## Fiel d Samplin g Referenc e Guid e



# Revisio n 6. 0 - UNCONTROLLE D DOCUMEN T

Decembe r

199 8

Orego n Departmen t

b f Environmenta l Qualit y Laborator y Divisio n 171 2 S.W
. Eleventh Avenu e Portland , Orego n 9720 1

### Tabl e o f Content s Decembe r 199 8 i I
. INTRODUCTIO N 1 II
. INFORMATIO N CONTACTS..
. 1 SAMPLIN G & ANALYTICAL INFORMATIO N 1 SAMPL E TRACKER

- '. / ORGANI C LABORATOR

Y - 2 INORGANI

C LABORATOR

Y - 2 AI RMONITORIN

G - : 2 WATE RMONITORIN

G - , 2 BIO-MONITORING

- 2 QUALIT Y ASSURANC

E - ^ '
. : 2 ADMINISTRATION

- 2 m . SAFET Y CONSIDERATION S 2 DE Q SAFETY COMMITTEE 3 PORTABLE "SNIFFERS " 3 CHEMICAL PRESERVATIVE S : 3 Preservative s commonl

y provide d 4 Materia l Safet

y Dat aSheet s (MSDS ) 4 IV
. INVESTIGATION S 5 ORGANIC S : : '. 5 VOLATIL E ORGANI

C COMPOUND S (VOC) 6 SEMI-VOLATIL

E ORGANI

C COMPOUND S (SEMI-VOLs , BNAs ) 6 PETROLEU

M I N SOIL S 6 OI L & GREASE : ..... 6 Other Organic s 6 INORGANIC S 7 METALS
. ; : 7 NUTRIENTS \8 BIOLOGICA

L OXYGE N DEMAN

D (BOD ) 8 TOXICITY CHARACTERISTI C LEACHIN G PROCEDUR E (TCLP ) : 8 BIOLOGICA

L '
. 9 FIELD ANALYSI S 1 0 DISSOLVE

D OXYGE N (DO) '. 1 0 ALKALINITY

, CONDUCTANCE, PH , ETC
. 1 0 V
. COMPLIANC E INSPECTION S 1 0 NPDES , WPC

F ; 1 0 SPLIT SAMPLIN

G O F STP' S FORCOMPLIANC E INSPECTION S 1 0 VI
. SAMPLIN G AN

D ANALYSI S PLAN 1 2 ADVANCE D NOTIC E O F PLANNE D SAMPLIN G ACTIVIT Y 1 3 VII
. QUALIT Y ASSURANC E
. , 1 5 DE Q LABORATOR

Y SAMPL E ACCEPTANC

E POLIC Y '. 1 5 VIII
. SAMPL E COLLECTIO N 1 6 WATE RSAMPLE S '.. k
. 1 7 Groundwater

1 7 Surfac e water

1 7 AIR: :i 8

### Tabl e o f Content s SOIL/SEDIMEN

T
. - 1 8 SUSPEC T H

W CONTAINERS 1 8 IX
. SUBMITTIN G SAMPLES , REQUES T FO RANALYSIS..
. 1 9 REQUES T FORANALYSI S FOR M .'
. 1 9 CHAI N OFCUSTOD Y 2 2 FIRS T CUSTOD

Y LEVE L •.,.2 2 SECON D CUSTOD

Y LEVE L '. '..2 2 SAMPL E SHIPMEN

T : 2 2 FIEL D NOTEBOOKS : 2 3 CORRECTIO

N T O DOCUMENTATION..,. : 2 3 APPENDI X A SAMPLIN G FO RVOLATIL E ORGANIC S 2 5 Contaminatio n 2 5 Preparatio n 2 5 Samplin g an

dDocumentatio n '
. 2 5 Sampl e Collectio n ; 2 5 APPENDI X B SAMPLIN G PROCEDUR E FO RDISSOLVED OXYGEN .....2 7 INTRODUCTION.. : „... ; ;2 7 SAMPL E COLLECTION ^ 2 7 SAMPL E PRESERVATION 2 7 APPENDI X C FIEL D FILTRATIO N PROCEDUR E 2 9 APPENDI X D LEGA L SAMPL E CHAIN-OF-CUSTOD Y PROCEDUR E ...3 1 Purpos e : : ; 3 1 Pre-samplin g 3 1 Sampl e Collectio n 3 1 Transfe r o f Custod y 3 2 Laborator y Custod y 3 2 Reference s , ; : 3 5 APPENDI X E SPIKES , SPIK E DUPLICATES ? 3 5 Surrogat e Spike s 3 7 PRESERVATIO

N CODE S 4 1 CONTAINE

RCODE S 4 1

### DE Q LAB : Fiel d Samplin g Referenc e Guide Decembe r 199 8 Revisio n 6. 0 - UNCONTROLLE D DOCUMEN

T Pag e 1 

# I
. Introductio n Th e goa l o f DE Q Lab' s Fiel dSamplin g Referenc e Guid e i s t o provid e Regiona l and Progra

mstaf f wit h information they needt o mak

e knowledgeabl e an

defficien t us e ofth e resource s availabl e fromth e Laborator y Division
. Laborator y service s availabl e include : broa dtechnica l capabilitie s i

n qualitativ e an

d quantitativ e inorganic , organic , microbiological , microscopic , an d biologica

l samplin g an

danalyse s o f

air , water , soil , sediment , an d tissue ; dat a validation , statistica

l dat aanalysis , an

dqualit y assurance ; analytica

l dat ainterpretation ; etc . Th e La b Divisio n i s comprise do f between 6 0 an

d 7 0 permanent

an d temporar

y staff , wit h cumulativ e experienc e considerably in exces s o f

60 0 years . Th e Divisio n i s divide dinto seven functiona l sections : Ai

r Monitoring , Wate

r Monitoring , Bio-monitoring , Inorgani c Lab , Organi c Lab , Qualit y Assurance , an

d Administration
. Eac h yea r th e La b log s in , analyzes , an

d report s dataon approximately 1400 separat e Cases , each consistin g o f from1 t o 7 5 samples
. Th e numbe

r o f individua l analyte s reporte dpe

r sampl e ca

n var y from1 t o 80 , o

r more . O n th e average . La b suppor t fo r Ai r Quality , Water

Quality , Hazardou s an

dSoli dWaste , an

d Environmenta

l Cleanu p Program s account fo r approximately 38% , 49% , 9% , an d6 % o f th e Lab' s resources , respectively'
. Th e DE Q Laborator

y i s locate da

t 171 2 S W Elevent h Avenue , Portland , O

R97201 , in th e Scienc e II Buildin g o n th e campu s o f Portlan d Stat

e University , between Mil

l an d Montgomer

y streets . I

t occupie s th e groun d and basemen t leve l floor s o n th e wes t

sid e ofth e building
. 

