Field Sampling Reference Guide 

Revision 6.0 - UNCONTROLLED DOCUMENT 

December 1998 

Oregon 

Department bf Environmental Quality 

Laboratory Division 

1712 S.W. Eleventh Avenue 

Portland, Oregon 97201 
Table of Contents 

December 1998 i 

I. INTRODUCTION 1 

II. INFORMATION CONTACTS... 1 

SAMPLING & ANALYTICAL INFORMATION 1 

SAMPLE TRACKER- '. / 

ORGANIC LABORATORY - 2 

INORGANIC LABORATORY - 2 

AIR MONITORING - : 2 

WATER MONITORING - , 2 

BIO-MONITORING- 2 

QUALITY ASSURANCE - ^ '. : 2 

ADMINISTRATION- 2 

m . SAFETY CONSIDERATIONS 2 

DEQ SAFETY COMMITTEE 3 

PORTABLE "SNIFFERS" 3 

CHEMICAL PRESERVATIVES : 3 

Preservatives commonly provided 4 

Material Safety Data Sheets (MSDS) 4 

IV. INVESTIGATIONS 5 

ORGANICS : : '. 5 

VOLATILE ORGANIC COMPOUNDS (VOC) 6 

SEMI-VOLATILE ORGANIC COMPOUNDS (SEMI-VOLs, BNAs) 6 

PETROLEUM IN SOILS 6 

OIL & GREASE : .....6 

Other Organics 6 

INORGANICS 7 

METALS. ; : 7 

NUTRIENTS \ 8 

BIOLOGICAL OXYGEN DEMAND (BOD) 8 

TOXICITY CHARACTERISTIC LEACHING PROCEDURE (TCLP) : 8 

BIOLOGICAL '. 9 

FIELD ANALYSIS 10 

DISSOLVED OXYGEN (DO) '. 10 

ALKALINITY, CONDUCTANCE, PH, ETC. 10 

V. COMPLIANCE INSPECTIONS 10 

NPDES, WPCF ; 10 

SPLIT SAMPLING OF STP'S FOR COMPLIANCE INSPECTIONS 10 

VI. SAMPLING AND ANALYSIS PLAN 12 

ADVANCED NOTICE OF PLANNED SAMPLING ACTIVITY 13 

VII. QUALITY ASSURANCE ., 15 

DEQ LABORATORY SAMPLE ACCEPTANCE POLICY '. 15 

VIII. SAMPLE COLLECTION 16 

WATER SAMPLES '.. k. 17 

Groundwater 17 

Surface water 17 

AIR : :i8 
Table of Contents 

SOIL/SEDIMENT .- 18 

SUSPECT HW CONTAINERS 18 

IX. SUBMITTING SAMPLES, REQUEST FOR ANALYSIS... 19 

REQUEST FOR ANALYSIS FORM .'. 19 

CHAIN OF CUSTODY 22 

FIRST CUSTODY LEVEL •.,.22 

SECOND CUSTODY LEVEL '. '..22 

SAMPLE SHIPMENT : 22 

FIELD NOTEBOOKS : 23 

CORRECTION TO DOCUMENTATION..,.: 23 

APPENDIX A SAMPLING FOR VOLATILE ORGANICS 25 

Contamination 25 

Preparation 25 

Sampling and Documentation '. 25 

Sample Collection ; 25 

APPENDIX B SAMPLING PROCEDURE FOR DISSOLVED OXYGEN .....27 

INTRODUCTION..: „...; ;27 

SAMPLE COLLECTION ^ 27 

SAMPLE PRESERVATION 27 

APPENDIX C FIELD FILTRATION PROCEDURE 29 

APPENDIX D LEGAL SAMPLE CHAIN-OF-CUSTODY PROCEDURE ...31 

Purpose :: ; 31 

Pre-sampling 31 

Sample Collection 31 

Transfer of Custody 32 

Laboratory Custody 32 

References , ;: 35 

APPENDIX E SPIKES, SPIKE DUPLICATES? 35 

Surrogate Spikes 37 

PRESERVATION CODES 41 

CONTAINER CODES 41 
DEQ LAB: Field Sampling Reference Guide December 1998 

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I. Introduction 

The goal of DEQ Lab's Field Sampling Reference Guide is to provide Regional and Program staff with information 

they need to make knowledgeable and efficient use ofthe resources available from the Laboratory Division. 

Laboratory services available include: broad technical capabilities in qualitative and quantitative inorganic, organic, 

microbiological, microscopic, and biological sampling and analyses of air, water, soil, sediment, and tissue; data 

validation, statistical data analysis, and quality assurance; analytical data interpretation; etc. 

The Lab Division is comprised of between 60 and 70 permanent and temporary staff, with cumulative experience 

considerably in excess of 600 years. The Division is divided into seven functional sections: Air Monitoring, Water 

Monitoring, Bio-monitoring, Inorganic Lab, Organic Lab, Quality Assurance, and Administration. Each year the 

Lab logs in, analyzes, and reports data on approximately 1400 separate Cases, each consisting of from 1 to 75 

samples. The number of individual analytes reported per sample can vary from 1 to 80, or more. On the average. 

Lab support for Air Quality, Water Quality, Hazardous and Solid Waste, and Environmental Cleanup Programs 

account for approximately 38%, 49%, 9%, and 6% of the Lab's resources, respectively'. 

The DEQ Laboratory is located at 1712 SW Eleventh Avenue, Portland, OR 97201, in the Science II Building on the 

campus of Portland State University, between Mill and Montgomery streets. It occupies the ground and basement 

level floors on the west side ofthe building. 

II. INFORMATION CONTACTS 

Inform the Laboratory as early as possible of your sampling event. Preferably prior to sample collection, to insure 

that both your needs and the Laboratory's are met in a timely manner. Contact the Sample Tracker for information 

on sample requirements (QA Manual), sampling equipment needs and availability, field preservation (QA Manual) 

or filtration requirements, sample transport, and scheduling. Speak to the appropriate Lab Manager about analytical 

capabilities that are available. 

For parameters having a short holding time (24 hours, or less refer to Table 2), schedule sample collection 

thoughtfully. Inform the Lab of your intent to sample, approximate number of samples, what you are looking for, 

and when samples will be delivered to the lab. Analysts need to be made aware of your needs and expectations so 

schedules and workloads can be adjusted to accommodate the work. 

Sampling & Analytical Information 

(503) - 229 - 5983 

SAMPLE TRACKERBob McCoy: Type of container for specific tests, general inorganic and organic sampling 

inquiries, sampling supplies, sample preservation, equipment, preliminary results. Status 

of analytical works in progress. 

Based on 1993 data, prior to reorganization, which combined BCD and HSW into one Division: WMC. 
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ORGANIC LABORATORY -

Dan Hickman: Organic and Physical Test Laboratory capabilities, sample requirements, 

methods, data interpretation. 

INORGANIC LABORATORYRon McCartney: Inorganic Laboratory capabilities, sample requirements, methods, data 

interpretation. 

METALSKaren Yates: Analytical methods, data interpretation, and test requirerrients. 

NONMETALSWilliam Calzaretta: Analytical methods, data interpretation, and specific test requirements. 

AIR MONITORINGJeff Smith: Air and meteorological monitoring procedures, capabilities, data interpretation. 

WATER MONITORINGGreg Pettit: Water sampling/monitoring procedures, equipment loans, sampling capabilities, 

data interpretation. Surface or groundwater, soils, sediments, estuaries, lakes, streams, . 

rivers, etc. 

BIO-MONITORING -

Rick Hafele: Specific information regarding biological or biotoxicity testing, interpretation of 

aquatic toxicity data, etc. 

QUALITY ASSURANCERaeAnn Haynes/Chris Redman/Paul McKay: General sampling and analytical QA/QC 

requirements and assistance, QA project plan development, data quality needs, data 

quality assessment, split sample results, coordination of QA requirements, etc. Status of 

data reports. 

ADMINISTRATIONRick Gates: Reassignment of work priorities, budgeting, cost recovery, overall Lab 

administration. 

III. Safety Considerations 

Any field activity or complaint investigation can lead into the realm ofthe unknown. Approach any complaint 

investigation as a potentially hazardous event. Obtain the proper training to recognize, deal with, and protect 

yourself from hazardous chemicals. If you have any questions about what you might be dealing with, utilize 

existing resources (e.g. MSDS, literature. Lab) and contact the appropriate authority {e.g. DEQ Health & Safety 
DEQ LAB: Field Sampling Reference Guide December 1998 

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Manager, Lab Managers, Safety Committee, etc.). The DEQ Safety Committee^ continually reviews safety and 

health needs. The Health & Safety Manager can recommend and supply the most appropriate Personal Protective 

Equipment. 

DEQ Safety Committee 

Gene Rushing 

Dale Chipman: 

Stan Okamoto: 

Susan Steronko 

Martin Loring: 

Cheryll Parr: 

Aim Cox: 

Dave St Louis: 

Bob Marshall: 

RaeAnn Haynes: 

Daniel Murphy: 

Portable " 

(DEQ Health and Safety Manager) 

MSD 

LAB 

VIP 

WQ 

WR 

NWR 

WMC 

ER 

LAB 

VIP 

Sniffers" 

229-6160 

229-6022 

229-5983 

731-3050 „ 

229-5415 

378-8240, x237 

229-6653 

229-5532 

(541)-278-4600 

229-5983 

731-3050 

Portable photoionization detectors (MicroTip'^" and HNuTM) are available to screen for toxic gases. The MicroTip is 

also capable of collecting an air sample in a bag for subsequent qualitative or quantitative analysis at the Lab. WMC 

has an Organic Vapor Analyzer (OVA) and Regions possess Combustible Gas Analyzers (CGA-GasTekTM). These 

are "sniffers," used to screen for hazards prior to site entry. Understand that they do not necessarily provide 

qualitative results {e.g. cannot always discriminate one pollutant from the next), nor are they always quantitative. 

Chemical Preservatives 

In order to stabilize samples for certain tests it is necessary to add a chemical preservative, in addition to immediate 

cooling, storage, and transport on ice. Failure to add the proper preservative, or amount, could result in samples 

deteriorating to the point of being useless for analysis. 

The DEQ Laboratory supplies sample preservative chemicals to agency persoimel on request. Staff requesting these 

chemicals is expected to become familiar with the necessary safety precautions and follow them, or to ask for 

assistance. 

Liquid preservatives are provided in 50 niilliliter re/Zo« bottles^ having integral dropper spouts with tethered 

closures. Sodium hydroxide is supplied in screw-cap plastic bottles containing less than 25 grams of pure caustic 

pellets. Each bottle is labeled with the appropriate hazard warnings and sealed in a Zip-Lock plastic bag to contain 

leakage, should the bottle closure fail in transit. Anv liquid observed inside the plastic bag should be assumed to be • 

leakage from the bottle, in which case the bag should be opened with caution, wearing hand and eye protection, and 

thoroughly rinsed with water. Solid sodium hydroxide pellets are deliquescent, that is, they absorb moisture from 

the air. This chemical is capable of absorbing enough moisture to put itself into solution. Make sure that lids are 

screwed down tightiy! 

^ As of June 1995. 

^ When these Teflon bottles become empty DON'T throw them away! They cost nearly $20 each. Retum them to the Lab so 

they can be refilled. 
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Preservatives commonly provided 

Concentrated Sulfuric Acid, H2SO4, 95+% 

Concentrated Nitric Acid, HNO3, 70+% 

Concentrated Phosphoric Acid, H3PO4, 85% 

Concentrated Hydrochloric Acid, HCL, 37% 

Solid Sodium Hydroxide, NaOH, 100% 

At the concentration supplied for sample preservation these chemicals are highly corrosive and capable of causing 

severe physical damage to skin, eyes, and clothing unless the proper precautions are observed. Treated with 

appropriate respect, and following a few simple rules, these chemicals should not cause injury. 

Material Safety Data Sheets (MSDS) 

One source of information on hazards associated with each of these chemicals, and the precautions that should be 

taken during use, are the Material Safety Data Sheets (MSDS). MSDS for each ofthe above chemicals mav be 

obtained from the Lab. 

When reading the MSDS keep in mind that you are dealing with less than 50 milliliters of liquid, and less than 25 

grams ofthe solid. Many ofthe precautions cited {e.g. respiratory protection, self-contained breathing apparatus, 

etc.) are intended for emergency response personnel dealing with bulk or industrial quantities ofthe material. 

The primary hazards posed by these chemicals are: 

• Chemical bums to the skin and eyes. 

• Chemical damage to clothing and footwear. 

All these chemicals are capable of causing Sever e an d permanen t damag e to the eyes. The following 

precautions must always be taken when handling acid or caustic for preserving samples: 

• Transport preservative containers in a restrained, upright position. 

• Wear appropriate protective eyewear. 

• Wear chemically resistant synthetic gloves. 

• Be prepared to deal with accidents. 

The Laboratory will provide, on request, protective eye wear, synthetic gloves, and "pH 6.9 buffer" which is useful 

to neutralize skin or clothing exposed to acid or caustic. We recommend that staff engaged in sample collection 

carry, at minimum, a one-gallon jug of water in their vehicle for washing in emergencies. 
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IV. Investigations 

[ OBSERVE AND DOCUMENT! 

Look for clues that suggest abnormal conditions e.g. sfressed vegetation, dead or dying insects or animals, soil 

staining, fiimes, crystals, oil, puddles of liquid, abandoned containers, unusual colors, odors, phase separations, etc. 

Whether or not to collect a sample is your decision. You must make the judgment whether or not your observations 

warrant chemical characterization ofthe material in question. If a sample is coUected it must represent the 

condition ofthe site as much as possible. 

If a sample is collected, get as much ofthe material as you can. The Laboratory needs a reasonable amount of 

sample to conduct tests. For safety consideration fill the bottle to the neck not to the cap. 

Field observations should be documented, using ink in a permanently, bound notebook. Photographs should be 

taken, if possible. If you feel that there is a potential enforcement action in the making, contact the Enforcement 

Section of Regional Operations to leam what type of evidence is needed to support an enforcement action. 

Appearance, odor, or nearby sources may suggest what to test for. 

