial Temp: 45C; ms on at 1.5 min

-Gradient is 8.0 c/min to final temp of 210 – hold final time 1.0min 

B. 50ng BFB direct injection: performed at the beginning of each analytical set and

every 12 hours of analysis. BFB introduction to the MS detector by purge and trap is

acceptable following the sequence procedure outlined in section C of the procedure

section.

1. Activate the MS Top Software

2. Select “Sequent-Edit sample log table”

3. Enter data file: date/year/cycle #

4. Enter current acquisition method

5. Enter sample information (example: “50ng BFB” )and press “ok”

6. Select “sequence-run”, enter “full method”

7. Data file directory (example“c:\hpchem\1\data\feb03”), press “ok”

8. When temperatures on GC oven equilibrate a “start” message will appear on the

acquisition computer. Inject 2μL of 25ppm 8260 IS/SURR mix.

9. Press start on GC oven
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10. Confirm BFB spectral scan and ion abundance criteria are calculated, plotted and

printed. Reanalysis of BFB and instrument maintenance must be performed if

any abundance criteria are not met.

C. Sequence Set Up

1. Enter and save sample information in GC/MS daily run log stored at the VOS

workstation. Include date, tube number, file name, reference number, reference

number suffix, sample preservation, client, project, site dilutions and

miscellaneous notes. For soil analysis includes injection volume, sample mass

and extraction volume.

2. Load samples at appropriate dilutions on MPM 16 and DPM 16

3. Press “SPL” on sample concentrator and enter range of tubes to be analyzed.

Press “start”.

4. When sample concentrator indicates “DSB-RDY” activate ms top software

5. Program sequence-enter data file names to be analyzed, acquisition method is

“AQ-8260” on the 5971 workstation.

6. At sample info section enter laboratory reference number, dilution and

miscellaneous sample information then press “ok”

7. Select “sequence-run”, enter “full method”

8. Data is saved to the server at “s:\appropriate subdirectory”, press “ok”, sequence

will start automatically when temperatures equilibrate.

D. Aqueous sample preparation/introduction.

1. Samples and standard solutions are allowed to warm to room temperature before

analysis. Insure sample containers have no headspace.

2. Calibration verification and instrument performance criteria are met prior to

sample analysis.

3. Pour sample to the top of the barrel of a 5ml-gas tight lure-lock syringe. Attach

the plunger and adjust the sample volume to 5mls. Add 10uL of 25ppm IS/Surr

mix to each 5mls of sample, QC, Line Check Blank and spike prior to loading

purge and trap.

4. If there is only one VOA vial for the sample, transfer the remaining sample to a

20ml VOA vial, sealed with zero headspace and stored until the analyst has

determined the first sample has been analyzed properly.

5. Attach the 5ml lure-lock syringe to the syringe valve on the purge device. Open

the valves and inject the sample to the purging chamber. Close the valve and

follow the procedure outlined in section IX.C. to purge the sample for 11mins.

6. Sample desorption to the GC is for 4min. at 180 degree C, followed by the trap

bake, which should not exceed 210 degrees C.

7. Dilutions are performed when compound concentration exceeds analytical

calibration range using volumetric flasks or syringes (class A).

8. Process the sample file through the current calibration method in the MS

ChemStation software after all quality control criteria have been met. Check the

integration of each peak to be quantitated upon.

E. Soil and Solid waste sample preparation/introduction.

1. Appendix A outlines the collection of soil samples in the field using methanol as

the sample preservation and extraction solvent.

2. Soil/Sludge in house extraction
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a. Weigh approximately 10g of soil on an analytical balance into a 40ml vial.

Steps to insure a homogeneous sample from the container should be taken.

Whenever practical, mix the contents of the sample container by shaking

without opening the vial. When shaking is not practical, quickly mix the

sample container contents with a narrow metal spatula prior to removing

sample fraction to be analyzed.

b. Add 5ml purge and trap grade methanol.

c. Shake samples gently for 2min and allow samples to settle in the dark,

refrigerated for 24 hours.

d. Analyze a fraction of the methanol extract in 5mls DI water following the

procedure outlined in section IX. D.

F. Tedlar bag air sample preparation/introduction.

1. Tedlar bags are analyzed at first available opportunity.

a. With gas tight syringe, extract no more than 100cc sample

b. When auto-sampler cycles to purge on a clean tube, open sample valve and

introduce sample at approximately 20mls /min.

c. Process results and associated QA/QC via external standard method of most

recent calibration

X. Calibration and Standardization (make/use/storage):

A. Prepare a 10 ppm Working Standard in methanol containing all 8260 analytes:

-50μL 200 ppm NSIQ2479 Custom VOC mix (or equivalent standard)

-5μL 2000 ppm Accustandard M-601C-10x (or equivalent standard)

-945μL Purge and Trap Methanol

-Store at < 0C in organic standard freezer

B. Prepare a 25 ppm Internal Standard/Surrogate Solution:

-500μL 200 ppm M-8260-IS IS Mix (or equivalent standard)

-500μL 200 ppm M-8260-SS Surr Mix (or equivalent standard)

-3000μL Purge and Trap MeOH.

-Store at < 0C in organic standard freezer

C. Analyze a series of calibration standards. The following concentrations historically

bracket a wide range of contamination observed in environmental samples with good

instrument performance. However, the analyst has the discretion to change initial

calibration point concentrations based on current instrument performance, reporting limit

requirements or other analytical needs. Analyze a 1.0ppb, 2.0ppb, 5.0ppb, 10ppb, 20ppb,

50ppb, 100ppb, 150ppb and 200ppb standard following the steps outlined in section

IX.C. The initial calibration must have a minimum of 5 points with an RSD of < 15%,

the low calibration standard should be at or below the laboratory reporting limit and the

range of standards should bracket all reported analytes. Sample dilution is required when

reported analytes exceed the analytical calibration range.

1. Good GC and column performance will produce symmetrical peaks with

minimal tailing.

2. The GC/MS software should recognize a GC peak in the appropriate

retention time window. If fewer than 99% of the compounds are recognized,

system maintenance is required.
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3. The Chemstation software will calculate the response factor for each analyte,

surrogate and isomer pair as follows.

RF = Ax Qis

 Ais Qx

Ax = Quantitation Ion Abundance of the Analyte

Ais = Quantitation Ion Abundance of the Internal Standard

Qx = Quantity of Analyte Purged

Qis = Quantity of Internal Standard

RF = Response factor

4. The mean RF from the analysis is calculated.

5. The standard deviation and relative standard deviation (RSD) from each

mean are calculated: RSD = 100*(SD/M). If the RSD exceeds 15%

reanalyze additional aliquots of calibration solution to obtain an acceptable

RSD. Perform instrument maintenance as needed if reanalysis of standards

does not provide an acceptable RSD.

D. Evaluation of Retention Times

1. The relative retention time of each target analyte should agree within

0.06 RRT units

E. Peak Integration

1. Peak integration should be consistent for all analytes. Refer to

laboratory integration SOP for detailed protocol.

2. Single peaks, the integration should begin at the start of the upward

slope of the peak and end at the bottom of the downward slope.

3. If there is a raised baseline, the analyst should be careful to not

integrate the raised baseline as part of the area of the target peak.

4. In the instance of co-elution isomer pairs, the baseline should start at

the beginning of the upward slope of the peak and remain level until

the slope of the valley of the two peaks is at its lowest level. If the

target peak is the second of a co-eluting pair, the baseline should be

drawn backwards to the same level. The valley of the co-eluting pair

should be less than 25% of the sum of the two peak heights or the pair

is reported as a total.

XI. Data Reduction and Interpretation:

A. Chemstation software calculates analyte and surrogate concentrations in water

samples as follows:

Cx = [(Ax) (Qis) 1000 ÷ (Ais) (RF) (V)]

V = Volume water in mls

RF = Response factor from initial calibration

Cx = Concentration in μg/L

Ax = Integrated Abundance of the quantitation ion of the Analyte

Ais = Integrated Abundance of the quantitation ion of the Internal Standard

Qis = Quantity of Internal Standard added to the sample
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B. Analyte concentration in soil samples:

Cs = Cx x 5 x VE+((M*(1-P))*1000)

 M x P VI

Where:

Cs = analyte concentration as μg/kg, dry

Cx = analyte concentration from instrument expressed as ng/ml

M = sample mass in grams

P = percent solid expressed as a decimal extraction

VE = extraction volume in μL

VI = Injection volume in μL

C. Qualitative Analysis-Compound identification is determined by satisfying two

criteria.

1. Elution of sample compound at the same GC relative retention time as the

standard analyte ± 0.06 RRT units.

2. Comparison of sample and standard mass spectrum.

a. All ions greater than 10% of the primary ion in the standard must be

present in the sample spectrum.

b. Relative intensities of secondary ions must agree within + or - 30%.

c. Identification of compounds not in the calibrated standard is

determined by comparing to library mass spectra

D. Percent Recovery of compounds in the continuing calibration standard, matrix

spike, matrix spike duplicate and independent laboratory fortified blank are

calculated as follows:

% Recovery = Measured Value * 100

 Target Value

E. The relative percent deviation (RPD) between the recovery (REC) from the

matrix spike (MS) and matrix spike duplicate (MSD) is calculated as follows:

RPD = ABS(MSREC-MSDREC) *100

((MSREC+MSDREC)/2)
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XII. Data Recording:

A. Sample data is electronically imported to the LIMS from the VOC/GCMS computer

after it has been reduced to a usable format. Current data reduction MACRO is

LIMSMAC.XLM stored at c:\EXCELFILES\REPORTS. on the VOC/GCMS

computer.

B. Record any Instrument Maintenance in the maintenance log for the PT/GC/MS

C. All standards opened and made are reported in the VOC standards log

D. Individual calibration standard and associated QC dilutions are recorded in the daily

run log.

E. Sample pH is measured using pH strips and recorded in the daily run log.

F. Analysts initial and date each sample chromatogram. The analyst will initial each

data sheet associated with that chromatogram. Sample chromatograms and data

sheets are filed sequentially with other organic chromatograms and stored for a

minimum of 3 years.

G. All QC, line check, blank data, MS, MSD and BFB Tune Criteria is printed and

stored sequentially by date with the VOC/GCMS QC Data and is stored for a

minimum of 5 years.

H. Individual QC data is entered to 8260 QC Spread Sheets to determine if acceptable

QA/QC Criteria has been attained prior to reporting each analytical batch. Data is

stored on VOC/GCMS computer (c:\EXCELQC\QC\CONTROL) and is tabulated

and printed annually.

I. Sample data is entered to LIMS with Analyst ID, Date, Units and analyte

concentration.

J. A hard copy of all quality control data is stored with the PT/GCMS data

K. Computer hard drive is backed up quarterly to a CD. This includes run log, QC

charts, and sample data, line standards, methods and QC standards. Sample data

acquired to the server is backed up daily.

L. Method hard copies are printed and stored with the PT/GCMS QC hard copies.

N. QC summary data packages are prepared for each analytical batch daily and

incorporate the following criteria.

1. Instrument run log-Includes date, time, analyst initials, auto-sampler tube #,

sample data file names, Reference #, container ID, Client, project, site ID,

dilutions, sample preservation verification, standard ID, Standard date reference

to standards log, standard dilution/prep., and Misc. notes

2. BFB tune spectra results.

3. GC/MS QA-QC Check Report – Documents Sample/Standard IS area compared

to the continuing calibration standard. Documents sample/standard analysis

within 12 hour BFB window. Performed as follows:

a. Load continuing calibration standard in software. Select pull down window

“ConCal” select “Save continuing ISDT response”

b. Select pulldown “ConCal”, Select “QA check report”

c. Name Data file unique to data set

d. Enter BFB Tune File for data set

e. Highlight samples/standards analyzed with data set and select for processing.

Press “process” key and print the tabulated summary

f. IS areas outside acceptance range (-50% to +100%) are flagged with “*”.

Files analyzed outside the 12 hour BFB are flagged “t”.

4. Continuing calibration (CC) raw data results with “Evaluate Continuing

Calibration Report” are printed. This report shows the comparison of the average

of the RRF from the initial calibration versus the RRF from the continuing
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calibration level. To print this report, load the CC file in the software, select pull

down “ConCal”, select “Evaluate data file as continuing cal to printer”.

Information is summarized as follows:

a. AvgRRF displays the average RF of all calibration levels of the initial

calibration.

b. CCRRF is the calculated RF for the CC data file. SPCC compounds are

verified here. (see section VIII. E. 2. For acceptance limits.

c. %Dev. is the absolute value of the percentage difference between the

AvgRRF and the CCRRF - %DEV=(AvgRRF-CCRRF)/AvgRRF*100

CCC compounds are verified here. Target compound recoveries are verified

here (+/- 25%).

d. Area % - The integrated area of the quantitation ion of the CC file is

compared with the same ion in the initial calibration at the same

concentration. CC IS area vs. the initial calibration is verified here (-50 to

+200%) - %AREA = (Ccarea/INITarea)*100

5. Laboratory fortified Ind. Standard, Blank raw data is printed. Percent recoveries

are compared to laboratory control charts for acceptance limits.

6. Method blank raw data is printed and system contamination is evaluated as

outlined in section VIII.G.

7. Matrix Spike and Matrix Spike Duplicate (MS/D) raw data is printed with a

MS/D report which summarizes analysis reproducibility and aids in the

determination of matrix interference. Generate report from software “tools” pull

down, select “MS/D recovery report” and follow software prompts. Report

summary is as follows:

a. Sample Conc – Indicates the concentration of analyte in the unknown

sample.

b. Spike Added – Concentration of compound added to unknown sample

c. Spike Res - The concentration of the MS compound in the MS sample

d. Dup Res - The concentration of the MS compound in the MS/D sample

e. Spike %Rec - % recovery of the MS compound in the MS Sample

Percent Recovery = (MS Conc.-Unknown Conc)*100/Spike Added

f. Dup %Rec - % recovery of the MS compound in the MS/D Sample

g. RPD – Relative % Deviation between MS/MSD recoveries

RPD=ABS(MSREC-MSDREC)*100/((MSREC+MSDREC)/2)

h. RPD QC Limits – 30% until laboratory control limits are established

i. % Rec QC Limits – entered from established laboratory control charts
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XIII. Instrument Maintenance/Trouble Shooting: Instrument maintenance is documented in the

maintenance section of the current instrument run log.

A. Injection port septa is replaced every 20 injections or as needed.

B. Poor response or failed tune criteria may be indicative of a dirty MS source. Follow

procedures in the HP MSD 5971 operator manual to clean the source.

C. No sample response or emission current indicates a worn of broken filament. Follow

procedures in the HP MSD 5971 operators manual to replace filaments or manually

switch to alternate filament on back of MSD.

D. A high baseline or poor instrument response may indicate a leak in the system.

Leaks will oxidize the column and shorten column life. Perform an air and water

check following any instrumental maintenance.

E. Varying surrogate and analyte response and excessive analyte carry over are common

with deteriorating traps. Replace the Vocarb 4000 in the Tekmar LCS-2 according to

the operating manual.

F. Varying response may indicate a contaminated injection port. Replace the injector

liner or salanize an old injection liner in accordance to HP GC oven 5890 operators

manual.

XIV. Method Modifications:

Purge flows most effective for O/I auto-sampler and trap are 20-25mls/min. Method

8260 recommends 25 to 40mls/min.

MS/MSD RPD upper control limit, recommended by NELAC, is defined as 3.27 times

the average RPD of minimum 30 data points. This reference was not found in literature

review as of 3/20/07.

The GC/MS operating systems are programmed to scan mass ranges between 42-

260AMU as opposed to 35-260AMU recommend by method 8260. The reduced range

effectively reduces baseline noise allowing for easier chromatogram interpretation. All

primary characteristic ions and qualifying ions for each compound are present at this

mass range. In instance where a broader mass range is required the laboratory will adjust

its scan range accordingly.
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XV. Bibliography/References:

EnviroQuant Chemstation, G1701BA Version b.01-00 © Hewlett-Packard 1989-1998

HP 5971A Mass Selective Detector Hardware Manual, edition 1 © Hewlett-Packard Feb.

1990, Publication # 05971-90011

HP 5890A Series II Programmable Cool on Column Inlet, eighth edition © HewlettPackard, Sept. 1995 Publication # 05890-90300

HP 5890A Series II Reference Manual, fifth edition © Hewlett-Packard, Sept.

1991Publication # 05890-90270

Method 8000b Determinative Chromatographic Separations, EPA SW-846 NTIS ,CD

ROM Version 2, Dec. 1997

Method 8260b– Volatile Organic Compounds by Gad Chromatography/Mass

Spectrometry (GC/MS), Revision 2, US EPA December 1996

Method 5035-Closed System Purge and Trap and Extraction for Volatile Organics in Soil

and Waste Samples, CD-ROM Revision 0, US EPA December 1996

Method 5030B-Purge and Trap for Aqueous Samples, CD-ROM Revision 2, US EPA

December 1996

XVI. Revision history

Revision #7 January 26, 2004

-Added Bibliography/Reference section; Added Revision History section; Added

sign off sheet.

-Edited typos; formatted tab sets and spacing; updated table of contents

-Added laboratory safety requirements

-Added NH gas additive compounds; Added priority pollutant compounds; Added

OMYA compounds.

-Added Tedlar bag requirements.

Revision #8 – April 7, 2005

-Edit for content and grammar

Revision #9 Began September 2006

 -Edited quality control to reflect discovered software capabilities and

 Documentation

Revision #9 Finished March 20,2007

 -Reviewed content, clarified software calculations, edits for grammar

 -Updated method modification section after literature review.

 -Adjusted table of contents for new page fit.

Revision #10 September 26, 2007

-Section VIII.H.2 Defined acceptance criteria for calibration models.

TABLE 1
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BFB (4-BROMOFLUOROBENZENE) MASS INTENSITY CRITERIA

 

 

m/z Required Intensity (relative abundance)

 

50 15 to 40 % of m/z 95

75 30 to 60% of m/z 95

95 Base peak, 100% relative abundance

96 5 to 9% of m/z 95

173 Less than 2% of m/z 174

174 Greater than 50% of m/z 95

175 5 to 9% of m/z 174

176 Greater than 95% but less than 101% of m/z 174

177 5 to 9% of m/z 176
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Appendix A

VOLATILE ORGANIC COMPOUND

SAMPLING WITH METHANOL PRESERVATION

Endyne is recommending to its clients that they modify their sampling procedure for Volatile Organic

Compounds (VOCs) in soil/solid matrices; SW-846 Method 5035.

The recommended protocol calls for the sampler to notify the laboratory approximately 1 week before

sampling date. Once notified the laboratory will prepare 40-ml vials for each site.

Preparation will involve adding exactly 10.0 ml of a high purity grade methanol (MeOH) to a 40-ml

vial and determining the exact weight, which will be recorded on the vial along with the date

prepared. A pen mark is made on the label to note the meniscus of the solvent at the time of

preparation.

The sampler will then add approximately 20.0 g of soil in the field to each vial. This is roughly

equivalent to 2 rounded tablespoons or 1.5 inches in the vial of a loosely packed soil or one heaping

tablespoon of a denser/damper soil. Once the soil has settled, there should be approximately one

centimeter of MeOH as a supernatant. The sampler should mark on the bottle the level of the

meniscus after sample addition, this will allow the laboratory to confirm that there was no sample loss

at the time of analysis.

The sampler will also include a 40.0-ml vial of soil sampled the standard way. This vial will be

used to determine percent solids as well as a back up in case of sample loss with the MeOH vial.

Once returned to the lab, the soil is ready for analysis. The weight of the sample will be determined

by the difference of the before and after weights.

Advantages:

-More accurate and generally higher analyte recoveries

Disadvantages:

-Poor sampling/handling procedure can result in greater erroneous results.

Hints:

- It is very important to not splash any of the MeOH out of the vial when collecting the

sample.

- Do not add any additional labels to the vial, as it will affect the sample weight.

- Keep vials refrigerated/even before sampling.

- Do not leave caps open for very long since MeOH evaporates quite quickly.

- After sampling, be sure to wipe the threads of the vial & cap with a clean tissue. Even

the slightest amount of dirt can prevent a good seal.

- Unused sample vials are stable for several weeks when refrigerated. Always confirm

that no methanol has evaporated from the vial by checking the meniscus line.
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Table 2

TABLE 2-SW 8260B Water Reporting Limits

Limit Limit

Parameter ug/L Parameter ug/L

Acetone 10.0 1,1-Dichloropropene 1.0

Benzene 1.0 cis-1,3-Dichloropropene 1.0

Bromobenzene 1.0 trans-1,3-Dichloropropene 1.0

Bromochloromethane 2.0 Diethyl Ether 10.0

Bromodichloromethane 1.0 Ethylbenzene 1.0

Bromoform 1.0 Hexachlorobutadiene 5.0

Bromomethane 5.0 2-Hexanone 10.0

2-Butanone 10.0 Isopropylbenzene 1.0

n-Butylbenzene 1.0 p-Isopropyltoluene 1.0

sec-Butylbenzene 1.0 Methylene Chloride 10.0

tert-Butylbenzene 1.0 4-Methyl-2-Pentanone 10.0

Carbon Disulfide 10.0 MTBE 2.0

Carbon Tetrachloride 1.0 Naphthalene 2.0

Chlorobenzene 1.0 n-Propylbenzene 1.0

Chloroethane 5.0 Styrene 1.0

2-Chloroethyl Vinyl Ether 20.0 1,1,1,2-Tetrachloroethane 2.0

Chloroform 1.0 1,1,2,2-Tetrachloroethane 2.0

Chloromethane 3.0 Tetrachloroethene 1.0

2-Chlorotoluene 1.0 Tetrahydrofuran 10.0

4-Chlorotoluene 1.0 Toluene 1.0

Dibromochloromethane 1.0 1,2,3-Trichlorobenzene 2.0

1,2-Dibromo-3-Chloropropane 2.0 1,2,4-Trichlorobenzene 2.0

1,2-Dibromoethane 2.0 1,1,1-Trichloroethane 1.0

Dibromomethane 2.0 1,1,2-Trichloroethane 1.0

1,2-Dichlorobenzene 1.0 Trichloroethene 1.0

1,3-Dichlorobenzene 1.0 Trichlorofluoromethane 2.0

1,4-Dichlorobenzene 1.0 1,2,3-Trichloropropane 2.0

Dichlorodifluoromethane 5.0 1,2,4-Trimethylbenzene 1.0

1,1-Dichloroethane 1.0 1,3,5-Trimethylbenzene 1.0

1,2-Dichloroethane 1.0 Vinyl Chloride 2.0

1,1-Dichloroethene 1.0 Xylenes, Total 2.0

cis-1,2-Dichloroethene 1.0 Isopropanol 50.0

trans-1,2-Dichloroethene 1.0 MITC 5.0

1,2-Dichloropropane 1.0 ETBE 2.0

1,3-Dichloropropane 1.0 TAME 2.0

2,2-Dichloropropane 1.0 t-Butanol 10.0

Isopropyl ether 2.0 Acrylonitrile 20.0

Acrolein 20.0

Note: Soil reporting limits are base on the sample percent solid, extraction mass, and extraction solvent

volume and therefore vary with each individual sample. See section XI for soil calculation conversion to

ug/kg, dry.

Note: Current MDL study can be referenced at “Wayne” C:/EXCELQC/QC/MDL. Hard copied and raw data are filed

with VOC QC data.
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I acknowledge that I have read this Standard Operating Procedure and agree

 to adhere to the Safety and Quality Control policies outlined within.

Name Date

 
Aqueous Solid

Method Method Calibration Lab. Fortified 

Detection Reporting Detection Reporting Verifivation Blank (QC) 

Compound Limit ug/L Limit ug/L Limit ug/Kg Limit ug/Kg % Recovery % Recovery Dichlorodifluoromethane 0.37 5.0 2.2 50.0 75 - 125 70 - 130 Chloromethane 0.70 3.0 9.5 30.0 75 - 125 70 - 130 Vinyl chloride 0.75 2.0 6.4 20.0 80 - 120 70 - 130 Bromomethane 0.85 5.0 10.2 50.0 75 - 125 70 - 130 Chloroethane 0.74 5.0 21.2 50.0 75 - 125 70 - 130 Trichlorofluoromethane 0.36 2.0 11.6 20.0 75 - 125 70 - 130 Diethyl ether 1.18 5.0 17.4 50.0 75 - 125 70 - 130 1,1-Dichloroethene 0.65 1.0 6.2 10.0 80 - 120 70 - 130 Acetone 2.50 10.0 52.0 100.0 75 - 125 70 - 130 Carbon disulfide 0.69 5.0 9.2 50.0 75 - 125 70 - 130 Methylene chloride 0.53 5.0 10.0 50.0 75 - 125 70 - 130 t-Butanol 6.20 20.0 125 200 75 - 125 70 - 130 MTBE 1.52 2.0 14.5 20.0 75 - 125 70 - 130 trans-1,2-Dichloroethene 0.50 1.0 9.2 10.0 75 - 125 70 - 130 Diisopropyl ether 0.68 2.0 6.1 20.0 75 - 125 70 - 130 1,1-Dichloroethane 0.50 1.0 6.8 10.0 75 - 125 70 - 130 ETBE 0.63 2.0 7.2 20.0 75 - 125 70 - 130 2-Butanone 1.07 10.0 43.6 100.0 75 - 125 70 - 130 2,2-Dichloropropane 0.59 2.0 5.8 20.0 75 - 125 70 - 130 cis-1,2-Dichloroethene 0.49 1.0 6.5 10.0 75 - 125 70 - 130 Bromochloromethane 0.69 2.0 3.2 20.0 75 - 125 70 - 130 

Control Limits 2010 EPA 8260B/624 - Aqueous & Soil Samples

Endyne, Inc.