# II
. INFORMATIO N CONTACT S Infor mth e Laborator

y a s early a s possibl e o f

you r samplin g event . Preferabl y prior t o sample collection , t o insur e tha t bot h you r need s an d th e Laboratory' s ar

e me t i n atimel y manner . Contac t th e Sample Tracke

r fo r information on sampl e requirement s (Q A Manual) , samplin g equipment need s an d availability , field preservatio n (Q A Manual ) o r filtration requirements , sampl e transport , an d scheduling
. Spea

k to th e appropriat

e La b Manage r about analytica l capabilitie s tha

t ar e available
. Fo r parameter s havin g ashor

t holdin g tim e (2 4 hours , o r les s refe r t o Tabl e 2) , schedul e sampl e collectio n thoughtfully
. Infor

mth e La b o f your inten t t o sample , approximat

e numbe r o f samples , wha

t yo u ar e lookin g for, an d when sample s will b e delivere dto th e lab
. Analyst s nee d t o b e mad e awar e o f you r need s an d expectation s s o schedule s an

dworkload s ca

n b e adjusted t o accommodat e th e work
. 

## Samplin g & Analytica l Informatio n 

## (503 ) - 22 9 - 598 3 SAMPL E TRACKER

Bo b McCoy : Typ e o f

containe r fo r specifi c tests , genera

l inorgani c an

d organi c samplin g inquiries , samplin g supplies , sampl e preservation , equipment , preliminar y results
. Statu s o f analytica l work s i n progress .

Base do n 199 3 data, prio r t o reorganization , whic

h combine dBC D an dHS W int o on e Division : WMC
.

### DEQLAB : Fiel d Samplin g Referenc e Guid e Decembe r 199 8 Revisio n 6. 0 - UNCONTROLLE D DOCUMEN

T Pag e 2 ORGANI C LABORATOR Y - Dan Hickman : Organi c an d Physica l Tes t Laborator y capabilities , sample requirements , methods , dat ainterpretation
. INORGANI C LABORATORY

Ro n McCartney : Inorgani c Laborator y capabilities , sampl e requirements , methods , data interpretation
. METALS



### Kare n Yates : Analytica

l methods , datainterpretation , an d tes t requirerrients
. NONMETALS



### WilliamCalzaretta : Analytica l methods , dat ainterpretation , an d specifi c tes t

requirements
. AI RMONITORING

Jef f Smith : Ai r

an d meteorologica

l monitorin g procedures , capabilities , datainterpretation
. WATE RMONITORING

Gre g Pettit : Wate

r sampling/monitorin g procedures , equipmen t loans , samplin g capabilities , datainterpretation
. Surfac e o r groundwater , soils , sediments , estuaries , lakes , streams , . rivers , etc . BIO-MONITORIN G - Ric k Hafele : Specifi c informatio n regardin g biologica l o r biotoxicit y testing , interpretatio n o f aquati c toxicit

y data , etc . QUALIT Y ASSURANCE

RaeAn n Haynes/Chri s Redman/Pau l McKay : Genera l sampling an

d analytica

l QA/Q C requirement s an

d assistance , Q

A projec t pla n development , dataqualit

y needs , data qualit y assessment , split

sampl e results , coordinatio n o f Q A requirements , etc . Statu s o f dat areports . ADMINISTRATION

Ric k Gates : Reassignment

o f wor k priorities , budgeting , cos t

recovery , overal l La

b administration
. 

# III
. Safet y Consideration s An y field activit

y o r complaint investigatio n ca

n lea dint o th e realmofth e unknown
. Approach an y complain

t investigatio n a s apotentially hazardou s event . Obtain th e prope r trainin g t o recognize , dea

l with , an d protec t yoursel f fromhazardou s chemicals
. I f you hav e an

y question s about

wha t you migh t b e dealin g with , utiliz e existin g resource s (e.g
. MSDS , literature
. Lab ) an d contac t the appropriat

e authorit y {e.g
. DE Q Healt

h & Safet y

### DE Q LAB : Fiel d Sampling Referenc e Guide Decembe r 199 8 Revisio n 6. 0 - UNCONTROLLE D DOCUMEN

T Pag e 3 Manager , La

b Managers , Safet

y Committee , etc.)
. Th e DE Q Safet y Committee

^ continually review s safet

y an d healt h needs
. Th e Healt

h & Safet y Manage r ca n recommendand suppl

y th e mos t appropriat

e Persona l Protectiv e Equipment
. 

### DE Q Safet y Committe e Gen e Rushin g Dal e Chipman : Sta n Okamoto : Susa n Steronko Marti n Loring : Cheryll Parr : Ai mCox : Dav e S t Louis : Bo b Marshall : RaeAnn Haynes : Danie l Murphy : 

## Portabl e " (DE Q Healt h an d Safet y Manager

) MS D LA B VI P W Q W R NW R WMC E R LAB VI P 

## Sniffers " 229-616 0 229-602 2 229-598 3 731-305 0 „ 229-541 5 378-8240 , x23 7 229-665 3 229-553 2 (541)-278-460 0 229-598 3 731-305 0

Portabl e photoionizatio n detector s (MicroTip'^ " an d HNuTM ) ar e availabl e t o scree

n fo r toxi c gases . Th e MicroTi

p i s als o capabl e o f

collectin g a

n ai r sampl e i n abag fo r subsequent

qualitativ e o

r quantitativ e analysi s a

t th e Lab
. WM

C ha s a n Organi c Vapor

Analyze r (OVA ) an

dRegion s posses s Combustibl e Ga s Analyzer s (CGA-GasTekTM)
. Thes e are "sniffers, " use d t o scree n fo r hazard s prio r

t o site entry . Understan d tha t the y d o no t necessarily provide qualitativ e result s {e.g
. canno t alway s discriminate on

e pollutan t

fro mthe next) , no

r ar e the y alway s quantitative
. 

### Chemica l Preservative s I n order t o stabiliz e sample s fo

r certai n test s i

t i s necessar

y t o addachemica

l preservative , i

n additio n to immediat

e cooling , storage , an

dtranspor t o n ice
. Failure to ad

dth e prope

r preservative , o

r amount , could result

i n sample s deterioratin g t o th e poin

t o f bein g useles s fo

r analysis
. Th e DE Q Laborator

y supplie s sampl e preservativ e chemical s t o agenc y persoimel o n request . Staf

f requestin g thes e chemical s i s expecte dt o becom e familia r wit h th e necessar

y safet y precaution s an

d follo w them , o

r t o ask fo r assistance
. Liqui d preservative s ar

e provide d i

n 5 0 niilliliter

re/Zo « bottles ^ havin g integra l droppe r spout s wit

h tethere d closures
. Sodiu

mhydroxid e i s supplie din screw-ca p plasti c bottle s containin g les s tha n 2 5 gram s o f

pure causti c pellets
. Eac h bottl e i s labele dwit h th e appropriate hazar

dwarning s an

d seale d i n aZip-Loc

k plasti c ba g t o contain leakage , shoul dth e bottl e closur e fai l i n transit
. An

v liqui dobserve d inside th e plasti c bag should be assumed to be • leakag e fromth e bottle , i

n which cas e th e bag should b e opene dwit h caution , wearin g han

d an d ey e protection , an

d thoroughl y rinse d wit

h water . Solidsodiumhydroxide pellet s are deliquescent , tha t is , they absor

b moistur e from th e air
. Thi s chemica

l i s capabl e o f

absorbin g enough moisture to pu t itsel f int o solution
. Mak

e sur e tha t lid s ar e screwe ddown tightiy !