, • / • ' \ ' ^ \ ^ CAUTION: , ^ , ' \- \ -: 

Be very cautious of unfamiliar odors / 

'"' ''A VOID opening unlabeled containers to make a preliminary assessment of sample, i 

(Be especially wary of containers that exhibit crystals around the cap, they could be extremely explosive 

organic peroxides Whin exposed to light or air, ethers can form peroxides^ that can_ easily detonate t) 

ORGANICS 

Organic substances may appear as tar, wax, oil, crystalline or amorphous solids, colored or colorless liquids. 

Samples may be odorless or their smell may be sweet, sour, biting, petroleum-like. Attempt to characterize the 

sample appearance and odor, and describe them on the Analysis Request Form. The more information you provide 

the better are the Lab's chances of identifying an "unknown" contaminant, and successfully quantifying it. 

Collect samples for organic analysis in DEQ Lab-supplied containers (see Table 2) which have been specially 

cleaned to eliminate interference. Because organic analytical methods are expensive it is imperative that samples be 

collected in acceptable containers to avoid having the analysis invalidated as a resuh of container contamination. If 

you are caught in a bind without the correct containers, call the Laboratory so we can work out an acceptable 

altemative. 

In peneral, plastic containers should NOT he used to collect .samples for organic analysis. 
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VOLATILE ORGANIC COMPOUNDS (VOC) 

VOCs are a large group of organic solvents, cleaners, and degreasers that evaporate at ambient temperature. 

Although they can volatilize quickly, frace amounts tend to persist in soils and water. This persistency, coupled with 

their mobility, makes groundwater contamination a primary concem following a spill or release of VOCs into the 

soil. When requesting VOC analysis, it is important to convey the type of situation you are investigating (dry 

cleaner, UST, spill, etc.) and whether or not you are interested in specific chemicals or materials such as gasoline, 

kerosene, trichlororethylene, or benzene. This information will help the lab choose an analytical method appropriate 

for your situation. Our default VOC method is Method 8260, a GC/MS procedure that analyzes for roughly 65 

volatile organics plus Tentatively Identified Compounds (TICs). Unfortunately not all VOCs can be analyzed using 

this method;' hence our need to know as much as possible about the possible contaminant source. 

SEMI-VOLATILE ORGANIC COMPOUNDS (SEMI-VOLs, BNAs) 

Semi-Vols {aka 8270Bor Base/Neutral-Acid Extractables, "BNA") comprises a large group of chemicals that 

include several categories: phenols, chlorophenols, phthalates, pentachlorophenol, polynuclear aromatics, and many 

others. The method covers approximately 85 specific analytes, and also provides provisional identification of 

additional analytes as Tentatively Identified Compounds (TlC's). As with VOCs the list of analytes is large, but not 

universal. Ifthe question arises whether or not a particular chemical can be tested for by this method, call the 

Organic Section at the Lab. 

PETROLEUM IN SOILS 

Methods for analysis are designated in Oregon's Soil Matrix Rules for Petroleum Underground Storage Tank 

Cleanups (OAR 340-122-350). Petroleum products in soil are first identified and then quantified by the Northwest 

Total Petroleum Hydrocarbon (NWTPH) methods: 

NWTPH-HCID is a qualitative screen to determine which petroleum products (ifany) is present, and what 

subsequent quantitative methods may be required. 

NWTPH-Gx is the quantitative method for gasoline. 

NWTPH-Dx is the quantitative method for diesel and other heavy oils. 

OIL & GREASE 

Classical "Oil & Grease" measured the polar (animal fats, vegetable oils, etc.) and non-polar (petroleum fiiels, 

mineral oils, etc.) Freon""^" extractable material in a sample. It was sometimes used in conjunction with EPA's Total 

Recoverable Petroleum Hydrocarbon method to distinguish between polar and non-polar components. DEQ Lab is 

using EPA Method 1664, n-Hexane Extractable Material (HEM), which can be used with silica gel cleanup to 

determine TPH or NWTPH Methods as appropriate. 

Other Organics 

Other common analyses used to identify or characterize unknovra organic contaminants include MBAS, 

Glycol/Fluorescein, Lignin-Tannin, Total Organic Carbon (TOC), Chemical Oxygen Demand (COD), Total 

Organic Halogens (TOX), and Formaldehyde. 

"•"MBAS . - - - -.^-- .. . .. __ 

A non-specific test for Methylene Blue Active Substances. Anionic surfactants, which may include LAS 

(Linear Alkylbenzene Sulfonates) other sulfonates and sulfate esters (colorimetric procedure). MBAS can 

detect the presence of detergents. 

Glycol/Fluorescein 
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Can identify antifreeze. Fluorescein is the ingredient responsible for antifreeze's vibrant green color, and is 

also a dye used to monitor water flow. Unlike glycol, fluorescein is not considered harmful to the 

environment. 

Lignin-Tannin 

A non-specific test for hydroxylated aromatic compounds found in lignin and tannin compounds 

(colorimetric procedure) characteristic of tree bark leaching. 

Total Organic Halogens (TOX) 

Measurement used to estimate total quantity of dissolved halogenated organic material in a water sample. 

Indicative of contamination by synthetic chemicals. 

PCBs and Chlorinated Pesticides v^ 

Both extracted by the same method, therefore a single container may be used to sample for these two 

analyses. Other organic tests require a separate container for each method of extraction. 

INORGANICS 

Inorganic contaminants tend to be crystalline, dissolved salts, or suspended solids in water. They include all 

combinations of elements, with the exception of compounds containing carbon, which are defmed as Organics. 

Inorganic acids and some caustics have a sharp, irritating odor. Collect inorganic samples in Laboratory supplied 

plastic containers described in Table 2. 

Characterization of unknown inorganic contaminants includes physical measurements (Total Suspended Solids, 

Total Solids, Turbidity, Conductance, and pH)", metals, and nutrient analysis. Turbidity, pH and orthophosphate 

samples have very short holding times, thus these analyses must be started immediately upon sample receipt. 

METALS 

Whether to request Dissolved, Total, or Total Recoverable Metals analysis is another decision you'll have to make. 

Dissolved metals are water soluble, defined as passing through a 0.45 micron filter, whereas total and total 

recoverable metals include those contained in particulate matter and thus less available to the enviroimient. The 

analytical difference between total and total recoverable metals is the severity ofthe acid digestion procedure 

utilized by the Lab to prepare samples for analyses. Total Metals digestion is more aggressive. Dissolved metals 

samples must be filtered in the field, immediately after collection and before adding acid preservative 

(Appendix C). Total Recoverable metals is a classification from the drinking water regulations. If Request for 

Analysis does not specify Dissolved or Total, Total Recoverable metals will be the test assigned. 

The Lab needs to know what level of sensitivity or detection your project requires, in order to select the appropriate 

analytical method. There are two choices: Inductively Coupled Plasma (ICP) and Graphite Furnace Atomic 

Absorption (GFAA). The ICP and GFAA methods have approximately the same minimum reporting limit, 

however, ICP is generally faster and cheaper. Reserve requests for GFAA to those situations where the method is 

specially required by the program such as a few drinking ^yater metals. 

Analyses for Mercury uses different digestion and analytical procedure than the other metals and a separate sample 

must be collected. Requests for mercury analysis must be specifically identified on the Request for Analysis, and 

separate samples collected, or it will not be performed. 

Physical measurements are performed by the Organic Laboratory Section. 
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NUTRIENTS 

Nutrients include Total Organic Carbon (TOC), Chemical Oxygen Demand (COD), Nitrate-Nitrite (NO3+NO2), 

Total Kjeldahl Nitrogen (TKN), Ammonia (NH3), Dissolved (OPO4), and Total (TPO4) Phosphate. These analytes 

can occur naturally at low levels in the ecological system. Elevated values are frequently indicative and a source of 

problems. Discharges from industry, municipal wastewater treatment plants, and agricultural operations can 

increase certain nutrient levels. Nitrogen nutrients are reported as mg/L of equivalent hifrogen, and phosphate 

nutrients are reported as mg/L equivalent phosphorous. 

There are a wide variety of chemical forms that phosphate can exist in, and be analyzed for^. Forms include Total, 

Total Reactive, Total Acid Hydrolyzable, Total Organic, Dissolved Reactive, Total Dissolved, Dissolved Acid 

Hydrolyzable, and Dissolved Organic. Notify the Lab well in advance ifany form other than Total or Dissolved 

Reactive phosphate are of interest. DEQ Lab uses the Molybdate-Ascorbic acid for Dissolved Reactive Phosphate 

(OPO4) on filtered samples, and Molybdate-Ascorbic acid proceeded by persulfate-autoclave digestion for Total 

Phosphate (TPO4). Methods used by other labs may vary, so data comparison could be difficult. 

Total Organic Carbon (TOC) 

A nonspecific test measuring organic carbon content of a water sample. Reported as milligrams of Carbon 

per liter. 

Chemical Oxygen Demand (COD) 

Measure ofthe oxygen equivalent of organic matter contained in a sample that is subject to oxidation by a 

strong chemical oxidant. 

BIOLOGICAL OXYGEN DEMAND (BOD) 

Samples may be held up to 48 hours, but less than 24 hours is preferred. BOD samples will be accepted between 

08:00 AM Tuesday and 12:00 AM Friday. Accepting BOD samples at any other time will require overtime work, 

and must be pre-approved by the Inorganic Section Manager. During the period following collection, and including 

transport to the Lab, biological samples must be kept cool on ice (4°C). 

TOXICITY CHARACTERISTIC LEACHING PROCEDURE (TCLP) 

TCLP extraction is used in RCRA to evaluate hazardous waste characteristic, replacing the EPtox Method. It is 

used to assess the leachability of metals and certain organics under precisely controlled conditions. TCLP 

procedures are also used in DEQ's Soil Cleanup Rules. 

When asking for "TCLP" on samples, be aware ofthe method's.limitations. TCLP extraction is an involved and 

relatively expensive method to run, depending on the nature ofthe samples. 

Samples having muhiple phases (water-oil, water-solid, oil-solid, water-oil-solid) are difficult to deal with under this 

protocol. Sufficient sample must be collected to provide an adequate quantity ofeaeh phase for both inorganic and 

organic TCLP extractions: approximately 500 grams of solid, or at least 1 liter of liquid. More sample material is 

required as the ratio of aqueous:solid (other) phase increases. If a sample contains less than 150 grams solid (other) 

phase in the conventional sample size, a larger quantity of sample is necessary just to run the TCLP inorganic tests. 

Table 4500-Pl. Standard Methods for the Analysis of Water and Wastewater. APHA-AWWA, 18th Edition, p. 4-109, (1992). 
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If TCLP organics, duplicate, matrix spike, or matrix spike duplicate analyses are requested considerably more 

sample is needed. According the TCLP protocol the Lab needs to have 100 grams of solid to perform the extraction. 

Extraction can be done on less material, but it compromises the integrity ofthe procedure and increases the 

likelihood of error. As a guideline, see Table 1. 

Table 1 

% Solid (other) 

2% 

5% 

10% 

15% 

20% 

Desirable Sample 

7.5 liters 

3.0 liters 

1.5 liters 

1.0 liters (« quart) 

0.5 liters (« pint) 

In general, a 1-gallon sample (* 3.8 liters) is a practical limit. 

When requesting TCLP on a sample it is more efficient for the Organic section to analyze for Totals {e.g. Total 

VOCs) first, and then to perform TCLP on any sample where a Total is observed that exceeds the TCLP Regulatory 

Limit. It serves no purpose to do a TCLP extraction, followed by analysis ofthe TCLP extract, if there isn't enough 

regulated substance in the sample in the first place to exceed the TCLP standard. On the other hand, it is more 

efficient for the Inorganic section to perform the TCLP extraction right away. Submitting samples for inorganic 

Total Metals, with the instmction that samples having high levels of regulated metals should be subjected to TCLP, 

will take considerably longer than simply requesting TCLP. 

Notice that TfVO TCLP protocols are listed in the Code of Federal Regulations: 1) 40 CFR Part 261, Appendix 

II, Method 1311 Toxicity Characteristic Leaching Procedure; and 2) 40 CFR 268, Appendix I, Toxicity 

Characteristic Leaching Procedure. The method in Part 261 is the revised version of Part 268, the original version. 

Furtiier, Part 261 was modified, effective June 29,1990, in 57 FR 55114-56117 (published November 24,1992). 

BIOLOGICAL 

Biological Oxygen Demand (BOD) is a nonspecific test used to evaluate consumption of Dissolved Oxygen (DO) 

by biological processes incubated at 20°C over a period of 5-days. It is a bioassay procedure that is normally 

applied to water samples, although it can be applied to sediment as well. BODs conventionally are done over a 5-

day period, however longer time periods are possible (e.g. 14-, 28-day). Special requests are necessary for any but 

the 5-day test. 

BODs can evaluate the oxygen depletion caused by carbonaceous material and nitrogen species (BOD), such as 

TKN and ammonia, carbonaceous material alone (CBOD), or nitrogen species alone (NOD). Special requests are 

necessary for any test other than BOD or CBOD. 

Biological samples are analyzed by both the Inorganic (BOD, CBOD) and microbiological lab (Coliform, E. Coli, 

etc.). Collect liquid samples in specially cleaned DEQ containers (referto Table 2). Lab must be notified prior to 

sampling. BOD samples for surface and receiving waters low in BOD are collected in special glass BOD bottles. It 

is desirable to determine Field DO on these samples, prior to sending to Lab (see procedure in Appendix B). When 

Field DO measurements aren't made, DO is less than 5 mg/L, or DO exceeds 120% Saturation, specify the B0DS2 

test on the Request for Analysis to inform the Lab analyst ofthe need to perform the initial DO or %Sat test. > 
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Bacterial samples will be accepted Monday through Thursday. Bacterial samples may be held for a maximum 

of 30 hours (time elapsed from collection to analysis). For Regulatory Purposes the holding time on bacterial 

samples is 6 hours! 

FIELD ANALYSIS 

DISSOLVED OXYGEN (DO) 

A significant indicator of stream health, low DO is frequently the primary cause for fish kills. Refer to Appendbc B 

for field analytical procedure. This analysis should be performed in the field because DO samples are not stable. 