160 James Brown Drive

Williston, Vermont

Page 1 of 4
Aqueous Solid

Method Method Calibration Lab. Fortified 

Detection Reporting Detection Reporting Verifivation Blank (QC) 

Compound Limit ug/L Limit ug/L Limit ug/Kg Limit ug/Kg % Recovery % Recovery 

Control Limits 2010 EPA 8260B/624 - Aqueous & Soil Samples

Endyne, Inc.

160 James Brown Drive

Williston, Vermont

Chloroform 0.40 1.0 4.8 10.0 80 - 120 70 - 130 Tetrahydrofuran 1.63 10.0 69.1 100.0 75 - 125 70 - 130 1,1,1-Trichloroethane 0.34 1.0 5.7 10.0 75 - 125 70 - 130 Carbon tetrachloride 0.36 1.0 7.1 10.0 75 - 125 70 - 130 1,1-Dichloropropene 0.56 1.0 6.8 10.0 75 - 125 70 - 130 Benzene 0.53 1.0 7.4 10.0 75 - 125 70 - 130 TAME 0.66 2.0 4.9 20.0 75 - 125 70 - 130 1,2-Dichloroethane 0.64 1.0 5.9 10.0 75 - 125 70 - 130 Trichloroethene 0.41 1.0 4.9 10.0 75 - 125 70 - 130 1,2-Dichloropropane 0.37 2.0 7.0 20.0 80 - 120 70 - 130 Dibromomethane 0.50 2.0 10.0 20.0 75 - 125 70 - 130 Bromodichloromethane 0.17 0.50 3.5 5.0 75 - 125 70 - 130 cis-1,3-Dichloropropene 0.33 1.0 5.8 10.0 75 - 125 70 - 130 MIBK 0.98 10.0 9.5 100.0 75 - 125 70 - 130 Toluene 0.35 1.0 5.7 10.0 80 - 120 70 - 130 trans-1,3-Dichloropropene 0.50 2.0 4.9 20.0 75 - 125 70 - 130 1,1,2-Trichloroethane 0.32 1.0 6.2 10.0 75 - 125 70 - 130 Tetrachloroethene 0.37 1.0 2.8 10.0 75 - 125 70 - 130 1.3-Dichloropropane 0.42 1.0 5.5 10.0 75 - 125 70 - 130 2-Hexanone 0.84 10.0 13.1 100.0 75 - 125 70 - 130 Dibromochloromethane 0.49 2.0 5.6 20.0 75 - 125 70 - 130 

Page 2 of 4
Aqueous Solid

Method Method Calibration Lab. Fortified 

Detection Reporting Detection Reporting Verifivation Blank (QC) 

Compound Limit ug/L Limit ug/L Limit ug/Kg Limit ug/Kg % Recovery % Recovery 

Control Limits 2010 EPA 8260B/624 - Aqueous & Soil Samples

Endyne, Inc.

160 James Brown Drive

Williston, Vermont

1,2-Dibromoethane 0.48 1.0 4.6 10.0 75 - 125 70 - 130 Chlorobenzene 0.29 1.0 6.4 10.0 75 - 125 70 - 130 Ethylbenzene 0.36 1.0 4.5 10.0 80 - 120 70 - 130 1,1,1,2-Tetrachloroethane 0.24 2.0 7.9 20.0 75 - 125 70 - 130 m & p - Xylene 0.76 2.0 11.6 20.0 75 - 125 70 - 130 o-Xylene 0.35 2.0 4.6 20.0 75 - 125 70 - 130 Styrene 0.33 1.0 6.0 10.0 75 - 125 70 - 130 Bromoform 0.56 2.0 7.1 20.0 75 - 125 70 - 130 Isopropylbenzene 0.45 1.0 7.0 10.0 75 - 125 70 - 130 1,1,2,2-Tetrachloroethane 0.88 2.0 9.1 20.0 75 - 125 70 - 130 Bromobenzene 0.32 1.0 5.1 10.0 75 - 125 70 - 130 n-Propylbenzene 0.37 1.0 4.8 10.0 75 - 125 70 - 130 1,2,3-Trichloropropane 0.54 2.0 6.2 20.0 75 - 125 70 - 130 2-Chlorotoluene 0.28 1.0 5.7 10.0 75 - 125 70 - 130 1,3,5-Trimethylbenzene 0.40 1.0 6.6 10.0 75 - 125 70 - 130 4-Chlorotoluene 0.21 1.0 3.9 10.0 75 - 125 70 - 130 tert-Butylbenzene 0.43 1.0 4.9 10.0 75 - 125 70 - 130 1,2,4-Trimethylbenzene 0.46 1.0 6.1 10.0 75 - 125 70 - 130 sec-Butylbenzene 0.45 1.0 5.0 10.0 75 - 125 70 - 130 4-Isopropyltoluene 0.46 1.0 5.7 10.0 75 - 125 70 - 130 1,3-Dichlorobenzene 0.49 1.0 5.8 10.0 75 - 125 70 - 130 

Page 3 of 4
Aqueous Solid

Method Method Calibration Lab. Fortified 

Detection Reporting Detection Reporting Verifivation Blank (QC) 

Compound Limit ug/L Limit ug/L Limit ug/Kg Limit ug/Kg % Recovery % Recovery 

Control Limits 2010 EPA 8260B/624 - Aqueous & Soil Samples

Endyne, Inc.

160 James Brown Drive

Williston, Vermont

1,4-Dichlorobenzene 0.38 1.0 4.7 10.0 75 - 125 70 - 130 n-Butylbenzene 0.29 1.0 4.7 10.0 75 - 125 70 - 130 1,2-Dichlorobenzene 0.28 1.0 5.1 10.0 75 - 125 70 - 130 1,2-Dibromo-3-chloropropa 0.98 2.0 7.7 20.0 75 - 125 70 - 130 

1,2,4-Trichlorobenzene 0.28 2.0 5.5 20.0 75 - 125 70 - 130 Hexachlorobutadiene 0.42 0.50 5.3 5.0 75 - 125 70 - 130 Naphthalene 2.14 2.0 9.0 20.0 75 - 125 70 - 130 1,2,3-Trichlorobenzene 0.32 2.0 7.4 20.0 75 - 125 70 - 130 

1/22/09 2/17/09

Surrogate

Dibromofluoromethane S1 70 - 130 70 - 130 Toluene-d8 S2 70 - 130 70 - 130 4-Bromofluorobenzene S3 70 - 130 70 - 130 

Specific instrument control charts may supersede value only when control range is less than default method 

Page 4 of 4
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Endyne, Inc.

160 James Brown Dr.

Williston, VT 05495

Phone: (802) 879-4333

Fax: (802) 879-7103

SEMIVOLATILE ORGANIC COMPOUNDS

METHOD EPA 8270C

Standard Operating Procedure

REVISED: September 26, 2007

Revision: 9

Technical Director: Date : 

Harry B. Locker Ph.D.

QA Officer: Date : 

Mark L. Fausel
Endyne, Inc. SVOC Method SW 8270C SOP

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TABLE OF CONTENTS

Section Pages

1. Overview 3-4

2. Summary of Method 4-5

3. Safety 5

4. Waste Disposal 5-6

5. Sample Collection, Preservation and Storage 6

6. Equipment and Supplies 6-7

7. Reagents and Standards 7-8

8. Interferences 8-9

9. Quality Control 9-14

10. Procedure 14-30

11. Data Reduction 30-31

12. Data Recording 31

13. Data Archiving 31-32

14. Instrument Maintenance 32-33

15. Trouble Shooting 34

16. Method Modifications 34

17. Bibliography/Reference 35

18. Revision History 35

Table 1 – DFTPP Key Ions/Ion Abundance Criteria 36

Table 2 – Calibration Check Compounds 36

Table 3 – Reporting Limits 37

Table 4 – Characteristic Ions 38-39

Sign Off Sheet 40
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1. Overview

1.1. Method 8270 is used to determine the concentration of semivolatile organic

compounds in extracts prepared from soil, water and solid waste matrices. The

following compounds are determined by this method:

Base/Neutral Extractable:

Anthracene Azobenzene Benzidine

Benzo(a)anthracene Benzo(b&k)fluoranthene Benzo(a)pyrene

Benzo(g,h,i)perylene Bis(2-chloroethyl)ether Bis(2-chloroethoxy)methane

Bis(2-ethylhexyl)phthalate Bis(2-chloroisopropyl)ether 4-Bromophenyl phenyl ether

Butyl benzyl phthalate Carbazole 4-Chloroaniline

1-Chloronaphthalene 2-Chloronaphthalene 4-Chlorophenyl phenyl ether

Chrysene Dibenzofuran Dibenzo(a,h)anthracene

Di-n-butylphthalate 1,3-Dichlorobenzene 1,2-Dichlorobenzene

1,4-Dichlorobenzene 3,3’-Dichlorobenzidine Diethyl phthalate

Dimethyl phthalate 2,4-Dinitrotoluene 2,6-Dinitrotoluene

Di-n-octylphthalate Fluoranthene Fluorene

Hexachlorobenzene Hexachlorobutadiene Hexachlorocyclopentadiene

Hexachloroethane Indeno(1,2,3-cd)pyrene Isophorone

1-Methylnapththalene 2-Methylnaphthalene Naphthalene

1-Naphthylamine 2-Naphthylamine 2-Nitroaniline

3-Nitroaniline 4-Nitroaniline Nitrobenzene

N-Nitrosodipheylamine N-Nitrosodimethylamine N-Nitrosodi-n-propylamine

N-Nitrosopiperidine Phenanthrene Pyrene

Pyridine 1,2,4-Trichlorobenzene

Acid Extractables:

Benzyl Alcohol 4-Chloro-3-methylphenol 2-Chlorophenol

2,4-Dichlorophenol 2,6-Dichlorophenol 2,4-Dimethylphenol

4,6-Dinitro-2-methylphenol 2,4-Dinitrophenol 2-Methylphenol

3&4-Methylphenol 2-Nitrophenol 4-Nitrophenol

Pentachlorophenol Phenol 2,4,5-Trichlorophenol

2,4,6-Trichlorophenol

1.2. Sample preparation techniques:

1.2.1. Method 3510 is a separatory funnel technique used to extract aqueous

samples.

1.2.2. Method 3550 is an ultrasonic technique used for soil samples.

1.3. Method 8270 can be used to quantify most neutral, acidic, and basic organic

compounds that are soluble in methylene chloride and capable of being eluted

without derivatization as sharp peaks from a gas chromatographic fused-silica

capillary column coated with a slightly polar silicone. Such compounds include

polynuclear aromatic hydrocarbons, chlorinated hydrocarbons and pesticides,

phthalate ester, organophosphate ester, nitrosamines, aromatic nitro compounds,

and phenols, including nitrophenols.
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1.4. The following compounds may require special treatment when being determined

by this method:

1.4.1. Benzidine can be subject to oxidative losses during solvent concentration.

Also, chromatography is poor.

1.4.2. Under the alkaline conditions of the extraction step, alpha-BHC, gammaBHC, Endosulfan I and II, and Endrin are subject to decomposition in the

inlet of the gas chromatograph, chemical reaction in acetone solution, and

photochemical decomposition.

1.4.3. Hexachlorocyclopentadiene is subject to thermal decomposition in the

inlet of the chromatograph, chemical reaction in acetone solution and

photochemical decomposition.

1.4.4. N-Nitrosodimethylamine is difficult to separate from the solvent under the

chromatographic conditions described. N-nitrosodiphenylamine

decomposes in the gas chromatographic inlet and cannot be separated from

diphenylamine.

1.4.5. Pentachlorophenol, 2,4-Dinitrophenol, 4-Nitrophenol, 4,6-Dinitro-2-

methylphenol, 4-Chloro-3-methylphenol, Benzoic acid, 2-Nitroaniline, 4-

Chloroaniline, and Benzyl alcohol are subject to erratic chromatographic

behavior, especially if the GC system is contaminated with high boiling

material.

1.4.6. Pyridine may perform poorly at higher injection port temperatures.

Consideration of the performance of other analytes is necessary when

lowering the injection port temperature.

1.5. The method detection limit (MDL) of Method 8270 ranges from 1.0 to 10ug/L.

Practical quantitation limit (PQLs) will be proportionately higher for sample

extracts that require dilution to avoid saturation of the detector.

1.6. This method is restricted to use by or under the supervision of analysts

experienced in the use of gas chromatograph/mass spectrometers and skilled in

the interpretation of mass spectra. Each analyst must demonstrate the ability to

generate acceptable results with this method.

2. Summary of Method

2.1. The samples are prepared for analysis by gas chromatography/mass spectrometry

(GC/MS) using the appropriate sample preparation technique and, if necessary,

sample cleanup procedures.

2.2. The semivolatile compounds are introduced into the GC/MS by injecting the

sample extract into a GC with a narrow-bore fused silica capillary column. The

GC column is temperature programmed to separate the analytes, which are then

detected with a MS.

2.3. Analytes eluted from the capillary column are introduced into the MS via direct

connection. Identification of target analytes is accomplished by comparing their

mass spectra with the electron impact spectra of authentic standards.
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Quantitation is accomplished by comparing the response of a major

(quantitation) ion relative to an internal standard using a minimum five-point

calibration curve.

3. Safety

3.1. This method involves the handling of chemicals outlined below. Each of these

chemicals may have specific associated hazards. Analysts must read and become

familiar with all elements of each chemical’s MSDS. Make special awareness of

the symptoms of exposure and potential routes of entry. Analysts must notify the

Safety Officer immediately if any symptoms of exposure are suspected.

3.2. PPE must be worn at all times in designated work areas. All applicable

engineering controls, such as fume hoods and splash shields, must be used when

performing analyses.

3.3. To ensure the safety of all laboratory personnel: work areas must be kept neat

and organized; equipment and bench-tops must be cleaned and sterilized, if

necessary, at the completion of each task; all containers must be properly labeled

as to the contents and hazard ratings; and spills need to be cleaned immediately

and completely.

3.4. Lab coats, nitrile gloves and protective eyeglasses are to be worn at all times

during analysis by this method and while handling any laboratory sample.

3.5. A thorough MSDS review of methylene chloride, sodium sulfate and all

laboratory calibration standards should be performed prior to analysis by this

method.

3.6. All standards are to be made in a fume hood away from heat sources.

3.7. This method uses reagents that may cause anemia, eye/liver/kidney/central

nervous disorders, reproductive disorders and cancer upon exposure. Stock

standards of these materials should be handled in fume hoods. Toxic gas

respirators should be worn when handling concentrated standards and samples.

4. Waste Disposal

4.1. Solvent Waste: All solvent waste must be disposed of in the solvent waste

satellite container, then placed in the larger container located in the hazardous

waste room. Note: a technician certified to do so can only dump solvent waste in

the hazardous waste room.

4.2. Water/Soil Waste: Solid and aqueous material must sit in a vented area until all

the solvent has been evaporated. Alternatively, wastewater may be collected in a

carboy and bubbled with the exhaust of the pump in the extraction lab hood. The

water can be flushed down the drain with copious amounts of tap water. Soil

waste is stored in a satellite container and disposed of in the solid waste

container in the hazardous waste room.
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4.3. Acid Waste should be contained separate from all other waste streams and

disposed of in the proper waste container in the hazardous waste room by a

technician who is trained to do so.

5. Sample Collection, Preservation and Storage

5.1. Sample Collection and Preservation

5.1.1. Collect water samples in 1L amber glass bottles with PTFE-lined screw

caps.

5.1.2. Adjust the pH to 5.0 - 9.0, using 6N HCl or 6N NaOH as needed. Store

the sample at 4o

C in a refrigerator and away from light.

5.1.3. Collect solids in 250mL amber glass bottle with PTFE-lined screw caps,

and refrigerate at 4o

C.

5.2. Storage

5.2.1. All samples are stored in the Extraction Lab refrigerator at 4o

C.

5.2.2. All extracts are stored in the Sample Extract refrigerator in the extraction

lab at 4o

C.

5.2.3. Standards are stored in the Extraction Lab and Organics Lab Standard

refrigerators at 4oC.

5.3. Holding Times

5.3.1. Extraction 

Waters: 7 days from sampling

Soils: 14 days from sampling

5.3.2. Analysis 

40 days from extraction

6. Equipment and Supplies

6.1. Gas Chromatograph/Mass Spectrometer (GC/MS)

6.1.1. Hewlett Packard 6890 Series GC

6.1.2. Agilent 5973 Network Mass Selective Detector

6.1.3. Agilent 7683B Series Injector

6.1.4. Dell desktop computer running Agilent MSD Chemstation D.02.00.275

6.1.5. Capillary Column - Rxi-5ms, 30m, 0.25 mmID, 0.25umdf (or equivalent)

6.1.6. 10ul, 23guage injector syringe

6.1.7. Merlin microseal – septa

6.1.8. Restek drilled uniliner with hole on bottom injection port liner (or

equivalent)

6.1.9. Vent Carbon Trap

6.1.10. Ultra-High Purity He gas supply

6.2. 1L and 250mL Amber glass bottles with PTFE-lined screw caps.
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6.3. 375 watt Ultrasonic Disrupter (Tekmar)

6.3.1. 3⁄4” horn (low concentration)

6.3.2. 1/8” tapered microtip attached to a 1⁄2” horn (high concentration)

6.4. 250mL Beakers

6.5. 500mL Erlenmeyer Flasks

6.6. Glass funnels

6.7. Various sized syringes

6.8. 2 Liter Teflon separatory funnels

6.9. 1 Liter graduated cylinder

6.10. 9” Glass Pasteur pipettes

6.11. 2mL and 4mL vials, Teflon septa caps, and micro inserts

6.12. Metal spatulas

6.13. Zymark TurboVap II concentrator

6.14. Zymark TurboVap II concentration vials

7. Reagents and Standards

7.1. Reagents Log

• All reagents are recorded in the Reagents Log when opened. The date

reagents are entered into the Reagents Log is then used to trace reagents on

the Extraction Log.

7.2. Reagents

• Reagent grade chemicals that conform to the specifications of the Committee

on Analytical Reagents of the American Chemical Society shall be used in all

tests. Other grades may be used, provided it is first ascertained that the

reagent is of sufficiently high purity to permit its use without lessening the

accuracy of the determination. Reagents should be stored in glass to prevent

the leaching of contaminants from plastic containers.

7.2.1. Acetone – Fisher Optima

7.2.2. Methylene chloride – GC Resolv

7.2.3. Methanol

7.2.4. Anhydrous granular sodium sulfate – Certified ACS

• Purify by heating to 400 oC for 4 hours in a shallow tray.

• The sodium sulfate log is kept by the analyst who is responsible for

baking the sodium sulfate in the muffle furnace. Reagent information as

well as baking information (time, temperature...) is recorded here.

7.2.5. De-ionized water – produced by Endyne, Inc

7.2.6. Pool sand – Methylene chloride rinsed

7.2.7. Glass wool – Silanated

7.2.8. Concentrated sulfuric acid

7.2.9. 10 N NaOH
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7.3. Standards

• Store standards at 4 oC in PTFE-sealed containers in the standards refrigerator

in the extraction lab.

• Ensure that all purchased standards are in solvents compatible with methylene

chloride.

• Standards purchased for QCS samples should come from a separate supplier

than calibration standards – when possible.

• Equivalent standards may be ordered from alternate sources.

7.3.1. Internal Standard Mix – AccuStandard, Z-014J, 4000ppm Internal

Standard Mix in methylene chloride.

7.3.2. Surrogate Standard Mix – AccuStandard, M-8270-SS, 4000ppm Method

8270 – Surrogate Standard in methylene chloride

7.3.3. Calibration Stock Standards – Restek, 31815, 8270/Appendix IX Kit

• Restek, 31850, 500-1000ppm 8270 MegaMix in methylene chloride

• Restek, 31625, 2000ppm Appendix IX Mix #1 in methylene chloride

• Restek, 31806, 1000ppm Appendix IX Mix #2 in methylene chloride

• Restek, 31030, 2000ppm 605 Benzidines Calibration Mix in MeOH

7.3.4. QCS/Independent Calibration Stock Standard – NSI Solutions, Inc., Q1261, 100ppm Custom BNA Spiking Mix in MeOH

7.3.5. QC/MS Spiking Stock Standards – AccuStandard, CLP-007 includes:

7.3.5.1. CLP-007A, 1.0mg/mL Base/Neutral in MeOH

7.3.5.2. CLP-007B, 2.0mg/mL Acids in MeOH

• These two standards are diluted together in MeOH to make a 200ppm

spiking standard.

7.3.6. Instrument Performance Check/DFTPP Tuning Standard – AccuStandard,

M625-TS-20X, 1,000ppm GC/MS Tuning Std for EPA Method 624/625 in

methylene chloride

8. Interferences

8.1. Raw GC/MS data from all blanks samples and spikes must be evaluated for

interferences. Determine if the source of interference is in the preparation and/or

cleanup of the samples and take corrective action to eliminate the problem.

8.2. Contamination by carryover can occur whenever high-concentration and co

concentration samples are sequentially analyzed. To reduce carryover, the

sample syringe must be rinsed with solvent between sample injections.

Whenever an unusually concentrated sample is encountered, it should be

followed by the analysis of a solvent to check for cross-contamination.

8.3. Sources

8.3.1. Contaminated solvents, reagents, or sample processing hardware.

8.3.2. Contaminated GC carrier gas, parts, column surfaces, or detector surfaces.
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8.3.3. Compounds extracted from the sample matrix to which the detector will

respond.

8.4. Prevention and Solutions

8.4.1. Common flexible plastics contain varying amounts of phthalate esters

which are easily extracted or leached from such materials during laboratory

operations. Interference from phthalate esters can best be minimized by

avoiding contact with any plastic materials and checking all solvents and

reagents for phthalate contamination

8.4.2. Glassware must be scrupulously cleaned. Clean all glassware as soon as

possible after use by rinsing with the last solvent used. This should be

followed by detergent washing with hot water, and rinses with tap water and

DI water. Drain the glassware and dry it in an oven at 130 oC for several

hours or rinse with MeOH and drain. Volumetric glassware should not be

subjected to heating. Store dry glassware in a clean environment.

9. Quality Control

9.1. Extraction

9.1.1. The following should be extracted at least 1 per set or 1 per 20 samples,

whichever is more frequent:

9.1.2. Laboratory Reagent Blank (LRB)

• 1.0L DI H2O or 30.0g pool sand spiked with 10uL of 4,000ppm Surrogate

Standard and 10uL of 4,000ppm Internal Standard

9.1.3. Laboratory Fortified Blank (LFB)/Laboratory Control Sample (LCS)

• 1.0L DI H2O or 30.0g pool sand spiked with 10uL of 4,000ppm Surrogate

Standard, 200uL of 200 ppm QC/MS spiking std in MeOH, and 10uL of

4,000ppm Internal Standard

• 400uL of 100ppm NSI Custom BNA Spiking Mix should be used

when a project requires that all reported analytes are evaluated in

the LCS.

• The stock QC/MS spiking mix should come from a source independent

from the calibration stock standard.

9.1.4. Laboratory Duplicate (LD)

• A sample aliquot taken in addition to the first, spiked 10uL of 4,000ppm

Surrogate Standard and 10uL of 4,000ppm Internal Standard, extracted,

and analyzed with an identical procedure to the first in order to measure

the precision associated with this laboratory procedure.

9.1.5. Laboratory Fortified Sample Matrix (LFM)

• A sample aliquot taken in addition to the first, and spiked the same as an

LFB to determine whether the sample matrix contributes bias to the

analytical results.

9.2. Method Blanks/LRB
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9.2.1. When samples that are extracted together are analyzed on separate

instruments or on separate analytical shifts, the method blank must be

analyzed on at least one of those instruments.

9.2.2. The method blank may be analyzed immediately after the calibration

verification standard, to ensure that there is no carryover from the standard,

or at another point in the analytical shift.

9.2.3. When sample extracts are subjected to cleanup procedures, the associated

method blank must also be subjected to the same cleanup procedures.

9.2.4. LRBs should have target compounds:

• Less than the reporting limit for the analyte;

• Less than 5% of the regulatory limit associated with an analyte;

• Less than 5% of the sample result for the same analyte, whichever is

greater.

9.2.5. If the method blank results do not meet the acceptance criteria above, then

the laboratory should take corrective action to locate and reduce the source

of the contamination and to re-extract and reanalyze any samples associated

with the contaminated method blank.

9.2.6. If method blank does not meet acceptance criteria and samples are past

holding times, reported data will be qualified “B” indicating that blank

contamination was observed at levels affecting analytical results.