^ A s o f Jun e 1995
. ^ Whe n thes e Teflo

n bottle s becom

e empt y DON' T thro

w the maway ! The

y cos t nearl y $2 0 each
. Retu

mthe mt o th e La b s o the y ca n b e refilled
.

### DEQ LAB : Fiel d Samplin g Referenc e Guid e Decembe r 199 8 Revisio n 6. 0 - UNCONTROLLE D DOCUMEN

T j Pag e 4 Preservative s commonl y provide d Concentrate d Sulfuri c Acid , H2SO4 , 95+ % Concentrate d Nitri c Acid , HNO3 , 70+ % Concentrate d Phosphori c Acid , H3PO4 , 85 % Concentrate d Hydrochlori c Acid , HCL , 37 % Soli dSodiu

mHydroxide , NaOH , 100 % A t th e concentratio n supplie dfo r sampl e preservatio n thes e chemical s ar e highl y corrosiv e an

d capabl e o f

causin g severe physica l damag e to skin , eyes , an dclothin g unles s th e prope r precaution s are observed
. Treate d wit h appropriate respect , an

dfollowin g afe

w simpl e rules , thes e chemical s shoul d no t caus e injury
. 

### Materia l Safet

y Dat aSheet s (MSDS ) On e sourc e o f

informatio n on hazard s associate dwit h each o f thes e chemicals , an

d th e precaution s tha

t should b e taken durin g use , ar

e th e Materia

l Safet y DataSheet s (MSDS)
. MSD S for eac h ofth e abov e chemical s mav b e obtaine dfro mth e Lab
. Whe n readin g th e MSD S keep i n min dtha t yo u ar e dealin g wit

h les s tha n 5 0 milliliter s o f

liquid , an d les s tha n 2 5 gram s ofth e solid
. Man

y ofth e precaution s cited {e.g
. respirator y protection , self-containe d breathin g apparatus , etc. ) ar e intende dfo

r emergenc y respons e personnel dealin g wit h bul k o r industria l quantitie s ofth e material
. The primar

y hazard s pose db

y thes e chemical s are :


### • Chemica

l bum s t o th e skin an

d eyes .
• Chemica

l damag e t o clothin g an

d footwear
. All thes e chemical s ar

e capabl e o f

causin g Sever e an d permanen t damag e t o th e eyes . The following precaution s mus t

alway s b e take n whe

n handlin g aci do

r causti c fo r preservin g samples :


### • Transpor

t preservativ e container s i

n arestrained , uprigh

t position
.
• Wea r appropriat

e protectiv e eyewear .
• Wea r chemically resistant

syntheti c gloves
.
• B e prepare d t o dea

l wit h accidents
. Th e Laborator

y wil l provide , o n request , protectiv e ey e wear , syntheti c gloves , an d "pH 6. 9 buffer " which i s usefu l to neutraliz e skin o

r clothin g expose d to acid o r caustic
. W

e recommen

d tha t staf f engage d i n sampl e collectio n carry , a t minimum , aone-gallo n ju g o f wate r i n their vehicl e fo r washin g i n emergencies
.

### DE Q LAB : Fiel d Sampling Referenc e Guide Decembe r 199 8 Revisio n 6. 0 - UNCONTROLLE D DOCUMEN

T Pag e 5 

# IV
. Investigation s [ OBSERV E AN D DOCUMENT ! Loo k fo r clue s tha t sugges t abnorma l condition s e.g . sfressedvegetation , dea d o r dyin g insect s o

r animals , soil staining , fiimes , crystals , oil , puddle s o f liquid , abandone d containers , unusua l colors , odors , phas e separations , etc . Whethe r o r no t t o collec t asampl e i s your

decision
. Yo

u mus t mak e th e judgmen t

whethe r o r no t your observation s warrant chemica l characterizatio n ofth e materia l i n question
. I f

asampl e i s coUected i t

mus t represen t

th e conditio n ofth e sit e a s muc h a s possible
. If asampl e i s collected , get

a s much ofth e materia

l a s you can . Th e Laborator y need s areasonabl e amoun t o f sampl e to conduc t

tests . Fo r safet y consideratio n fill th e bottl e t o th e neck no t t o th e cap . Fiel d observation s shoul d b e documented , usin g in k i n apermanently , boun d notebook
. Photograph s should b e taken , i f possible
. If

yo u fee l tha t there i s apotentia

l enforcemen

t actio n in th e making , contac t th e Enforcemen

t Sectio n of Regiona l Operation s t o lea

mwha t typ e o f evidenc e i s neede d t o suppor t a n enforcemen

t action
. Appearance , odor , o r

nearb y source s ma y sugges t wha t t o tes t for
.



### , • / • ' \ ' ^ \

^ CAUTION : , ^ , ' \- \

- : B e ver y cautiou s o f unfamilia rodor s /

'" ' '' A VOI D openin g unlabele d container s to mak e apreliminar

y assessment

o f sample , i (B e especiall y war

y o f container s tha

t exhibit crystal s aroun dth e cap , the y coul d be extremel

y explosive organi c peroxide s Whin expose dto ligh t o r air , ether s can for

mperoxides^ that

can

_easil y detonate t

) 

### ORGANIC S Organi c substance s ma

y appea r a s tar , wax , oil , crystallin e o r amorphou s solids , colore d o r colorles s liquids
. Sample s ma

y b e odorles s o

r their smell ma y b e sweet , sour , biting , petroleum-like
. Attemp t t o characteriz e th e sampl e appearanc e an

dodor , an d describ e the

mo n th e Analysi s Reques t

Form
. Th e mor

e information yo

u provide th e better ar e th e Lab' s chance s o f

identifyin g a

n "unknown " contaminant , an d successfull

y quantifying it
. Collec t sample s fo

r organi c analysi s i

n DE Q Lab-supplie dcontainer s (se e Tabl e 2 ) which hav e bee n speciall y cleane d to eliminate interference
. Becaus e organi c analytica l method s ar

e expensiv e i

t i s imperativ e tha

t sample s b e collecte di n acceptabl e container s t o avoi dhavin g th e analysi s invalidate d a s aresuh o f containe r contamination
. I f you are caugh

t i n abin dwithou t th e correc t

containers , call th e Laborator y s o w e ca

n wor k ou t a n acceptabl e altemative
. I n peneral , plasti c container s shoul d NO T h e use d t o collec t .sample s fo rorgani c analysis
.