Dissolved oxygen can change rapidly after sample collection, depending on temperature, barometric pressure, and 

other dissolved gases. 

ALKALINITY, CONDUCTANCE, PH, ETC. 

Other field analyses include Alkalinity, Conductance, pH, Temperature, Turbidity, and filtration. Obviously sample 

temperature will change, but pH may also change over short periods of time. It is recommended that pH be 

measured in the field whenever possible. Some samples require filtration in the field because the solubility of some 

substances depends on temperature and pH. 

V. Compliance Inspections 

NPDES, WPCF 

Refer to DEQ or EPA inspection procedures or guidelines, and review Permit requirements. Ifthe source is required 

to report self-monitoring test data to the agency, and you intend to investigate the source's analytical capability, 

collect split samples. Samples will be analyzed by both the source lab and DEQ Lab, resulting in an Inter-laboratory 

comparison. Leave a split-sample analysis form (Form 1 or Form II)* with the source. Request that they fill in their 

test results and retum it to the DEQ QA chemist at the Laboratory as soon as possible. It is not necessary to limit 

requested analysis to Pennit parameters. DEQ lab will perform any reasonable analyses and prepare a split 

comparison report. 

The Lab would appreciate advance notice of split sampling. Intra-laboratory splits are a usefiil QC measurement 

for our lab, as well as the source's lab. The DEQ lab will only hold its data until we have completed work on it. The 

field inspector is responsible for insuring that the source reports their results to the Lab QA chemist as quickly as 

possible, particularly when a comparison is wanted. Lab would appreciate receiving a monthly forecast of 

compliance split sampling schedules. 

SPLIT SAMPLING OF STP'S FOR COMPLIANCE INSPECTIONS 

Split samples should be collected in a single large container, homogenized, and then poured into separate, clean 

sample bottles: one portion for the source and one portion for DEQ. Collecting one grab sample for the source and a 

second, separate grab sample for DEQ is not the same thing. To limit variance to analytical technique alone, it is 

imperative that both the Source and DEQ Lab analyze samples that are as near identical as possible. 

Common sewage treatment plant (STP) Split Sample parameters are Fecal Coliform (FC), E.Coli, Total Suspended 

Solids (TSS), pH, and Biological Oxygen Demand (BOD). Depending on the source's Permit, a sample for CBOD 

Obtain blank forms from QA Section, DEQ Lab. 
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may be split also. The DEQ lab measures pH on all BOD samples, even though not all STP's follow this procedure. 

Because of limited holding time requirements these samples must be received at the Lab as follows. 

BACTERIAL samples (fecal coliform, KColi) must be received no later than Noon on Thursday. For LEGAL 

samples, the maximum holding time of 6 hours must be adhered to, whereas routine samples can be held up to a 

maximum of 30 hours. Bacterial samples are routinely analyzed using the Membrane Filtration (MF) method. 

When analysis for a "non-routine" organism (E.Coli, total coliform, fecal strep) is required, notify the Lab in 

advance so that special media can be prepared' for the test. 

BOD samples must be received no later than NOON oh Friday. If it is necessary to sample between Noon 

Friday and 08:00 AM on Tuesday, the lab will have to schedule someone to come in the following weekend to 

complete the test. Special authorization is required, prior to collection and shipment of samples, which will be 

received by the Lab after 12:00 on a Friday. Unauthorized samples that do not fit the routine time frame may not be 

analyzed. 

Normal procedure is to collect a 24-Hr composite sample ofthe influent and a 24-Hr composite ofthe effluent for 

BODs, TSS, and pH. A grab sample ofthe effluent is taken, after the Chlorine Contact Chamber, for Fecal 

Coliform (FC) and E.Coli. The Composite influent and effluent samples should be collected in 1000 ml "STP 

polys", and the FC/EC grab sample should be collected in a sterile wide-mouth 125 ml "S bottle" containing sodium 

thiosulfate to destroy excess chlorine. Composite effluent samples cannot be used for FC/EC samples because of 

their lengthy chlorine exposure (up to 24 hours). 

The STP staff should take their own samples from the same composite and grab sample as the DEQ inspector. The 

DEQ Lab and the STP lab should begin testing at approximately the same time. Agree upon a time for test set-up. 

and make a note of it on the field sheet. Usually the inspector will arrange for test set-up at ten o'clock A.M. on the 

day following the sampling. ^ 

Write "Split" on the top of Request for Analysis form, 

along with agreed upon "set-uptime." 

Leave a copy ofthe "Split Sample Results Report" form (Form I or II) with the STP staff, with instmctions to mail 

the completed form to DEQ Lab QA Section as soon as they have completed thek analyses. 

Time of sampling must be noted on the Request for Analysis form for all samples, along with residual chlorine 

measurement. 

Microbiological analysis is perfomied by the Oregon Health Division Laboratory. Without advanced notice, when special 

media is required, the test may not be performed. 
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VI. SAMPLING AND ANALYSIS PLAN 

I - ' 

A Sampling and Analysis Plan (SAP) is a combination Laboratory Analysis and Field Sampling Plan. Basically it 

should describe What you are going to do. Who will do it. How Many there will be. Where and When you'll do it, 

and How it will be done. A SAP should be developed before any samples are submitted to the Lab, with the 

exception of complaint and routine compliance inspections. SAPs for projects on which DEQ Lab performs 

analytical work must be approved and signed by the Lab QA Mane^er. Contact the QA Section for assistance. 

To plan workloads tbe Lab expects to receive a Sampling and Analysis Plan when: 

• Sampler is requesting a complicated suite of tests on more than five samples, 

• Sampling event involves collection and analysis of more than ten samples, or 

' Multiple sampling events planned over a period of time (e.g. quarterly, monthly, etc.). . 

At a minimum, the Lab expects to be provided with a list of how many sampling sites there will be, what type of 

sample will be collected (e.g. soil, groundwater, sediment, etc.), analyses that will be requested (e.g. VOCs, NO's, 

TKN, TCLP, Total or Dissolved metals, TPH-?, BOD5, etc.), when samples will be collected and when delivered to 

Lab, Quality Assurance samples that are necessary, and when you need to have the data (e.g. ASAP, 2 weeks, 4 

weeks, 6 weeks, etc.). The name ofthe Project Manager, phone number, and a Fund Code assigned by the Business 

Office for the Lab to charge work ori the project must be included. 

This can be accomplished in the form of either a single narrative page or a simple table, as in the example that 

follows. 
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Project: 

Project Manager: 

Fund Code: 

Sampling Date(s): 

Delivery to Lab: 

Desired Turnaround: 

FRED'S KOI EMPORIUM 

Bart Simpson [503-229-xx36] 

WXYZ 

May 34-35, 1995 

May 35, 1995 , late in afternoon 

3 weeks 

Matrix 

Surface Water 

Sediment 

Groundwater 

Soil 

# sample sites 

3 

4 

5 

3 

analytes 

BODs, NHj, VOC, Pesticides, pH, 

Alkalinity, Conductivity 

Pesticides, VOC, TKN 

Total Arsenic & Lead 

VOC, pH, Dissolved Arsenic & Lead, 

pesticides 

Pesticides, TCLP and Total metals (As & 

Pb) 

-i-QA 

1 Duplicate 

1 matrix spike 

transport blank 

1 duplicate 

transport blank 

1 duplicate 

1 matrix spike 

transport blank 

1 duplicate +1 

matrix spike for 

each TCLP 

When the Lab receives this information we can see what our schedule is like, and plan to accommodate your 

samples. The SAP also permits the Sample Tracker to prepare the appropriate number and type of sampling 

containers you will need ahead of time. However, be forewarned: there are a limited number of instmments and 

analysts available to do certairi types of testing (e.g. GC/MS-VOC, Semi-Vols, ICP-metals, etc.). 

It is pmdent to allow for some flexibility in the scheduling of your sampling event and specific tumarourid times. If 

someone else has already booked up that time period we may ask that you reschedule your sampling event, or 

extend the turnaround time. There is also the possibility, however remote, that an unscheduled Criminal-Legal case 

might preempt your time slot. Criminal-Legal cases receive priority over all other pending work. In any event we 

will do our best to get the work done if it's too late to reschedule, and you will be kept informed ofthe progress of 

your project's analyses. 

Request rapid turnaround time (1-2 weeks, or less) only when it is absolutely necessary. The Lab recognizes that 

this may be appropriate on occasion, but it should not be employed routinely or as a matter of convenience. 

Advanced Notice of Planned Sampling Activity 

The "form" on page 18 has been designed to facilitate informing the Laboratory at the earliest possible time, with 

the least inconvenience to you, of sampling activities that are coming up. Either the first or both pages can be filled 

out and Faxed to the Lab as soon as the information is available to you. 

Lab FAX number; 229-6924 

When the FAX is received it will be filed in a central location, which everyone involved will check daily. Thus, if 

the regular liaison person is not available, the information will still reach those involved. This form will provide the 

Lab with the workload planning information it needs for the work requested. Once this form has been sent, if there 

are anv changes, please send an update. 
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Page 14 

W\w&\ 5lMij^i^ m ° [5 Ml M Bi.'.I°sgiL[^,L.[ ,..»4rf> ,..(%, . 

i Page 1 
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Vll. QUALITY ASSURANCE 

The term quality assurance describes the system of activities intended to provide evidence to the producer or user of 

a product or service that it meets predefined standards of quality with a stated level of confidence^. It consists of 

related but independent activities: quality control and quality assessment. Quality control describes those activities 

and procedures used intemally (within the lab) to produce consistent and reliable data. Quality assessment deals 

with activities to independently evaluate data quality, after it's produced. 

Scientifically valid test data does not just happen. It results from hard work and considerable cost, in both time and 

money. The costs to produce low quality, unreliable data is obviously less than the costs to produce high quality, 

reliable data. However in the long mn it could cost considerably more for poor quality data ifthe site has to be resampied, sample analyses repeated, or a case is thrown out of court because of poor quality data. It is impossible to 

provide high quality analytical data on low quality samples. 

It is the DEQ Lab's Policy to give higher priority to data quality over data quantity. However analytical data 

can only be as good as the samples analyzed. Samples that are not representative ofthe matrix being assessed, those 

collected in insufficient amounts for the analytical method used, or samples contaminated by sampling or handling 

procedures cannot be made representative, increased in quantity, or uncontaminated by Lab efforts. The Lab must 

assume that everything in the sample container constitutes the sample, that the sample was collected and preserved 

properly, and that it does not contain extraneous contamination. 

Due to the sophistication of today's measurement techniques, and their cost, considerable planning is necessary to 

insure that test data is meaningfiil. The goal is to collect an appropriate number of high quality samples that 

represent the environmental entity being tested. Reduced numbers of samples require even better planning to insure 

that gaps in the data set, caused by omissions or post-analysis data rejection, don't weaken conclusions or preclude 

decision-making. 

DEQ Laboratory Sample Acceptance Policy 

It is DEQ Laboratory policy to accept samples for analysis, and report analysis results, for samples that meet the 

following minimum requirements upon receipt at Laboratory: 

1. Complete sample documentation including: 

sample description, 

sample matrix (liquid, solid, sludge, sediment), 

sample classification (grab, continuous, composite), and 

date and time of collection, 

collector's name(s), 

program/project identification (fund code), 

sampling location (including latitude-longitude and elevation), or permanent LASAR' Station Number, 

and special remarks describing the sample, if appropriate. 

2. Sample container(s) appropriate for sample type and analysis requested; 

• preservation(s) (or lack of preservative), and 

* Taylor, J.K., Quality Assurance of Chemical Measurements, (Chelsea, MI: Lewis Publishers, 1987). 

' Laboratory Analytical Storage And Retrieval 
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3. Parameter/Method fieco/Mmenrferf HoMi/ig rime not exceeded; and 

4. . Adequate quantity of sample to accommodate tests requested by collector, judged appropriate by lab supervisor, 

or stipulated in Sampling and Analysis Plan (SAP) by project manager. " -

5. Minimum Sampling Plan submitted'" when more than five (5) samples submitted, including 

• Number of samples (by matrix), iricluding QA (dupes, matiix spikes & duplicates, blanks, etc.), 

• project manager, 

• whom to report data to, 

• analyses (tests) requested, and 

• Detection limit needed [qualitative screen, drinking water Maximum Contaminant Limit (MCL), 

Toxicity Characteristic Leaching Procedure (TCLP), NPDES permit compliance, etc.]., 

Sample(s) failing to meet the above criteria may be analyzed, depending on the circumstances, but the data will be 

unambiguously flagged when reported as having been compromised due to deficiency in one or more ofthe 

elements listed above. Release of data from compromised samples will be deferred awaiting the necessary 

documentation. 

Documentation ofany of these elements may be furnished at any time up to that time when the flagged data is 

released from the Laboratory, preferably as soon as possible. If all acceptance criteria are consequently met, 

qualifying flag will be expunged frpm the report, on condition that data quality is not affected. 

VIII. Sample Collection 

Collecting a representative sample can be difficult, but it is the most crucial in the process of obtaining valid data. 

Collect duplicate samples to measure variability from sample-to-sample. This QA measure can substantiate your 

data by demonstrating that your samples are, indeed, representative ofthe population being measured. 

An important factor in collecting a representative sample is the use of proper sample containers and appropriate 

preservation. Samples should always be collected in containers supplied by the Lab. This insures that the 

container has been properly cleaned. When the container is filled, the Lab is insured they will have enough sample 

to do the test requested. Samples submitted to the lab that are not in a Lab supplied container {e.g. mayormaise, 

pickle, or peanut butter jars) are likely to be rejected for analysis. Samples must also be properly preserved or they 

may be rejected. Refer to Table 2. 

10 ^ 

Failure to submit a sampling plan could result in holding times being exceeded due to prior scheduled work in the Lab. 
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Notice that some "Preservation Codes" following Table 2 call for adding ')c',' drops of a preservative to a "y" size 

container: It is important when containers are ?iof full of sample that a proportiohate.quantity of preservative 

be added (e.g. If a 500-ml container-is.only.half-fiill, and preservation requires 12 drops of cone, sulfuric acid/500 

ml, use only- 6 drops of acid for this bottle.). 