9.2.7. Blank subtraction is not permitted.

9.2.8. Method blanks and/or solvent blanks may be used to check for

contamination by carryover from a high-concentration sample into

subsequent samples.

9.2.9. When analysis of such blanks is not possible the analyst should review the

result for at least the next two samples after the high-concentration sample.

9.2.9.1. If the analytes in the high-concentration sample are not present in

subsequent samples, the lack of carryover has been demonstrated.

9.2.9.2. If there is evidence that carryover may have occurred, then the

affected samples should be reanalyzed.

9.3. LFB/LCS sample

9.3.1. The LFB consists of an aliquot of a clean (control) matrix similar to the

sample matrix and of the same weight or volume. It is fortified at the same

concentration as the matrix spike.

9.3.2. Recovery calculations are as follows:

%Recovery = ((Cs – Cu)/ Cn)*100 where:

• Cs = Measured concentration of the spiked sample aliquot

• Cu = Measured concentration of the unspiked sample aliquot (use 0

for the LFB)

• Cn = Nominal (theoretical) concentration increase that results from

spiking the sample or the nominal concentration of the spiked aliquot
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9.3.3. The LFB should fall within established laboratory control limits. In the

absence of control limits, 70-130% may be used.

9.3.4. If the LFB falls outside of acceptance limits, the laboratory should take

the following corrective action:

9.3.4.1. Check to be sure that there are no errors in the calculations or

standard solutions. If errors are found, recalculate the data accordingly.

Examine chromatograms for interfering peaks and integrated peak

areas.

9.3.4.2. Check instrument performance. If an instrument performance

problem is found, correct the problem and re-analyze the extracts as

well as all associated sample extracts.

9.3.4.3. If no instrument problem is found, the analytical batch should be

re-extracted and re-analyzed if still within holding time.

9.3.4.4. If upon re-analysis (of initial extract or re-extracted extract), the

recovery is again not within limits, affected analytes should be

qualified “QA” indicating that associated QA/QC did not meet

laboratory guidelines.

9.4. Matrix Spike (MS)/LFM sample

9.4.1. A duplicate field sample is fortified with a known amount of analyte in

order to document the effect of the matrix on method performance.

9.4.2. Matrix spikes are fortified with the same amount of analyte as the

LFB/LCS.

9.4.3. Matrix Spike recoveries are not calculated if the fortified concentration is

<20% of the background concentration of the sample.

9.4.4. Recoveries for Matrix Spike samples are calculated in the same manner as

the LFB/LCS and must meet established control limits.

• In the absence of control limits, 70-130% may be used.

9.4.5. When the results of a matrix spike analysis indicates a potential problem

due to the sample matrix itself (a positive of negative bias) the LFB/QCS

results are used to verify that the laboratory can perform the analysis in a

clean matrix.

9.4.6. If it is determined that the matrix is biasing quantitation, affected analytes

are to be qualified “M+” or “M-“ indicating a positive or negative bias due

to the sample matrix.

9.4.7. If both the LFB and MS fall outside of acceptance limits, follow the

corrective action outlined for the LFB/QLCS (sec. VII.C.4).

9.5. Duplicate/LD

9.5.1. A duplicate sample is analyzed along side the sample in order to measure

the precision associated with this method.

9.5.2. Precision is an estimate of the relative percent difference (RPD) of the

concentrations for the analysis of the unspiked samples.
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RPD = ((C1-C2)/((C1+C2)/2))*100 where:

• C1 = measured concentration of the first sample aliquot

• C2 = measured concentration of the second sample aliquot

9.5.3. Acceptance limits for precision are +/- 30% RPD

9.5.4. Duplicates that fall outside acceptance criteria should be qualified as

“DS,” indicating that there were disparate results between laboratory

duplicate analyses.

9.6. Surrogates

9.6.1. In addition to the fortification of all QA/QC samples with 10uL of

4,000ppm surrogate standard, all field samples must also be fortified and

evaluated versus in-house acceptance criteria.

9.6.2. Surrogate recoveries is calculated as: (Recovered Surrogate Concentration

/ Surrogate Target Concentration) * 100

9.6.3. Surrogate recoveries must fall within established acceptance limits. If

surrogate recoveries are outside of acceptance limits the following steps

should be taken.

9.6.3.1. Check to be sure that there are no errors in the calculations or

surrogate standard solutions. If errors are found, recalculate the data

accordingly. Examine chromatograms for interfering peaks and

integrated peak areas.

9.6.3.2. Check instrument performance. If an instrument performance

problem is found, correct the problem and re-analyze the extract.

9.6.3.3. Some samples may require dilution in order to bring one or more

target analytes within the calibration range or to overcome significant

interferences with some analytes. This may result in the dilution of the

surrogate responses to the point that the recoveries cannot be measured.

If the surrogate recoveries are available from a less-diluted or undiluted

aliquot of the sample or sample extract, those recoveries may be used

to demonstrate that the surrogates were within the QC limits, and no

further action is required. However, the results of both the diluted and

undiluted (or less-diluted) analysis should be provided to the data user.

9.6.3.4. If no instrument problem is found, the sample should be reextracted and re-analyzed if still within holding time.

9.6.3.5. If upon re-analysis (of initial extract or re-extracted extract), the

recovery is again not within limits, Surrogate value reported to the

client must be qualified as “NR” indicating that the surrogate falls

outside laboratory QA/QC parameters.

9.7. Internal Standard Response – If the area for any of the internal standards in a

QA/QC or field sample changes by a factor of two (-50% to +100%) from that in

the midpoint standard level of the most recent valid initial calibration sequence,

the sample must be reanalyzed. If, upon reanalysis, the IS response is still
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unacceptable, the sample may be re-extracted if within holding time or reported

with a qualifier on affected analytes stating that the associated internal standard

recovery did not meet laboratory acceptance criteria.

9.8. Quality Control Sample/Independent Calibration Verification

9.8.1. A 40ug standard is diluted from the 100ppm Custom BNA Spiking Mix

from NSI in methylene chloride.

9.8.2. This standard is analyzed immediately after the last initial calibration

standard and evaluated as if it were a Calibration Verification Standard (sec.

10.3).

9.8.3. If the QCS does not meet the calibration verification criteria, a newly

prepared QCS standard must be acquired and evaluated. If the new QCS

does not meet calibration verification criteria all calibration standards must

be evaluated for proper preparation, possible concentration and degradation.

New calibration standards should be prepared and a new initial calibration

should be run and evaluated with a QCS.

9.9. Demonstration of Capability (DOC)

9.9.1. Prior to extracting samples for clientele, a new extractionist must extract 4

LFB samples at the standard QC concentration. These LFB must be

analyzed as other laboratory samples and then processed according to the

following acceptance criteria:

9.9.1.1. Calculate the average concentration and the standard deviation for

each parameter using the four results

9.9.1.2. The average % Recovery must fall within established control limits

for LFBs, and the percent standard deviation must be less than 20%.

9.10. Method Detection Limits (MDL)/Reporting Limits

9.10.1. An MDL study should be performed once a year.

9.10.1.1. Seven low-level LFBs are extracted. To determine the MDL for

each analyte and surrogate, the standard deviation of the seven values

is multiplied by 3.14.

9.10.1.2. The target concentration of the low-level QCs should be 2.5-5

times the calculated MDL value.

9.10.1.3. Method Detection Limit should be no greater than one-fifth the

Reporting Limit.

9.10.2. The reporting limit is based on achieving the requested detection limits of

our clients as well as being below known environmental action limits. The

laboratory takes into account known interferences, such as contamination

peaks. It should be no less than 5 times the MDL.

9.10.3. For established reporting limits refer to Table 3.

9.11. Limits, Tables, and Charts
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9.11.1. Tables of surrogate and analyte recoveries from LFBs and LFMs are

maintained, and updated annually. Surrogate data is established from field

samples and LFB and LFM data come from LFBs and Matrix Spike

samples.

9.11.2. Limits are based on the previous chronological year’s data, unless

significant modification has been made to the methodology in which case

limits are established after the first twenty samples have been analyzed.

9.11.2.1. Control Limits: parameter average +/- 3(Standard Deviation)

9.11.2.2. Warning Limits: parameter average +/- 2(Standard Deviation)

9.11.2.3. Control Charts must be separated by matrix and extraction

procedure (Ex: Soil by Sonication, Soil by Soxhlet, Soil by

Continuous)

9.11.2.4. Up to date Control Charts are kept in the 8270 analyst’s

workspace.

9.12. Qualifying Data

• Any deviations from the above outlined quality control as well as any sample

container, preservation or holding time discrepancies, outlined in Section 5,

are noted on the final report.

10. Procedure

10.1. Extraction Log – An 8270/625 Extraction Log is to be filled out for every

extraction batch and kept in the extraction log binder in the extraction lab.

Copies of the extraction log are to be stapled to the Login Reports and given to

the analyst when extractions have been completed.

10.2. Separatory Funnel Liquid-Liquid Extraction (SW-846 Method 3510C) for full

8270 and TCLP analysis. Method 3510C allows the following pH adjustment

steps to be reversed to better separate acid and neutral waste components. This

will be performed at the analyst discretion.

10.2.1. *Pre-rinse all extraction apparatus with MeCl2 before use.

10.2.2. Using a 1-L graduated cylinder, measure 1-L of sample. Alternatively, if

the entire contents of the sample bottle are to be extracted, mark the level of

the sample on the outside of the bottle. If high analyte concentrations are

anticipated, a smaller sample volume may be taken and diluted to 1-L with

DI.

10.2.3. 1-L of DI H2O is to be used for the blank and QC sample.

10.2.4. Spike 10ul of the 4,000ppm 8270 surrogate spiking solution into each

sample (including blanks, QC samples and matrix spike samples) in the

graduated cylinder (or sample bottle) and mix well.

10.2.5. For the sample in each batch selected for use as a matrix spike sample and

the QC sample, spike 200ul of the 200ppm 8270 QC/MS spiking standard.
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10.2.6. Check the pH of the sample with wide-range pH paper to ensure a neutral

pH between 5 and 9.

10.2.7. Quantitatively transfer the sample from the graduated cylinder (or sample

bottle) to the 2-L separatory funnel and adjust the pH to > 11 using 10N

NaOH. Shake sample in separatory funnel to ensure mixing and check the

pH using narrow-range pH paper. Add more 10N NaOH, if necessary, to

achieve a pH > 11.

10.2.8. Use 60mL of methylene chloride to rinse the cylinder (or bottle) and

transfer this rinse solvent to the separatory funnel.

10.2.9. If the sample was transferred directly from the sample bottle, refill to the

mark made in Sec. 10.2.2. with water and then measure the volume of

sample that was in the bottle.

10.2.10. Seal and shake the separatory funnel vigorously for 2 minutes with

periodic venting to release excess pressure. The automatic shaker may be

employed on the high setting for 2 minutes after the separatory funnel has

been shaken by hand and vented periodically for 30 seconds.

• Methylene chloride creates excessive pressure very rapidly;

therefore, initial venting should be done immediately after the

separatory funnel has been sealed and shaken once. The

separatory funnel should be vented into a hood to avoid exposure

of the analyst to solvent vapors.

10.2.11. Allow the organic layer to separate from the water phase for a

minimum of 10 minutes. If the emulsion interface between layers is more

than one-third the size of the solvent layer, the analyst must employ

mechanical techniques to complete the phase separation.

• The optimum technique depends on the sample and may include

stirring, filtration of the emulsion through glass wool,

centrifugation, or other physical methods.

10.2.12. Decant the solvent extract through a glass funnel containing sodium

sulfate and into a 500mL Erlenmeyer flask.

• Plug a glass funnel with glass wool and add sodium sulfate until it

is 2-3cm above the glass wool plug.

10.2.13. Repeat the extraction (Sec. 10.2.10 to 101.2.12) two more times

adding fresh 60mL portions of methylene chloride directly to the separatory

funnel.

10.2.14. Adjust the pH to < 2 using concentrated sulfuric acid. Shake sample

in separatory funnel to ensure mixing and check the pH using narrow-range

pH paper. Add more concentrated sulfuric acid, if necessary, to achieve a

pH <2.

10.2.15. Add 60mL methylene chloride to the separatory funnel, seal and shake

vigorously for 2 minutes with periodic venting to release excess pressure.

The automatic shaker may be employed on the high setting for 2 minutes

after the separatory funnel has been shaken by hand and vented periodically

for 30 seconds.

• Methylene chloride creates excessive pressure very rapidly;

therefore, initial venting should be done immediately after the
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separatory funnel has been sealed and shaken once. The

separatory funnel should be vented into a hood to avoid exposure

of the analyst to solvent vapors.

10.2.16. Allow the organic layer to separate from the water phase for a

minimum of 10 minutes. If the emulsion interface between layers is more

than one-third the size of the solvent layer, the analyst must employ

mechanical techniques to complete the phase separation.

• The optimum technique depends on the sample and may include

stirring, filtration of the emulsion through glass wool,

centrifugation, or other physical methods.

10.2.17. Decant the solvent extract through a glass funnel containing sodium

sulfate and into a 500mL Erlenmeyer flask.

• Plug a glass funnel with glass wool and add sodium sulfate until it

is 2-3cm above the glass wool plug.

10.2.18. Repeat the extraction (Sec. 10.2.15 to 101.2.17) two more times

adding fresh 60mL portions of methylene chloride directly to the separatory

funnel.

10.2.19. On the final extraction, rinse the sodium sulfate with two 30ml

portions of methylene chloride and collect with the rest of the extract in the

500mL Erlenmeyer flask.

10.2.20. Perform the concentration using the TurboVap Concentration Method

(Sec. 10.6)

10.3. Separatory Funnel Liquid-Liquid Extraction (SW-846 Method 3510C) for

PAH analysis.

10.3.1. *Pre-rinse all extraction apparatus with MeCl2 before use.

10.3.2. Using a 1-L graduated cylinder, measure 1-L of sample. Alternatively, if

the entire contents of the sample bottle are to be extracted, mark the level of

the sample on the outside of the bottle. If high analyte concentrations are

anticipated, a smaller sample volume may be taken and diluted to 1-L with

DI.

10.3.3. 1-L of DI H2O is to be used for the blank and QC sample.

10.3.4. Spike 10ul of the 4,000ppm 8270 surrogate spiking solution into each

sample (including blanks, QC samples and matrix spike samples) in the

graduated cylinder (or sample bottle) and mix well.

10.3.5. For the sample in each batch selected for use as a matrix spike sample and

the QC sample, spike 200ul of the 200ppm 8270 QC/MS spiking standard.

10.3.6. Check the pH of the sample with wide-range pH paper to ensure a neutral

pH between 5 and 9.

10.3.7. Quantitatively transfer the sample from the graduated cylinder (or sample

bottle) to the 2-L separatory funnel.

10.3.8. Use 60mL of methylene chloride to rinse the cylinder (or bottle) and

transfer this rinse solvent to the Separatory funnel.

10.3.9. If the sample was transferred directly from the sample bottle, refill to the

mark made in Sec. 10.3.2. with water and then measure the volume of
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sample that was in the bottle.

10.3.10. Seal and shake the Separatory funnel vigorously for 2 minutes with

periodic venting to release excess pressure. The automatic shaker may be

employed on the high setting for 2 minutes after the Separatory funnel has

been shaken by hand and vented periodically for 30 seconds.

• Methylene chloride creates excessive pressure very rapidly;

therefore, initial venting should be done immediately after the

separatory funnel has been sealed and shaken once. The

separatory funnel should be vented into a hood to avoid exposure

of the analyst to solvent vapors.

10.3.11. Allow the organic layer to separate from the water phase for a

minimum of 10 minutes. If the emulsion interface between layers is more

than one-third the size of the solvent layer, the analyst must employ

mechanical techniques to complete the phase separation.

• The optimum technique depends on the sample and may include

stirring, filtration of the emulsion through glass wool,

centrifugation, or other physical methods.

10.3.12. Decant the solvent extract through a glass funnel containing sodium

sulfate and into a 500mL Erlenmeyer flask.

• Plug a glass funnel with glass wool and add sodium sulfate until it

is 2-3cm above the glass wool plug.

10.3.13. Repeat the extraction (Sec. 10.3.10 to 101.3.12) two more times

adding fresh 60mL portions of methylene chloride directly to the separatory

funnel.

10.3.14. On the final extraction, rinse the sodium sulfate with two 30ml

portions of methylene chloride and collect with the rest of the extract in the

500mL Erlenmeyer flask.

10.3.15. Perform the concentration using the TurboVap Concentration Method

(Sec. 10.6)

10.4. Ultrasonic Extraction (SW-846 Method 3550B)-Low Concentration, <

20mg/kg.

10.4.1. The following steps should be performed rapidly to avoid the loss of the

more volatile extractable compounds.

10.4.2. *Pre-rinse all extraction apparatus with methylene chloride before use.

10.4.3. Weigh approximately 30g of sample into a 500ml beaker. Record the

weight to the nearest 0.01g. 30g of methylene chloride rinsed pool sand are

to be used for the blank and QC sample.

10.4.3.1. Samples must be well mixed prior to weighing. Dump entire

contents of sample into a tared beaker, remove any foreign objects

(sticks, leaves and rocks) and thoroughly mix the sample with a

spatula. Replace sample into original sample container leaving 30g in

the beaker to be extracted.

10.4.3.2. Nonporous or wet samples (gummy or clay type) that do not have

a free flowing sandy texture must be mixed with 60g of anhydrous
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sodium sulfate, using a spatula. If required, more sodium sulfate may

be added.

10.4.3.3. After addition of sodium sulfate, the sample should be free

flowing.

10.4.4. Spike 10ul of the 4,000ppm surrogate standard solution onto all samples,

matrix spike samples QC samples and blanks.

10.4.5. For the sample in each batch selected for use as a matrix spike sample and

the QC sample, spike 200ul of the 200ppm 8270 QC/MS spiking standard.

10.4.6. Immediately add 100mL of 1:1 acetone/methylene chloride. Method

3550B allows for the use of other extraction solvents, provided the analyst

can demonstrate adequate performance for the compounds of interest in the

sample matrix. This will include MDL and DOC studies. Associated

QA/QC with the extraction set must meet laboratory acceptance limits.

10.4.7. Tune sonicator daily or after changing the horn (use 3⁄4 inch horn).

10.4.7.1. Ensure that the probe is not immersed in liquid and that it does not

come in contact with anything.

10.4.7.2. Set PULSER to OFF.

10.4.7.3. Set OUTPUT CONTROL to “10”

10.4.7.4. Set POWER SWITCH to ON. The switch will illuminate.

10.4.7.5. Momentarily depress TUNE SWITCH and rotate the tuner

clockwise or counterclockwise until a minimum (not maximum)

reading (usually <20) is obtained on power monitor.

10.4.7.6. Set OUTPUT CONTROL to “10”

10.4.7.7. Set % DUTY CYCLE to “50”

10.4.7.8. Set TIMER to “180S”

10.4.7.9. Set PULSER to ON position

10.4.8. Before each sample, place the probe tip in fresh 1:1 acetone/methylene

chloride and energize the power supply for a few seconds to remove any

residue.

10.4.9. Place the bottom surface of the tip of the 3⁄4 inch disrupter horn about 1⁄2

inch below the surface of the solvent, but above the sediment layer. If the

horn comes in contact with the sediment output is reduced.

10.4.10. Press START on sonicator and extract ultrasonically for 3 minutes,

with output control knob set to 10 (full power) at 50% duty cycle. Do not

use microtip probe.

• It is highly advisable to wear earplugs during the sonication process to

prevent possible damage to one’s hearing.

10.4.11. Decant the solvent extract through a glass funnel containing sodium

sulfate and into a 500mL Erlenmeyer flask.

• Plug a glass funnel with glass wool and add sodium sulfate until it is

2-3cm above the glass wool plug.

10.4.12. Repeat the extraction two or more times with two additional 100mL

portions of 1:1 acetone/methylene chloride. Decant off the solvent after

each ultrasonic extraction. On the final ultrasonic extraction, pour the entire

sample onto the sodium sulfate and rinse with two 50ml portions of 1:1

acetone/methylene chloride.
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10.4.13. Perform the concentration using the TurboVap Concentration Method

(Sec. 10.6)

10.5. Ultrasonic Extraction (SW-846 Method 3550B)-High Concentration,

>20mg/kg

10.5.1. The following steps should be performed rapidly to avoid the loss of the

more volatile extractable compounds.

10.5.2. Transfer approximately 2g (record weight to the nearest 0.01g) of wellmixed sample to a 40mL VOA vial. Wipe the mouth of the vial with a

Kimwipe to remove any sample material. Record the exact weight of the

sample taken.

10.5.3. Add 2g anhydrous sodium sulfate to the sample in the 40mL vial and mix

well.

10.5.4. Spike 25ul of the 4,000ppm surrogate standard solution onto all samples,

matrix spike samples QC samples and blanks.

10.5.5. For the sample in each batch selected for use as a matrix spike sample and

the QC sample, spike 100ul of the 1,000ppm CLP-007A, Base/Neutral

QC/MS stock standard and 50ul of the 2,000ppm CLP-007B, Acid QC/MS

stock standard.

10.5.6. Immediately add 10.0ml methylene chloride to the vial.

10.5.7. Tune sonicator daily or after changing the horn (use 1/8 inch-tapered

microtip).

10.5.7.1. Ensure that the probe is not immersed in liquid and that it does not

come in contact with anything.

10.5.7.2. Set PULSER to OFF.

10.5.7.3. Set OUTPUT CONTROL to “5” **Never exceed this level with

the microtip.**

10.5.7.4. Set POWER SWITCH to ON. The switch will illuminate.

10.5.7.5. Momentarily depress TUNE SWITCH and rotate the tuner

clockwise or counterclockwise until a minimum (not maximum)

reading (usually <20) is obtained on power monitor.

10.5.7.6. Set OUTPUT CONTROL to “5”

10.5.7.7. Set % DUTY CYCLE to “50”

10.5.7.8. Set TIMER to “120S”

10.5.7.9. Set PULSER to ON position

10.5.8. Before each sample, place the probe tip in fresh methylene chloride and

energize the power supply for a few seconds to remove any residue.

10.5.9. Disrupt the sample with the 1/8 inch tapered microtip ultrasonic probe for

2 minutes at output control setting 5 and with a 50% duty cycle.

10.5.10. Loosely pack a disposable Pasteur pipette with 2-3cm glass wool.

Filter approximately 4ml of extract through the glass wool into a 4ml vial.

• Note final volume in Extraction Log as 10.0ml.

10.5.11. Spike 10ul of 4,000ppm 8270 Internal Standard mix into the 4mL

extract and proceed to Vial Labeling and Extract Archival (Sec. 10.7). If

performing Silica Gel Cleanup do not spike IS and proceed to Section 10.8.
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10.6. Turbo Vap Concentration Method (nitrogen blowdown technique)

10.6.1. *Pre-rinse all extraction apparatus with MeCl2 before use.

10.6.2. Transfer a maximum 200-mL of the extract to a 200-mL TurboVap

concentrator vial. As the volume in the concentrator vial decreases,

additional extract can be added.

10.6.3. Place the concentrator vial into the TurboVap II workstation at a water

bath temperature of 42o

C. If the concentrator vials are initially full, start

with a low gas pressure and increase the pressure as the volume in the vial

decreases. Operate at a maximum gas pressure of 15psi (1.0 bars).

10.6.4. Caution: when the volume of solvent is reduced below 1-mL, analytes

may be lost.

10.6.5. When the solvent volume reaches ~1.5-mL (at the bottom of the tapered

part of the vial) remove the vial from the water bath.

10.6.6. With a 9.0” Pasteur pipette, use the entire sample volume to rinse the

lower, tapered portion of the concentrator vial a couple of times. Transfer

the extract to a 4-mL vial.

10.6.7. Repeat Step 5, two times with fresh 1-mL portions of methylene chloride.

10.6.8. Bring extract up to a final volume of 4-mL with methylene chloride.

10.6.9. Spike 10ul of 4,000ppm 8270 Internal Standard mix into the 4mL extract

and proceed to Vial Labeling and Extract Archival (Sec. 10.7). If

performing Silica Gel Cleanup do not spike IS and proceed to Section 10.8.

10.7. Vial Labeling and Extract Archival

10.7.1. All sample extracts are to be archived in 4.0-mL vials in the sample

extract refrigerator for a minimum of 40 days.

10.7.2. For each sample, a portion of the extract to be analyzed is to be transferred

to a 2.0-mL vial lined with a 500uL micro-insert if necessary. If matrix is a

solid, the extraction analyst should prepare a 2-mL vial and cap it without

transferring the extract. This will allow suspended particles to settle to the

bottom. The 8270 analyst will transfer the extract before analysis on the

GC/MS.

10.7.3. All vials are to be labeled with the following:

10.7.3.1. Method ID (8270) & Matrix

10.7.3.2. Sample Reference Number

10.7.3.3. Extraction Date

10.7.3.4. Extraction Analyst Initials

10.8. Silica Gel Cleanup Method for PAH compounds (SW-846, Modified Method

3630C).