### DE Q LAB : Fiel d Sampling Referenc e Guide Decembe r 199 8 Revisio n 6. 0 - UNCONTROLLE D DOCUMEN

T Pag e 6 VOLATIL E ORGANI C COMPOUND S (VOC ) VOC s are alarg e group o f organi c solvents , cleaners , an ddegreaser s tha

t evaporat e a t ambien t temperature . Although they ca

n volatiliz e quickly , frace amount s ten d t o persis t i n soil s an d water . Thi s persistency , coupled wit h their mobility , make s groundwate r contaminatio n aprimar

y concemfollowing aspill o r releas e o f VOC s int o th e soil
. Whe n requestin g VO C analysis , i t i s important

t o conve y th e typ e o f

situatio n yo u are investigatin g (dr y cleaner , UST , spill , etc. ) an dwhethe r o r no t yo u ar e intereste di

n specifi c chemical s o r

material s suc h a s gasoline , kerosene , trichlororethylene , o r benzene
. Thi s informatio n wil l help th e la b choos e a n analytica

l metho d appropriat

e fo r you r situation
. Ou

r defaul t VO C metho di s Metho d 8260 , aGC/M S procedur e tha t analyze s fo

r roughl y 6 5 volatil e organic s plu s Tentatively Identifie dCompound s (TICs)
. Unfortunatel y no t al l VOC s ca

n b e analyzed usin g thi s method; ' henc e ou

r need t o kno w a s much a s possibl e about th e possibl e contaminant

source . 

### SEMI-VOLATIL E ORGANI C COMPOUND S (SEMI-VOLs , BNAs ) Semi-Vol s {ak

a8270Bor Base/Neutral-Aci dExtractables , "BNA" ) comprise s alarg e group o f chemical s tha t include severa

l categories : phenols , chlorophenols , phthalates , pentachlorophenol , polynuclea r aromatics , an

d man y others
. Th e metho dcover s approximately 8 5 specifi c analytes , an dals o provide s provisiona

l identificatio n o f additiona l analyte s a s Tentatively Identifie dCompound s (TlC's)
. A s wit h VOC s th e lis t

o f analyte s i s large , but

not universal
. Ifth e questio n arise s whethe r o r not aparticula

r chemica l ca n b e teste d fo

r by thi s method , call th e Organi c Sectio n a

t th e Lab
. 

### PETROLEU M I N SOIL S Method s fo

r analysi s ar

e designate di

n Oregon' s Soi l Matri x Rule s for Petroleu mUndergroun d Storag e Tan k Cleanup s (OA

R340-122-350)
. Petroleumproduct s i n soi l are firs t

identified an

d then quantifie d b

y th e Northwes t Tota l Petroleu mHydrocarbo n (NWTPH ) methods : NWTPH-HCI D i s aqualitativ e screen t o determin e which petroleumproduct s (ifany ) i s present , an d wha t subsequent

quantitativ e method s ma

y b e required
. NWTPH-G x i s th e quantitativ e metho dfo r gasoline
. NWTPH-D x i s th e quantitativ e metho d fo r diesel an dothe r heav y oils
. 

### OI L & GREAS E Classica l "Oi l & Grease " measure dth e pola r (anima l fats , vegetabl e oils , etc. ) an d non-pola

r (petroleumfiiels , minera l oils , etc. ) Freon""^" extractabl e materia l i n asample
. It

wa s sometime s use d in conjunctio n wit h EPA' s Tota

l Recoverabl e Petroleu mHydrocarbo n metho dt o distinguis h betwee n pola r an d non-pola

r components . DE Q La

b i s usin g EP A Metho d1664 , n-Hexan e Extractabl e Materia l (HEM) , which ca

n b e used wit

h silic agel cleanu

p to determin e TP

H o r NWTP H Method s a s appropriate
. 

### Othe r Organic s Other commo n analyse s use d t o identif y o r characteriz e unknovr

aorgani c contaminant s include MBAS , Glycol/Fluorescein , Lignin-Tannin , Tota l Organi c Carbo n (TOC) , Chemica l Oxyge n Deman d (COD) , Tota l Organi c Halogen s (TOX) , an dFormaldehyde
. "•"MBA S
. - - - -.^-

- . . . . . _ _ A non-specifi c tes t

fo r Methylen e Blu e Activ e Substances
. Anioni c surfactants , which ma y include LAS (Linea r Alkylbenzen e Sulfonates ) othe r sulfonate s an

d sulfat e ester s (colorimetri c procedure)
. MBA S ca n detec t th e presenc e of

detergents
. Glycol/Fluorescei n

### DE Q LAB : Fiel d Sampling Referenc e Guid e Decembe r 199 8 Revisio n 6. 0 - UNCONTROLLE D DOCUMEN

T Pag e 7 Ca n identif y antifreeze
. Fluorescei n i s th e ingredient responsibl e fo

r antifreeze' s vibrant

green color , an

d i s als o ady e used t o monitor

wate r flow. Unlik

e glycol , fluorescein i s not considere d harmfu

l to th e environment
. Lignin-Tanni n A non-specifi c tes t

fo r hydroxylate daromati c compound s foun d i n lignin and tanni n compound s (colorimetri c procedure ) characteristi c o f tre e bar k leaching
. Tota l Organi c Halogen s (TOX ) Measurement

usedt o estimat

e tota l quantit y o f dissolve dhalogenate d organi c materia l in awate r sample
. Indicativ e o f

contaminatio n b

y syntheti c chemicals
. PCB s an d Chlorinate dPesticide s v ^ Bot h extracte d b

y th e sam e method , therefor

e asingl e containe

r ma y b e use d t o sampl e fo

r thes e tw o analyses
. Othe

r organi c test s require aseparate container fo r each metho d o f

extraction
. 

## INORGANIC S Inorgani c contaminant s ten dt o b e crystalline , dissolve dsalts , o r suspende d solid s i

n water . The

y include all combination s o f

elements , wit

h th e exceptio n o f

compound s containin g carbon , whic h ar e defme d a s Organics
. Inorgani c acid s and som

e caustic s hav e asharp , irritatin g odor
. Collec t inorgani c sample s i

n Laborator

y supplied plasti c container s describe din Tabl e 2
. Characterizatio n o f

unknown inorgani c contaminant s include s physica l measurement s (Tota

l Suspended Solids , Tota l Solids , Turbidity , Conductance , an dpH)" , metals , an

dnutrient analysis
. Turbidity , p

H an d orthophosphat

e sample s hav e ver y shor t

holdin g times , thu s thes e analyse s mus t b e starte d immediately upon sampl e receipt
. 