Collecting representative samples of liquid matiices requires deciding what it is you want to represent. Are you 

interested in the effluent itself, the impact ofthe effluent on its receiving water at the point where they mix {mixing 

zone), or the impact the effluent is having 100 meters downstream from its point of discharge? Should a 

"background" sample be collected upstream ofthe discharge point? Collecting a representative sample of a 

multiphase waste in a steel drum presents different problems than collecting a sample of "pure product." Does a 

representative soil sample" include rocks, vegetation, or sticks? Considering these and similar questions before 

sampling will determine what your sample represents. 

It is up to the sampler to determine what constitutes a "sample," and what it "represents." Unless the Laboratory is 

told otherwise, whatever is in the container is "sample." It is imperative that the sampler inform the Lab when 

interested only in specific fractions of a sample, and it's also necessary to make certain that there is sufficient 

quantity ofthe fraction of interest to successfully perform the analyses. If you're not sure, call the Laboratoiy and 

ask. 

Samples "split" with a source or suspected violator must be as close to identical as it is possible to achieve. Ifthe 

source or suspected violator intends to have the sample analyzed by their own lab it would be pmdent to have their 

lab contact DEQ Lab to agree on what portion each lab defines as the "sample." If one lab screens out and discards 

the large rocks, while the other retains them, the concentration of analyte in the two samples will be significantly 

different. 

WATER SAMPLES 

The Water Quality Monitoring (WQM) section collects samples for WQ, HSW, and WMC projects. WQM 

' sampling procedures may be found in their Mode of Operation Manual (MOM), which includes procedures for 

sampling rivers, stteams, estuaries, lakes, groundwater wells, soil, shellfish, fish, and sediment. All long-term 

sampling performed by Lab personnel requires an approved SAP and/or Quality Assurance Project Plan (QAPjP). 

Groundwater 

Monitoring wells without dedicated pumps may be sampled using bailers. Some bailers are expensive and difficult 

to decontaminate. Disposable bailers are available from the Lab Sample Tracker on request. 

Collect drinking water or irrigation well samples by first purging water lines. Fill sample container directly from 

tap, unless sample is to be split. Insure that split samples are homogeneous: fill large clean container, mix and pour 

into appropriate containers. Samples collected in purge vials for VOC analyses cannot be split in this manner. They 

must be filled individually, directly from the tap or bailer (Appendix A). 

Groundwater wells must be properly "developed." All sub-samples from a given site should be representative. 

Surface water 

Samples are best collected using a stainless steel bucket. The collection container should first be rinsed with 

sample, to wash out previous sample. Collect a fresh sample. Avoid dipping bottle into sample, if possible; pour 

DEQ Lab has received sainples containing large roclcs, coins, unfired .22 rifle ammunition, etc. 
DEQ LAB: Field Sampling Reference Guide December 1998 

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from collection container, with minimal agitation, into sample bottle. Residue from the outside surface ofthe 

container, or your hands, could contaminate samples and/or expose you to hazardous materials. If a stainless 

sampling container is not available, dip bottle directly into sample, install lid, and wipe off outside of container with 

paper towel. 

AIR 

The Air Quality Monitoring (AQM) section collects samples for AQ Program projects. The AQM Procedures 

Manual contains sampling procedures for pollutant gases (CO, SO2, O3, and NOx), PMio and Suspended 

Particulate, and canister gas sampling. Air sampling/monitoring equipment is highly specialized, requires 

considerable logistic support, and is not generally available for use outside of AQM. Anyone interested in 

proposing a monitoring/sampling project should contact AQM Supervisor. 

DEQ Lab has sampling capability for PUF and Bubbler samples, and subsequent analyses for PAH (TO-4), volatile 

toxics (TO-14), and carbonyls (aldehydes & ketones using TO-11). 

Air particulate material can be analyzed for specific source-related chemicals, wood fiber, asbestos, etc. Techniques 

for particulate samplirig include Particle Fallout Samplers and "Sticky Paper." Evacuated Stainless Steel canisters 

passively sample ambient air which is retumed to the Lab and subjected to gas chromatographic analyses for ttace 

organics (e.g. solvents, gasoline, BTEX, etc.). 

SOIUSEDIMENT 

Use a stainless steel spoon or disposable plastic scoop to collect soil/sediment samples. The plastic scoops are -

useful for soft soils and those contaminated with organics, which are difficult to clean off. It is common practice to 

composite several subsamples of soil to obtain a representative sample of an environmental condition. Composite 

sampling is achieved by collecting several roughly equal sub-samples and thoroughly mixing to form one sample. 

Select soil that contains as few large rocks as possible, unless you wish the rocks included in the analysis. 

Subsurface soils can be collected while wells are being drilled, during excavation, or using a hollow-core soil drill. 

The Lab has no special equipment to collect subsurface soils, beyond using augers and core samplers. 

SUSPECT HW CONTAINERS 

Use a disposable bailer on bulk containers, such as 55-gallon dmms, storage tanks, etc. At least one-half foot depth 

of product is required for the bailer to function. The lab also supplies disposable glass tubes (approximately 4 feet 

long) that may be used to "pipette" product out of large containers. Either process is messy. Take an ample supply 

of clean water and paper towels to clean off sample bottles. Wear disposable surgical gloves to protect hands. 

Decontaminate all sampling equipment, except disposable variety, before retuming it to the lab. Do not return or 

transport any contaminated sampling equipment in ice chests with samples! Spraying with water is generally 

adequate. Carry a squirt bottle or water-filled pump-type garden sprayer to remote sites. Make your own 

arrangements to dispose of wastes generated during sampling {i.e. disposable equipment, wash water, surgical 

gloves, and paper towels). The lab has no disposal facilities or resources to accommodate disposal of wastes 

that accumulate when you decontaminate equipment. The Lab will not store or dispose of purge water. 
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IX. SUBMITTING SAMPLES, Request for Analysis 

Include the following information on the Request for Analysis form: sampling site description and nearest town; 

date and time collected; sampler's name; program to be charged (Fund Code, Project Billing Code); purpose for 

sampling; description for each discrete sampling location; container ID number(s) (in spaces provided); and request 

analysis for a specific analyte by name or test group, NOT method nuriiber. 

To insure that the correct person receives the data report, enter one or more names in the upper right hand space 

labeled: "Report Data To: ." On Requests for Analysis without anyone listed, data will be reported to the 

sample submitter. 

REQUEST FOR ANALYSIS FORM 

The Request for Analysis form is an important element for logging samples into the Laboratory, and serves as 

documentation linking analytical data in LIMS with the appropriate project or monitoring event. Certain 

information on the form is absolutely necessary. Such information as the Sampling Project Location/Site should be 

kept short, but be as descriptive as possible. 

When a sampling event is only one of several, make certain that the same project name is used on each Request for 

Analysis for each sampling event. As each case is completed and reported out a database is updated which links the 

project name with appropriate case numbers and date of reporting. If several sampling events related to the same \ 

project are listed using different names, it may be impossible to connect them in the fiiture. 

The Request for Analysis form usually contains the only information the Lab has about sample origin, possible 

contaminants and sources, conditions of collection, etc. It would be helpful, when the field sampler has kept a field 

notebook, if pertinent information was transcribed onto these forms. Information, such as "suspect cyanide in 

samples," "diesel spill," "samples contain elemental mercury," should be noted as a safety waming to the Sample 

Tracker and Analysts that will subsequentiy be handling the samples. 

Staffsubihittirig.samplesfor the LUST Program must have an Incident Log Nuniber'to include on the Request for 

AnalysisForm.-Thisinsures.thatproperresourcesareusedtopay foranalysis. . , , "; '" ' 

Waste Management andCleahup projects must have a unique Project Billing Co(le'assigried to each project through 

the.Business 6ffi'ce"if CbstlVecoveiy is (or may become) involved." The Laboratory niustbe informed what this • -

code,is before, or at the time, samples are submitted. . •',-. ' ,".-_,'• ' " ' 
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DEPARTMENT OF ENVIRONMENTAL QUALITy LABORATORi'DIVISION 

REQUEST FORANALYSIS Case Number:. 

Locatiar/SitB;_ 

Collecledby:_ 

DaleSanpbd:_ 

FtrdCcde 

ReoauedatLsb:. 

_ .. DateFfeporied _ 

Ffeporl Data To: 

Ccnunsncs 

ITEM 

• # 

1 

2 

.....3.... 

4 ... 

5.. . 

.....P..... 

: SANPLING POINT : 

: DESCRPTION 

SarrpbCcrtai-eraooatJrg : 

to testis] requested' " 

Nutrients 

Base 

DO 

BOD : 

Metals 

Oroaric 

Misc 

Misc' '• TESTE) REQUIRED . 

•••—:•—-—••••••• - •--•••• • 

: Laboratoty Goitiinents:_ 

. Contact Saiihple TracKwfotpropisr sampling containers and preseivalioii procedure at 503.229-5983 

DEQ Lab "Request For Analysis" 

It is obvious that Collected By, Date Sampled, Purpose, and Report Data To are important fields to be completed 

by the sampler. The Lab will fill in the Date Samples Received. 

Fltzseflag on the Request for Analysis samples known or suspected to contain sewage, cyanide, toxic 

solvents or heavy metals, etc. This is safety information for the Sample Tracker and Analysts who will 

subsequently handle the container and sample material. 

Always keep in mind that the Holding Time for a sample begins when the sample is collected, not when it arrives at 

the Laboratory. This could lead to problems for samples having extremely short holding time, such as BOD5 or 

Turbidity (48 hours), and Chromium"^' (24 hours). Should a sample be delivered so late as to exceed the holding 

time the test will be performed, but results will be reported as an ''estimate" and the data flagged. 

Each "item" should include a concise Sampling Point Description of where, or sample identification number, and 

when (time) sample taken. Tt is helpfiil to have the sampler note the matrix (surface water, groundwater, soil, 

sediment, etc.). 

The complete (alpha + numeric) sample bottle number should be entered under Sample Container According to 

Test(s) Requested in the appropriate column to the right of "sampling point description." If containers aren't under 
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the correct column it's not a big problem. From the container prefix the Lab knows what analj^es come out ofeaeh 

bottle. 

"Test(s) Required" should include each analyte, or type of analyte, you are interested in having a sample item 

tested for. Try to be as specific as possible. The Lab will assign methods appropriate to the analytes you are 

looking for. 

Even though you (or your contractor) have provided a Sampling & Analysis Plan (SAP), donot expect the 

Sample Tracker to'sort out yoursamples and fill outtheRequestfor Analysis, based on your SAP. Tracker 

does not have time to do this. . " - •,,.,_ _ 

• Note on "Request For Analysis" whether preservatives were added,^which preservative, and the 

amount.' ' • < 

The DEQ Lab Information Management System (LIMS) assigns a unique "Case Number" to each batch of samples 

that are logged in. A case number might be assigned to all samples from a specific project on a given sample day, or 

all samples collected during an ambient monitoring event spaiming more than one day. In no event will a case 

number be assigned to include samples from different monitoring projects. 

Case Numbers have sbc digits. The first two digits represent the year, followed by four digits assigned sequentially 

by LIMS and representing the order the cases were logged in during the year. Possible case numbers for any year 

range from YYOOOl to YY9999. 

Each Case has at least one "item," representing a distinct sampling site. A Case may have an unlimited number of 

"items." In tum, each "item" consists of one or more uniquely numbered {e.g. P105, DM456, R207, B002459, etc.) 

sample containers, depending on the type(s) of test(s) the samples were collected for. 

The container numbers, sizes, and materials are a result ofthe various chemical preservations and quantity of sample 

required to test for different analytes. Tests for several analytes, having identical preservation requirements, are 

frequently performed on a single bottle. It's obvious that a bottle preserved with nitric (TM-poly) or sulfiiric acid 

(R-poly) cannot be analyzed for nitrate, sulfate, pH, alkalinity, conductivity, etc.; however, those tests can be 

performed on a bottle (e.g. P-poly) where the only preservation is refrigeration at 4°C. 

Based on the analytes you request, and your DQOs (when specified), the Lab will assign an appropriate analysis 

method. Analytical procedures used by DEQ Lab comply with requirements ofthe applicable federal regulations; 

[e.g. National Interim Primary Drinking Water Regulation (NIPDWR), NPDES, RCRA] and are EPA approved'^ 

methods. All procedures are referenced to current published literature. If DQOs are not specified the Lab will 

employ their default method for the test. DEQ Lab Methods are listed in the most recent Laboratory Quality 

Assurance Plan. 

Occasionally non-standard methods may need to be developed when a standard method is not available, or when 

interfering substances influence the performance of a standard method. Non-standard methods will be appropriately 

validated, documented, and noted on the data record. 

40 CFR 136, SW-846, Standard Methods, etc. 
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CHAIN OF CUSTODY 

Two levels of Chain-of-Custody have been developed to eliminate some ofthe paperwork associated with 

maintaining a rigorous Chain-of-Custody. It should be noted that custody level has no bearing whatsoever on 

analytical data quality; it only documents who had the sample in their possession at any particular time. 

FIRST CUSTODY LEVEL 

Intended for routine, ambient monitoring, and samples unlikely to become involved in litigation. No formal 

custody transfer is documented. Samples are treated routinely, which includes: analyses using EPA 

approved methods; replicate analyses, matrix spikes, and QC standards using method and EPA QC criteria 

on a 1:20 frequency; comparison against historical data, if it exists; data review for consistency, 

completeness, precision and accuracy; QA review of duplicate sample data; and standardized reporting on 

the Laboratory LIMS. FIRST CUSTODY LEVEL samples will be discarded upon completion of 

analyses and report of results. 

SECOND CUSTODY LEVEL 

Includes everything in FIRST LEVEL, plus custody is thoroughly documented through every transfer from 

sampler to Lab, to and from secure storage, custody during analysis in laboratory, and retention of 

remaining sample under secure storage as evidence. 

Sample remaining after analyses are finished, or empty container when sample is exhausted during 

analyses, will be retained in secure storage until release is approved in writing by program or sampler (see 

Appendix D). Samples handled at the THIRD CUSTODY LEVEL are suitable for Criminal Actions. 