10.8.1. Place a large drying column in a clamp on a ring stand.

10.8.2. Pack a wad of glass wool down into the tip of a large drying column.

10.8.3. Fill the column with 3-4” of silica gel.
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10.8.4. Rinse the column with 20mls of Methylene Chloride but do not let the

column go dry.

10.8.5. Once almost all of the Methylene Chloride is through the column place the

column in a clean TurboVap Tube and transfer the extract onto the column

via pipet.

10.8.6. Rinse the old TurboVap tube with 3, 2ml aliquots of Methylene Chloride

and transfer these onto the column.

10.8.7. Let the solvent flow through the column without applying pressure. This

may take awhile.

10.8.8. Rinse the column with at least 20mls of Methylene Chloride.

10.8.9. Finally, gently blow the last bit of solvent through the column with a large

pipet bulb.

10.8.10. Repeat the concentration using the TurboVap Concentration Method

(Sec. 10.6)

10.9. Analysis

10.9.1. A single-column analysis is performed using a 0.25mm ID Restek Rxi5ms capillary column (or equivalent).

10.9.2. MSD Chemstation D.02.00 software is employed to operate the GC/MS

and acquire/store raw data on the Chemist (8270) computer.

10.9.3. GC operating conditions are determined by the analyst and recorded in the

following places:

• Temperature, pressure and injection programs are all saved as

acquisition method AQ-8270x. These conditions are printed and filed

with the calibration method and chromatograms after a new calibration

method is created.

10.9.4. Established operating conditions are used for both calibration and sample

analyses.

10.9.5. All analyses of calibration standards, LRBs, LFBs, LFMs, LDs, and field

samples must be recorded in the “5973 Run Log” file located on the Chemist

computer.
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10.10. Dilutions

10.10.1. Some samples may require dilution in order to bring one or more

target analytes within the calibration range or to overcome significant

interferences with some analytes.

10.10.2. Dilutions are made using methylene chloride and adjusting the amount

of IS to 40ug.

10.10.3. Dilutions must be re-analyzed with all necessary calibration

verification requirements being met.

10.11. Percent Solids

10.11.1. Dry weight, used for soil calculations, is determined by measuring the

percent solids of the sample.

10.11.2. The BOD/Solids analyst determines percent solids using EPA Method

160.3.

10.12. Initial Calibration:

10.12.1. Instrument Performance Check – Decafluorotriphenylphosphine

(DFTPP) analysis performed every 12 hours to confirm that the mass

spectrometer is tuned properly for 8270 analysis. The mass intensities are

then compared to the tune criteria listed in Table 1.

10.12.1.1. Three scans (the peak apex scan and the scans immediately

preceding and following the apex) are acquired and averaged.

Background subtraction is required and must be accomplished using a

scan no more than 20 scans prior to the elution of DFTPP. The

background subtraction should be designed to eliminate column bleed

or instrument background ions. Do not subtract part of the DFTPP

peak.

• MSD Chemstation software is used to automatically evaluate the

DFTPP.

• All subsequent standards, field samples and QA/QC samples

associated with a DFTPP analysis must use the identical MS

instrument conditions.

• If all tune criteria is not met, system maintenance (possibly

including re-tuning the MS) and reanalysis of the DFTPP are

required until performance is acceptable.

10.12.1.2. A 25ng of DFTPP is analyzed at the start of each data set and

every 12 hours of analysis by injecting 1uL of a 25ppm DFTPP tuning

standard.

10.12.1.3. Also included in the mix are Benzidine and Pentachlorophenol to

monitor peak shape and total recovery. These compounds are very

susceptible to active site degradation and peak tailing. They should be

present at their normal responses and no peak tailing should be visible.
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10.12.1.4. Also included is 4,4’-DDT which degrades to DDE and DDD.

Degradation byproducts must be less than 20% of DDT peak area in the

total ion chromatogram (TIC). Evaluation can be performed by

integrating all three peaks and using the area counts to calculate

percent breakdown using the following formula:

((area DDD + area DDE) / (area DDD + area DDE + area DDT)) x 100

10.12.1.5. If degradation is excessive and/or chromatography is poor, the

injection port may require cleaning. It may also be necessary to clip

off 20-40 cm from the head of the column.

10.12.2. Calibration Standards

10.12.2.1. All calibration standards are recorded in the GC/MS SVOC

Standards log at the 8270 workstation. Standards opened and used in

the extraction lab are recorded in the Extraction Lab Standards log.

10.12.2.2. A minimum of five calibration standards is required for calibration

curves using average of response factor and linear regression models; a

minimum of six calibration standards are needed for a quadratic

regression curve fit model.

10.12.2.3. Because of the number of compounds analyzed by Method 8270, it

may be necessary to use multiple curve fit models for calibration.

Also, the response of all the compounds in the calibration standards are

not equal and it is therefore necessary to include additional calibration

standards in the initial calibration so that there are sufficient calibration

points within the calibration range for all compounds.

10.12.2.4. Typically, a minimum of 10 calibration standards ranging in

concentration from 0.5ug to 100ug are prepared by diluting a primary

dilution standard (PDS) containing 200ppm target compounds and

surrogate compounds to 4ml with methylene chloride. 40ug of all

internal standards is added to each calibration standard. Typical

calibration standard concentrations are 0.5, 1.0, 2.0, 5.0, 10, 20, 40, 50,

60, 80 and 100ug.

10.12.3. 1uL of each calibration standard (containing internal standards) is

analyzed.

10.12.4. An internal standard calibration procedure is used for initial

calibration.

10.12.5. System Performance Check Compounds (SPCCs)

10.12.5.1. A system performance check must be performed to ensure that

minimum average response factors (RFs) are met before the calibration

curve is used. SPCCs are: N-nitroso-di-n-propylamine;

hexachlorocyclopentadiene; 2,4-dinitrophenol; and 4-nitrophenol.
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10.12.5.2. The minimum acceptable average RF is 0.050. These SPCCs

typically have very low RFs (0.1-0.2) and tend to decrease in response

as the chromatographic system or the standard material begins to

deteriorate.

10.12.5.3. If the minimum response factors are not met, the system must be

evaluated and corrective action must be taken before sample analysis

begins. Possible problems include standard mixture degradation,

injection port inlet contamination, contamination at the head of the

column and active sites in the column or chromatographic system.

10.12.6. Calibration Check Compounds (CCCs)

10.12.6.1. The purpose of the CCCs is to evaluate the calibration from the

standpoint of the integrity of the system. High variability for these

compounds may be indicative of system leaks or reactive sites on the

column.

10.12.6.2. Calculate the mean response factor and the relative standard

deviation (RSD) of the response factors for each target analyte. The

RSD should be less than or equal to 15% for each target analyte.

However, the RSD for each individual CCC (see table 2) must be less

than or equal to 30%

10.12.6.3. If the RSD for any CCC is greater than 30%, then the

chromatographic system is too reactive to begin sample analysis.

Clean or replace the injection port liner and/or capillary column, then

repeat the calibration procedure.

10.12.7. Evaluation of retention times – The relative retention time (RRT) of

each target analyte in each calibration standard should agree within

0.06RRT units.

10.12.8. Calibration Range and the Linearity of Target Analytes

10.12.8.1. Due to the quantity of target analytes analyzed by Method 8270, it

may be necessary to narrow the calibration range for individual

analytes by removing data points from either extreme ends of the

calibration range to achieve linearity.

10.12.8.2. The method quantitation limit (MQL) is established by the

concentration of the lowest standard analyzed during the initial

calibration. Hence narrowing the calibration range by changing the

concentration of the lowest standard will, by definition, change the

MQL. The analyst must ensure that the MCL is at least as low as the

reporting limit and preferably one calibration point below that level.

10.12.8.3. It is prohibited to remove data points from within a calibration

range while retaining the extreme ends of the calibration range. There

must also be a minimum of 5 standards (6 standards if using the

quadratic regression model) remaining for the calculation of the RSD.
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10.12.8.4. When employing a linear or quadratic curve fit model for a target

analyte, in addition to meeting the acceptance criteria for that model, it

must also have an RSD less than or equal to 30% when fit with an

average of response factor model. If this is unachievable the system

must be evaluated. Corrective action must be taken before a new initial

calibration is analyzed.

10.12.9. Quality Control Sample/Independent Calibration Verification

10.12.9.1. A 40ug standard is diluted from the 100ppm Custom BNA Spiking

Mix from NSI in methylene chloride.

10.12.9.2. This standard is analyzed immediately after the last initial

calibration standard and evaluated as if it were a Calibration

Verification Standard (sec. 10.3).

10.12.9.3. If the QCS does not meet the calibration verification criteria, a

newly prepared QCS standard must be acquired and evaluated. If the

new QCS does not meet calibration verification criteria all calibration

standards must be evaluated for proper preparation, possible

concentration and degradation. New calibration standards should be

prepared and a new initial calibration should be run and evaluated with

a QCS.

10.12.10. Calibration Models

10.12.10.1. Linear Calibration Using the Response Factor

10.12.10.1.1. The MSD Chemstation Environmental Data Analysis

software is used to determine the RF and relative standard

deviation (RSD) for each analyte from a minimum of five

calibration standards.

10.12.10.1.2. If the RSD is less than or equal to 15% over the calibration

range the response factor may be used to determine sample

concentrations.

10.12.10.1.3. If the RSD exceeds 15% or at the discretion of the analyst,

another calibration method listed below may be used.

10.12.10.2. Linear Calibration Using a Least Squares Regression

10.12.10.2.1. The MSD Chemstation Environmental Data Analysis

software is used to perform a linear regression of the instrument

response versus the concentration of a minimum of five

calibration standards.

10.12.10.2.2. A weighted least squares regression may be used if

replicate multi-point calibrations have been performed. For all

other instances an unweighted least squares method should be

used.
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10.12.10.2.3. The analyst should not force the line through the origin nor

include the origin as an additional calibration point. The intercept

is to be calculated from the data points.

10.12.10.2.4. The regression calculation will generate a correlation

coefficient (r) that is a measure of good fit. When r is greater or

equal to 0.990 this calibration method may be used to determine

sample concentration.

10.12.10.3. Non-linear Calibration Using a Quadratic Model

10.12.10.3.1. The MSD Chemstation Environmental Data Analysis

software is used to perform a quadratic calibration of the

instrument response versus the concentration of a minimum of six

calibration standards.

10.12.10.3.2. The curve may not be forced through the origin nor may

the origin be included as a calibration point.

10.12.10.3.3. Weighting using a quadratic calibration model may

significantly improve its accuracy.

10.12.10.3.4. A coefficient of the determination greater than or equal to

0.990 indicates that the curve may be used to determine sample

concentration.

10.12.10.3.5. The quadratic model is not to be used to compensate for

detector saturation at higher concentrations or to avoid proper

instrument maintenance.

10.12.10.4. Whichever calibration option is employed, analyte and

surrogate concentrations must fall within the calibration range in order

for calculations to be valid. Dilutions may be necessary in order to

bring analyte concentrations within this range.

10.12.10.5. Individual analytes and surrogates within the method may be

calibrated using any of the three methods described above.

10.12.10.6. If initial calibration does not meet acceptance criteria the

following steps need to be taken:

10.12.10.6.1. Check to be sure that there are no errors in the calculations

or preparation of calibration standard solutions. If a standard is

found to be prepared wrong a new standard should be made and

injected.

10.12.10.6.2. Examine chromatograms for interfering peaks and

integrated peak areas. If coelution with contaminant peaks is an

issue, instrument conditions may need to be changed to achieve

better separation or new calibration standards may need to be

made with new reagents.

10.12.10.6.3. Check instrument performance. If an instrument

performance problem is found, correct the problem and re-analyze

the initial calibration standards.

10.12.10.6.4. If no instrument problem is found and reanalysis of initial
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calibration standards is unsuccessful, new calibration standards

must be made.

10.13. Calibration Verification – consists of three steps that are performed at the

beginning of each 12-hour analytical shift.

10.13.1. Prior to the analysis of samples or calibration standards, inject 25ng of

the DFTPP standard into the GC/MS system. The resultant Mass Spectrum

for DFTPP must meet the criteria given in Table 1 before sample analysis

begins. These criteria as well as other IPC criteria (Sec. 10.12.1) must be

demonstrated each 12-hour shift during which samples are analyzed.

10.13.2. The initial calibration for each compound of interest should be verified

once every 12 hours prior to sample analysis, using the sample introduction

technique and conditions used for samples. This is accomplished by

analyzing a calibration standard at a concentration near the midpoint

concentration (40ug) for the calibration range of the GC/MS. The results

from the calibration standard analysis should meet the verification

acceptance criteria provided in sections 10.2.4 through 10.2.7.

10.13.3. A method blank should be analyzed after the calibration standard, or at

any other time during the analytical shift, to ensure that the total system is

free of contaminants. If the method blank indicates contamination, then it

may be appropriate to analyze a solvent blank to demonstrate that the

contamination is not a result of carryover from standards or samples. See

section 9.2 for method blank performance criteria.

10.13.4. SPCCs – A system performance check must be made during every 12-

hour analytical shift. Each SPCC in the calibration verification standard

must meet a minimum response factor of at least 0.050. This is the same

check applied during the initial calibration in section 10.1.5.

10.13.5. CCCs

10.13.5.1. After the system performance check is met, the CCCs listed in

Table 2 are used to check the validity of the initial calibration. Use

percent difference when performing the average of response factor

model calibration. Use percent drift when calibrating using a

regression fit model.

10.13.5.2. If the percent difference for each CCC is less than or equal to 20%,

then the initial calibration is assumed to be valid. If the criterion is not

met for any one CCC, then corrective action must be taken prior to the

analysis of samples. If the CCCs are not included in the list of analytes
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for a project, and therefore not included in the calibration standards,

then all analytes must meet the 20% difference or drift criterion.

10.13.6. Internal Standard retention time – the retention times of the internal

standards in the calibration verification standard must be evaluated

immediately after or during data acquisition. If the retention time for any

internal standard changes by more than 30 seconds from that in the midpoint standard level of the most recent initial calibration sequence, then the

chromatographic system must be inspected for malfunctions and corrections

must be made as required. When corrections are made, reanalysis of

samples analyzed while the system was malfunctioning is required.

10.13.7. Internal standard response – if the EICP area for any of the internal

standards in the calibration verification standard changes by a factor of two

(-50% to +100%) from that in the mid-point standard level of the most

recent initial calibration sequence, the mass spectrometer must be inspected

for malfunctions and corrections must be made, as appropriate. When

corrections are made, reanalysis of samples analyzed while the system was

malfunctioning is required.

10.14. GC/MS Analysis of Samples

10.14.1. Inject a 1-2ul aliquot of the sample extract into the GC/MS system,

using the same operating conditions that were used for the initial calibration.

The sample to be injected must contain 40ug of base/neutral and acid

surrogates (assuming 100% recovery). The injection volume must be the

same volume used for the calibration standards.

10.14.2. If the response for any quantitation ion exceeds the initial calibration

range of the GC/MS system, the sample extract must be diluted and reanalyzed. Additional internal standard must be added to the diluted extract

to maintain the same concentration as in the calibration standards (40ug).

10.14.3. Internal standard response in all field and QA samples must meet the

same criteria as the calibration verification standard (Sec. 10.2.7) to

effectively check drifting method performance, poor injection execution, and

anticipate the need for system inspection and/or maintenance. If the criteria

is not met, affected samples must be reanalyzed.

10.15. Qualitative Analysis – the qualitative analysis identification of compounds

determined by this method is based on retention time and on comparison of the

sample mass spectrum, after background correction, with characteristic ions in a

reference mass spectrum. The reference mass spectrum must be generated by the

laboratory using the conditions of this method. The characteristic ions from the

reference mass spectrum are defined as the three ions of greatest relative

intensity, or any ions over 30% relative intensity, if less than three such ions
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occur in the reference spectrum. Compounds are identified when the following

criteria are met.

10.15.1. The intensities of the characteristic ions of a compound must

maximize in the same scan or within one scan of each other. Selection of a

peak by a data system target compound search routine where the search is

based on the presence of a target chromatographic peak containing ions

specific for the target compound at a compound-specific retention time will

be accepted as meeting this criterion.

10.15.2. The RRT of the sample component is within +/- 0.06 RRT units of the

RRT of the standard component.

10.15.3. The relative intensities of the characteristic ions agree within 20% of

the relative intensities of these ions in the reference spectrum. (Example: for

an ion with an abundance of 50% in the reference spectrum, the

corresponding abundance in a sample spectrum can range between 30% and

70%.)

10.15.4. Structural isomers that produce very similar mass spectra should be

identified as individual isomers if they have sufficiently different retention

times. Sufficient GC resolution is achieved if the height of the valley

between two isomer peaks is less than 25% of the sum of the two peaks.

Otherwise, structural isomers are identified as isometric pairs.

Diastereomeric pairs that may be separable by the GC should be identified,

quantitated and reported as the sum of both compounds by the GC.

10.15.5. Identification is hampered when sample components are not resolved

chromatographically and produce mass spectra containing ions contributed

by more than one analyte. When gas chromatographic peaks obviously

represent more than one sample component, appropriate selection of analyte

spectra and background spectra is important.

10.15.6. Examination of extracted ion current profiles of appropriate ions can

aid in the selection of spectra and in qualitative identification of compounds.

When analytes coelute, the identification criteria may be met, but each

analyte spectrum will contain extraneous ions contributed by the coeluting

compound.

10.16. Unidentified Peak (UIP) Reporting

10.16.1. For samples containing components not associated with the calibration

standards, a library search may be made for the purpose of tentative

identification.
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10.16.2. The concentration of any non target analytes identified in the sample

should be estimated by rearranging the formula:

RF = (As x Cis) / (Ais x Cs)

Where:

RF = 1 (assumed)

As = peak area of the unknown compound from the TIC

Ais = peak area of the nearest IS from the TIC

Cs = Concentration of the unknown compound in ug.

Cis = Concentration of the internal standard in ug.

10.16.3. The resulting concentration should be reported in a UIP report

indicating: the qualitative identification; that the value is an estimate; and

the % quality match with the data system library.

10.17. Quantitative Analysis

10.17.1. Once a compound has been identified, the quantitation of that

compound will be based on the integrated abundance of the primary

characteristic ion from the EICP.

10.17.2. The data analysis software using the initial calibration data may be

used to determine the concentration in the extract.

10.17.3. Structural isomers that produce very similar mass spectra should be

quantitated as individual isomers if they have sufficiently different retention

times. Sufficient GC resolution is achieved if the height of the valley

between two isomer peaks is less than 25% of the sum of the two peaks.

Otherwise, structural isomers are quantitated as isometric pairs.

Diastereomeric pairs that may be separable by the GC should be summed

and reported as the sum of both compounds.

11. Data Reduction

11.1. Aqueous calculations

11.1.1. Calculated analyte masses in micrograms (ug) are divided by the volume

of sample in liters (L) resulting in calculated sample concentrations in ug/L.

11.1.2. Concentrations may also need to be adjusted for dilutions by multiplying

the final concentration by the dilution factor.

11.2. Soil calculations

11.2.1. Soils are reported out as a dry weight concentration using the equation:

Cs = Cex/(Ms*(PS/100)
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where;

Cs = Concentration in the sample (ug/Kg, dry)

Cex = Calculated mass in ug of analyte in the final extract

Ms = Mass of the sample in Kg

PS = Percent solid

11.2.2. Concentrations may also need to be adjusted for dilutions by multiplying

the final concentration by the dilution factor.

12. Data Recording

12.1. Locating the 8270 Chain-of-Custody and extracted samples

12.1.1. The Chain-of-Custody for extracted 8270 samples will be found in the

bins dedicated to methods of the Organic Department labeled “8270”.

12.1.2. Extracted samples are located in the Organics Department refrigerator

found in the extraction lab.

12.1.3. Enter the individual sample information found on the Extraction Log sheet

into the Excel Run-log (“5973”).

12.2. Data from MSD Chemstation is directly imported into the LIMS system using

a Microsoft Excel macro. The macro calculates the reported values taking into

consideration: volume/mass extracted; percent solid (soils only); and post

extraction dilutions.

12.3. Target Compounds

12.3.1. If analyte concentration is below the reporting limit, report “< (Reporting

Limit)”

12.3.2. As long as it is within the calibration curve, report that value. Otherwise,

dilute the sample and rerun OR add additional standards to the calibration

tables.

13. Data Archiving

13.1. Hard Copies

13.1.1. All QC packets from method analyses are to be kept for 5 years.

13.1.2. QC packets are separated by method and kept in the filing cabinet near the

8270 workstation or in banker boxes (the most recent QC packets are kept in

the filing cabinet, space permitting, while all others are kept in folders in

labeled banker boxes beneath the workstation).

13.1.3. Only the previous and present year QC data are kept on the premises. All

other QC data is kept in the Endyne storage facilities.

13.1.4. Hard copies of all chromatograms are saved as data packets by order ID

with all other Organic data packets.
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13.2. Electronic Backup

13.2.1. An electronic backup of all new data files should occur at least once a

month.

13.2.2. Data is archived in 8270-525 Backup in the Shared folder on the Server.

13.2.3. Annually, data is backed up on CD-R.

14. Instrument Maintenance

14.1. Recalibration

14.1.1. In addition to recalibration being necessary when calibration verification

does not meet acceptance criteria, significant maintenance activities or

hardware changes may also require recalibration.

14.1.2. Maintenance that should not automatically require recalibration:

14.1.2.1. Changing septa; compressed gas cylinders; syringes; moisture,

hydrocarbon, or oxygen traps; split seals; column fittings; inlet liners.

14.1.2.2. Other procedures include breaking off or changing a guard column

or cleaning the inlet.

14.1.2.3. Whenever such procedures are performed, the analyst must

demonstrate that the results for a calibration verification standard meet

the acceptance criteria.

14.1.3. Maintenance that automatically requires recalibration:

14.1.3.1. Changing, replacing, or reversing the column; and replacing the

injection port.

14.1.3.2. Changing or replacing the column will also require that the

retention time windows be redetermined.

14.1.3.3.Cleaning the MS source; changing the electron multiplier, ion source

chamber or injection port all require recalibration.

14.2. Maintenance Log

14.2.1. In the Instrument Maintenance Log found on a separate sheet in the 5973

Run Log, enter any problems that have arisen with any methods and how the

problem was solved. Also log in any changes made to the instrument (i.e.

gas flow changes, column changes, injection port changes, etc.).

14.2.2. Each entry must be accompanied by the Date and Analyst’s Initials

14.3. Standards Log

14.3.1. Whenever any standard is opened or made up, enter the date, analyst’s

initials, source of standard, type and concentration, and detailed steps as to

how the standards were prepared.

14.4. Maintenance
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14.4.1. General

14.4.1.1. The Merlin Micro Seal is good for more than 2000 injections.

However, if the traditional septa are used, they must be changed every

30 or so runs.

• Occasional inspection of the microseal for coring or cracking is

recommended.

14.4.1.2. Replace injection port liner every 100-150 injections; whenever

standard degradation is evident

14.4.1.3. Replace injection port orange O-Rings if dried and cracking

14.4.1.4. Replace column ferrules when cutting the column

14.4.2. Injection Port Liner Cleaning

• Rinse with MeCl2

• Rinse with HNO3

• Rinse with HCl

• Rinse with DI

• Rinse with MeOH

• Dry with N2

• Rinse for 30 seconds with silanating agent

• Rinse with Toluene

• Rinse with MeOH

• Dry with Nitrogen

14.4.3. Changing a Column

14.4.3.1. Vent the MS

14.4.3.2. Lower all GC temperatures (oven and injector) to < 70o

C

14.4.3.3. Remove the detector end of the column first

14.4.3.4. Plug the detector end of the column with and injection port septa

14.4.3.5. Remove the injector end of the column and plug it into the septa.

14.4.3.6. Remove the old column from the oven and install the new column

in the injection port. Ensure there is carrier gas flow by dipping the tail

end of the column into solvent and condition the column for a couple of

hours outside the MS.

14.4.3.7. After conditioning, position the column in the MS so that 2-3mm

of column is sticking beyond the end of the transfer line.

14.4.3.8. Close and pump down the MS. Additional conditioning of the

column may be necessary.

15. Trouble Shooting

15.1. No Signal

15.1.1. Switch to alternate filament.

15.1.2. Check for MS malfunctions.
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15.2. Noisy / High Baseline

15.2.1. Using an air duster, check for leaks into the MS by spraying at system

seals and the MS transfer line. Monitor ion scans in manual tuning window

for primary ions of fluorinated compound in air duster.

15.2.2. Use a leak detector to check for helium leaks in connections in the supply

line and the injection port.

15.2.3. Double check column insertion distances.

15.3. High or Low Column Flows / Head Pressure Not Adjustable

15.3.1. Split vent lines may be contaminated with sample waste. To resolve this

problem, rinse the purge lines with MeOH and blow dry.

15.3.2. The column may be plugged. Check the detector and injector ends of the

column for blockage

15.4. No Head Pressure

15.4.1. Make sure the injector column fittings are tight.

15.4.2. Make sure the septum is not leaking.

15.5. Reduction in Response / Coelution of Certain Analytes

15.5.1. There may be active sites in the injector / column. Try changing the

injection port liner, gold plated seal, septa, or removing 1-2 loops of column.