### METAL S Whether t o reques t Dissolved , Total , o r

Total Recoverabl e Metal s analysi s i s another decisio n you'l l hav e to make
. Dissolve d metal s ar

e wate r soluble , defineda s passin g throug h a0.4 5 micron filter, wherea s tota l an d tota l recoverabl e metal s include thos e containe di n particulate matte

r an d thu s les s availabl e t o th e enviroimient
. The analytica l differenc e between tota

l an dtotal recoverabl e metal s i s th e severit y ofth e aci d digestio n procedur e utilize db y th e La b to prepar

e sample s fo

r analyses
. Tota

l Metal s digestio n i s mor

e aggressive
. Dissolve d metal s sample s mus t

b e filtere di n th e field , immediatel y afte r collectio n an d befor e addin g aci d preservativ e (Appendi x C)
. Tota

l Recoverabl e metal s i s aclassificatio n fromth e drinkin g wate r regulations
. I f

Reques t fo r Analysi s doe s no t

specif y Dissolve d o

r Total , Tota

l Recoverabl e metal s wil l b e th e tes t assigned
. Th e La b need s t o kno w wha

t leve l o f sensitivit y o r detectio n you r

project requires , i

n orde r t o selec t th e appropriat

e analytica l method
. Ther

e ar e tw o choices : Inductivel y Couple d Plasm a(ICP) an d Graphite Furnac e Atomi c Absorptio n (GFAA)
. Th e ICP an dGFA A method s hav e approximately th e sam e minimu mreportin g limit , however , IC P i s generally faste r an d cheaper
. Reserv e request s fo r GFA A to thos e situation s wher

e th e metho d i s specially require db

y the progra

msuc h a s afe w drinkin g ^yate

r metals
. Analyse s fo

r Mercur y use s differen

t digestio n an

danalytica

l procedur e tha n th e othe r metal s an d aseparat

e sampl e mus t b e collected
. Request s fo

r mercur y analysi s mus t

b e specifically identified o n th e Reques t

fo r Analysis , an

d separate sample s collected , o r i t will not b e performed
. Physica l measurement

s ar e performe db y th e Organi c Laborator y Section
.

### DE Q LAB : Fiel d Sampling Referenc e Guid e Decembe r 199 8 • Revisio n 6. 0 - UNCONTROLLE D DOCUMEN

T Pag e 8 NUTRIENT S Nutrient s include Tota

l Organi c Carbo n (TOC) , Chemica l Oxyge n Demand (COD) , Nitrate-Nitrite (NO3+NO2) , Tota l Kjeldah l Nitroge n (TKN) , Ammoni a(NH3) , Dissolve d (OPO4) , an d Tota l (TPO4 ) Phosphate
. Thes e analyte s ca n occur naturally a

t lo w level s i

n th e ecologica

l system . Elevate dvalue s ar e frequently indicativ e an

d asourc e o f problems
. Discharge s fromindustry , municipa l wastewate

r treatment plants , an d agricultura

l operation s ca

n increas e certai n nutrient

levels
. Nitroge n nutrient s are reporte d a s mg/ L of equivalent

hifrogen , an

d phosphat

e nutrient s are reporte da s mg/ L equivalent

phosphorous
. Ther e ar e awide variet

y o f chemica l forms tha

t phosphat e ca n exis t in , an d b e analyze d for^
. Form s include Total , Tota l Reactive , Tota

l Aci dHydrolyzable , Tota

l Organic , Dissolve dReactive , Tota l Dissolved , Dissolve d Aci d Hydrolyzable , an

dDissolve dOrganic
. Notif y th e La b wel l i n advanc e ifan y for

mothe r tha n Tota l o r Dissolve d Reactiv e phosphat

e are o f interest
. DE Q La

b use s th e Molybdate-Ascorbi c aci d fo r Dissolve d Reactiv e Phosphat e (OPO4) o n filtered samples , an

dMolybdate-Ascorbi c aci dproceede d by persulfate-autoclav e digestio n fo r Tota l Phosphat e (TPO4)
. Method s use db y othe r lab s ma y vary , s o datacompariso n coul d b e difficult
. Tota l Organi c Carbo n (TOC ) A nonspecifi c tes t

measurin g organi c carbo n content o f awate r sample
. Reporte d as milligram s o f Carbon pe r liter
. Chemica l Oxyge n Deman d(COD ) Measur e ofth e oxygen equivalen

t o f organi c matte

r containe di

n asampl e tha

t i s subject t o oxidatio n b

y a stron g chemica

l oxidant
. 

### BIOLOGICA L OXYGE N DEMAND (BOD ) Sample s ma

y b e hel d u

p to 4 8 hours , bu

t les s tha n 2 4 hour s i s preferred
. BO D sample s wil l b e accepted betwee n 08:0 0 A M Tuesda y and 12:00 A

M Friday
. Acceptin g BO D sample s a t an y other tim e wil l requir

e overtim e work , an d mus t b e pre-approve db

y th e Inorgani c Sectio n Manager
. Durin g the perio d followin g collection , an d includin g transpor t t o th e Lab , biologica

l sample s mus t

b e kept coo l on ic e (4°C)
. 

### TOXICIT Y CHARACTERISTI C LEACHIN G PROCEDUR E (TCLP ) TCL P extractio n i s usedi

n RCR A to evaluat

e hazardou s wast e characteristic , replacin g the EPto x Method
. It i s used t o asses s th e leachabilit y o f metal s an d certai n organic s unde

r precisely controlle d conditions
. TCL P procedure s ar

e als o used i

n DEQ' s Soi l Cleanu p Rules
. Whe n askin g fo

r "TCLP " o n samples , b e awar

e ofth e method's.limitations
. TCL P extractio n i s a

n involved an

d relativel y expensiv e metho d t o run , dependin g o n th e natur

e ofth e samples
. Sample s havin g muhipl e phase s (water-oil , water-solid , oil-solid , water-oil-solid ) ar e difficul t to dea l wit h unde r thi s protocol
. Sufficien

t sampl e mus t

b e collecte d t o provide a

n adequat e quantit y ofeae h phas e fo

r bot h inorgani c an

d organi c TCL

P extractions : approximately 50 0 gram s o f solid , o r a t leas t 1 liter o f liquid
. Mor

e sampl e materia

l i s require da s th e rati o o f

aqueous:soli d(other) phas e increases
. If asample contain s les s tha

n 15 0 gram s soli d (other

) phas e i n th e conventiona

l sampl e size , alarge

r quantit y o f sampl e i s necessar

y jus t to ru n th e TCL P inorgani c tests . Tabl e 4500-Pl
. Standar

dMethod s fo r th e Analysis o

f Wate r an d Wastewater

. APHA-AWWA

, 18t h Edition, p . 4-109 , (1992)
.

### DE Q LAB : Fiel d Samplin g Referenc e Guide

Revisio n 6. 0 - UNCONTROLLE D DOCUMEN

T Decembe r 199 8 Pag e 9 I f TCLP organics , duplicate , matri x spike , o r matri x spik

e duplicat e analyse s ar

e requeste d considerably mor e sampl e i s needed
. Accordin g th e TCL P protoco l th e La

b need s t o hav e 10

0 gram s o f

soli d to perfor

mth e extraction
. Extractio n ca

n b e don e o

n les s material , bu t

i t compromise s th e integrit

y ofth e procedur

e an d increase s th e likelihoo do f

error . A s aguideline , se e Tabl e 1
. 