SAMPLE SHIPMENT 

Transport samples to the Lab immediately after collection. Notify the Sample Tracker (229-5983) prior to 

sample collection to allow adequate time for scheduling analysis, advance preparation, and/or technical 

assistance. Ship samples'^, packed on ice in a sealed ice chest available from the lab, via Greyhound. The 

Lab has prepaid Greyhound shipping labels available. For shipment of legal samples, refer to "Legal 

Chain-of-Custody Procedures" Appendix D. 

Ship samples to: 

DEQ Laboratories 

1712 SW 11th Avenue 

Portland, OR 97201 

If possible, hand deliver samples to the Laboratory. We are located on the Portland State University campus in the 

Science II Building, on 11th Avenue between Clay and Montgomery. Parking in front ofthe building is restricted to 

15 Minutes and Official Use Only (i.e. State licensed vehicles). Private cars will quickly be cited by Campus 

Security. You may obtain a temporary parking pass from the Lab receptionist, allowing you more time to conduct 

business. " ' " ^ -

Samples ONLY, via public carrier. Not preservative chemicals, decon solvents, or other sanctioned hazardous materials. 
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VOLATILE ORGANICS: To avoid cross-contamination of samples during shipment, seal 

samples and "Transport Blank" vials in ziplock bags. 

BACTERIAL samples {fecalcoliform, E.Coli) must be received no later than 1200 hours 

(Noon) on Thursday. 

For Legal bacterial/microbiological samples, the maximum holding time of 6 hours must be adhered to, whereas 

routine samples can be held for a maximum of 30 hours. Analysis for a "non-routine "organism {E.Coli, total 

coliform, fecal strep) is required, notify the Lab well in advance so that special media can be prepared for the test. 

Microbiological testing is currently performed exclusively by the Oregon Health Division Lab, in the adjacent 

building. 

BOD: Samples must be received no later than 1200 hours on Friday. ' " 

If it is necessary to sample between 12:00 Friday and 08:00 on Tuesday, the Lab will need to schedule someone to 

come in on the weekend. Special notification is required prior to collection and shipment of samples. 

FIELD NOTEBOOKS 

A bound field notebook should be maintained to provide a daily record of significant events, observations, and 

measurements during field investigations. This record should include field measurements, personnel, personal and 

weather observations, and physical conditions. All entries in field notebooks should be made, signed, and dated jn 

ink. Field notebooks should be kept as a permanent record. 

These notebooks are intended to provide sufficient data, observations, and documentation to enable participants to 

reconstruct events that occurred during an activity, and to refresh their memory when called upon to give testimony 

during legal proceedings. 

CORRECTION TO DOCUMENTATION 

All original data recorded in field notebooks, chain-of-custody records, and other forms must be written in 

INK. None of these documents should be destroyed or thrown away, even if they are^ecome illegible or contain 

inaccuracies that require a replacement document. . ' 

If an error is made on a document assigned to an individual, that individual must make corrections by crossing a 

single line through the error, enter the correct information, and initial the correction. 
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Appendix A SAIVIPLING FOR VOLATILE ORGANICS 

Contamination 

Because ofthe sensitivity ofthe analytical technique (0.5 parts per billion), and potential for sample contamination, 

volatile organics sampling is somewhat complex. It is important that all steps be followed. Every effort must be 

made to avoid contamination, and to document where contamination might originate (e.g. field, transport, lab 

blanks). 

Preparation 

Notify the Organic Lab before collecting any volatile organic samples. The laboratory will prepare the following 

vials upon proper notification and scheduling: 

1. LAB BLANK Two vials filled by Sample Tracker with purified water and kept in the Organic Lab for 

later analysis. 

2. TRANSPORT BLANK Two vials filled with purified water to accompany samples throughout the sampling 

run. Do NOT open these vials in the field. Retum to the Lab with samples. 

3. TRANSFER BLANK Three vials, filled with purified water by laboratory personnel, carried to the sampling 

site where the Sampler transfers the contents to two fresh vials. 

4. SAMPLE VIALS The Sampler is provided with sufficient duplicate numbered vials for DUPLICATE 

sampling at each site. Duplicate vials are distinguished by "-A" and "-B" to designate 

first and second sample, respectively. 

Sampling and Documentation 

i. The laboratory will provide the Sampler with pre-numbered vials for the Samples, Lab Blanks, and Transport 

Blanks. These vial numbers must be listed on the "Request for Analysis". 

2. Transport Blanks are NOT to be opened, and are to accompany the Samples at all times. 

3. The Sampler is required to prepare two Transfer Blanks at the sampling site, using water supplied by the 

laboratory. . 

4; All samples are collected in REPLICATE, and immediately refrigerated. 

5. Samples should be delivered to the Laboratory without delay. 

Sample Collection 

A. Collect volatile organic samples in paired sets of 40-ml glass purge vials with Teflon-lined (non-reactive) 

septums in the lids, labeled "A" and "B". Fill two vials, in the order "A" followed by "B," from the same spurce 

with as little time-lapse as possible between them. Fill vials all the way to the top and a little above, generating a 

positive meniscus. No air bubbles should pass through the sample as the bottle is filled, or be trapped in the sample 
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when the bottle is sealed. A positive meniscus at the top ofthe bottle will help ensure that no air is trapped inside 

when cap is screwed on. Place the vials in a plastic bag, close the top, and put the bag in a cooler with ice. Ship the 

samples to the lab as soon as possible. 

CAUTION! 

Some purge vials from the DEQ Lab are pre-acidifiedfor preservation. Each vial contains 10 drops of 

concentrated hydrochloric acid. Acidified containers normally give off fumes, which should not be inhaled If 

spilled on clothes or skin, flush immediately with copious amounts of cool water. 

In addition to duplicate sample vials from each site, a sampling event should include vials for Lab, Transport, and 

Transfer blanks. When sampler desires Matrix Spikes(MS) or Matrix Spike Duplicate(MSD) samples, he must 

collect and submit additional vials for analysis. Vials for MS or MSD analyses must be clearly designated as a 

separate item on the Request for Analysis form. 

Note the number ofeaeh purge vial on the "Request for Analysis Form" with a site description, date and time sample 

was taken, as each sample is collected. 

B. When sampling from a tap, open the tap and allow the system to flush until the water temperature has 

stabilized (usually 5-10 min.). Adjust flow to about 500 ml/min and collect duplicate samples from the flowing 

stream. The sampler should ensure that the tap is free of aerator, strainer, and hose attachment or water purification 

device. 

C. When sampling from an open body of water fill a 1 quart bottle or clean beaker with sample, and carefully 

fill duplicate sample bottles from the container. 

D. When sampling wells with a bailer the VOC sample should be collected from the first bailer-fiill after 

purging well. Precautions should be taken to prevent aeration of sample. 

E. When sampling a chlorinated water supply for volatiles it is necessary to preserve the samples with 25-mg 

Ascorbic acid, then acidify with 2 drops 1:1 hydrochloric acid to destroy any chlorine that may be present. Do 

not use 40-ml vials that alreadv contain HCl. If this is not done the free chlorine can react with some volatiles, 

producing chlorinated compounds that did not exist in the original sample. 

Check VOC vials for Air Bubbles 

Invert vial and tap on solid surface.".If present, air bubbles will rise 
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Appendix B SAMPLING PROCEDURE FOR DISSOLVED OXYGEN 

INTRODUCTION 

Use this procedure for field preservation of water and wastewater samples for dissolved oxygen. 

The preservation method employs dry reagent pillows to "fix" the dissolved oxygen for later 

analysis. Manganous ion reacts with the dissolved oxygen present in the alkaline solution to 

form a manganese (IV) oxide hydroxide floe. Azide ion is added to suppress interference by 

nitrite, which reacts with the free iodine generated during analysis. Following acidification, 

reduce the manganese (IV) floe with iodide; then titrate the free iodine produced with sodium 

thiosulfate (or PAO) titrant. 

SAMPLE COLLECTION 

Collect water samples in a clean 300-ml BOD bottle to overflowing with minimal aeration. This ensures that there 

will be no air bubbles trapped in the bottle. Replace ground glass stopper until you are ready to add reagent pillows. 

SAMPLE PRESERVATION 

1. Remove glass stopper and add contents of one Manganous Sulfate Powder Pillow. Replace cap and invert 

several times to facilitate mixing. 

2. Remove glass stopper and add contents of one Alkaline Iodide-Azide Reagent Powder Pillow. Insert 

stopper and invert bottle several times to mix. A flocculent precipitate will form. It will be brownish-orange if 

dissolved oxygen is present or white if oxygen is absent. 

3. Allow the sample to stand until the floe has settled. Again invert the bottle several times to mix, and let 

stand until the floe settles. 

4. Transport samples immediately to the Lab. Store in the dark at 10-20°C during transport. Preserved 

samples can be held for up to 8 hours prior to final titration. 

NOTES: 

a. If DO is for Initial D.O. measurement used in BOD determinations a second bottle must be collected 

simultaneously and sent to the lab in a cooler with ice (do not add anything to this bottle). The cooler must be 

carefully packed to protect the sample containers. 

b. When collecting for Lab BOD measurement, and BOD is expected to be greater than 5 mg/L, collect an 

additional P-poly of sample for BOD dilution setups, instead ofthe second BOD bottle. 

c. Remember to schedule DOs and B0D5s with laboratory so that personnel can be scheduled to perform 

analyses 
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Appendix C FIELD FILTRATION PROCEDURE 

APPARATUS 

The filtering apparatus consists of a wide-mouth jar, rubber stopper with filter funnel base and filter inserted, and 

removable magnetic filter funnel. Use a hand-operated vacuum pump to filter the sample. Filters used must be 0.45 

micron cellulose membrane (47 mm diameter). 

OPERATION 

1. Remove cap from clean 250 ml "DP", or "DM", poly bottle; place in center of filtering jar. 

2. Place rubber stopper (with filter base) firmly in jar opening, with filter stem inside poly sample bottle. 

(Vacuum cannot be produced unless jar is securely sealed). 

3. Place filter membrane on filter base grid. (Make certain that blue separator disk is not attached to 

membrane). 

4. Place fiinnel over filter. 

5. Pour approximately 250 ml of sample into the fiinnel. Evacuate the filtering jar (using hand vacuum pump) 

until sample begins to pass through filter. If sample is very turbid, filter several small volumes, replacing 

filter membrane as it becomes plugged, until container is frill. 

6. Remove poly sample bottle fi-om the Mason filtering jar. Rinse filter grid and funnel between samples with 

distilled water. 
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Appendix D LEGAL SAMPLE CHAIN-OF-CUSTODY PROCEDURE 

Purpose 

To provide appropriate support to litigation the Department must demonstrate the integrity of samples submitted for 

analysis, and test results, by documenting chain of possession or custody. 

Written procedures must be available and followed whenever samples destined to become evidence are collected, 

transferred, stored, analyzed, or discarded. Their primary objective is to create an appropriate and accurate record 

that can be used to trace the possession of a sample from its collection, through analysis, until its infroduction as 

evidence. A sample is considered to be i« ctw/oiiv if it is: 

a. In actual physical possession. 

b. In view, after being in physical possession. 

c. In physical possession, and then placed in secure storage. 

d. In a secured area where access is resfricted to authorized personnel. 

Pre-sampling 

Prior to any "Legal" sample collection the Inorganic, Organic, and QA Mafiagers at the Laboratory should be 

appraised ofthe project's regulatory objectives, proposed sampling locations and procedures, matrices, analytical 

requirements, and chain-of-custody procedures to be followed. This is especially true for any project collecting 

LEGAL samples, or when non-routine sampling procedures are employed. 

When criminal action is contemplated the potential litigant also must be informed that samples are to be collected. 

Since analytical results may be used as evidence, the potential litigant is entitied to collect duplicate samples and 

have them analyzed by someone else, or observe the analysis being done by the DEQ Laboratory. 

Sample Collection 

The minimum number of persons should be involved, and each should be trained in proper collection and handling 

of samples. 

Written procedures for collection, preservation, and handling, specific for each sample type and analysis must be 

followed, and any deviations documented. 

Field records must be complete, dated, and initialed at the time the sample is collected. Fill out the Request for 

Analysis form, providing at least the following information: 

a. Specific sampling location 

b. Date and time sample collected 

c. Purpose 

d. Sample container number 

e. Preservatives added and quantity 

f. Analyses required 

g. Pertinent field data (e.g., pH, temperature) 

h. Nameof collector(s): 

A separate, bound field log book is highly desirable. The necessity, and the specific information to be recorded 

therein must be determined prior to sampling, hy the project manager 
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The sample collector is responsible for the care and custody ofthe samples (including documentation) until the 

samples are properly shipped to the Laboratory, or custody is transferred to another person. 

Color slides or photographs ofthe sampling location are recommended to facilitate identification and subsequent 

recollection by the sample collector(s). Sign and write date, time, and location on the back ofeaeh photo. Handle 

photographs according to chain-of-custody procedures. Keep arid protect negatives (if appropriate) as part ofthe 

documentation. 

Transfer of Custody 

When transferring possession/custody of samples the date and time of fransfer must be recorded, and all persons 

involved must sign the record. The sample collector is responsible for proper packaging, security, and fransport of 

samples to the Laboratory for analysis, as well as providing all necessary sample documentation. 

Samples shipped to the Laboratory, either by mail or private carrier, must be in a shipping container sealed with 

security tape or a Numbered Security Seal. 

The number embossed on the security seal must be recorded on the Request for Analysis 

form, which accompanies the samples. - ^ 

Once locked, a wire cutter is required to remove the seal, assuring the integrity ofthe samples. The sample collector 

should retain a copy ofthe Request for Analysis form. The Laboratory as part ofthe permanent chain-of-custody 

documentation will retain copies of receipts from post offices, or bills of lading. 

Adhesive-backed "security seals", which theoretically^sustain damage when removed, cannot always be 

relied upon. Experience has shown these seals do not adhere to some plastic ice chests (e.g. they can be 

removed without damage!). 

An effective security tape is filament packing tape wrapped several times completely around the cooler. The tape 

should be signed or initialed and dated using a permanent marker pen across the tail-end of the'tape. 

Shipment of a secure cooler/ice chest via bus does not require signature by the bus company agent to document 

custody transfer for either SECOND CUSTODY LEVEL. 