15.5.2. Check column flow. If flow is too high or too low, coelution and/or

tailing may occur.

15.5.3. Check column insertion distance into the MS.

16. Method Modifications

16.1. Sec. 10.4, Method 3550B calls for the solvent to be decanted through filter

paper after sonication. Endyne filters through muffled sodium sulfate and glass

wool to remove particulate and further dry the extract.

17. Bibliography/Reference

Method 8270C Semivolatile Organic Compounds by GC/MS. Revision 3.

USEPA, SW-846, December 1996.

Method 8000B Determinative Chromatographic Separations, Revision 2. USEPA,

SW-846, December 2006.
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Method 3500B, Organic Extraction and Sample Preparation, Revision 2. USEPA,

SW-846, December 2006.

Method 3510C, Separatory Funnel Liquid-Liquid Extraction, Revision 3. USEPA,

SW-846, December 2006.

Method 3550B, Ultrasonic Extraction, Revision 2. USEPA, SW-846, December

2006.

Method 3630C, Silica Gel Cleanup, Revision 3. USEPA, SW-846, December

2006.

18. Revision History

Revision #7, April 6, 2005

-Revised safety section

-Updated QC section

-Added Table #3 – Detection Limits

-Added Bibliography

-Added Revision History

-Added sign off sheet

Reviewed Method: March 2006

Revision #8, April 4, 2007, Matthew White

Complete revision of the SOP, which includes:

-Clarification of calibration models

-Updated QA/QC criteria including corrective action and qualifying data

-Revised extractions, which now include method numbers and high and 

low level soil extractions

-Detailed sections on initial calibration and calibration verification

Revision #9, September 20, 2007

-Section 10.2.10 & 10.2.15 & 10.3.10 Defined 2 minute extraction shake.

-Section 10.2 Defined option of reversing extraction pH sequence.

-Section 10.4.6 Defined the acceptability of using alternate extraction

solvents in the sonication method.
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TABLE 1. DFTPP KEY IONS AND ION ABUNDANCE CRITERIA 

 Mass Ion Abundance Criteria 

51 30-60% of mass 198

68 < 2% of mass 69

70 < 2% of mass 69

127 40-60% of mass 198

197 < 1% of mass 198

198 Base peak, 100% relative abundance

199 5-9% of mass 198

275 10-30% of mass 198

365 > 1% of mass 198

441 Present but less than mass 443

442 > 40% of mass 198

443 17-23% of mass 442

 

a

J.W. Eichelberger, L.E. Harris, and W.L. Budde. “Reference Compound to Calibrate

Ion Abundance Measurement in Gas Chromatography-Mass Spectrometry”, Analytical

Chemistry, 47, 995 (1975).

TABLE 2. CALIBRATION CHECK COMPOUNDS (CCC) 

Base/Neutral Fraction Acid Fraction

Acenaphthene 4-Chloro-3-methylphenol

1,4-Dichlorobenzene 2,4-Dichlorophenol

Hexachlorobutadiene 2-Nitrophenol

Diphenylamine Phenol

Di-n-octyl phthalate Pentachlorophenol

Fluoranthene 2,4,6-Trichlorophenol

Benzo(a)pyrene
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TABLE 3.

Reporting Limit Reporting Limit

Compound Waterug/L Soilug/Kg Compound Waterug/L Soilug/Kg

Acenaphthene-d (IS) NA NA 2,4-Dinitrophenol 20.0 400.

Acenaphthene 2.0 40.0 2,6-Dinitrophenol 20.0 400.

Acenaphthylene 2.0 40.0 2,4-Dinitrotoluene 5.0 100.

Aniline 5.0 100. 2,6-Dinitrotoluene 5.0 100.

Anthracene 2.0 40.0 Fluoranthene 2.0 40.0

Benz(a)anthracene 2.0 40.0 Fluorene 2.0 40.0

Benzidine 15.0 300. Hexachlorobenzene 5.0 100.

Benzo(a)pyrene 2.0 40.0 Hexachlorobutadiene 5.0 100.

Benzo(b)fluoranthene 2.0 40.0 Hexachlorocyclopentadiene 20.0 400.

Benzo(k)fluoranthene 2.0 40.0 Hexachloroethane 5.0 100.

Benzo(g,h,i)perylene 2.0 40.0 Indeno(1,2,3-cd)pyrene 2.0 40.0

Benzyl alcohol 10.0 200. Isophorone 2.0 40.0

Bis(2-chloroethoxy)methane 5.0 100. 1-Methylnaphthalene 2.0 100.

Bis(2-chloroethyl) ether 5.0 100. 2-Methylnaphthalene 2.0 100.

Bis(2-chloroisopropyl) ether 10.0 200. 2-Methylphenol 5.0 100.

Bis(2-ethylhexyl) phthalate 5.0 100. 3-Methylphenol 5.0 100.

4-Bromophenyl phenyl ether 2.0 40.0 4-Methylphenol 5.0 100.

Butyl benzyl phthalate 5.0 100. Naphthalene-d (IS) NA NA

Carbazole 10.0 200. Naphthalene 2.0 40.0

4-Chloroaniline 5.0 100. 1-Naphthylamine 10.0 200.

4-Chloro-3-methylphenol 10.0 200. 2-Naphthylamine 10.0 200.

1-Chloronaphthalene 2.0 40.0 2-Nitroaniline 20.0 400.

2-Chloronaphthalene 2.0 40.0 3-Nitroaniline 10.0 200.

2-Chlorophenol 5.0 100. 4-Nitroaniline 20.0 400.

4-Chlorophenyl phenyl ether 2.0 40.0 Nitrobenzene 2.0 40.0

Chrysene 2.0 40.0 2-Nitrophenol 10.0 200.

Chrysene-d (IS) NA NA 4-Nitrophenol 10.0 200.

Dibenz(a,h)anthracene 2.0 40.0 N-Nitrosodi-n-butylamine 5.0 100.

Dibenzofuran 2.0 40.0 N-Nitrosodi-n-propylamine 10.0 200.

1,2-Dichlorobenzene 2.0 40.0 N-Nitrosodiphenylamine 5.0 100.

1,3-Dichlorobenzene 2.0 40.0 N-Nitrosopiperidine 10.0 200.

1,4-Dichlorobenzene-d (IS) NA NA N-Nitrosodimethylamine 5.0 100.

1,4-Dichlorobenzene 2.0 40.0 Pentachlorophenol 15.0 300.

3,3'-Dichlorobenzidine 5.0 100. Perylene-d (IS) NA NA

2,4-Dichlorophenol 5.0 100. Phenanthrene 2.0 40.0

Di-n-butyl phthalate 5.0 100. Phenanthrene-d (IS) NA NA

Di-n-octyl phthalate 5.0 100. Phenol 5.0 100.

Diethyl phthalate 5.0 100. Pyrene 2.0 40.0

2,4-Dimethylphenol 5.0 100. 1,2,4-Trichlorobenzene 2.0 40.0

Dimethyl phthalate 5.0 100. 2,4,5-Trichlorophenol 10.0 200.

4,6-Dinitro-2-methylphenol 50.0 2,000. 2,4,6-Trichlorophenol 10.0 200.
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TABLE 4.

Compound Primary Ion Confirmation Ion(s)

Acenaphthene-d (IS) 164 162,160

Acenaphthene 154 153,152

Acenaphthylene 152 151,153

4-Aminobiphenyl 169 168,170,115

Aniline 93 66,65

Anthracene 178 176,179

Benz(a)anthracene 228 229,226

Benzidine 184 92,185

Benzoic acid 122 105,77

Benzo(a)pyrene 252 253,125

Benzo(b)fluoranthene 252 253,125

Benzo(k)fluoranthene 252 253,125

Benzo(g,h,i)perylene 276 138,277

Benzyl alcohol 108 79,77

Bis(2-chloroethoxy)methane 93 95,123

Bis(2-chloroethyl) ether 93 63,95

Bis(2-chloroisopropyl) ether 45 77,121

Bis(2-ethylhexyl) phthalate 149 167,279

4-Bromophenyl phenyl ether 248 250,141

Butyl benzyl phthalate 149 91,206

Carbofuran 164 149,131,122

4-Chloroaniline 127 129,65,92

4-Chloro-3-methylphenol 107 144,142

1-Chloronaphthalene 162 127,164

2-Chloronaphthalene 162 127,164

2-Chlorophenol 128 64,130

4-Chlorophenyl phenyl ether 204 206,141

Chrysene 228 226,229

Chrysene-d (IS) 240 120,236 12

Dibenz(a,h)anthracene 278 139,279

Dibenzofuran 168 139

1,2-Dichlorobenzene 146 148,111

1,3-Dichlorobenzene 146 148,111

1,4-Dichlorobenzene-d (IS) 152 150,115

1,4-Dichlorobenzene 146 148,111

3,3'-Dichlorobenzidine 252 254,126

2,4-Dichlorophenol 162 164,98

Di-n-butyl phthalate 149 150,104

Di-n-octyl phthalate 149 167,43

Diethyl phthalate 149 177,150

2,4-Dimethylphenol 122 107,121

Dimethyl phthalate 163 194,164

1,4-Dinitrobenzene 168 75,50,76,92,122

1,3-Dinitrobenzene 168 76,50,75,92,122

1,2-Dinitrobenzene 168 50,63,74

4,6-Dinitro-2-methylphenol 198 51,105

2,4-Dinitrophenol 184 63,154
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TABLE 4. cont.

Compound Primary Ion Confirmation Ion(s)

2,6-Dinitrophenol 162 164,126,98,63

2,4-Dinitrotoluene 165 63,89

2,6-Dinitrotoluene 165 63,89

Diphenylamine 169 168,167

Fluoranthene 202 101,203

Fluorene 166 165,167

Hexachlorobenzene 284 142,249

Hexachlorobutadiene 225 223,227

Hexachlorocyclopentadiene 237 235,272

Hexachloroethane 117 201,199

Indeno(1,2,3-cd)pyrene 276 138,227

Isophorone 82 95,138

1-Methylnaphthalene 142 141

2-Methylnaphthalene 142 141

2-Methylphenol 107 108,77,79,90

3-Methylphenol 107 108,77,79,90

4-Methylphenol 107 108,77,79,90

Naphthalene-d (IS) 136 68

Naphthalene 128 129,127

1-Naphthylamine 143 115,89,63

2-Naphthylamine 143 115,116

2-Nitroaniline 65 92,138

3-Nitroaniline 138 108,92

4-Nitroaniline 138 65,108,92,80,39

Nitrobenzene 77 123,65

2-Nitrophenol 139 109,65

4-Nitrophenol 139 109,65

N-Nitrosodiethylamine 102 42,57,44,56

N-Nitrosodi-n-butylamine 84 57,41,116,158

N-Nitrosodi-n-propylamine 70 42,101,130

N-Nitrosodiphenylamine 169 168,167

N-Nitrosopiperidine 114 42,55,56,41

N-Nitrosopyrrolidine 100 41,42,68,69

Pentachlorophenol 266 264,268

Perylene-d (IS) 264 260,265 12

Phenanthrene 178 179,176

Phenanthrene-d (IS) 188 94,80 10

Phenol 94 65,66

Pyrene 202 200,203

1,2,4-Trichlorobenzene 180 182,145

2,4,5-Trichlorophenol 196 198,97,132,99

2,4,6-Trichlorophenol 196 198,200
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I acknowledge that I have read this Standard Operating Procedure and agree

 to adhere to the Safety and Quality Control policies outlined within.

Name Date

 
Parameter

Method 

Detection 

Limit ug/L

Reporting 

Limit ug/L

Calibration 

Verification 

% Recovery

Ext. Lab 

Fortified 

Blank 

% Recovery

Matrix 

Spike % 

Recovery

Duplicate 

% 

Difference

N-Nitrosodimethylamine 0.590 10.0 80 - 120 < 30 %

Pyridine 0.844 10.0 80 - 120 < 30 %

Aniline 0.894 10.0 80 - 120 < 30 %

Phenol 0.327 5.0 80 - 120 14 - 36 12 - 36 < 30 %

2-Chorophenol 0.755 5.0 80 - 120 39 - 87 28 - 85 < 30 %

bis(2-chloroethyl) Ether 0.907 5.0 80 - 120 < 30 %

1,3-Dichlorobenzene 0.885 2.0 80 - 120 < 30 %

1,4-Dichlorobenzene 0.983 2.0 80 - 120 23 - 73 18 - 78 < 30 %

1,2-Dichlorobenzene 0.979 2.0 80 - 120 < 30 %

Benzyl Alcohol 0.880 20.0 80 - 120 < 30 %

2-Methylphenol 0.674 5.0 80 - 120 < 30 %

bis(2-chloroisopropyl)Eth 0.837 5.0 80 - 120 < 30 %

N-Nitrosodi-n-propylamin 0.893 5.0 80 - 120 45 - 87 32 - 88 < 30 %

3&4-Methylphenol 0.695 10.0 80 - 120 < 30 %

Hexachloroethane 1.11 5.0 80 - 120 < 30 %

Nitrobenzene 0.956 5.0 80 - 120 < 30 %

N-Nitrosopiperidine 0.860 10.0 80 - 120 < 30 %

Isophorone 0.952 2.0 80 - 120 < 30 %

2-Nitrophenol 0.809 10.0 80 - 120 < 30 %

2,4-Dimethylphenol 0.201 5.0 80 - 120 < 30 %

bis(2-chloroethoxy)Metha 0.870 5.0 80 - 120 < 30 %

2,4-Dichlorophenol 0.837 5.0 80 - 120 < 30 %

1,2,4-Trichlorobenzene 1.10 2.0 80 - 120 30 - 82 22 - 87 < 30 %

Naphthalene 0.135 2.0 80 - 120 < 30 %

4-Chloroaniline 0.983 5.0 80 - 120 < 30 %

2,6-Dichlorophenol 0.882 5.0 80 - 120 < 30 %

Hexachlorobutadiene 1.30 5.0 80 - 120 < 30 %

N-Nitrosodi-n-butylamine 0.735 5.0 80 - 120 < 30 %

4-Chloro-3-methylphenol 0.754 10.0 80 - 120 45 - 115 44 - 107 < 30 %

2-Methylnaphthalene 0.087 2.0 80 - 120 < 30 %

1-Methylnaphthalene 0.059 2.0 80 - 120 < 30 %

Control Limits 2010 EPA 8270C Aqueous

Endyne, Inc.

160 James Brown Drive

Williston, Vermont

Page 1 of 6
Parameter

Method 

Detection 

Limit ug/L

Reporting 

Limit ug/L

Calibration 

Verification 

% Recovery

Ext. Lab 

Fortified 

Blank 

% Recovery

Matrix 

Spike % 

Recovery

Duplicate 

% 

Difference

Control Limits 2010 EPA 8270C Aqueous

Endyne, Inc.

160 James Brown Drive

Williston, Vermont

Hexachlorocyclopentadien 0.818 20.0 80 - 120 < 30 %

2,4,6-Trichlorophenol 0.890 10.0 80 - 120 < 30 %

2,4,5-Trichlorophenol 0.939 10.0 80 - 120 < 30 %

2-Chloronaphthalene 0.935 2.0 80 - 120 < 30 %

1-Chloronaphthalene 0.994 2.0 80 - 120 < 30 %

2-Nitroaniline 0.845 20.0 80 - 120 < 30 %

Dimethylphthalate 0.988 5.0 80 - 120 < 30 %

2,6-Dinitrotoluene 0.992 10.0 80 - 120 < 30 %

Acenaphthylene 0.135 2.0 80 - 120 < 30 %

3-Nitroaniline 0.778 20.0 80 - 120 < 30 %

Acenaphthene 0.129 2.0 80 - 120 45 - 98 33 - 103 < 30 %

2,4-Dinitrophenol 0.577 20.0 80 - 120 < 30 %

Dibenzofuran 0.951 2.0 80 - 120 < 30 %

4-Nitrophenol 0.325 20.0 80 - 120 14 - 59 12 - 61 < 30 %

2,4-Dinitrotoluene 0.939 10.0 80 - 120 50 - 97 31 - 98 < 30 %

1-Naphthylamine 1.57 10.0 80 - 120 < 30 %

2-Naphthylamine 0.810 10.0 80 - 120 < 30 %

Fluorene 0.123 2.0 80 - 120 < 30 %

Diethylphthalate 1.04 5.0 80 - 120 < 30 %

4-Chlorophenylphenyleth 1.17 2.0 80 - 120 < 30 %

4-Nitroaniline 1.15 20.0 80 - 120 < 30 %

2-Methyl-4,6-dinitropheno 0.598 50.0 80 - 120 < 30 %

N-Nitrosodiphenylamine 0.990 5.0 80 - 120 < 30 %

Azobenzene 1.03 5.0 80 - 120 < 30 %

4-Bromophenylphenyleth 1.01 2.0 80 - 120 < 30 %

Hexachlorobenzene 1.07 5.0 80 - 120 < 30 %

Pentachlorophenol 1.15 20.0 80 - 120 42 - 135 27 - 128 < 30 %

Phenanthrene 0.120 2.0 80 - 120 < 30 %

Anthracene 0.079 2.0 80 - 120 < 30 %

Carbazole 1.05 5.0 80 - 120 < 30 %

Di-n-butylphthalate 1.07 5.0 80 - 120 < 30 %

Page 2 of 6
Parameter

Method 

Detection 

Limit ug/L

Reporting 

Limit ug/L

Calibration 

Verification 

% Recovery

Ext. Lab 

Fortified 

Blank 

% Recovery

Matrix 

Spike % 

Recovery

Duplicate 

% 

Difference

Control Limits 2010 EPA 8270C Aqueous

Endyne, Inc.

160 James Brown Drive

Williston, Vermont

Fluoranthene 0.094 2.0 80 - 120 < 30 %

Benzidine 0.534 20.0 80 - 120 < 30 %

Pyrene 0.078 2.0 80 - 120 62 - 122 45 - 128 < 30 %

Benzylbutylphthalate 0.933 5.0 80 - 120 < 30 %

Benzo(a)anthracene 0.071 2.0 80 - 120 < 30 %

Chrysene 0.081 2.0 80 - 120 < 30 %

3,3'-Dichlorobenzidine 0.819 5.0 80 - 120 < 30 %

bis(2-ethylhexyl)phthalate 1.70 5.0 80 - 120 < 30 %

Di-n-octylphthalate 0.906 5.0 80 - 120 < 30 %

Benzo(b)fluoranthene 0.097 2.0 80 - 120 < 30 %

Benzo(k)fluoranthene 0.120 2.0 80 - 120 < 30 %

Benzo(a)pyrene 0.068 2.0 80 - 120 < 30 %

Indeno[1,2,3-cd]pyrene 0.099 2.0 80 - 120 < 30 %

Dibenz(a,h)anthracene 0.114 2.0 80 - 120 < 30 %

Benzo(g,h,i)perylene 0.097 2.0 80 - 120 < 30 %

12/31/09 12/31/09

Acid Surrogates

2-Fluorophenol (E.S.) 80 - 120 16 - 50 16 - 50

Phenol-d5 (E.S.) 80 - 120 11 - 42 11 - 42

2,4,6-Tribromophenol (E.S.) 80 - 120 45 - 124 45 - 124

BN Surrogates

Nitrobenzene-d5 (E.S.) 80 - 120 34 - 107 34 - 107

2-Fluorobiphenyl (E.S.) 80 - 120 31 - 102 31 - 102

Terphenyl-d14 (E.S.) 80 - 120 55 - 133 55 - 133

Page 3 of 6
Parameter

Method 

Detection 

Limit 

ug/Kg

Reporting 

Limit 

ug/Kg

Calibration 

Verification 

% Recovery

Ext. Lab 

Fortified 

Blank % 

Recovery

Matrix 

Spike % 

Recovery

Duplicate 

% 

Difference

N-Nitrosodimethylamine 56.7 400 80 - 120 < 30 %

Pyridine 312 800 80 - 120 < 30 %

Aniline 10.6 800 80 - 120 < 30 %

Phenol 46.7 200 80 - 120 26 - 97 31 - 92 < 30 %

2-Chorophenol 48.1 200 80 - 120 30 - 96 30 - 94 < 30 %

bis(2-chloroethyl) Ether 44.4 200 80 - 120 < 30 %

1,3-Dichlorobenzene 44.0 80 80 - 120 < 30 %

1,4-Dichlorobenzene 46.9 80 80 - 120 31 - 78 26 - 80 < 30 %

1,2-Dichlorobenzene 46.3 80 80 - 120 < 30 %

Benzyl Alcohol 36.4 800 80 - 120 < 30 %

2-Methylphenol 45.6 200 80 - 120 < 30 %

bis(2-chloroisopropyl)Et 42.6 200 80 - 120 < 30 %

N-Nitrosodi-n-propylami 44.1 200 80 - 120 46 - 85 31 - 87 < 30 %

3&4-Methylphenol 38.8 400 80 - 120 < 30 %

Hexachloroethane 39.5 200 80 - 120 < 30 %

Nitrobenzene 53.8 200 80 - 120 < 30 %

N-Nitrosopiperidine 38.5 400 80 - 120 < 30 %

Isophorone 41.0 80 80 - 120 < 30 %

2-Nitrophenol 51.5 400 80 - 120 < 30 %

2,4-Dimethylphenol 42.5 200 80 - 120 < 30 %

bis(2-chloroethoxy)Meth 42.0 200 80 - 120 < 30 %

2,4-Dichlorophenol 41.0 200 80 - 120 < 30 %

1,2,4-Trichlorobenzene 47.1 80 80 - 120 37 - 86 32 - 90 < 30 %

Naphthalene 6.07 80 80 - 120 < 30 %

4-Chloroaniline 12.4 200 80 - 120 < 30 %

2,6-Dichlorophenol 42.5 200 80 - 120 < 30 %

Hexachlorobutadiene 49.1 200 80 - 120 < 30 %

N-Nitrosodi-n-butylamin 42.0 200 80 - 120 < 30 %

4-Chloro-3-methylpheno 55.6 400 80 - 120 48 - 108 41 - 111 < 30 %

2-Methylnaphthalene 2.90 80 80 - 120 < 30 %

1-Methylnaphthalene 1.95 80 80 - 120 < 30 %

Endyne, Inc.

160 James Brown Drive

Williston, Vermont

Control Limits 2010 EPA 8270C Solid

Page 4 of 6
Parameter

Method 

Detection 

Limit 

ug/Kg

Reporting 

Limit 

ug/Kg

Calibration 

Verification 

% Recovery

Ext. Lab 

Fortified 

Blank % 

Recovery

Matrix 

Spike % 

Recovery

Duplicate 

% 

Difference

Endyne, Inc.

160 James Brown Drive

Williston, Vermont

Control Limits 2010 EPA 8270C Solid

Hexachlorocyclopentadie 18.0 800 80 - 120 < 30 %

2,4,6-Trichlorophenol 49.6 400 80 - 120 < 30 %

2,4,5-Trichlorophenol 41.7 400 80 - 120 < 30 %

2-Chloronaphthalene 42.9 80 80 - 120 < 30 %

1-Chloronaphthalene 46.7 80 80 - 120 < 30 %

2-Nitroaniline 65.9 800 80 - 120 < 30 %

Dimethylphthalate 38.8 200 80 - 120 < 30 %

2,6-Dinitrotoluene 61.7 400 80 - 120 < 30 %

Acenaphthylene 6.38 80 80 - 120 < 30 %

3-Nitroaniline 34.5 800 80 - 120 < 30 %

Acenaphthene 6.57 80 80 - 120 49 - 95 50 - 91 < 30 %

2,4-Dinitrophenol 264 800 80 - 120 < 30 %

Dibenzofuran 41.2 80 80 - 120 < 30 %

4-Nitrophenol 44.9 800 80 - 120 30 - 98 25 - 101 < 30 %

2,4-Dinitrotoluene 67.5 400 80 - 120 48 - 106 36 - 101 < 30 %

1-Naphthylamine 18.6 800 80 - 120 < 30 %

2-Naphthylamine 13.0 800 80 - 120 < 30 %

Fluorene 6.61 80 80 - 120 < 30 %

Diethylphthalate 37.8 200 80 - 120 < 30 %

4-Chlorophenylphenyleth 38.2 80 80 - 120 < 30 %

4-Nitroaniline 51.5 800 80 - 120 < 30 %

2-Methyl-4,6-dinitrophen 56.3 2000 80 - 120 < 30 %

N-Nitrosodiphenylamine 40.7 200 80 - 120 < 30 %

Azobenzene 38.3 200 80 - 120 < 30 %

4-Bromophenylphenyleth 40.7 80 80 - 120 < 30 %

Hexachlorobenzene 39.3 200 80 - 120 < 30 %

Pentachlorophenol 87.6 800 80 - 120 32 - 120 41 - 118 < 30 %

Phenanthrene 6.15 80 80 - 120 < 30 %

Anthracene 4.35 80 80 - 120 < 30 %

Carbazole 44.0 200 80 - 120 < 30 %

Di-n-butylphthalate 51.1 200 80 - 120 < 30 %

Page 5 of 6
Parameter

Method 

Detection 

Limit 

ug/Kg

Reporting 

Limit 

ug/Kg

Calibration 

Verification 

% Recovery

Ext. Lab 

Fortified 

Blank % 

Recovery

Matrix 

Spike % 

Recovery

Duplicate 

% 

Difference

Endyne, Inc.