## Tabl e 1 % Soli d(other ) 2 % 5 % 10 % 15 % 20 % Desirabl e Sampl e

7. 5 liter s 3. 0 liter s 1.5 liter s 1. 0 liter s ( « quart) 0. 5 liter s ( « pint ) I n general , a1-gallo

n sampl e ( * 3. 8 liters ) i s apractica l limit
. Whe n requestin g TCLP o

n asampl e i

t i s more efficien

t fo r th e Organi c sectio n t o analyz e fo r Total s {e.g
. Tota

l VOCs ) first, an

dthen t o perfor

mTCLP on an

y sampl e where aTota

l i s observe d tha

t exceed s th e TCL

P Regulator

y Limit
. It serve s n o purpos e t o d

o aTCL P extraction , followedb

y analysi s ofth e TCL

P extract , i f

there isn' t enough regulate dsubstanc e in th e sampl e i n th e first plac e t o exceed th e TCLP standard
. O n th e othe r hand , i t i s mor e efficien t fo r th e Inorgani c sectio n t o perfor mth e TCL

P extractio n righ

t away . Submittin g sample s fo r inorgani c Tota l Metals , wit

h th e instmctio n that

sample s havin g hig

h level s o f regulate d metal s shoul d b e subjected to TCLP , wil l take considerably longe r tha n simply requestin g TCLP
. Notic e tha t TfV O TCL P protocol s ar e liste d i n th e Cod e o f

Federa l Regulations : 1 ) 4 0 CF RPar t 261 , Appendix II , Metho d131 1 Toxicit

y Characteristi c Leachin g Procedure ; an d 2 ) 4 0 CF

R268 , Appendix I , Toxicit

y Characteristi c Leachin g Procedure
. Th e metho di n Par t 26 1 i s th e revise d versio n of Par t 268 , th e origina

l version
. Furtiier , Par

t 26 1 wa s modified , effectiv e Jun e 29,1990 , i n 5 7 F R55114-5611 7 (publishe d Novembe r 24,1992)
. 

## BIOLOGICA L Biologica l Oxygen Demand(BOD ) i s anonspecifi c tes t used t o evaluate consumptio n o f Dissolve d Oxyge

n (DO ) b y biologica

l processe s incubate da

t 20° C ove r aperio d o f

5-days
. It

i s abioassa

y procedur

e tha t i s normall y applie dto wate

r samples , althoug h i t

ca n b e applie d t o sedimen

t a s well
. BOD s conventionally ar e done ove r a5

- da y period , howeve

r longe r time period s ar e possibl e (e.g
. 14- , 28-day)
. Specia l request s ar

e necessar y fo r an y bu t th e 5-da y test . BOD s ca n evaluate th e oxyge

n depletio n cause db

y carbonaceou s materia

l an d nitrogen specie s (BOD) , suc h a s TK N an d ammonia , carbonaceou s materia l alon e (CBOD) , o

r nitrogen specie s alon e (NOD)
. Specia l request s ar

e necessar y fo r an y tes t othe r tha n BO D o r CBOD
. Biologica l sample s ar

e analyze db

y bot h th e Inorgani c (BOD , CBOD ) an d microbiologica

l la b (Coliform , E
. Coli , etc.)
. Collec t

liqui dsample s i

n speciall y cleane d DE Q container s (refert o Tabl e 2)
. La b mus t b e notifie d prio r

t o sampling
. BOD sample s fo r surfac e an

d receivin g water s lo

w i n BOD ar e collecte d i

n specia l glas s BO D bottles
. It i s desirabl e to determin e Fiel dD O on thes e samples , prio r t o sendin g to La

b (se e procedur

e i n Appendix B)
. Whe

n Fiel d D O measurement s aren' t made , D O i s les s tha

n 5 mg/L , o

r D O exceed s 120 % Saturation , specif y th e B0DS 2 tes t o n th e Reques t

fo r Analysi s t o infor

mth e La b analys t ofth e nee d t o perfor

mth e initia

l D O o r %Sa t test . >

### DE Q LAB : Fiel d Sampling Referenc e Guide Decembe r 199 8 Revisio n 6. 0 - UNCONTROLLE D DOCUMEN

T Pag e 1 0 Bacteria l sample s wil l b e accepte dMonda y throug h Thursday
. Bacteria l sample s ma

y b e hel d fo

r amaximu m o f 3 0 hour s (tim

e elapse dfromcollectio n t o analysis)
. Fo r Regulator y Purpose s th e holdin g time on bacteria l sample s i s 6 hours ! 

## FIEL D ANALYSI S DISSOLVE D OXYGEN (DO ) A significan

t indicator o f strea mhealth , lo w D O i s frequently th e primar y caus e fo r fish kills
. Refe

r to Appendb

c B fo r fieldanalytica

l procedure
. Thi s analysi s shoul db e performed i n th e field becaus e D O sample s ar e no t stable
. Dissolve doxyge

n ca n chang e rapidly afte

r sampl e collection , dependin g on temperature , barometri c pressure , an d othe r dissolve dgases . 

### ALKALINITY , CONDUCTANCE , PH , ETC
. Othe r fieldanalyse s include Alkalinity , Conductance , pH , Temperature , Turbidity , and filtration. Obviousl y sampl e temperature will change , but pH ma y als o chang e ove

r shor t period s o f

time
. It i s recommende d tha

t p H b e measure din th e fieldwheneve r possible
. Som

e sample s requir

e filtration in th e field becaus e th e solubilit y o f som e substance s depend s on temperatur e an dpH
. 

# V
. Complianc e Inspection s NPDES , WPC F Refe r t o DE Q o r EP A inspectio n procedure s o

r guidelines , an

d revie w Permi t

requirements
. Ifth e sourc e i s require d t o repor t self-monitorin g tes t

datat o th e agency , an

dyo u intend t o investigat

e th e source' s analytica

l capability , collec t spli t samples
. Sample s wil l b e analyze dby bot h th e sourc e la

b an d DE Q Lab , resultin g i

n a n Inter-laborator

y comparison
. Leav e asplit-sampl e analysi s for m(For m1 o r For mII) * wit h th e source . Reques t

tha t the y fill i n their tes t result s an dretu mi t t o th e DE Q Q

A chemis t a t th e Laborator

y a s soon a s possible
. It

i s not necessar y t o limi t requeste danalysi s t o Penni t parameters . DE Q la

b will perfor

man y reasonabl e analyse s an

d prepare asplit compariso n report . Th e La b woul dappreciat e advanc e notic e o f spli t sampling
. Intra-laborator

y split s ar e ausefiil Q

C measuremen

t fo r ou r lab , a s well a s th e source' s lab
. Th e DE Q la b will onl y hold it s dat aunti l w e hav e complete d wor k on it
. The field inspector

i s responsibl e fo

r insurin g tha

t th e sourc e report s their

result s t o th e La

b Q A chemis t a s quickl y a s possible , particularly whe

n acompariso n i s wanted
. La b wouldappreciat

e receivin g amonthl

y forecas t o f complianc e split

sampling schedules
. 