The sample collector must complete a Chain-of-Custody form for SECOND CUSTODY LEVEL samples 

(Criminal) that are delivered directly to the Laiboratory. The sample collector will receive a copy to acknowledge 

receipt ofthe samples by the Sample Tracker. 

Laboratory Custody 

The Sample Tracker is the principal custodian of samples in the Laboratory. The QA Chemist, Inorganic and 

Organic Laboratory Managers, and Laboratory Division Administrator are also designated to act as sample 

custodians. Samples should be handled by a^minimum number of persons. 

The Laboratory maintains locked refrigerators exclusively for storing SECOND CUSTODY LEVEL samples. A 

log book in which to record sample transfers, and a secure place to keep Chain-of-Custody forms accompanies each 

refrigerator. 
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The Sample Tracker, or designated altemate, receives incoming samples and documents receipt of SECOND 

CUSTODY LEVEL samples with a multi-part NCR Chain-of-Custody form. Information required by the form: 

a. Date and time received 

b. Number of sample containers received 

c. Date samples were collected 

d. Name of collector 

e. Name of person delivering samples 

f. Description and identification number of sample containers 

g. Signature ofthe person delivering and person receiving the samples. 

// is always appropriate to make written comments on the Request for Analysis or 

Chain-of-Custody form conceming the integrity or condition of samples. 

The person delivering samples gets the Pink copy, the White copy goes to the Laboratory Office Manager for filing, 

and the Yellow copy remains with the samples. 

Ifthe samples have been mailed or shipped to the Laboratory, the Padlock Security Seal number must be 

recorded on the Chain-of-Custody form. Transportation receipts are attached to the White copy for filing, 

and the Pink copy given to the sample collector to acknowledge receipt. 

SECOND CUSTODY LEVEL samples are distributed for analysis or secured in a locked refrigerator, as 

' appropriate. The Yellow copy ofthe Chain-of-Custody form must be kept with samples. 

All laboratory documentation and logs are filled out as usual, but the samples are identified as "LEGAL" to alert the 

. analyst ofthe need to follow custody procedures. 

The laboratory area is designated a secure area, and access is resfricted to authorized personnel only. 

Laboratory personnel are responsible for the care and custody ofthe sample, once it is in their possession. They 

should be prepared to testify that the sample was in their view, or secured in the Laboratory, at all times while in 

their custody. 

Approved methods for laboratory analysis will be used and documented. All analytical results are recorded irf 

bound notebooks, retained as a permanent record in the Laboratory, as well as on LIMS. 

When sample analyses are complete the unused portion of sample must be returned to secure storage until data is 

reported out ofthe Laboratory. 

Unused portion of samples logged into the Laboratory under FIRST CUSTODY LEVEL will be 

discarded as soon as the analytical data is reported. 

SECOND CUSTODY LEVEL (Criminal) samples will be discarded/destroyed only by order ofthe 

Division Administrator after consultation with enforcement officials, when it is verified that samples are no 

longer required. The date and time of destruction is recorded on the Yellow copy ofthe Chain-of-Custody 

form, which is initialed and filed with the White copy. 
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References 

NPDES Compliance Sampling Manual. U.S. EPA 0-241-037/44, Enforcement Division, Office of Water 

Enforcement, 1977 

Handbook for Analytical Quality Confrol in Water and Wastewater Laboratories. U .S. EP A 600/4-79-019, 

EMSL - Cincinnati, Office of Research and Development, March, 1979.SPIKES, SPIKE DUPLICATES? 

What is meant by Matrix Spikel Matrix Spike Duplicate? The concept can be very conflising. 

Matrix Spikes (MSs) are useful for assessing the analytical bias of a method, i.e. systematic errors arising 

from unstable calibration standards, matrix effects, interferences, elevated blanks, instrument shifts, analyst bias, etc. 

Matrix Spike Duplicates (MSDs) are just as the name describes: a duplicate ofthe Matrix Spike. MSDs 

are usefiil for assessing analytical precision, i.e. random errors arising from instrument instability, faulty technique, 

tolerances, etc.. Analytical precision can also be determined by analysis of two portions ofthe same sample, e.g. 

duplicate samples, without spiking. Analysis offield duplicate samples can be used to assess field sampling 

precision. Various methods developed under different programs (CWA, SDWA, & RCRA) require MSs and MSDs 

at a frequency from 5 to 10% ofthe samples collected. 

Most analytical methods are developed using relatively clean samples under well confrolled conditions. 

When the method is applied by a real-world analyst to a real-world sample matrix containing chemical compounds 

that interfere with the method, by either reducing or enhancing the recovery ofthe analyte of interest, we are said to 

have a bias. Although it may not appear logical, it is not uncommon to add an accurately known quantity of analyte 

to a sample, analyze it, and get back considerably less or more than 100% of what was added. In most cases bias is 

characterized by occurring in the same direction, e.g. for a given analyst-matrix-method combination the results are 

nearly always biased in the same direction, either high or low. 

The degree of bias and precision in test data is a result of both systematic and random error in both the 

sampling and analytical phases ofthe project. Assessing which uncertainty is attributable to which activity is not a 

precise science, given the limited amount of data associated with each individual project and unique matrix. 

Theoretically the sample, MS, and MSD analyses are performed on identical 'portions of homogeneous 

sample material originating in a single sample container. This is doable for some types of sample, e.g. aqueous, or 

very finely divided, dry solid (e.g. powdered sand), but it is not possible for every sample matrix or method. The 

key to this admonition is that the sampled material must be homogeneous, and there must be enough sample quantity 

to prepare and analyze several portions ofthe same sample. 

The basis for this technique is that by analyzing a portion ofthe original sample, as it comes from the field, 

we determine the concentration of those analytes in aU portions of that sample, including those portions we 

subsequently spike (MS and MSD) with a known concenfration of analyte. 

It is necessary to find the analyte concentration in the un-spiked, original sample material before it is possible to 

calculate the recovery ofthe added (spiked) concentration. Matrix spike recovery is calculated as follows: 

„ .,' ^„ „ Observed Concentration 

Percent Spike Recovery = lOOx-

(Spike Concentration)-I-(Initial Concentration) 
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Where: Observed Concentration = concentration of analyte found in spiked sample 

Spike Concentration = concenfration of analyte spike added 

Initial Concentration = concenfration of analyte in un-spiked sample 

Uncertainty may be created when sample, MS, and MSD are collected as separate, discreet samples; a 

question of homogeneity arises, particularly for soils or solids, raising concems about the relevance of MS & MSD 

analyses. The probability of collecting two or more soil grab samples, even out ofthe same hole, and have them be 

identical is practically non-existent. For valid samples for spiking collect multiple grab samples, mix them together 

to produce a homogeneous composite, and then sub-sample the composite. Although it would be best to send a 

single, bulk sample to the Lab, ifthe composite is thoroughly mixed it could be packaged in multiple containers. 

This approach should work for semi-volatiles, pesticides, TPH, herbicides, PAH, and PCBs in soil. 

Ideally the diagram below is the way MS & MSD samples should originate, not by collecting separate grab 

samples for each entity. 

Field Activity Composite 

Initial Sample 

Analyze as Matrix 

Spike Duplicate 

Concentration "y" 

Concentration 

« x " 4- "v" : 

Concentration 

«._M t a„, , . 

Mixing a composite of soil grab samples is generally not a valid approach for Volatile Organic samples; 

samples for VOCs should be disturbed as little as possible to preclude loss of volatiles. Instead it is better to collect 

several smaller grab samples Eind place them in the container undisturbed. 

At the present time there is a logistic issue at the Lab: making certain that those organic samples where a 

MS & MSD are requested are spiked and analyzed. It arises from the way the Laboratory Information Management 

System (LIMS) identifies samples, assigns tests, and generates work lists for the analysts. To minimize this 

difficulty we have requested that samples, MS samples, and MSD samples each be logged into LIMS as a separate 

item in separate containers. Although this works for us, it's not rigorously producing MS or MSD data. We assume 

that material in^ll the containers is homogeneous; 

The quantity of sample submitted can hamper doing MS and MSD analyses. With soils it is less of a 

concem, because relatively small quantities of sample are necessary for analyses. However for aqueous samples the 

method requires that "...around 1 liter of sample..." be exfracted. An "X" or "L" glass jar contains a quart or pint of 
DEQ LAB: Field Sampling Reference Guide December 1998 

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sample, respectively. This does not allow performing muhiple analyses on a single container of liquid for 

semivolatiles, pesticides, herbicides, etc., because it takes one fiill container for each analysis. 

Surrogate Spikes 

In many organic analytical methods. Surrogate Spikes'^ are added to each sample analyzed, as a quality 

control measure. Percent recovery of these surrogates must fall within a specific range for the analysis to be 

considered "acceptable." A Surrogate is a stable compound that is chemically similar to the analytes being analyzed 

for, but either isotopically labeled or else does not occur as a natural or manmade substance normally observed in 

envirbnmental samples. Examples include D6-Benzene (benzene with all six hydrogens replaced by deuterium), 

bromofluorobenzene, various di- or tri-substituted fluorobenzenes, etc.. 

Problems can occur with surrogate recoveries on samples containing elevated concenfrations of one or 

more analytes. Surrogate spikes are prepared at a concentration to function within the normal calibration range of 

the analytical instrument. Observation of very high concentrations of one or more analytes requires the sample be 

diluted to bring these elevated concentrations within the valid concenfration range. Substantial sample dilution often 

results in dilution ofthe surrogate concentration to a level that is below their detection limit. Although surrogate 

recovery may appear bad, it may not be when all the facts are known. 

Anywhere from one to three surrogate compounds per method, depending on the method. 
Table 2 Analyte/Container 

ANALYTE 

Acidity 

Alcohols i 

Alkalinity > 

Asbestos (bulk) | 

Ash free dry weight 

BTU 

BODS (Sfream BOD5 initial DO performed in field) 

BOD5 (DO<5mg/L and/or initial DO performed in lab) 

CBOD 

NBOD^ 

Chloride 

Chlorine 

Chlorophyll a 

Chlorinated Pesticides/PCBs 

COD 1 

E. Coli. ; 

Fecal coliform, non-chlorinated 

Fecal coliform, chlorinated 

Total coliform, chlorinated 

Color 

Conductivity 

Copper 8 Quinolinate 

Corrosivity • 

Cyanide 

Dissolved Oxygen (DO) 

Ethylene Dibromide (EDB) 

Flash Point 

Fluorescein 

Fluoride 

Formaldehyde 

Glycol 

Hardness (calc.) 

Herbicides 

Hydrocarbon ID 

Iodine 

CONTAINER 

P,T 

X 

P,T 

Z 

L,Z 

BOD bottle 

P 

BOD bottle, P 

2X BOD bottle, P 

DP, DT 

BOD bottle 

Chlorophyll Tube 

X,L 

R,V 

Plastic Bac-T 

Narrow mouth bottle 

Wide mouth bottle 

Wide mouth bottle 

P,T 

P,T 

X,L 

P 

BOD bottle, P 

3 x 2 

L 

X 

DP 

X 

X 

DP,DT 

X,L 

X,L 

DP 

MIN. QUANTITY 

100 ml 

50 ml 

100 ml 

200 g 

200 g 

300 ml 

500 ml 

300 ml 

600 ml 

100 ml 

300 ml 

8 ml 

800 ml 

50 ml 

75 ml 

75 ml 

75 ml 

75 ml 

50 ml 

50 ml 

800 ml 

500 ml 

300 ml 

2 X 40 ml 

200 g 

800 ml 

50 ml 

800 ml 

800 ml 

200 ml 

800 ml 

800 ml 

200 ml 

PRESERVATION 

A 

A 

-A 

B 

A 

B 

G 

A 

G 

G 

C 

G 

H 

A 

D 

A 

A 

A 

A 

A 

A 

A 

A 

J 

I 

G 

A 

A 

C 

A 

A 

C 

A 

A 

C 

HOLDING TIME' 

14 days 

14 days 

72 hours 

N/A 

30 days 

48 hours 

48 hours 

48 hours 

48 hours 

28 days 

Immediate^ 

3.5 weeks 

7 days to extract* 

28 days 

6 hours Legal, 30 hours routine 

6 hours Legal, 30 hours routine 

6 hours Legal, 30 hours routine 

6 hours Legal, 30 hours routine 

48 hours 

28 days 

7 days to extract'' 

14 days 

0.5 h, 8h"* 

14 days 

30 days 

30 days 

28 days 

30 days 

30 days 

28 days 

7 days to extract* 

7 days to extract* 

14 days 
ANALYTE 

Ketones-Aldehydes 

Lignin-Tannin 

MBAS 

METALS' ••. •.,-. • 

Chromium +6 

Mercury 

Boron, Silica, Common Cations 

Other Metals 

Dissolved Metals 

Metals in solids 

Methane gas 

Nitrogen: Ammonia nitrogen 

Nitrogen: Nitrite nitrogen 

Nitrogen: Nitrate+Nitrite nitrogen 

Nifrogen; Total Kjeldahl Nitrogen 

Oil & Grease 

Organotins (TBT, etc.) 

Ortho Phosphate 

Polynuclear Aromatic Hydrocarbons (PAH) 

PCB 

Pentachlorophenol 

Percent Fat 

Percent Sulfiir 

PH 

Phenolics 

Pheophytin a 

Phthalates 

Propane in water 

Sediment moisture 

Sediment Partical Sizing 

Sediment Oxygen Demand (SOD) 

Semivolatile Organics (PPOE, BNA) 

Sulfate 

Sulfides 

Percent Solids 

Solvents 

Suspended Solids 

CONTAINER 

Cartridge 

P 

P 

TM 

TH 

DP, DT 

TM 

DM 

L,Z 

Tedlar bag 

R,V 

P,R,V 

R,V 

.R,V 

X,L 

Polycarbonate 

DP 

X,L 

X,L 

X,L 

Foil 

L 

P,T,0 

X,L 

Chlorophyll tube 

X,L 

B 

S 

S 

S 

X,L . 