160 James Brown Drive

Williston, Vermont

Control Limits 2010 EPA 8270C Solid

Fluoranthene 5.73 80 80 - 120 < 30 %

Benzidine 120 800 80 - 120 < 30 %

Pyrene 5.43 80 80 - 120 58 - 109 49 - 113 < 30 %

Benzylbutylphthalate 65.1 200 80 - 120 < 30 %

Benzo(a)anthracene 4.95 80 80 - 120 < 30 %

Chrysene 4.89 80 80 - 120 < 30 %

3,3'-Dichlorobenzidine 24.2 200 80 - 120 < 30 %

bis(2-ethylhexyl)phthalat 78.3 200 80 - 120 < 30 %

Di-n-octylphthalate 124 200 80 - 120 < 30 %

Benzo(b)fluoranthene 4.01 80 80 - 120 < 30 %

Benzo(k)fluoranthene 6.15 80 80 - 120 < 30 %

Benzo(a)pyrene 9.48 80 80 - 120 < 30 %

Indeno[1,2,3-cd]pyrene 5.37 80 80 - 120 < 30 %

Dibenz(a,h)anthracene 5.12 80 80 - 120 < 30 %

Benzo(g,h,i)perylene 5.34 80 80 - 120 < 30 %

12/31/09 12/31/09

Acid Surrogates

2-Fluorophenol (E.S.) 80 - 120 25 - 111 25 - 111

Phenol-d5 (E.S.) 80 - 120 45 - 108 45 - 108

2,4,6-Tribromophenol (E.S.) 80 - 120 36 - 146 36 - 146

BN Surrogates

Nitrobenzene-d5 (E.S.) 80 - 120 28 - 110 28 - 110

2-Fluorobiphenyl (E.S.) 80 - 120 41 - 109 41 - 109

Terphenyl-d14 (E.S.) 80 - 120 58 - 117 58 - 117

Page 6 of 6
Document Control Copy on Buff colored paper. Any other color is not official version 

Endyne, Inc. 

160 James Brown Dr. 

Williston, VT 05495 

Phone: (802) 879-4333 

Fax: (802) 879-7103 

Alkaline Digestion for 

Chromium VI 

in Solid Samples 

Method SW 3060A 

Standard Operating Procedure

Written: March 8, 2006 

Technical Director: Date : 

Harry B. Locker Ph.D. 

QA Officer: Date : 

Mark L. Fausel 
Endyne, Inc. Chromium VI Method SW 3060A SOP 

160 James Brown Drive Effective 03/31/06 

Williston, VT 05495 Page 2 of 8 

Document Control Copy on Buff colored paper. Do not duplicate 

TABLE OF CONTENTS

Section Page

I – Overview 3 

II – Safety 3 

III – Waste Disposal 3 

IV – Sample Collection, Preservation & Storage 3 

V – Equipment & Supplies 3-4 

VI – Reagents & Standards 4 

VII – Interferences 4 

 VIII – Quality Control 4-5 

IX – Analytical Procedure 5 

X – Calibration & Standardization 6 

XI – Data Reduction 6 

XII – Data Recording 6 

XIII – Trouble Shooting 6 

XIV – Method Modifications 6 

 XV – Revision History 6 

 XVI – References 7 

Analyst Attestation 8 
Endyne, Inc. Chromium VI Method SW 3060A SOP 

160 James Brown Drive Effective 03/31/06 

Williston, VT 05495 Page 3 of 8 

Document Control Copy on Buff colored paper. Do not duplicate 

Overview: 

This method is an alkaline digestion and is used to solubilize water soluble/insoluble 

Cr(VI) compounds in solid/soil samples. The digested samples are then analyzed for 

Cr(VI) by method SW 7196A, a spectrophotometric method employing the reaction of a 

coloring agent diphenylcarbazide with Cr(VI). Please refer to SOP SW 7196A for 

further details. 

I. Safety: 

 

A. This method involves the handling of the chemicals outlined below. Each of these 

chemicals may have specific associated hazards. Analysts must read and become 

familiar with all elements of each chemical’s MSDS. Make special awareness of the 

symptoms of exposure and potential routes of entry. Analysts must notify the Safety 

Officer immediately if any symptoms of exposure are suspected. 

B. Personal protective equipment i.e. gloves goggles and lab coat must be worn at all times 

in designated work areas. All applicable engineering controls, such as fume hoods or 

splash shields, must be used when performing analyses. To ensure the safety of all 

laboratory personnel; work areas must be kept neat and organized, equipment and 

bench-tops must be cleaned and sterilized, if necessary, at the completion of each task, 

all containers must be properly labeled as to contents and hazard ratings and spills 

cleaned immediately and completely. 

II. Waste Disposal: 

A. Cr(VI) solutions or waste materials that are generated are dumped in the metals waste 

satellite container found underneath the fume hood on the inorganic floor. 

B. When the satellite container is full contact one of the hazardous waste personnel who is 

fitted with a respirator and properly trained in hazardous waste disposal, to dispose of 

metals waste in the proper corrosive liquid drain. 

C. Cr(VI) spills are to be treated with ascorbic acid or another reducing agent to reduce 

Cr(VI) as well as Cr(III). 

III. Sample Collection, Preservation and Storage: 

A. Samples should be collected in clean plastic or glass containers that do not contain 

stainless steel. 

B. Samples are to be stored at 4°C until the time of digestion. 

C. Cr(VI) is stable in properly stored samples for 30 days from the date of sample. 

D. The digestate is stable for 7 days from the date of digestion. 

IV. Equipment & Supplies: 

1. Digestion vessels: 250mL/500mL Erlenmeyer flasks 

2. 50mL/100mL graduated cylinder 

3. Volumetric flasks, varying sizes 

4. Vacuum filtration apparatus 

5. Filter membranes (0.90um glass filter) & (0.45um cellulose filter) 

6. Stirring hot plates 

7. Volumetric pipettes 
Endyne, Inc. Chromium VI Method SW 3060A SOP 

160 James Brown Drive Effective 03/31/06 

Williston, VT 05495 Page 4 of 8 

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8. Calibrated pH meter (refer to pH SOP) with stirring device 

9. Calibrated balance (refer to balance SOP) 

10. Thermometer capable of measuring 100 ̊C and with NIST traceable calibration 

11. Magnetic stir bars 

12. 250mL beakers 

V. Reagents & Standards: 

1. Nitric Acid (HNO3): 5.0M analytical reagent grade. Do not use concentrated HNO3

to make 5.0M solution if it has a yellow tinge as this is an indication of 

photoreduction of NO3 to NO2, a reducing agent for Cr(VI). 

2. Laboratory reagent grade water 

3. Digestion Solution: 

1) 20g Sodium Hydroxide 

2) 30g Sodium Carbonate 

brought up1000mL volumetrically with reagent water; pH must be 11.5 or 

greater 

4. Magnesium Chloride anhydrous (MgCl2) 

5. Phosphate Buffer: 

1) 8.71g K2HPO4

2) 6.80g KH2PO4

brought up 100mL volumetrically with reagent water; pH must around 7 

6. Potassium Dichromate, 1000ppm soluble spiking solution 

1) Dissolve 0.2829g H2Cr2O7 in a 100mL volumetric flask with reagent water 

2) Prepare 10ppm working stock solution by adding 1mL of 1000ppm stock to 

100mL reagent water volumetrically. 

3) Prepare all laboratory QC’s and soluble matrix spikes from 10ppm working 

stock. 

7. Lead Chromate (PbCrO4), insoluble matrix spike. 

8. ERA Hexavalent Chromium Soil QC – Independent QC 

9. ERA blank soil for metals digestion. 

 

VI. Interference: 

This method is usually free from interferences. However, certain reducing/oxidizing 

substances may interfere with the results of the analytical method if the chromium 

concentration is relatively low and the reducing/oxidizing substances are high. The 

addition of Mg with phosphate buffer is designed to suppress oxidation in the digestion. 

 

VII. Quality Control: 

A. All samples and QA are analyzed via method SW 7196A and quality control is 

pertinent to that method. (refer to SOP SW 7196A) 

B. A laboratory reagent blank must be prepared with the ERA blank soil and analyzed 

with each digestion batch. The recovery must be 1/10 less than the MDL as defined 

in method SW 7196A. 

C. A laboratory QC prepared at varying concentrations from the10ppm Potassium 

Dichromate stock must be spiked to the ERA blank sand and digested and analyzed 

with each digestion batch. Recovery must be 100 ± 20%. 
Endyne, Inc. Chromium VI Method SW 3060A SOP 

160 James Brown Drive Effective 03/31/06 

Williston, VT 05495 Page 5 of 8 

Document Control Copy on Buff colored paper. Do not duplicate 

D. An independent soil QC from ERA must be digested and analyzed with each 

digestion batch. Recovery must be within the certified accepted range as defined by 

the ERA certificate of analysis. 

E. A separately prepared duplicate sample must be analyzed each digestion batch. 

Duplicates samples must have a relative percent difference of ≤ 20%. 

F. Both a soluble and insoluble digestion spike must be prepared and analyzed during 

each digestion batch. The soluble digestion spike is analyzed at 0.2ppm (2mL, 

10ppm working stock added predigestion). The insoluble digestion spike is prepared 

by adding 20mg of Lead Chromate to the sample prior to digestion. The acceptance 

range for both matrix spike recoveries is 75-125%. 

G. Any data that falls outside of the above stated criteria are either redigested/analyzed 

or qualified with the appropriate qualifier. 

H. All in-house prepared reagents and standards must be properly labeled and have 

preparation and expiration dates noted on them. 

I. All reagents and standards must be properly documented with manufacture, lot 

numbers and expiration dates as well as a brief description of preparation in the 

miscellaneous logbook. 

 

VIII. Analytical Procedure: 

1. Weigh and record in logbook a known amount of homogeneous sample into a clean 

labeled 250mL Erlenmeyer flask. Samples may need to be ground prior to weighing. 

For blanks and QC’s weigh 2.5g ±0.1g. 

2. Add appropriate volume of spiking solution from 10ppm working stock to QC’s and 

matrix spikes. 

3. Add 50mL ± 1mL digestion solution to each sample, QC and blank using a graduated 

cylinder. 

4. Add approximately 400mg MgCl2 and 0.5mL phosphate buffer to each sample and 

cover with watch glasses. 

5. Stir samples continuously with out heat for five minutes on the stirring hot plate with 

magnetic stir bars. 

6. Adjust the temperature setting of each stirring hot plate to 185oC. 

7. Monitor temperatures with thermometer until they reach 90-95oC. Maintain 

temperature for at least 60 minutes with continuous stirring. 

8. Turn off heat on all hot plates and maintain stirring while the samples gradually cool. 

9. Filter each sample individually through a glass filter, rinsing the digestion vessel with 

three successive portions of reagent water. Rinse the filter and apparatus with 

reagent water. 

10. Collect filtrate and transfer to a 250mL beaker. Discard solid portion of the sample 

in proper waste recepticle. 

11. Adjust pH with constant stirring of filtered sample drop by drop with 5M HNO3 until 

the pH is 7.5 ± 0.5. 

12. Filter pH adjusted sample through a 0.45um cellulose filter and collect filtrate in a 

250mL beaker. 

13. Transfer sample to a 100mL or 200mL volumetric flask and bring up to the mark 

with reagent water. Record final volume in logbook. 

14. Analyze samples for Cr(VI) via method SW 7196A. 
Endyne, Inc. Chromium VI Method SW 3060A SOP 

160 James Brown Drive Effective 03/31/06 

Williston, VT 05495 Page 6 of 8 

Document Control Copy on Buff colored paper. Do not duplicate 

IX. Calibration & Standardization: 

A. Calibrate pH meter prior to each use (refer to pH SOP). 

B. Calibrate balance once a week (refer to balance SOP). 

C. Calibrate thermometer yearly against NIST traceable thermometer (refer to 

thermometer SOP). 

X. Data Reduction: 

 Refer to SOP for method SW 7196A for all calculations. 

XI. Data Recording: 

A. All data pertaining to the digestion, data and calculations are to be recorded in the 

miscellaneous logbook. 

B. All results are recorded as mg/kg 

C. Refer to SOP for method SW 7196A for further information on data recording. 

 

XII. Troubleshooting: 

1. Some samples upon pH adjusting form a gel. Filter samples through another glass 

filter rather than 0.45um cellulose filter. 

XIII. Method Modifications: 

1. Method SW 3060A describes procedures for indicating the reductive nature of the 

samples in the event the matrix spike falls outside accepted limits. This is so that that 

data may be accepted without qualifying it. Not all sample matrixes are compatible 

with the digestive procedures and for the sake of time and resources, data that falls 

outside of the strict matrix spike criteria is flagged as such and reported to the client. 

2. Method SW 3060A states that 2.50g of sample is to be analyzed, for the sake of 

minimizing the reductive potential of the samples it may be necessary to digest a 

smaller known amount such as 1g. 

3. Method SW 3060A states that the final volume is to be 100mL. The final volume of 

the sample may be brought up to any volume as long as the final volume is noted in 

the logbook. 

XIV. Revision History:

N/A 

XV. References:

1. Alkaline Digestion for Hexavalent Chromium. Method SW 3060A. CD-ROM, 

Revision 1, December 

I acknowledge that I have read this Standard Operating Procedure and agree 

 to adhere to the Safety and Quality Control policies outlined within. 
Endyne, Inc. Chromium VI Method SW 3060A SOP 

160 James Brown Drive Effective 03/31/06 

Williston, VT 05495 Page 7 of 8 

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 Name Date 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 
Document Control Copy on Buff colored paper. Any other color is not official version 

Endyne, Inc. 

160 James Brown Dr. 

Williston, VT 05495 

Phone: (802) 879-4333 

Fax: (802) 879-7103 

CHROMIUM VI 

Method SW 7196A 

Standard Operating Procedure

REVISED: March 25, 2010 

Revision #: 6 

Technical Director: Date : 

Harry B. Locker Ph.D. 

QA Officer: Date : 

Mark L. Fausel 
Endyne, Inc. Chromium VI Method SW 7196A SOP 

160 James Brown Drive Revision #5, Effective 3/25/10 

Williston, VT 05495 Page 2 of 8 

Document Control Copy on Buff colored paper. Do not duplicate 

TABLE OF CONTENTS

Section Page

I – Overview 3 

II – Safety 3 

III – Waste Disposal 3 

IV – Sample Collection, Preservation & Storage 3 

V – Equipment & Supplies 3-4 

VI – Reagents & Standards 4 

VII – Interferences 4 

VIII – Quality Control 

 4-5 

IX – Analytical Procedure 5 

X – Calibration & Standardization 6 

XI – Data Reduction 6 

XII – Data Recording 6-7 

XIII – Trouble Shooting 7 

XIV – Method Modifications 7 

 XV – Revision History 7 

 XVI – References 7 

 

 Analyst Attestation 8 
Endyne, Inc. Chromium VI Method SW 7196A SOP 

160 James Brown Drive Revision #5, Effective 3/25/10 

Williston, VT 05495 Page 3 of 8 

Document Control Copy on Buff colored paper. Do not duplicate 

I. Overview: 

This method is used to determine the concentration of dissolved Chromium VI 

(hexavalent chromium) in the absence of interfering amounts of substances such as Mo, 

V, and Hg. This is done by colorimetric reaction with diphenylcarbazide in acid solution. 

This is suitable for water samples, EP/TCLP characteristic extracts as well as soil samples 

that have been digested via method SW3060A. This method may also be applicable to 

certain domestic and industrial wastes provided that no interfering substances are present. 

II. Safety: Health=3 Fire=0 Reactivity=0 

A. This method involves the handling of the chemicals outlined below. Each of these 

chemicals may have specific associated hazards. Analysts must read and become 

familiar with all elements of each chemical’s MSDS. Make special awareness of the 

symptoms of exposure and potential routes of entry. Analysts must notify the Safety 

Officer immediately if any symptoms of exposure are suspected. 

B. Personal protective equipment i.e. gloves goggles and lab coat must be worn at all 

times in designated work areas. All applicable engineering controls, such as fume 

hoods or splash shields, must be used when performing analyses. To ensure the 

safety of all laboratory personnel; work areas must be kept neat and organized, 

equipment and bench-tops must be cleaned and sterilized, if necessary, at the 

completion of each task, all containers must be properly labeled as to contents and 

hazard ratings and spills cleaned immediately and completely. 

III. Waste Disposal: 

A. Cr(VI) solutions or waste materials that are generated are dumped in the metals 

waste satellite container found underneath the fume hood on the inorganic floor. 

B. When the satellite container is full contact one of the hazardous waste personnel to 

dispose of metals waste in the proper corrosive liquid drain. 

C. Cr(VI) spills are to be treated with ascorbic acid or another reducing agent to 

reduce Cr(VI) as well as Cr(III). 

IV. Sample Collection, Preservation and Storage: 

 

1. Samples should be collected in clean plastic or glass containers that do not contain 

stainless steel. 

2. Samples are to be stored at 4°C until the time of digestion. 

3. Water samples must be analyzed 24 hours from the time of collection. 

4. Cr(VI) is stable in properly stored soil samples for 30 days from the date of sample. 

5. The digestate is stable for 24 hours from the date of digestion. 

V. Equipment & Supplies: 

1) Spectrophotometer set at 540nm 

2) Appropriate absorption cell 

3) Pipettes, graduated/volumetric for sample dilutions 

4) 25mL sample cups 

5) 100mL volumetric flasks 
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VI. Reagents & Standards: 

1. Potassium Dichromate, 1000ppm soluble spiking solution 

1) Dissolve 0.2829g K2Cr2O7 in a 100mL volumetric flask with reagent 

water 

2) Prepare 10ppm working stock solution by adding 1mL of 1000ppm stock 

to 100mL reagent water volumetrically. 

3) Prepare all laboratory QC’s and soluble matrix spikes from 10ppm 

working stock. 

2. Diphenyl Carbizide Solution in acetone 0.125gm DC in 25 mls Acetone kept in the dark 

3. Concentrated H2S04

4. Reagent grade water 

 

VII. Interferences: 

This method is usually free from interferences. However, certain substances such as 

hexavalent Mo/Hg may form color, however the color intensity tends to be much lower 

than that of chromium. Concentrations of up to 200ppm Mo and Hg can be tolerated, V 

up to 10X the concentration of Cr will not cause trouble. Iron at levels greater than 1ppm 

may produce a yellow color but is usually not very strong. 

 

VIII. Quality Control: 

A. Demonstration of Capability (DOC) 

Prior to extracting samples for clientele, a new analyst must prepare 4 LFB samples 

at the standard QC concentration. These LFB must be analyzed as other laboratory 

samples and then processed according to the following acceptance criteria: 

1. Calculate the average in mg/L and the standard deviation for each parameter 

using the four results. 

2. The average % recovery must fall within 80-120% of the target result, and the 

percent standard deviation must be less than 20%. Analysts must perform annual 

DOC (demonstration of capability) by analyzing 4 mid-range QC’s. Values must 

have an average percent recovery and a percent standard deviation <20. DOC 

results are turned into the lab manager. 

B. An MDL must be run yearly. Run 7 standards that are roughly 2-5X estimated 

detection limit based on the calibration line and are calculated according to the Code of 

Federal Regulations chapter 1 part 136 appendix b. The MDL benchsheet is stapled to 

the miscellaneous logbook. 

C. A line calibration must be performed each analytical day and the correlation must be 

0.995 or greater. A line calibration is made from the 10ppm stock Potassium 

Dichromate solution into a 100ml volumetric flask as follows: 

0.02ppm = 0.2mL 

0.05ppm = 0.5mL 

0.10ppm = 1.0mL 

0.25ppm = 2.5mL 

0.50ppm = 5.0mL 

1.00ppm = 10.0mL 

D. A lab reagent blank is run 1 every 10 samples. 
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E. An undigested Line Check at varying concentrations is run 1 every 10 samples. Results 

should be +20%. 

F. Laboratory fortified matrix samples are run 1 every sample matrix or 10 samples, 

which ever comes first. For example, 100ul of 10ppm stock Potassium Dichromate can 

be added to 10mls of water sample to form a 0.1ppm spike. Results must be +30%. 

G. Duplicate water samples are run 1 per set or 1 every 10 samples. The relative 

difference must be ≤ 20%. 

H. One of the two following QC protocols must be performed for each batch of digested 

soil samples: 

(a) An independent soil QC prepared at varying concentrations from the10ppm 

Potassium Dichromate stock must be spiked to the blank Teflon chips and digested 

and analyzed with each digestion batch. Recovery must be 100 ± 20%. (refer to SOP 

SW 3060A). 

I. A separately prepared duplicate sample must be analyzed each digestion batch. 

Duplicate samples must have a relative percent difference of ≤ 20%. (refer to SW 

3060A) 

J. A soluble digestion spike must be prepared and analyzed during each digestion batch. 

The soluble digestion spike is analyzed at 0.2ppm (2mL, 10ppm working stock added 

predigestion). 

K. Any data that falls outside of the above stated criteria are either redigested/analyzed or 

qualified with the appropriate qualifier. 

L. All in-house prepared reagents and standards must be properly labeled and have 

preparation and expiration dates noted on them. 

M. All reagents and standards must be properly documented with manufacture, lot 

numbers and expiration dates as well as a brief description of preparation in the Cr+6 

log. 

IX. Analytical Procedure: 

1. Turn on the spectrophotometer and set the wavelength to 540nm. 

2. Add 10mL of each line point to a labeled sample cup and add 0.2mls 

Diphenylcarbazide solution. 

3. Add two drops of concentrated H2S04 and allow reacting for 5 minutes. 

4. Zero the spectrophotometer by following the instrument instructions. 

5. Once the reaction has occurred in the line points, from lowest concentration to the 

highest, pour of an aliquot into a clean sample cell, place it in the spectrophotometer 

and record the absorbance in the logbook. 

6. Repeat steps 2-5 for all samples, line checks and blanks. All results are given in 

absorbance. 

7. If a sample is turbid or has a discoloration to it, it may be necessary to zero that 

specific sample against itself without color reagent. If this is performed for a 

particular sample be sure to rezero the spectrophotometer with reagent water prior to 

analyzing other samples. 
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X. Calibration & Standardization: 

The spectrometer software performs the linear regression and provides an output of line 

and the correlation coefficient. 

XI. Data Reduction: 

1. The spectrometer software converts the absorbance to a mg/L value 

2. For samples with no observable Cr6+ the reporting limit is the lowest point on the 

line. 

3. Water samples are reported out as ppm or mg/L. 

4. Soil digested samples must be converted from mg/L to mg/kg. The calculation is as 

follows: 

A x D x E/ B x C = mg/kg 

 Whereas: 

 A= Concentration observed in the digestate (ppm) 

 B= Initial moist sample weight (g) 

 C= % Solids/100 

 D= Dilution Factor 

 E= Final digest volume (mL) 

5. Duplicate relative percent difference calculation is as follows: 

 (S-D)/[(S+D)/2] 

 Whereas: 

 S= Initial sample result 

 D= Duplicate sample result 

6. Spike recovery calculation is as follows: 

[(SSR –SR)/SA] x 100 

 Whereas: 

 SSR= Spike sample result 

 SR= Unspiked sample result 

 SA= Spike added 

XII. Data Recording: 

1. All digestion information, data and final results are recorded in a computer file saved 

in the Metals Subdirectory 

2. Water results are recorded in LIMS as mg/L. 

3. Soil results are recorded in LIMS as mg/kg. 

4. Results are to be recorded with 2 significant figures 

XIII. Troubleshooting: 

1. If samples are turbid or have a color, rezero the sample against itself without reagent 

to obtain a proper absorbance value or try filtering the sample. See section IX. 

2. If the correlation is not at 0.995 or above, drop points on the line and plug in the 

numbers again to get the best fit. If there are only five points to begin with, it will be 

necessary to make a new calibration from the 10ppm stock and try again. 
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XIV. Method Modifications: 

1. It is stated in the original SOP that it may be appropriate to treat all standards and line 

points as the samples, indicating the possibility to digest the line calibration. 

However, when spoken to ERA, although digesting the line may help to compensate 

for possible loss of Cr6+ during digestion, as long as the QA values fall within 

mandated limits, line digestion is not necessary. 

2. The method states that every sample must be spike to ensure that a reducing agent is 

not affecting the color reaction and thereby the results. This protocol is impractical 

and the random matrix spike requirements should be enough to fulfill this criterion. 

If reducing reagent is suspected, obtain a fully prepared sample and add 0.1ppm 

matrix spike from the 10ppm stock as would be done with a water sample and 

analyze if according to section IX. 

XV. Revision History:

Rev. # 3- Wrote SOP according to new SOP format 

Rev. #4- Rewrote SOP according to using a new spectrophotometer as well as the 

implementation of the digestion method SW 3060A. Amended Health and Safety and 

QA QC sections. Added Method Modifications, Revision History, References and 

Analyst Attestation. 