### SPLI T SAMPLIN G O F STP' S FO RCOMPLIANC E INSPECTION S Split sample s shoul db e collecte d in asingl e larg e container , homogenized , an d then poure d int

o separate , clea

n sampl e bottles : one portio n fo r th e sourc e an

don e portio n fo

r DEQ
. Collectin g one gra

b sampl e fo

r the sourc e an

d a second , separat

e gra b sampl e fo

r DE Q i s no t

th e sam e thing
. To limit

varianc e to analytica

l techniqu e alone , i

t i s imperativ e tha

t bot h th e Sourc e an

dDE Q La b analyz e sample s tha

t ar e a s nea r identica l a s possible
. Common sewag e treatmen

t plan t (STP ) Split

Sampl e parameter s ar

e Feca l Colifor m(FC) , E.Coli , Tota

l Suspended Solid s (TSS) , pH , an

d Biologica

l Oxygen Demand(BOD)
. Dependin g o n th e source' s Permit , asample fo r CBOD
Obtai n blan k form s fromQ A Section, DE

Q Lab
.

### DE Q LAB : Fiel d Sampling Referenc e Guide Decembe r 199 8 Revisio n 6. 0 - UNCONTROLLE D DOCUMEN

T Pag e 1 1

ma y b e spli t also
. Th e DE Q la

b measure s p H o

n all BO D samples , even thoug h no t all STP' s follow thi s procedure
. Becaus e o f

limite dholdin g tim e requirement s thes e sample s mus t b e receive d a

t th e La b a s follows
. BACTERIA L sample s (feca l coliform , KColi ) mus t

b e receive d n o late r

tha n Noo n o n Thursday
. Fo r LEGA L samples , th e maximu

mholdin g time o f

6 hour s mus t

b e adhere d to , wherea s routin e sample s ca n b e hel d u

p to a maximumo f

3 0 hours
. Bacteria

l sample s are routinel y analyze dusin g th e Membran e Filtratio n (MF ) method
. Whe n analysi s fo

r a"non-routine " organis m(E.Coli , tota l coliform , feca

l strep ) i s required , notif

y th e La b i n advanc e s o tha

t specia l medi aca n b e prepared ' fo

r th e test . BO D sample s mus t

b e receive dn o late r

tha n NOO N o h Friday
. I f i t i s necessar

y t o sampl e betwee

n Noon Frida y an d08:0 0 A M o n Tuesday , th e la

b wil l hav e to schedul e someon e to com e i n th e following weekend t o complete th e test . Specia

l authorizatio n i s required , prio r to collectio n an

d shipmen t o f samples , whic h wil l b e receive d by th e La

b afte r 12:00 o n aFriday
. Unauthorize d sample s tha t d o no t fit th e routin e tim

e frame ma

y no t b e analyzed
. Norma l procedure i s t o collec t

a24-H r composit e sampl e ofth e influen

t an d a24-H r composit e ofth e effluen

t fo r BODs , TSS , an

dpH
. A gra

b sampl e ofth e effluen

t i s taken , after

th e Chlorin e Contac t

Chamber , fo

r Feca l Colifor m(FC ) an d E.Coli
. Th e Composite influen t an d effluen t sample s shoul d b e collecte d i n 100 0 m l "ST P polys" , an d th e FC/E C gra

b sampl e shoul db e collecte d i n asteril e wide-mout

h 12 5 m l " S bottle " containin g sodiu m thiosulfate t o destro y exces s chlorine
. Composit e effluen t sample s canno t

b e use d fo

r FC/EC sample s becaus e o f thei r length y chlorin e exposur

e (u p t o 2 4 hours)
. Th e ST P staf f shoul dtake their

own sample s fromth e sam e composit

e an d gra b sampl e a s th e DEQ inspector
. Th e DE Q La b andth e ST

P la b shoul dbegi n testin g a

t approximately th e sam

e time. Agre e upon atime fo r tes t set-up . and make anote o f

i t o n th e field sheet
. Usuall y th e inspector wil l arrang e fo

r tes t set-u p a t te n o'clock

A.M
. on th e da y followin g th e sampling
. ^ Writ e "Split " o n th e to p o f

Reques t fo r Analysi s form , alon g wit h agree dupo n "set-uptime. " Leav e acop

y ofth e "Split

Sampl e Result s Report " for m(For mI o r II ) wit h th e ST P staff , wit h instmction s t o mail th e complete dfor

mt o DE Q Lab Q

A Sectio n a s soo n a s the y hav e complete d the k analyses
. Time o f samplin g mus t

b e note do

n th e Reques t

fo r Analysi s for

mfo r al l samples , alon g wit

h residua l chlorin e measurement .

Microbiologica

l analysi s i s perfomie

db y th e Orego n Healt h Divisio n Laboratory
. Withou

t advance d notice , whe

n specia l medi ai s required, th

e test ma y no t b e performed
.

### DE Q LAB : Fiel d Samplin g Referenc e Guide Decembe r 199 8 Revisio n 6. 0 - UNCONTROLLE D DOCUMEN

T Pag e 1 2 

# VI
. SAMPLIN G AN D ANALYSI S PLA N

I - ' A Samplin g an

dAnalysi s Pla

n (SAP) i s acombinatio n Laborator y Analysi s an

d Fiel d Sampling Plan
. Basically i t shoul d describ e Wha t

yo u ar e going to do
. Wh o wil l d o it
. Ho w Man y ther e wil l be
. Wher e an

d Whe n you'l l d

o it , an d Ho w i t wil l b e done
. A SA

P shoul db e developed befor e an y sample s ar

e submitte d t o th e Lab , wit

h th e exceptio n o f

complaint an d routin e complianc e inspections
. SAP s fo r project s o n which DEQ La

b perform s analytica l wor k mus t b e approve dan

dsigne db y th e La b Q A Mane^er
. Contac t

th e Q A Sectio n fo

r assistance
. T o pla n workload s tb e La b expect s t o receiv e aSamplin g an dAnalysi s Pla n when : • Sample r

i s requestin g acomplicate dsuit e of test s o n mor e tha n five samples , • Samplin g even t

involve s collectio n an d analysi s o f mor e tha n te n samples , o r ' Multipl e samplin g event s planne dove r aperio d of

tim e (e.g
. quarterly , monthly, etc.)
. . A t aminimum , th e La

b expect s t o b e provide d wit h alis t o f ho w man y samplin g site s there wil l be , wha t typ e o f sampl e wil l b e collecte d(e.g
. soil , groundwater , sediment , etc.) , analyse s tha t will b e requeste d (e.g
. VOCs , NO's , TKN , TCLP , Tota

l o r Dissolve dmetals , TPH-? , BOD5 , etc.) , whe n sample s wil l b e collecte d an d when delivere d t o Lab , Qualit

y Assuranc e sample s tha

t are necessary , an

d whe n yo u nee d t o hav e th e data(e.g
. ASAP , 2 weeks , 4 weeks , 6 weeks , etc.)
. Th e nam e ofth e Project

Manager , phone number , an d aFun d Cod e assigne d b

y th e Busines s Offic e fo r th e La b t o charg e wor

k or i th e project

mus t be included
. Thi s ca n b e accomplishe di n th e for mo f eithe r asingl e narrativ e pag e o

r asimpl e table , a s in th e exampl e tha t follows
.