DP,DT 

BOD Bottle 

Z 

B 

P,0 

MIN. QUANTITY 

Air samples 

50 ml 

250 ml 

100 ml 

300 ml 

100 ml 

100 ml 

100 ml 

100 g 

500 ml 

50 ml 

50 ml 

50 ml 

50 ml 

800 ml 

800 ml' 

100 ml 

800 ml 

800 ml 

800 ml 

5 grams of tissue 

200 ml 

100 ml 

500 ml 

8 ml 

10 g, 800 ml 

40 ml 

1000 g 

IL 

1000 g 

800 ml, 10 g 

100 ml 

300 ml 

200 g 

40 ml 

200 ml 

PRESERVATION 

N 

A 

A 

A 

F 

C 

E 

C,E 

A 

D 

A 

D 

D 

D(cwA) or E(RCRAi 

M 

C 

A 

A 

A 

N 

A 

A 

L 

H 

A 

G 

A 

A 

A 

A 

C 

K 

B 

G 

A 

HOLDING TIME" 

7 days to extract* 

N/A 

48 hours 

24 hours 

14 days 

6 months 

6 months 

6 months 

6 months 

14 days 

28 days 

48 hours 

28 days 

28 days 

28 days 

180 days to extract* 

48 hours 

7 days to extract* 

7 days to extract* 

7 days to extract* 

6 months 

14 days 

Immediate^^ 

28 days 

3.5 weeks 

7 days to extract* 

14 days 

@NA 

6 months 

7 days to extract* 

28 days 

7 days 

@NA 

14 days 

7 days 
ANALYTE 

Thiocyanate \ 

TCLP 

Total Dissolved Solids 

Total Organic Carbon 

Total Organic Carbon (Soil) 

Total Organic Halides 

Total Phosphate 

Total Solids 

Total Volatile Solids 

Turbidity i 

Volatile Aromatics ' 

Volatile Organics ! 

Woodstove Catalyst , 

CONTAINER 

P 

TM, A, X, L, S 

P 

R,V 

L 

Amber, TOX bottle 

R 

P 

P 

P 

Bx2,L 

Bx2,L 

TSP Filter 

MIN. QUANTITY 

50 ml 

200 g" 

200 ml . 

20 ml 

100 g 

10 g, 200 ml 

100 ml 

100 ml 

200 ml 

50 ml 

2 X 40 ml, 5 g 

2 x 40 ml, 5 g 

PRESERVATION 

A 

A 

A 

D 

A 

DfRCRAi or E(cwA> 

D 

A 

A 

A 

G 

G 

B 

HOLDING TIME* 

7 days to extract* 

7 days 

28 days 

28 days 

14 days to extract* 

28 days 

7 days 

7 days 

48 hours 

14 days 

14 days 

Holding times less than or equal to 72 hours are printed in bold text. 

^ Nifrogenous BOD determined by difference between BOD & CBOD. 

' Chlorine samples analyzed within 0.5 to 24 hours after sample collection are reported as estimates. Samples older than 24 hours are rejected. 

* Samples held up to 40 days after extraction. 

Analyze immediately. Winkler allows stabilization & holding for 8 hours until titration. 

^^ pH samples older than 36 hours are reported as estimates. 

'^ Ifthe sample contains filterable solids, collect sufficient volume to contain 200 g of solids. Refer to DEQ's field sampling reference guide. 
Preservation Codes 

A = Refrigerate on ice at 4oC. 

B = No preservation required, but should be kept on ice at 4oC. 

C = Filter in Field (0.45 |i filter), and refrigerate at 4oC. 

D = Add 12 drops cone. H2S04 to 500 ml bottle and refrigerate. [H2S04 = Sulftiric Acid] 

E = Add 25 drops cone. HN03 to 250 ml bottle and refrigerate. [HN03 = Nitt-ic Acid] 

F = Add 50 drops cone. HN03 to 500 ml bottle and refrigerate. 

G = No air space in container; refrigerate at 4oC. 

H = Filter in field; store in acetone with Magnesium Carbonate; freeze with dry ice; avoid light! 

I = Add alkaline Potassium iodide and Manganous sulfate; refrigerate!, (See sampling procedure for 

Dissolved Oxygen) 

J = Add 4- 5 pellets of solid potassium or sodium hydroxide to 1000 ml bottle; pH > 10; refrigerate. 

K = Add Zinc acetate. Potassium hydroxide to pH > 9; exclude air; refrigerate. 

L = Add cone. H3P04 to pH < 4; Methyl orange and 1 g Copper sulfate; refrigerate. 

[H3P04=Phosphoric acid]. 

M = Ship on dry ice (freeze); allow 1 inch headspace for expansion of sample. 

N = Wrap in clean aluminum foil and freeze. 

Container Codes 

ORGANICS IN WA TER: 

X = New, 1000 ml amber glass jar with Teflon lined lid. 

B = New, 40 ml glass vial with Teflon septum; or Amber, 4 oz. TOX bottle. 

METALS IN WATER: 

TM = New, 250 ml polyethylene bottle. 

DM = New, 250 ml polyethylene bottle. 

TH = New, 500 ml polyethylene bottle. 

SURFACE WATER: 

P = Reused, 1000 ml polyethylene bottle. 

DP = Reused, 250 ml polyethylene bottle for filtered sample. 

R = Reused, 500 ml polyethylene bottle for samples preserved with H2SO4. 

LANDFILLS: 

T = 

DT = 

V = 

Reused, 1000 ml polyethylene bottle. 

Reused, 250 ml polyethylene bottle for filtered sample. 

Reused, 500 ml polyethylene bottle for samples preserved with H2SO4. 

SOLIDS: 

Z 

S 

L 

= "Zip-Loc" baggies. 

= New, 1000 ml polyethylene bottle. 

= New 500 ml (1 pint) Mason jar. 

WASTE WATER: 

STP = Reused, 1000 ml polyethylene bottle. 

5 = Reused, 250 ml sterile polycarbonate bottle. 

R = Reused, 500 ml polyethylene bottle for samples preserved with H2SO4. 

MIXED PHASE: 

TL = Reused, 2000 ml or 4000 ml polyethylene bottle. 

TS = Reused, 500 ml clear glass jar. 

5 = New, 1000 ml polyethylene wide mouth bottle. 
Table 3 CHEMICAL GROUPS, BY ORGANIC ANALYTE 

ALCOHOLS 

Methanol 

1-Propanol 

iso-Propanol 

Ethanol 

n-Butanol 

2-Propanol 

CHEMICAL OXYGEN DEMAND (COD) 

Nonspecific test to measure oxygen depletion potential of a water sample assuming all materials are chemically 

oxidized to their highest oxidation state: reported as mg oxygen per liter. 

CHEMICAL MASS BALANCE CARBON (CMB) 

Nonspecific test that measures elemental carbon and organic carbon on suspended particulate samples, along 

with various metals and chemical species. 

CYANIDE 

Total Cyanide 

* Must request Cyanide Amenable to Chlorination when seeking to determine characteristic waste criteria 

under RCRA. 

HERBICIDES 

2,4-D 

Dicamba 

2,4-DB 

MCPP 

Hydrocarbon ID (HCID) 

Kerosene 

Stoddard Solvent 

Thinner 

Gasoline 

Mineral Spirits 

N-P PESTICIDES 

Guthion 

Demeton-S 

Coumaphos 

Dimethoate 

Fensulfothion 

Phosdrin 

Disulfoton 

Fenthion 

Dibrom 

Tetrachlorvinphos 

Sulfotep 

Oil AND GREASE 

Dichlorprop 

Dalapon 

Dinoseb 

2,4,5-T 

Fuel Oil #1 

Fuel Oil #2 (Diesel) 

Fuel Gil #4 

Fuel Oils #5, #6 (Bunker) 

Sulprofos 

Diazinon '" 

Phorate 

Fenchlorophos 

EPN 

Malathion 

Parathion-ethyl 

Tokuthion 

Tefraethylpyrophosphate 

Silvex 

MCPA 

Picloram 

Chlorpyrifos 

Dichlorvos 

Prophos 

Merphos 

Parathion-methyl 

Trichloronate 

Non-specific test for hydrocarbon-like compounds containing -CH2- linkages (infra-red technique looking for 

C-H stretch). 
CHLORINATED PESTICIDES 

a-BHC 

P-BHC 

5-BHC 

r-BHC (Lindane) 

Heptachlor 

Aldrin 

Heptachlor epoxide 

p,p'-DDE 

Dieldrin 

Endrin 

p,p'-DDD 

Endosulfan II 

p,p'-DDT 

Endrin Aldehyde 

POLYNUCLEAR AROMATIC HYDROCARBONS (PAHs) 

Acenaphthene 

Acenaphthylene 

Anthracene 

Benzo(a)anthracene 

Benzo(a)pyrene 

Chrysene 

Fluoranthene 

Fluorene 

Heptacosane 

Naphthalene 

Azulene 

Dibenzofuran 

Dibenzothiophene 

Phenanthrene 

Pyrene 

Acridine 

Carbazole 

Benzo(b)fluoranthene 

p,p'-Methoxychlor 

Endrin ketone 

Chlordane 

Toxaphene 

Endosulfan sulfate 

Endosulfan 1 

Benzo(k)fluoranthene 

Perylene 

Dibenzo(a,h)anthracene 

Indeno( 1,2,3-c,d)pyrene 

Benzo(g,h,i)perylene 

POLYCHLORINATED BIPHENYLs (PCBs) 

Aroclor 1016 Aroclor 1248 

Aroclor 1221 Aroclor 1254 

Aroclor 1232 Aroclor 1260 

Aroclor 1242 Aroclor 1262 

PHENOLICS 

Non-specific test for phenolic-like compounds (colorimefric procedure in which sensitivity is inversely related 

to the number of substitutions on the aromatic ring). If specific phenols are required, see semi-volatile organic 

exfractables. Will not measure pentachlorophenol. 

SEMIVOLA TILE ORGANICs (Priority Pollutants Organic Extractables) 

Acenaphthene 

Acenaphthylene 

Aldrin 

a-BHC 

Anthracene 

Endosulfan sulfate 

Benzo(a)anthracene 

Benzo(a)pyrene 

Benzo(b)fluoranthene 

b-BHC 

bis(2-chloroethoxy)methane 

bis(2-chloroethyl)ether 

bis(2-chloroisopropyl)ether 

bis(2-Etiiylhexyl)phthalate 

4-bromophenyl Phenyl Ether 

Butylbenzylphthalate 

4-Chloro-3-methylphenol 

2-Chloronaphthalene 

2-Chlorophenol 

4-Chlorophenylphenyl Ether 

2,4-Dinittotoluene 

2,6-Dinitrotoluene 

di-n-octyl phthalate 

Endosulfan I 

Endosulfan II 

Benzo(g,h,i)perylene 

Endrin 

Endrin aldehyde 

Fluoranthene 

Fluorene 

Y-BHC 

Heptachlor 

Heptachlor epoxide 

Hexachlorobenzene 

Hexachlorobutadiene 

Hexachlorocyclopentadiene 

Hexachloroethane 

Isophorone 

2-Methyl-4,6-dinifrophenol 

2-Methylphenol 

Indeno( 1,2,3-c,d)pyrene 

Dibenzo(a,h)anthracene 

1,2,4,5-Tetrachlorobenzene 

Dibenzofuran 

Diethylphthalate 

Pyrene 

Endosulfan cyclic sulfate 

bis(2-ethylhexyl)adipate 

Benzo(k)fluoranthene 

2,4,5-TrichlorophenoI 

trans-Nonachlor 

2,4,6-Trichlorophenol 

2,4-Dinitrophenol 

1,2,4-Trichlorobenzene 

Dimethyl phthalate 

2,3,4,6-Tetrachlorophenol 

2,4-Dimethyphenol 

2,3,5,6-Tetrachlorophenol 

Dieldrin 
Chrysene 

4,4'-DDD 

4,4'-DDE 

4,4,-DDT 

6-BHC 

Dibutyl phthalate 

1,2-Dichlorobenzene 

1,3-Dichlorobenzene 

1,4-Dichlorobenzene 

3,3'-DichIorobenzidene 

2,4-Dichlorophenol 

4-Methylphenol 

Naphthalene 

Nitrobenzene 

2-Nifrophenol 

4-Nifrophenol 

N-Nitrosodimethylamine 

N-Nifroso-di-(n-propyI)amine 

N-Nifrosodiphenylamine 

Pentachlorophenol 

Phenanthrene 

Phenol 

Plus Tentatively Identified Components (TICs) in the Sample Extra 

SOLVENTS 

Acetone 

2-Propanol 

Methyl isobutyl ketone (MIBK) 

VOLA TILE AROMA TICs (B 

Benzene, 

o-Xylene 

VOLATILE ORGANICs (VO 

Chloromethane 

Vinyl chloride 

Bromomethane ^ 

Chloroethane N 

Trichlorofiuoromethane 

Acrolein (2-Propenal) 

1,1-Dichloroethy Iene 

Methylene chloride 

trans-1,2-Dichloroethylene 

1,1-Dichloroethane 

2,2-Dichloropropane 

cis-1,2-Dichloroethylene 

2-Butanone (MEK) 

Bromochloromethane 

Chloroform 

1,1,1-Trichloroethane 

Carbon tetrachloride ^ 

Benzene 

1,2-Dichloroethane 

Trichloroethylene 

1,2-Dichloropropane 

Bromodichloromethane 

2-Chloroethyl vinyl ether 

cis-1,3-Dichloropropene 

4-Methyl-2-pentanone (MIBK) 

Hexachloro-1,3-Butadiene 

¥*l 

Methyl ethyl ketone (MEK) 

Ethyl acetate 

. 

TEX) 

Toluene 

m-Xylene 

Q 

Toluene 

frans-1,3-Dichloropropene 

1,1,2-Trichlorethane 

1,1,2,2-Tefrachloroethylene 

1,3-Dichloropropane 

Dibromochloromethane 

1,2-Dibromoethane (EDB) 

Chlorobenzene 

Ethyl benzene 

1,4-/1,3-Dimethylbenzene 

1,2-Dimethylbenzene 

Styrene 

Bromoform 

Bromobenzene 

1,1,2,2-Tefrachloroethane 

n-Propyl benzene 

2-Chlorotoluene 

4-Chlorotoluene 

1,2,4-Trimethylbenzene 

1,3-Dichlorobenzene 

4-Isopropyltoluene 

1,4-Dichlorobenzene 

1,2-Dichlorobenzene 

n-Butylbenzene 

1,2,4-Trichlorobenzene 

T- A_A ; i_. ¥ j ^:r:-. j /"" ] » 

Ethylbenzene 

p-Xylene 

/T^T/~'« \ Plus Tentatively Identified Compounds (TICs) 

TOTAL ORGANIC CARBON (TOC) 

Nonspecific test that measures organic carbon content of a water sample as milligrams of Carbon per liter. 
TOTAL ORGANIC HALIDES (TOX) 

Nonspecific test that measures total halide (fluorine, chlorine, bromine, iodine) content of an organic exfract. 