Rev. #5 – analysis time for soils is 24hours and made modifications in reference to new 

digestion procedure. Opened spiking criteria to allow analyst to choose level. 

Rev. #6 – Changed LFM target and calculator use. 

XVI. References:

1. Alkaline Digestion for Hexavalent Chromium. Method SW 3060A. CD-ROM, Revision 1, 

December 

2. Chromium, Hexavalent (Colorimetric). Method 7196A. CD-ROM, Revision 1, July 

1992. 
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I acknowledge that I have read this Standard Operating Procedure and agree 

 to adhere to the Safety and Quality Control policies outlined within. 

 Name Date 

 

 

 

 

 

 

 

 

 

 

 
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Endyne, Inc.

160 James Brown Dr.

Williston, VT 05495

Phone: (802) 879-4333

Fax: (802) 879-7103

MERCURY IN SOLID OR SEMISOLID WASTE

Method SW 7471A

Standard Operating Procedure

REVISED: October 3, 2007

Revision #: 5

Technical Director: Date : 

Harry B. Locker Ph.D.

QA Officer: Date : 

Mark L. Fausel
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TABLE OF CONTENTS

Section Page

I – Overview 3

II – Safety 3

III – Waste Disposal 3

IV – Sample Collection, Preservation and Storage 3

V – Equipment and Supplies 4

VI – Reagents and Standards 4

VII – Interferences 4

VIII – Quality Control

5

IX – Analytical Procedure 5

X – Calibration 7

XI – Data Reductions 9

XII – Data Recording 9

XIII – Instrument Maintenance 9

XIV – Troubleshooting 9

XV – References 10

XVI -- Revision History 10

XVII – Method Modifications 10

XVIII SOP Attestation 11
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I. Overview:

 This method employs the Perkin Elmer FIMS 100 ( Flow Injection Mercury System) a

dedicated Atomic Absorption Spectrometer, for determination of mercury in soils,

sediments, bottom deposits and sludges.

 Prior to analysis, the solid or semi-solid samples must be prepared according to the

procedures discussed in this method.

 This cold-vapor atomic absorption method is based on the absorption of radiation at the

253.7 nm wavelength by mercury vapor. The mercury is reduced to the elemental state and

aerated from solution in a closed system. The mercury vapor passes through a cell positioned

in the light path of the atomic absorption spectrophotometer. Absorbance (peak height) is

measured as a function of mercury concentration.

II. Safety:

This method involves the handling of the chemicals outlined below. Each of these

chemicals may have specific associated hazards. Analysts must read and become

familiar with all elements of each chemical’s MSDS. Make special awareness of the

symptoms of exposure and potential routes of entry. Analysts must notify the Safety

Officer immediately if any symptoms of exposure are suspected.

PPE must be worn at all times in designated work areas. All applicable engineering

controls, such as fume hoods or splash shields, must be used when performing analyses. 

To ensure the safety of all laboratory personnel; work areas must be kept neat and

organized, equipment and bench-tops must be cleaned and sterilized, if necessary, at the

completion of each task, all containers must be properly labeled as to contents and hazard

ratings and spills cleaned immediately and completely.

III. Waste Disposal:

Samples that do not contain mercury may be flushed down the drain with copious amounts

of water. Samples containing mercury, as well as all standards and QC samples, must be

disposed of in the Hazardous Waste drum. Expired hollow cathode lamps may not be placed

in the trash; they are considered hazardous waste since they contain the target element(s). 

Lamps should be disposed of in an appropriate waste stream or returned to the vendor for

recycling.

IV. Sample Collection, Preservation, and Storage:

A. Collection:

Samples are collected in plastic and glass bottles of various sizes.

B. Labeling:

All samples are assigned a sample number, plus a unique identifier suffix to indicate

preservative and bottle type.
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C. Preservation:

Non-aqueous samples, or those known to react violently with acid preservation, are

stored in the inorganics refrigerator below 4oC and analyzed as soon as possible.

D. Storage:

Samples are stored in the inorganic fridge.

V. Equipment and Supplies:

Digestion Tubes with screw caps

Block digester capable of maintaining 95οC +/- 5οC

Volumetric Flasks, Various Sizes Class A

Perkin Elmer FIMS 100

Absorption Cell

Argon, Compressed Gas

VI. Reagents and Standards:

Reductant #1 - 12% W/V Sodium Chloride and 12% W/V Hydroxylamine hydrochloride in 

 DI. Ex. Dilute to 30g of each compound to 250 mL

Reductant #2 – 1.1% Stannous Chloride in 3% HCl. Ex. 6gÆ200mls

Nitric Acid, concentrated, Trace Metal Grade

5% Nitric Acid

Hydrochloric, concentrated, Trace Metal Grade

3% Hydrochloric Acid

Potassium Permanganate, 5% W/V ex. 50gÆ1L

Mercury Stock Standard

Aqua Regia – 40 mLs DI, 30 mLs Conc HCL, 10 mLs conc HNO3

Anti Foam from Sigma

NOTE: All incoming reagents, standards, dry chemicals and acids shall be marked with the

date of receipt, date of opening, and date of expiration. Dry chemicals shall be used within

20 years, and concentrated acids shall be used within 10 years of the date of receipt or before

the manufacturer’s expiration date, which ever is sooner.

VII. Interferences:

The vapor generation technique demands a high standard of care: scrupulous cleanliness is

essential in all laboratory procedures; standards and samples must be meticulously prepared

and carefully handled; and strict precautions must be taken to avoid contamination of the

apparatus.

VIII. Quality Control

A. ( See Table A in the “SOP” SOP for more detailed definitions of the following)

1. Demonstration of Capability (DOC). Each new analyst performs a set of four midrange LFBs. The LFBs should be prepared as one sample, then split into four
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aliquots. The percent standard deviation and average percent recovery are

determined for each analyte. Each must be less than 20% to ensure proper capability

of the analyst for that method. This process is repeated annually for each metals

analyst.

2. Method Detection Limit (MDL).

a. An MDL is run annually for each element. The final calculated MDL value

must be at least 1⁄2 the reporting limit and the MCL. MDLs should be

prepared in a manner identical to that of sample analysis.

b. Seven to ten QCs are made at at concentration 2-5 times highger than the

expected MDL.

c. The MDL is calculated by taking the standard deviation of the values and

multiplying by the appropriate number from the chart from the Code of

Federal Fregulations Appendix B to part 136 of Chapter 1 (7 is 3.143, 8 is

2.998, 9 is 2.896and 10 is 2.821).

3. Calibration Check/Verification (or Instrument Performance Check – IPC). The

concentrations of the calibration verification shall be varied within the established

calibration range.

4. Laboratory Reagent Blank (LRB).

5. Laboratory Fortified Blank (LFB or Independent QCS)

6. For all determinations the laboratory must analyze a calibration blank and line

check (IPC) at the start of the sample run, after every tenth sample (or more

frequently, if required) and at the end of the sample run.

7. The percent recovery for IPC’s must be +/-10%.

8. The calibration blanks can not be greater than 1/10 of the measured concentration

of any sample in the associated sample batch; or exceed the concentration present

in the samples or be greater than 1/10 of the regulatory limit.

9. Percent Recovery for the LFB must be +/-10%.

10. Duplicate samples are run every batch or every 20 samples

11. LFM samples are run every 20 samples or when results are questionable. Percent

recovery for LFM’s must be +/-30%.

12. LFM’s are acceptable as Independent QC’s.

13. If data does not meet the criteria outlined above, it may be used, but MUST be

noted on the final client report.
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IX. Analytical Procedure:

Digestion:

1) Turn on block digester and set at 95oC.

2) Prepare a rack of digestion tubes by labeling with the sample identification nos. Record

sample reference number on the Mercury page of the metals digestion log. Record all

pertinent information concerning reagents and standards.

3) Prepare a blank and 0.5, 1, 2, and 4 ppb standards from a 1 ppm Mercury solution - each

at a volume of 25 mLs with 5% Nitric acid . Prepare QC's at 2 ppb in digestion tubes. 

Samples may also be run against the water line since the absorbances have proven to be

the same for both lines.

4) A duplicate (LD) and spike (LFM) should be run with each project or C.O.C. with a

minimum of one dup and spike per digestion. The spike target may be between 3-5 ppb.

5) Using the soils spreadsheet calculate the amount of sample needed to yield a desirable

detection limit. Weigh out that amount of sample (in three separate weights to assure a

representative sample) into a digestion tube. Use 1 gram for dry solids, 5 grams for

dewatered sludges and 25 grams for watery sludges. Record the mass of each sample

used on the mercury page of the digestion log.

6) After samples and standards are prepared, add1 mL of DI to each tube. Add 1.5 ml of

Aqua regia and mix thoroughly. Heat 10 min in 950C block digestor then allow to cool.

7) Add 4.0 mL Potassium Permanganate to each tube. Mix thoroughly. Allow to sit for

15 minutes. If purple color does not persist then add an additional 3.0 mLs Potassium

Permanganate to each tube. If it fades again repeat process with less sample.

8) Place in block digestor for 30 minutes at 950

C covered loosely with green caps.

9) Remove bottles from block and cool for 20 min. Add 2.0 mls Reductant #1 to each

tube, and swirl until all purple particles are gone. Bring all samples back to 40mls

volume with 5% nitric acid.

10) Allow samples to cool to room temperature, filter, and dilute (using digested blank)

before analysis.

Analysis:

1) Turn on the Argon carrier gas should be set for 52 Psig.

2) Switch on the FIMS

3) Allow Hg lamp to warm-up at least one-half hour before use.

4) Switch on the computer, start windows then Winlab 32

5) Verify that tubing configuration is correct.

6) Set the argon gas flow to 70-100 mls per minute.

7) Remove the reductant and carrier tubes from DI

8) Fill SnCl2 (reductant) and 3%HCl ( carrier) solutions and empty waste containers

9) Place the carrier tube ( yellow/blue) into the carrier solution 3% HCL

10) Place the reductant tube ( red/red) into the SnCl2 reductant solution.

11) Check for cleanliness. If tubes are dirty, replace before analysis.

12) Swing the pump pressure levers over the and press the pump tube magazines against the

rollers.

13) Under Toolbar: Open Method and select mercury method

14) Under Toolbar: select HG
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15) Enter Sample Info.: Name the file.

16) Enter sample information for each autosample location starting at location 8

17) Save sample information file

18) Under Tools: Open Automated Analysis Control: Under Select Sample Info. select

Location: enter location of sample tubes to be analyzed.(i.e. 8-20)

19) Open: Results Data Set update the file name where you plan to save the data.

20) Open Peak display, Calibration display, and Results display to ensure run quality.

21) Under Analysis open Rebuild List then select Analyze All

22) Autorun sequence begins.

23) Insure that there is not an excessive amount of foam in the gas/liquid separator during

analysis.

24) When analysis is complete, place all three tubes back in DI for five minutes and then air

dry for 5 minutes.

25) Shut off power to FIMS and release tubes from pump rollers.

26) Place the carrier and reductant tubes in DI water.

X. Calibration:

A. Calibration is performed by analyzing a series of digested standards from zero to

4ppb. The Perkin Elmer Windlab 32 software will then prepare a calibration curve by

plotting instrument response versus standard concentration. The calibration line may

be digested or undigested. For an undigested line, follow the digestion procedure

listed in IX and omit step #9.

B. A digested calibration line is often stable for several weeks.

C. For instrument operating conditions refer to the following from Method Editor:

Method Hg 7471

Spectrometer

Element : Hg Wavelength (nm) : 253.7

Signal

Type : AA Measurement : Peak height Smoothing : 9pts

Read Parameters

Time 20 sec Delay Time 0.0sec BOC Time 2sec

Replicates ...Same for all Samples : 2

Operation

Sample volume 500ul Use Amalgam? No

Step Time Pump1 Pump2 Valve Remotes

(sec) speed speed position 2 3 4 5 6 7 8 9 10

Prefill 15 120 0 Fill

1 10 120 0 Fill

2 15 120 0 Inject
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Read Step 2 Steps to repeat 1 to 1 Number of repeats 0

Wash Frequency : After all solutions Wash Location : 0

Normal Cycles : 1 Use FIAS steps : 1 to 1

Equation : Linear, calculated intercept Max Decimal places : 3 Max Sig. Figs. ; 4

Cal. Units ; ug/L Sample Units ; ug/L

ID Concentration A/S Loc

Calib Blank Calib. Blank 1

Standard 1 Calib Standard 1 0.5 2

Standard 2 Calib Standard 2 1 3

Standard3 Calib Standard 3 2 4

Standard4 Calib Standard 4 4 5

When opening this method manually: clear cal. Curves and construct new cal. Curves

When using this method in a multimethod sequence: start by constructing new cal. Curves

Check: Samples, QC samples

Limits:

Precision check signal : Conc. (cal. units)

Signal Limits : 1.00ug/L

If signal > limit and RSD 20% then action

Out of Limit actions : Reanalyze 1 time

Check Range on : Samples, QC Samples

Overcal. Limit : 110% of cal. Range Take action after 1 replicate

Alternate Method : Hg

A/S Count as Subtract

QC Sample ID Loc Sample Reagent Blk

QC1 ICV 2ppb 4 No No

QC2 ICB 6 No No

QC3 LFB 2ppb 7 No No

QC4 CCV 2ppb 4 No No

QC5 CCB 6 No No

QC1 ICV 2ppb Conc. 2 Lower limit 1.8 Upper limit 2.2

QC2 ICB Conc. 0 Lower limit –2 Upper limit 1

QC3 LFB 2ppb Conc. 2 Lower limit 1.8 Upper limit 2.2

QC4 CCV 2ppb Conc. 2 Lower limit 1.8 Upper limit 2.2

QC5 CCB Conc. 0 Lower limit –2 Upper limit 1

After After

QC Sample ID Init. Cal Recal Periodic Freq At End

QC1 ICV 2ppb Yes Yes No 10 No
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QC2 ICB Yes Yes No 10 No

QC3 LFB 2ppb Yes Yes Yes 20 No

QC4 CCV 2ppb No No Yes 10 Yes

QC5 CCB No No Yes 10 Yes

Frequency : Variable

Count : Samples

When QCs fail : Times to retry – 1

When all Tries Fail – Recal and repeat after trouble shooting.

XI. Data Reduction:

Insure that any dilutions are factored into the final result.

Solid samples are reported as mg/kg, dry wt. The calculations may be performed using an

Excel spreadsheet. The calculation is as follows:

 (Conc. in PPM)(Vol. In L)(1000) = Mg/Kg, dry wt.

 (% Solid)(Mass in G) 

XII. Data Recording:

1. All analyses are recorded on the Mercury page of the Metals Digestion Log Each log

sheet should include the sample reference number, analyst’s name, and concentrations for

standards, LFB’s, and LFM’s

2. Record final data in the LIMS databank.

3. Raw data is stored in the binder labeled “AA Metals” located in the Inorganics

laboratory.

4. For long-term storage, data is stored in a banker’s box labeled “AA Raw Data”.

5. Data from the hard drive C is backed up onto the partitioned D drive

XIII. Instrument Maintenance:

A. Refer to instruction manual for preventative maintenance procedures for the Perkin

Elmer FIMS.

B. Replace sample and reagent tubes on when they appear discolored or worn.

C. Quarterly check gas supply for leaks. 

D. Record any maintenance performed in the maintenance log.

XIV. Troubleshooting:

A. If condensation is present in the flow cell, install and turn on a heat lamp over spec. to

facilitate approximately a 10ο

C rise in the ambient temperature in the cell.

B. Filter soil samples to prevent a clog in the sample line, using a 2.0 um Teflon fiber filter.

C. Rinse sample line thoroughly with DI between high samples
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D. There should be gentle bubbling in the gas-liquid separator. If not, disconnect the inlet

line to the absorption cell, allow the separator chamber to fill up with DI, then re-attach

inlet line. Still no bubbling, remove inlet line and clean out with compressed air.

E. If contamination is suspected compare the EHT voltage on the optimization page with the

original value from the beginning of the run. An elevated voltage indicates that there is

Hg in the system.

XV. References

Method 7471A: Mercury in Solid or Semisolid Waste (Manual Cold-Vapor Technique)

Revision 1,September 1994, EPA Test Methods for Evaluating Solid Waste Physical/

Chemical Methods, Version 2. EPA SW 846, December 1997 United States

Environmental Protection Agency.

Electronic Code of Federal Regulations, 40 CFR – Chapter 1 – Part 136 – Appendix B. :

Definition and Procedure for the Determination of the Method Detection Limit –

Revision 1.11.

XVI. Revision History

May 14, 2003

March 26, 2004

April 17, 2006

XVII. Method Modifications/Analyst Notes:
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XVIII. SOP Attestation

I acknowledge that I have read this Standard Operating Procedure and agree

 to adhere to the Safety and Quality Control policies outlined within.

Name Date

 
 Cyanide EPA 335.4 / 9012A 

Revised 04-May-10 Rev#6 

 Created: 21-Sep-04 

Page 1 of 1616

Controlled Document - DO NOT PHOTOCOPY 

Standard Operating Procedure 

Cyanide

Distillation Method EPA 335.4 

Potable & Non-Potable Water Method EPA 335.4 

Total Cyanide in Solids EPA 9012A 

Solid Samples Prep Method 9010B 

Revision: 6 

Endyne, Inc. 

315 New York Road, Suite 85 

Plattsburgh, NY 12903 

Approved for Distribution:_______________________________ 

Approval Date:_______________________________ 

Out of Service Date:________________________ 
 Cyanide EPA 335.4 / 9012A 

Revised 04-May-10 Rev#6 

 Created: 21-Sep-04 

Page 2 of 1616

Controlled Document - DO NOT PHOTOCOPY 

1. Identification of Test Method 

METHOD #: EPA 335.4, 9012A 

TITLE: Cyanide 

ANALYTE: Free and Total Cyanide 

INSTRUMENTATION: Seal AQ2 Discrete Analyzer, Midi-Dist Distillation 

Apparatus

2. Applicable Matrix: 

2.1. This method is applicable to the concentration of Free and Total Cyanide 

in drinking and surface waters, domestic and industrial wastes, and 

solids. 

3. Method Detection Limit:

3.1. See Methods Manual Appendix A for current MDL and PQL numbers. 

4. Scope and Application, Components: 

4.1. This method covers the determination of cyanide in drinking, surface and 

saline waters, domestic and industrial wastes, and solids. 

4.2. The method is based upon reactions that are intended to be specific for 

cyanide.

5. Summary of Test Method: 

5.1. This method is the Endyne-Plattsburgh adaptation of methods EPA 335.4 

and EPA 9012A. 

5.2. The midi-distillation system is used to process Total Cyanide samples 

prior to their analysis in the AQ2 discreet analyzer. 

5.3. In the distillation process, cyanide as hydrocyanic acid (HCN) is released 

from cyanide complexes by means of a reflux-distillation operation and 

adsorbed in a scrubber containing sodium hydroxide solution. The 

cyanide ion in the absorbing solution is then determined colorimetrically 

on the AQ2. 

5.4. In the colorimetric determination, cyanides are converted to cyanogen 

chloride by reaction with chloramine-T (N-Chloro-p-toluenesulfonamide 

sodium salt). The cyanogen chloride then reacts with pyridine and 

barbituric acid to form a reddish-violet colored complex. The absorbance 

of this complex is measured spectrophotometrically at 578 nm. 

6. Definitions: 

6.1. CYANIDE – Cyanide (CN) ion and complex cyanides converted to 

hydrocyanic acid (HCN) by reaction in a reflux system of a mineral acid 

in the presence of magnesium ion. 

6.2. FREE CYANIDE – The fraction of cyanide that is reactive prior to 

the distillation step. Samples analyzed for SDWA compliance monitoring 

are reported as free cyanide. 
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6.3. BATCH – Environmental samples that are prepared and/or 

analyzed together with the same process and personnel, using the same 

lot(s) of reagents. 

6.4. PREPARATION BATCH – A set of samples composed of one to 20 

environmental samples of the same NELAC-defined matrix, meeting the 

above-mentioned criteria and with a maximum time between the start of 

processing of the first and last sample in the batch to be 24 hours. The 

preparation batch determines the frequency of the quality control sample 

to be processed. 

6.5. ANALYTICAL BATCH – A set of samples composed of prepared 

environmental samples (extracts, digestates, or concentrates) which are 

analyzed together as a group. An analytical batch can include prepared 

samples originating from various environmental matrices and can 

exceed 20 samples. 

6.6. CALIBRATION BLANK (CB) – A volume of reagent water in the 

same matrix as the calibration standards, but without the analyte. 

6.7. CALIBRATION STANDARD (CAL) – A solution prepared from the 

primary dilution standard solution or stock standard solutions. The CAL 

solutions are used to calibrate the instrument response with respect to 

analyte concentration. 

6.8. METHOD BLANK (MB) – An aliquot of reagent water or blank 

matrices that are treated exactly as a sample including exposure to all 

glassware, equipment, solvents, reagents, internal standards, and 

surrogates that are used with all other samples in the batch. The MB is 

used to determine if method analytes or other interferences are present 

in the laboratory environment, the reagents, or the apparatus. 

6.9. LABORATORY CONTROL STANDARD (LCS) (however named, 

such as laboratory fortified blank, spiked blank, or QC check sample) – A 

sample matrix, free from the analytes of interest, spiked with verified 

known amounts of analytes or a material containing known and verified 

amounts of analytes. It is generally used to establish intra-laboratory or 

analyst specific precision and bias or to assess the performance of all or 

a portion of the measurement system. 

6.10. LABORATORY DUPLICATES (LD) – Aliquots of a sample taken 

from the same container under laboratory conditions and processed and 

analyzed independently. Analysis of laboratory duplicates indicates 

precision associated with laboratory procedures but not with sample 

collection, preservation, or storage procedures. 

6.11. QUALITY CONTROL CHECK SAMPLE (QCS) – A sample 

containing analytes of interest at known concentrations (true values). 

The QCS is obtained for a source external to the laboratory or is 
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prepared from standards obtained from a different performance using 

test materials that have been prepared independently from the normal 

preparation process. 

6.12. METHOD DETECTION LIMIT (MDL) – A statistical calculation of 

the lowest concentration at which an analyte can be detected with 99 

percent confidence that the analyte concentration is greater than zero. 

6.13. MINIMUM LEVEL (ML) – The lowest standard used in the 

calibration.

6.14. MAXIMUM CONTAMINANT LEVEL (MCL) - The highest level of a 

contaminant that is allowed in drinking water. MCLs are set as close to 

level at which there are no known or expected health risks as feasible 

using the best available treatment technology and taking cost into 

consideration. MCLs are enforceable standards.

7.0. Interferences: 

7.1. Thiocyanates are a positive interference. 

7.2. Oxidizing agents, such as chlorine, decompose most of the 

cyanides. Test the sample with potassium iodide – starch paper. A 

blue color indicates the need for treatment with ascorbic acid. If 

needed, add ascorbic acid one crystal at a time until the sample yields 

no color change. Add an additional 0.06g of ascorbic acid for each liter 

of sample. This step should be done in the field during sample 

collection. 

7.3. Sulfides adversely affect the colorimetric procedure. If a drop of the 

sample on lead acetate test paper indicates the presence of sulfide, 

treat 25 mL more of the stabilized samples (pH>/=12) than that required 

for the cyanide determination with powdered cadmium carbonate. 

Yellow cadmium sulfide precipitates if the sample contains sulfide. 

Repeat this operation until a drop of the treated sample solution does 

not darken the lead acetate test paper. Filter the solution through a dry 

filter paper into a dry beaker and, from the filtrate, measure the sample 

to be used for analysis. Avoid a large excess of cadmium and a long 

contact time in order to minimize a loss by complexation or occlusion of 

cyanide. Record the treatment in the cyanide logbook. (NOTE: The 

sample may alternatively be subcontracted to another ELAP accredited 

lab to be treated for the interference and analyzed).

8.0. Safety: 

8.1. Safety glasses, gloves and labcoat are required. The toxicity or 

carcinogenicity of each reagent used in this method has not been fully 

established. Each chemical should be regarded as a potential health 

hazard and exposure should be as low as reasonably achievable. 

Cautions are included for known extremely hazardous materials. 
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8.2. A reference file of Material Safety Data sheets (MSDS) is available 

to all personnel involved in the chemical analysis. A formal safety plan 

is also available. 

8.3. The following chemicals have the potential to be highly toxic or 

hazardous, for detailed explanations consult the MSDS. 

Chloramine-T: causes burns, sensitization by inhalation, contact 

with acids liberates very toxic gas 

Pyridine: highly flammable, toxic by ingestion, inhalation, and 

skin contact 

Cyanide standards: toxic, contact with acids liberates toxic gas 

Barbituric Acid: irritating to eyes, skin, and respiratory tract 

Hydrochloric Acid: causes severe burns 

Sodium Hydroxide: causes severe burns 

9.0. Equipment and Supplies: 

9.1. Analytical balance capable of accuracy to the nearest 0.0001 g. 

9.2. Glassware - Class A volumetric flasks and pipettes. Glass or plastic 

containers as required. 

9.3. SEAL AQ2 discrete analyzer with Test and Reagent Parameters 

programmed for this cyanide application. 

9.4. Reflux distillation apparatus consistent with sample pre-treatment 

procedure described in USEPA method 335.4. 

10.0. Reagents and Standards: 

10.1. PREPARATION OF REAGENTS: Use of ASTM Type II water for all 

solutions. All standards and reagents must be prepared using 

ammonia-free water. 

10.1.1. Collection Reagents: 

10.1.1.1. Ascorbic Acid: Crystal (CASRN-50-81-7) 

10.1.1.2. 10N Sodium Hydroxide: Place a 500mL volumetric flask in 

a cold water bath in a fume hood. Turn on the hood. Add 

250mL of deionized water to the flask. Add 200g of solid 

NaOH to the deionized water in the flask. Swirl to mix. 

After the solution has cooled and the NaOH has dissolved, 

fill the flask to volume with deionized water. Invert to mix. 

10.1.1.3. Cadmium Carbonate: Powdered (CASRN- 513-78-0) 

10.1.2. Distillation Reagents: 

10.1.2.1. 0.25 N Sodium Hydroxide (see section 10.1.3.1.) 

10.1.2.2. Sulfamic Acid (NH2SO3H): (CASRN-212-57-3) 

10.1.2.3. 18N Sulfuric Acid (1:1): Place a 500mL volumetric flask in 

a cold water bath in a fume hood. Turn on the hood. With 
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a graduated cylinder, add 250mL of deionized water to the 

flask. With a graduated cylinder, slowly add 250mL of 

concentrated sulfuric acid to the flask, swirling 

occasionally. The flask will get very hot and water will 

evaporate. After the flask has cooled to room temperature, 

add deionized water to bring the volume up to 500mL. 

Invert to mix. Store at room temperature in a glass 

stoppered glass container. 

10.1.2.4. Magnesium Chloride Solution: Weigh 51g of Magnesium 

Chloride crystals into a beaker. Rinse the crystals into a 

100mL volumetric flask using a funnel and deionized water. 

Bring to 100mL volume. Invert to mix. Store at 4C in a 

plastic container. 

10.1.3. AQ2 Reagents: 

10.1.3.1. Sodium Hydroxide, 0.25 N: From a stock solid NaOH: 

Dissolve 20g of NaOH in 2L of DI water. Invert to mix. 

Caution: This solution will get hot during mixing. 

From a traceable 10N NaOH solution: Pipette 25mL of 

10N Sodium Hydroxide into a 1L volumetric flask. Bring to 

volume with deionized water, cooling in an ice bath as the 

water is added. Invert to mix. 

10.1.3.2. Phosphate Buffer: Dissolve 138 g of sodium dihydrogen 

phosphate in 900 mL deionized water and dilute to 1 Liter. 

Refrigerate this reagent. 

NOTE: This reagent may be purchased ready to use from 

EST Analytical. 

10.1.3.3. Chloramine-T: Dissolve 1.0 g of chloramine-T (N-Chlorop-toluenesulfonamide sodium salt) in 100 mL deionized 

water. Prepare fresh daily. 

NOTE: This reagent may be purchased ready to use from 

EST Analytical. 

10.1.3.4. Pyridine Barbituric Acid: Place 3.75 g of barbituric acid in 

a 250 mL volumetric flask and add just enough deionized 

water to wash the sides of the flask and wet the barbituric 

acid. Add 18.75 mL of pyridine and mix. Add 3.75 mL 

concentrated hydrochloric acid, mix and cool to room 

temperature. Dilute to 250 mL with deionized water and 

mix well to ensure complete solution of the barbituric acid. 

Stored in a dark bottle at a cool temperature, this solution 

should be stable for up to 6 months. THIS REAGENT 

MUST BE PREPARED IN A FUME CUPBOARD – TAKE 

EXTREME CARE! 

NOTE: This reagent may be purchased already prepared. 
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NOTE: For lowest detection limits, chill the pyridine 

barbituric acid reagent and perform gravity filtration at the 

time of use.

10.2. PREPARATION OF STANDARDS: 

10.2.1. Stock standard solution (1000 mg CN/L): Dissolve 2.51 g of 

potassium cyanide and 2.0 g of potassium hydroxide in 900 mL 

of deionized water and mix. Dilute to 1 Liter in a volumetric flask. 

If necessary, standardize with 0.0192N silver nitrate to 

appropriate concentration (1 mL = 1 mg CN). 

NOTE: A traceable stock 1000mg/L cyanide standard may be 

purchased ready to use. 

10.2.2. Intermediate stock standard solution (1 mg CN/L): Dilute 1 

mL stock standard (1000 mg CN/L) to 1 Liter with 0.25N NaOH 

reagent. 

10.2.3. Preparation of Working standard solutions: 

Concentration μg CN/L 0 1 4 10 25 50 75 150 200 250 

Volume (mL) Intermediate 

stock standard diluted as 

indicated with deionized 

water 

0 1 1 1 25 25 15 150 20 25 

Final Volume, mL 100 1000 250 100 1000 500 200 1000 100 100 

Note: Working standards are to be brought to volume using 0.25N NaOH.

11.0. Sample collection, preservation and storage: 

11.1. Samples should be collected in plastic bottles. All bottles 

must be thoroughly cleaned and thoroughly rinsed to remove 

soluble material from containers. Sample volume must be large 

enough to treat the samples for interferences as needed and 

analyze the sample with all applicable quality control parameters. 

The recommended sample size is 1L. 

11.2. Oxidizing agents such as chlorine decompose most of the 

cyanides. In the field, test a drop of the sample with potassium 

iodide-starch test paper (KI starch paper); a blue color indicates the 

need for treatment. Add ascorbic acid, a few crystals at a time, until 

a drop of sample produces no color on the indicator paper. Then 

add an additional 0.6 g of ascorbic acid for each liter of sample 

volume. The sample may then be preserved with sodium 

hydroxide. 

11.3. Samples must be preserved with 2 ml of 10N sodium 

hydroxide per liter of sample (pH ≥12) at time of collection. 

11.4. Samples should be analyzed as rapidly as possible after 

collection. If storage is required the samples must be stored in a 
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refrigerator or in an ice chest filled with water and ice to maintain 

temperature at <= 6C. Samples must be analyzed within 14 days. 

11.5. Solid samples are collected in plastic or glass containers and 

must be chilled to 4C until analysis. 

12.0. Quality Control: 

12.1. Analyze one sample duplicate and one matrix spike per 

preparation batch or 10% of samples, whichever is more frequent. 

Duplicate determinations must agree within 20% of each other. 

Matrix spike recoveries must be 80-120%. Note: Matrix spikes that 

fall outside the acceptance criteria require that only the spiked 

sample be qualified as this problem is matrix or solution related, not 

system related. 

12.2. One CCV (Continuing Calibration Verification) must be run 

with each batch. The CCV concentration must agree within 10% of 

its acceptable value. In addition, a distilled standard (or lab-fortified 

blank) must be analyzed with each batch. The distilled standard 

must be within 10% of its non-distilled value. 

12.3. One QC (Quality Control) sample must be run with each 

batch. The QC is distilled with the preparation batch. The value 

must fall within its acceptable range. 

12.4. A lab blank must be distilled with the preparation batch and 

the value must be below the PQL. Blank results greater than the 

PQL indicate a possible source of contamination. 

13.0. Calibration and Standardization: 

13.1. The standard curve is a 2nd order polynomial equation. A 

minimum correlation coefficient of 0.995 must be achieved to 

accept the calibration. If this value is not achieved, the analytical 

system is judged to be out of control, and the problem must be 

immediately identified and corrected. 

13.2. The initial calibration must be verified using a second source 

or certified standard that has a concentration within the calibrated 

range. Compute the percent recovery using the following equation: 

% x 100

K

D

recovery =

13.3. Where, D = Determined concentration of analyte in the 

calibration standard, K = actual concentration of the analyte in the 

calibration standard 

13.4. Verify the calibration using a calibration standard every ten 

samples or every analytical batch. 
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13.5. If % recovery of calibration verification falls outside the +

10% acceptance limit, the analytical system is judged to be out of 

control, and the problem must be immediately identified and 

corrected and the analytical batch reanalyzed. 

13.6. At least one standard should be taken through the distillation 

process with each batch. The distilled and undistilled standard 

must be within 10% of each other. 

14.0. Procedure: 

14.1. Midi-Distillation: NOTE: Drinking water samples to be 

reported for SDWA compliance monitoring, skip to section 

14.2. 

14.1.01. Pour 50mL of sample into the reflux flask (the back row of 

tubes). Samples may be diluted by pipetting the sample 

volume then bringing the tube up to a total of 50mL with 

deionized water. For solid samples use 1 g of sample and fill 

the tube up to 50mL with deionized water. Record the weight. 

14.1.02. Pour 50mL of 0.25N NaOH into the absorber flask (the front 

row of tubes). 

14.1.03. Add 3 glass boiling beads and 2 drops of antifoam to the 

reflux flask. Repeat steps 14.2.01 to 14.2.03 for each sample. 

14.1.04. Assemble the reflux impinger, absorber impinger, and 

tubing. 

14.1.05. Turn on the cold water tap to the cold fingers, keep the water 

at a higher flow than will be required for the distillation. 

Starting at the left-most side of the Midi-Dist apparatus, hold 

each cold finger parallel with the block and jiggle it lightly to 

remove air bubbles. After air bubbles are removed, assemble 

the cold finger and repeat the process, moving to the right, for 

the rest of the tubes. After all air bubbles are removed adjust 

the flow down to the level required for the distillation. Set the 

flow at 6 GPH per sample (per block). The tubing is split such 

that each block will read the flow for the samples in that block 

only. 

14.1.06. Turn on the vacuum pumps. Adjust the vacuum valves to 

obtain approximately 3 bubbles/second in the reflux flask. 

Allow vacuum draw for at least 5 minutes. Note: the vacuum 

may need to be slightly higher for solid samples so that the 

solids are suspended in the reflux flask.

14.1.07. To reduce interferences from nitrate and nitrite, add 0.2 g of 

sulfamic acid through the air inlet above the reflux flask. Rinse 
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down with a small amount of water. Let the flask bubble for 3 

minutes. 

14.1.08. Inject 5 mL of 18N Sulfuric Acid through the air inlet above 

the reflux flask. Rinse down with a small amount of water. Let 

the flask bubble for 5 minutes. 

14.1.09. Inject 2 mL of magnesium chloride solution through the air 

inlet. Rinse down with a small amount of water. Repeat if 

foaming occurs. 

14.1.10. For the LabCrest Midi-Dist, turn on the red rocker switch and 

turn the dial to 105. For the Glastron Midi-Dist, turn on the 

heating mantle. The timer has been programmed to ramp the 

temperature to 150C in 10 minutes, hold that temperature for 1 

1⁄2 hour and then turn off the heat. At the end of the run the 

unit will shut off. Leave the samples in the block for another 

15 minutes with the vacuum and cooling fingers on. 

14.1.11. Close each valve, disconnect the absorber, then starting at 

the right open the valve to draw all solution from the frit. Close 

valve and remove frit. 

14.1.12. After the Midi-Dist apparatus have cooled to below 100C 

disconnect the reflux flask from the absorber flask. Place the 

impingers in a tote of tap water to be washed. Turn off the 

vacuum valves for each position. Turn off the vacuum pumps. 

Turn of the cold water tap to the cold fingers. 

14.1.13. Collect the samples from the absorber flasks. This solution 

is now ready for analysis. If the samples will not be analyzed 

immediately they must be stored at <=6C until analysis. 

14.1.14. For solid samples being reported on a dry-weight basis, 

weigh approximately 5g of sample into a pre-dried, preweighed crucible. Place in a drying oven at 103C until a 

constant weight is reached. Calculate the percent solids of the 

sample. Note: The sample used must be a different aliquot 

than that used for the CN determination.

14.2. AQ2 Analysis: 

14.2.01. All parameters necessary to run calibration standards, 

QC's and unknown samples for this method are preprogrammed in the AQ2 software. 

14.2.02. The AQ2 analyzer's computer and software serve to 

control and monitor all mechanical functions, 

mathematical computations, sample data storage and 

report generation. 
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SCHEDULING:

14.2.03. Open a new schedule and select the WW reagent set. 

In the column labeled “type” skip rows 1, 2 and 3 (these 

are pre-programmed into the method to be the curve 

standard and undistilled CCB and CCV). In row 4 enter 

your method blank as “MB”. This is the start of the 

distilled preparation batch. 

14.2.04. In the column labeled “Sample ID” in rows 5 and 6 

enter the distilled CCV (as “CCV xx mg/L”) and the 

second source QC (as “QC#xxxxxx”). The “type” column 

will show “u1” and “u2” indicating that the CCV and QC 

will be treated as AQ2 unknowns. This guarantees that 

the standards will be treated the same as the samples. 

14.2.05. Starting in row 7 enter each sample, including 

duplicates and matrix spikes, as unknowns. After all 

samples are entered, highlight the column “Requested 

tests” to the right of each scheduled sample and 

standard. Select the test cyanide by clicking on “CN” in 

the test box above the schedule. 

14.2.06. Save the schedule: Click “file” at the top left-hand 

side of the screen. Click “save”. If any piece of the 

schedule is missing (ie. Forgot to select a test) then a 

prompt will show up asking if you really want to save. 

Cancel the save and fix the problem. Note: If you click 

save with pieces missing all or part of your schedule will 

disappear and you will have to start over. 

14.2.07. Place the standards and samples into a sample wheel 

according to the location in the schedule. Each 2mL 

sample cup must be completely filled. Place the sample 

wheel on the AQ2 and tighten the lock in the center of the 

wheel. 

SETUP: 

14.2.08. Replace any used reaction segments. Fill the 

deionized water reservoir. Empty waste containers. 

Place the waste tubing into the empty glass waste 

container. (CN AQ2 waste must be entered into the 

cyanide waste container after each run). 

14.2.09. The reagents are to be placed into their reagent 

wedges and placed on the AQ2 as follows: 

 Pyridine-Barbituric Acid: Reagent Wedge 11 

 Phosphate Buffer: Reagent Wedge 9 
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 Chloramine-T: Reagent Wedge 10 

 0.25N NaOH: Reagent Wedge 1 

 RUN: 

14.2.10. Double click on the “RUN” icon at the top left-hand 

side of the screen. Select the cyanide schedule from the 

list of trays and click “OK”. 

14.2.11. Check the box for “set tube counter to zero”. Click 

“OK”. The run will start. 

14.2.12. The AQ2 will analyze the samples in the order that 

they are on the screen. Samples that are over the 

calibration range will be rescheduled at a dilution (dilutes 

with 0.25N NaOH from reagent wedge 1) then ran again 

at the end of the run. If samples are auto-diluted in this 

manner they will show up blue on the screen. If any 

samples are auto-diluted then the last CCV and CCB on 

the run must be manually rescheduled after the run has 

been completed in order to bracket the diluted samples. 

Samples that remain over range must be rescheduled 

with a manual dilution with 0.25N NaOH. The run must 

always end with a CCV and CCB set. 

14.2.13. After the run is complete, the prompt at the top lefthand side of the screen will show “Finished” in red. 

Assess the quality controls. To accept the run, click the 

“acceptance” icon along the left-hand side of the screen. 

Select the cyanide run. Click “Accept All”. A prompt will 

show up asking if you want to permanently accept the 

run. Accept the run and a screen will open with the 

printable results for the bench notebook.

For information regarding analyzer maintenance and 

troubleshooting refer to the relevant sections of the Operator 

Manual. 

14.3. Cleanup: 

14.3.01. Distillation flasks are cleaned in the Miele glassware 

washer. Glass beads are washed by hand in the sink 

then dried and re-used. 

14.3.02. The reflux impingers and absorber impingers are 

soaked in hot tap water. Change the water each time it 

cools for at least 3 cycles, being careful to remove the 

water from the tubes between each step. After 3 washes 

with hot tap water, rinse the impingers well with flowing 

hot tap water then place them into a tub of deionized 
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water over night. In the morning, drain the water from the 

impingers and allow them to dry completely before 

putting the apparatus back together. 

NOTE: The tubes and impingers must be periodically 

acid washed to remove staining and other residue. Acid 

washing is completed with HCl or H2SO4 and tap water. 

The acid wash sign MUST be posted above the sink 

during acid washing. 

NOTE: The tubes and impingers do not have to be dried 

completely if they are going to be used again immediately 

after the cleaning process. 

14.3.03. The distillation blocks may be cleaned with damp 

paper towels. Check the system for leaks and damage 

after each run. 

14.3.04. The AQ2 has an automatic cleaning process at the 

shutdown of each run. The AQ2 waste must be emptied 

into the cyanide waste container. Rinse the container 

into the waste with a small amount of water. Follow the 

end-of-day prompts to shutdown the equipment for the 

night. 

15.0. Calculations: 

15.1. AQ2 Results are reported in ug CN/L. 

15.2. Sample results that fall below the practical quantitation limit 

(PQL), must be reported as <. 

15.3. Results entered into LabTask must be converted from ug/L 

to mg/L and reported as mg/L CN. 

15.4. The EPA Maximum Contaminant Level (MCL) is 0.2 mg/L 

(posted on the EPA website http://www.epa.gov/safewater/contaminants/index.html). 

15.5. For solid samples, calculate the result in mg/Kg (dry weight 

basis) based on the weight used in the distillation. The EXCEL 

spreadsheet for the calculation is saved on the server at: 

\\Server1\public\1 Plattsburgh Lab Task\Cyanide Solids.XLS. The calculations page 

must be printed and filed with the q-list. 

Calculation: mg/kg dry = (mg/L x final vol (L) x 1000)

 (mass (g) x %s as a decimal) 
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16.0. Method Performance: 

16.1. Studies to determine the Method Detection Limit (MDL) and 

Practical Quantitation Limit (PQL) are completed at least annually 

per SAP EL00029. 

16.2. Proficiency testing is completed at least twice annually per 

SAP EL0047 and passing the best two out of three is required. 

16.3. Tracking of the quality control results is completed with each 

run. 

17.0. Pollution Prevention: 

17.1. Completed samples that contain no cyanide are disposed of 

via the sanitary sewer. 

17.2. Leftover sample volume is stored in the sample archive 

fridge for 1 month. Samples that contain no cyanide can be 

disposed of via the sanitary sewer. Samples that contain cyanide 

are labeled “Contains Cyanide Do Not Dump” (go to 17.5.01). 

17.3. Expired hydrochloric acid and sodium hydroxide are 

neutralized and disposed of via the sanitary sewer. 

17.4. AQ2 waste is stored in the waste chemical disposal area 

until in can be disposed of as hazardous waste by a certified waste 

disposal company. 

17.5. Expired cyanide standards, quality control standards, and 

samples containing cyanide are stored in the “waste storage” area 

until they can be reacted with household bleach then disposed of 

via the sanitary sewer. 

17.5.01. To treat cyanide samples or standards, place the 

sample in a beaker in the fume hood. While stirring, add 

sufficient chlorine to maintain a chlorine residual. Check 

for the presence of chlorine with KI-starch indicator strips. 

Allow standards to remain in the hood for at least 1 hour. 

Check again for chlorine. If chlorine has dissipated, add 

more chlorine and repeat the process. Once a chlorine 

residual has been maintained for 1 hour, flush the sample 

down the fume hood drain with copious amounts of 

water. 

17.6. Samples treated with cadmium carbonate must be stored 

and disposed of as hazardous waste. 

18.0. Data Assessment and acceptance criteria: 

18.1. Quality control parameters must be met. See section 12. 

19.0. Corrective action for out-of-control data: 

19.1. Check reagents. 

19.2. Check for proper heating of the Midi-Dist sample tubes. 
 Cyanide EPA 335.4 / 9012A 

Revised 04-May-10 Rev#6 

 Created: 21-Sep-04 

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19.3. Complete the AQ2 troubleshooting and maintenance. 

20.0. Contingencies for handling out-of-control data: 

20.1. Repeat the analysis. 

21.0. Waste Management: 

21.1. Refer to SAP# EL0005 

22.0. References: 

22.1. Methods for Chemical Analysis of Waters and Wastes, U.S. 

Environmental Protection Agency: Method 335.4, Rev.1, 1993. 

22.2. Total Cyanide in Drinking, Saline and Surface Waters, and 

Domestic and Industrial Wastes, SEAL Method NO:EPA-130-A Rev 

3, USEPA Method 335.4, Range 3-250 ug CN/L, Revision Date: 01-

Jun-05. 

22.3. Total Cyanide in Drinking, Surface and Groundwater and 

Wastewater, Endyne Inc - Randolph Lab (formerly SciTest), SOP 

No. IC-024, Revision 5.0, Date: 3/8/2006. 

22.4. Andrews Glass Company LabCrest ® Midi-Dist TM Cyanide 

Distillation System Model 110-10 Operation Manual, Andrews 

Glass Company, EP Document #3100. 

22.5. Glastron TM Instruction Manual Enviro Midi-Dist Distillation 

System, Glastron Inc. 

22.6. EPA Method 9010B, Total and Amenable Cyanide: 

Distillation, Revision 2, December 1996. 

22.7. EPA Method 9012A, Total and Amenable Cyanide 

(Automated Colorimetric, with offline distillation), Revision 1, 

December 1996. 

23.0. Tables, diagrams, flowcharts and validation data: 

23.1. TEST PARAMETERS for the up to 2.5 mg CN/L RANGE

PARAMETER AQ2 SETTING 

Test Name CYANIDE 335.4 

Chemistry type End point 

Decimals 3 

Units ug/L 

Number of mixes 1 

Reaction time (seconds) 480 

Sample volume (μL) 250 

Water volume (μL) 0 
 Cyanide EPA 335.4 / 9012A 

Revised 04-May-10 Rev#6 

 Created: 21-Sep-04 

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Number of reagents 3 

1. Phosphate Buffer (μL) 100 

2. Chloramine-T (μL) 25 

3. Pyridine Barbituric acid (μL) 240 

Reagent 3 Delay (sec) 85 

Filter (nm) 578 

Flowcell wash 2 

Flowcell prime 1 

Polynomial order 1 

Date Tech Revision 

# 

Revisions 

14-Jan-08 CAL 2 Changed to method EPA 335.4, Rev.1, ELAP#9119. Updated 

reagents, distillation procedure, and QC requirements. Added to 

section 7.3 that samples containing sulfide interference may be 

subcontracted. Added section 17.6. 

10-Jun-09 CAL 3 Added references to Free Cyanide – drinking water analyzed for 

SDWA compliance monitoring are reported as free cyanide. 

22-Sep-09 CAL 4 Updated the acceptance criteria for duplicate and matrix spike 

acceptance. Added the use of antifoam to prevent bumping in the 

distillation step. 

10-Mar-10 CAL 5 Added info from methods 9010B and 9012A to include solid 

samples. Added to 14.1.10 and 14.1.11 the process to properly 

disconnect the samples from the unit. 

04-May-10 CAL 6 Added sections 14.1.14 (percent solids determination) and 15.5 

(solids calculation). 

 
ATTACHMENT 6 
 Elemental Analysis of Water and Sludge Samples as 

 Submitted by Endyne, Inc of Williston,Vt. 

1. Samples are logged into our accounting system and assigned a unique identification 

job number. Date received is recorded and a contract review is completed. 

2. Sample preparation:

a. Water samples: The entire Water sample submitted is weighed to three 

significant figures and then digested in the appropriate stabilizing acid for the 

elements of interest (see list below). The digested solution is then brought back to 

the original weight with deionized water. 

b. Sludge samples: A 0.5 gram aliquot of a Sludge sample is weighed to three 

significant figures, in duplicate, and digested in the appropriate stabilizing acid(see 

list below). The digested solution is then diluted to weight to 100 fold with 

deionized water. 

c. Reagent blanks are prepared in the same manner as the samples. 

3. Standards and QC controls: Standards of 0 and 10ppm are prepared for the 

elements of interest in the same acid matrix as the samples. QC Controls are also 

acid matrix matched to the samples and are prepared at 1ppm and 0.1 ppm. All 

standards and controls are prepared weight/weight and are Nist traceable. 

4. Analysis: The samples are then analyzed by ICP-OES on a PE 3300RL instrument 

according to the manufacturer’s specifications. The instrument is calibrated with 

each use for the elements of interest only. Appropriate dilution factors are entered 

into the analysis program so the resulting concentration reported is that of the ‘as is’ 

delivered sample. 

Elements of Interest Stabilizing Acid Elements of Interest Stabilizing Acid 

 Gold Aqua regia(HCL+HNO3) Strontium HNO3 

 Iridium Aqua regia(HCL+HNO3) Tantalum HNO3 + HF 

 Lanthanum HNO3 Tin HCL 

Palladium Aqua regia(HCL+HNO3) Titanium HNO3 + HF 

 Platinum Aqua regia(HCL+HNO3) Zirconium HCL 

Rhodium Aqua regia(HCL+HNO3) 

Note: When analyzing for Pt, the same prep and standards procedure is used as 

for all other elements in this SOP ensuring aqua regia is used as the stabilizing 

acid. The analysis is performed as in step 4, utilizing Pt wavelengths 214.423nm 

and 265.945nm