TOTAL PETROLEUM HYDROCARBON (TPH) 

Hydrocarbon ID analysis performed on soil sample. Based on ID result, analysis may be followed up with TPH-G, 

TPH-D, and/or a modified version of method 418.1. 
Table 4 ICAP TEST GROUPS 

The Inductively Coupled Argon Plasma (ICAP) instrument is capable of simultaneously scanning a single sample 

for multiple trace metals. To simplify logging in samples to LIMS for multiple trace metals a number of Test 

Groups have been designated to meet the needs of different program objectives {e.g. landfill monitoring wells, 

groundwater, surface water, drinking water, etc.). 

It is frequently more cost-effective to analyze for a Test Group, than to analyze for a single metal. The various "test 

Groups" are listed below: 

Element 

Aluminum 

Antimony 

Arsenic 

Barium 

Beryllium 

Boron 

Cadmium 

Calcium 

Chromium 

Cobalt 

Copper 

Hardness as CaC03 

Iron 

Lanthanum 

Lead 

Lithium 

Magnesium 

Manganese 

Molybdenum 

Nickel 

Phosphorus 

Potassium 

Rubidium 

Selenium 

Silica 

Silver 

Sodium 

Strontium 

Sulfur 

Thallium 

Tin 

Titanium 

Tungsten 

Vanadium 

Zinc 

Zirconium 

INDMl 

• 

' 

y^ 

-

• 

• 

• 

• 

•^ 

V' 

•" 

• 

INDM2 

• 

• 

i^ 

PPMl 

• 

• 

V 

• 

• 

V 

V 

V 

^ 

• 

V 

PPM2 

• 

V 

V 

V 

V 

TPMl 

/ 

• 

V 

• 

• 

• 

• 

SCAN 

y ' 

• 

• 

• 

V 

• 

V 

V 

• 

• 

V 

V 

V 

V 

^ 

• 

• 

V 

• 

• 

^ 

• 

• 

• 

• 

• 

• 

y^ 

• 

/ 

• 

V 

•' 

• 

V 

• 
Table 5 UNITS & CONVERSIONS 

Metric System 

The basic units of measurement in the metric system are the meter, gram, and Uter, all ofthe rest are multiples of these quantities using 

an exponent of 10. 

Prefix Symbol Multiple Decimal Name 

10'^ 

10'' 

10'-

10' 

10^ 

10^ 

10^ 

10^ 

10-

10-' 

10-^ 

10-' 

10-' 

10-' 

1 liter = 1000 milliliters = 1,000,000 microliters = 1000 cm^ 

1 kilogram = 1000 grams = 1,000,000 milligrams = 1,000,000,000 micrograms 

1 cm' H2O = 1 cc H2O = 1 milliliter H2O = 1 gram H2O 

Conversions 

Exa 

Peta 

Tera 

Giga 

Mega 

Kilo 

Hecto 

Basic unit: 

Cent! 

Milli 

Micro 

Nana 

Pico 

Femto 

Atto 

E 

P 

T 

G 

M 

k 

h 

c 

m 

|i 

n 

P 

f 

a 

1,000,000,000,000,000,000 

1,000,000,000,000,000 

1,000,000,000,000 

1,000,000,000 

1,000,000 

1,000 

100 

meter, gram^ liter -

0.01 

0.001 

0.000,001 

0.000,000,001 

0.000,000,000,001 

0.000,000,000,000,001 

0.000,000,000,000,000,001 

Quintillion 

Quadrillion 

Trillion 

Billion 

million 

thousand 

hundred 

hundredth 

thousandth 

millionth 

billionth 

^ trillionth 

quadrillionth 

quintillionth 

Unit 

Acre 

Acre 

Acre 

Barrel (petroleum) 

Bushel 

Chain (surveyor's) 

Cord (wood) 

Cup 

Degree (temperature) 

Fathom 

Foot 

Foot 

Foot" 

Foot' 

Foot' 

Gallon, liq. (US) 

Grain 

Gram 

Hectare 

Inch 

inch^ 

inch' 

Kilogram 

Kilometer 

Kilometer^ 

knot (nautical) 

league (nautical) 

Liter 

Liter 

Meter 

Meter^ 

Meter' 

Metric Equivalent 

0.40468564 hectares 

40468564 meters 

0.0040468564 sq. kilometers 

158.98729 liters 

35.23907 liters 

20.1168 meters 

3.624556 cubic meters 

0.2365882 liters 

°C =(5/9)(°F-32) 

1.8288 meters 

30.48 centimeters 

0.3048 meters 

929.0304 cm' 

28.316846 liters 

0.028316846 meter' 

3.785411784 liters 

64.79891 milligrams 

1000 milligrams 

10000 meters' 

2.54 centimeters 

6.4516 centimeters' 

16.387064 cm' (or milliliters) 

0.001 metric ton . 

1000 meters 

100 hectares 

1.852 kilometers/hr 

5.559552 kilometers 

0.001 meter' 

1000 milliliters (or cm') 

100 centimeters 

10000 cm' 

1000 liters 

English Equivalent 

43560 square feet 

4840 yards 

0.0015625 sq. miles 

.42 gallons 

4 pecks 

66 feet 

128 cubic feet 

8 ounces liquid (US) 

°F = °C (9/5)+32 

6 feet 

12 inches 

0.333333 yards 

144 in' 

7.480519 gallons (US) 

1728 in' 

4 quarts, liq.(US) 

0.00228571 ounces (advp) 

0.03527396 ounces (advp) 

2.4710538 acres 

0.08333333 feet 

0.00694444 feet' 

0.0346320 pints, liq. 

2.204623 pounds 

0.62137119 miles 

247.10538 acres 

1.151 miles/hr 

3 nautical miles 

1.056688 quarts, liq. 

1.093613 yards 

1.195990 yards' 

1.307951 yards' 
Unit 

Micron 

Mil 

mile, nautical 

mile, statute 

ounce, advp 

ounce, liquid 

Pace 

pint, liquid 

point (typographical) 

pound, advp 

quart,, liquid 

Rod 

section (US) 

Tablespoon 

Teaspoon 

ton, metric 

ton, short 

yard 

yard' 

yard' 

Metric Equivalent 

0.000001 meter 

0.0254 millimeters 

1.852 kilometers 

1.609344 kilometers 

28.349523125 grams 

29.57353 milliliters 

76.2 centimeters 

0.473176473 liter 

0.3514598 millimeter 

453.59237 grams 

0.946352946 liter 

5.0292 meter 

2.5899881 kilometer' 

14.78676 milliliters 

4.928922 milliliters 

1000 kilograms 

907.18474 kilograms 

0.9144 meter 

0.83612736 meters' 

764.554857984 liters 

English Equivalent 

0.0000394 inch 

0.001 inch 

1.1507794 miles 

5280 feet or 8 fiirlongs 

437.5 grains 

0.0625 pint, liquid 

30 inches 

0.5 quart, liquid 

0.013837 inch 

16 ounces, advp 

2 pints, liquid 

5.5 yards 

Imile' . 

3 teaspoons 

0.33333333 tablespoons 

2204.623 pounds 

2000 pounds 

3 feet 

9 feet' 

27 ft'or 201.974 gallons 

Perspective 

part-per-million 

part-per-billion 

part-per-trillion 

ppm 

ppb 

ppt 

1 mg/kg. 

1 UgAcg, 

Ipg/kg, 

1 mg/L 

\\iP/L 

Ipg/L1,000,000 ppt = 1,000 ppb = 1 ppm 

One ppm: 1 inch in 15.782 miles or 1 second in 11.57 days 

One ppb: 1 inch in 15782 miles or 1 second in 31.71 years 

One ppt: 1 inch in 15,782,828 miles or 1 second in 31,710 years 

Percentage 

.Percent means parts-per-hundred. Seldom used as a unit of environmental analytical measurement, because it is too large. 

Percent, % 

1 

0.1 

0.01 

0.001 

0.0001 

0.00001 

ppm 

10,000 

1000 

100 

10 

1 

0.1 
Form I 

DEPARTMENT 

Intar-Laboira' 

8TAL QUALBP 

Source Name: _ 

Contact Person: 

Address: 

DEQ Case Number: 

Sample Date: 

Phone: 

Collected By: Region/Division: 

Analyte 

CBOD* 

BOD 

Suspended 

Solids 

Fecal 

Coliform* 

Chlorine 

Residual 

pH 

FIELD MEASUREMENTS* 

Influent 

- .'• ' 

. 

•'• • 

Effluent 

grab 

Effluent 

composite 

Other Parameters (Fill in test) 

- ' • / 

-

- • _ 

; 

1 ' 

, ' -.^ • 

,-

.^ 

SOURCE SAMPLE RESULTS 

Influent 

MF 

MPN 

' 

Effluent 

grab 

MF 

MPN 

Effluent 

composite 

MF 

MPN 

-

DEQ LAB RESULTS 

Influent 

MF 

, 

-^ -

' 

'~ 

•" 

Effluent 

grab 

MF 

, -

- , 

Effluent 

composite 

. MF 

Shaded area for DEQ use. 

•DEQ sampler enter your field measurements, if taken; indicate whether they are estimates. 

•CBOD is when nitrification inhibitor is used in the BOD test. 

•Indicate if analysis is by MPN or MF. 

Date/Time BOD's set up at source lab: 

Date/Time FCs set up at source lab: 

Date/Time BOD's set up at DEQ lab: 

Date/Time FCs set up at DEQ lab: 

Fill in your split sample results and mail to: 

DEQ Lab 

1712 SW 11t h Ave. 

Portland , OR 97201 

Attn : QA Chemist 
Form II 

Source Name: _ 

Contact Person: 

Address: 

OREQOM DEPARTS TOP ENVDRONI 

-Laboratory Split Comparison 

Sample Date: 

8TAL QUALBP 

DEQ Case Number: 

Collected By: 

Phone:_ 

Region/Division: 

Analysis FIELD MEASUREMENTS* 

Sample 

A 

-

,'" 

' 

1 

Sample 

f< 

'i 

! ' 

,t 

•c 

Sample 

C 

-

'' 

SOURCE SAMPLE RESULTS 

Sample 

A 

Sample 

B 

' • 

Sample 

C 

Sample 

D 

Date/Time 

Analysis 

set up 

DEQ LAB RESULTS 

Sample 

A 

:'^^.:':^''^:-!^i^^!-:'^;i:-:'i-iii 

w^ww:::^:::'^:: 

;lii?il|l| 

5 %•:;:: •;•?;&:-?»;, 

W;§M 

llllll l 

11111111 

Sample 

B 

liiiii 

liiiiiii 

:^^i:^^i-^"-::'-vS-;;i'::;^:-^ 

;:f;-:;::;;f.v:;:sfft,;ii::: 

W:^':}^x''h 

•M::ii<-':i:&\: 

iiiiilli 

Iiiiil 

Sample 

C 

:iilii;p;|f| 

:":>!•:- ':• r^^^-::.:- ^ 

•;;;i;^.r':.•;, ••^'x:v:.:;^ y 

*:lS;S?:E4;;f;iJK:y::; 

iiiliiliS 

Sample 

D 

liiiiiii 

liiiiiii ii-'iiv^v;'. :--';';*-\'-v-' 

iiii:;,vW|i;i: :? 

Date/Time 

Analysis 

set up 

iiiiiliili-^i 

•••'^^•y ': ^i^^x^x;--"-'- : i*V/.',? ^ 

^•'y.:iy :•'::.'-::/}.:'•:' 

M^:'.:::3fi^'iv:MM---h 

!:-'^^'i^-:: . ;•>•!•:•:•:':'i^.-i-iv'.''-' :']-S:.-' ••:'i- : 

Sample 

A 

B 

C 

D 

Sample point description • 

(ie. Effluent comp.). 

$:'''^':.-,:y:M::'WiMXm 

ii::S::|-:ffil:;!l®:^liillil£|i:i^^ 

|i||||iii|||ii|||ii 

iliiiliiili iiliiiiBiiiili 

Container number 

SOURCE DEQ* 

' . 

Fill in your split sample results and mail to: 

1712 

DEQ 

SW 

Portland , 

Attn 

Lab 

11th 

OR 

^•^ ^ 

Ave . 

97201 

QA Chemist | 

Shaded area for DEQ use. 

•DEQ sampler enter your field measurements. If taken; indicate whether they are estimates. 

•DEQ sampler is responsible for completing this column. 

Need assistance with tliis form? Contact tlie QA chemist at (5031 229-5983. 
Location/Site: 

Collected by: _ 

Purpose: 

Comments: 

DEPARTMENT OF ENVIRONMENTAL QUALITY 

Request for Analysis 

Date Sampled:. 

Fund Code: 

Case No. 

Date Received in Lab: 

Date Reported: 

Report Data to; 

ltem# 

1 

2 

3 

4 

5 

6 

Sampling Point Description 

(include time) 

• 

-

PFO Bucket #: 

~ 

- - =^-=^ 5ii:i;_ : =i : 

Test(s) Required 

Lead, TPART, TASK, % VOL, PFOUP, PFODN 

Lead, TPART, TASH, % VOL, PFOUP, PFODN 

Lead, TPART, TASH, % VOL, PFOUP, PFODN 

Lead, TPART, TASH, % VOL, PFOUP, PFODN 

y 

Lead, TPART, TASH, % VOL, PFOUP, PFODN 

Lead, TPART, TASH, % VOL, PFOUP, PFODN 

Laboratory Comments: 

Contact Sample Tracker for proper sampling containers and preservation procedure. (503) 229-5983