### DE Q LAB : Fiel d Samplin g Reference , Guid e Revisio n 6. 0 - UNCONTROLLE D DOCUMEN

T Decembe r 199 8 Pag e 1 3 Project : Projec t Manager : Fun d Code : Samplin g Date(s) : Delivery t o Lab : Desire dTurnaround : FRED' S KO I EMPORIU M Bar t Simpso n [503-229-xx36 ] WXY Z Ma y 34-35 , 199 5 Ma y 35 , 199 5 , late i

n afternoon 3 week s Matri x Surfac e Wate

r Sedimen t Groundwate

r Soil #sampl e site s

3
4 5 3 analyte s

BODs , NHj , VOC , Pesticides , pH , Alkalinity , Conductivit

y Pesticides , VOC , TK

N Tota l Arseni c & Lea

d VOC , pH , Dissolve d Arseni c & Lead ,

pesticide s Pesticides , TCL

P an dTotal metal s (A s & Pb ) -i-Q A 1 Duplicate 1 matrix spik

e transpor t blan k 1 duplicat e transpor t blan k 1 duplicat e 1 matri x spik

e transpor t blan k 1 duplicat e + 1 matrix spik

e fo r each TCL P When the La

b receive s thi s informatio n w e ca n see wha t our schedul e i s like , an

d pla n t o accommodat

e you r samples
. Th e SA

P als o permit s th e Sampl e Tracke r to prepare th e appropriate numbe r an d typ e o f samplin g container s yo u wil l nee d ahea do f time
. However , b e forewarned : there ar e alimite d numbe

r of instmment s an

d analyst s availabl e t o d

o certair i type s o f testin g (e.g
. GC/MS-VOC , Semi-Vols , ICP-metals , etc.)
. It i s pmdent t o allo w fo

r som e flexibilit y in th e schedulin g o f

you r samplin g even

t an d specifi c tumarouri d times
. If someon e els e ha s alread

y booke du

p that tim e perio d w e ma

y as k tha t you reschedul e you

r samplin g event , o

r exten d th e turnaroun dtime
. There i s als o th e possibility , howeve r remote , tha

t a n unschedule d Criminal-Lega l cas e might preemp t you r tim e slot
. Criminal-Lega

l case s receiv e priorit

y ove r al l othe r pending work
. I

n an y even t w e wil l d o ou r bes t to get th e wor k don e i f it' s to o lat

e t o reschedule , an

d you wil l b e kep t

informe d ofth e progres s o f you r project' s analyses
. Reques t rapi dturnaroun d tim e (1- 2 weeks , o r less ) onl y whe n i t i s absolutely necessary . The La b recognize s tha

t thi s ma y be appropriat

e o n occasion , but

i t shoul dnot

b e employe droutinely o

r as amatte r o f convenience
. 

### Advance d Notic e o f Planne d Samplin g Activit y Th e "form " o

n pag e 1 8 ha s been designe d t o facilitat e informin g th e Laborator

y a t th e earlies t

possibl e time, wit

h th e leas t inconvenienc e to you , o f

samplin g activitie s tha

t are comin g up . Either

th e first o r bot h page s ca n b e filled ou t an dFaxedto th e La

b a s soon a s th e information i s availabl e t o you . 

### La b FA X number ; 229-692 4 Whe n th e FA X i s receive di

t wil l b e filedi

n acentra l location , whic h everyon e involved will chec k daily
. Thus , i f th e regula r liaiso n perso n i s no t

available , th e information wil l stil l reac h thos e involved
. Thi s for mwil l provide th e La b wit h th e workloa

dplannin g informatio n i

t need s fo r th e wor k requested
. Onc e thi s for

mha s bee n sent , i f ther e ar e an v changes , pleas e sen d a n update
.

### DEQ LAB : Fiel d Sampling Referenc e Guid e Revisio n 6. 0 - UNCONTROLLE D DOCUMEN

T Decembe r 199 8 Pag e 1 4 

## 5lMij^i^ ° [ 5 M l M Bi.'.I°sgiL[^,L. [ 

# W\w&\ m ,..»4rf > ,..(%,
.

i Pag e 1

### DE Q LAB : Fiel d Sampling Referenc e Guid e Decembe r 199 8 Revisio n 6. 0 - UNCONTROLLE D DOCUMEN

T Pag e 1 5 

# Vll
. QUALIT Y ASSURANC E Th e ter mqualit y assuranc e describe s th e systemo f activitie s intende d t o provid e evidenc e to th e produce r o r use r o f aproduc t o r servic e tha

t i t meet s predefine dstandard s o f qualit y wit h astate d leve

l o f confidence^
. I

t consist s o f relate d bu t

independent

activities : qualit

y contro l an

dqualit y assessment . Qualit

y contro l describe s thos e activitie s an d procedure s use dintemally (within th e lab ) t o produc e consistent and reliabl e data
. Qualit

y assessmen

t deal s wit h activitie s t o independently evaluat e dat aquality , afte

r it' s produced
. Scientifically vali dtes t

dat adoe s not

jus t happen
. It

result s fromhar

d wor k an d considerabl e cost , i

n bot h time an d money . Th e cost s t o produc e lo w quality , unreliabl e dat ai s obviously les s tha n th e cost s t o produc e high quality , reliabl e data
. However

i n th e lon g m

n i t coul dcos t

considerabl y mor

e fo r poor qualit y dat aifth e site ha s t

o b e re sampied , sampl e analyse s repeated , o r acas e i s throw n out

o f cour t becaus e o f

poor qualit y data
. I t i s impossibl e t

o provid e hig h qualit

y analytica

l datao n lo w qualit

y samples
. I t i s th e DE Q Lab' s Polic y t o giv e highe r priorit y t o dat aqualit y ove r dat aquantity
. Howeve

r analytica l data ca n only b e a s goo d a s th e sample s analyzed
. Sample s tha t ar e no t representativ e ofth e matrix bein g assessed , thos e collecte d in insufficien

t amount s fo

r th e analytica

l metho d used , o

r sample s contaminate d b

y samplin g o

r handling procedure s canno t

b e mad e representative , increase di n quantity , o r

uncontaminate d by La

b efforts
. Th e La

b mus t assum e tha

t everythin g i

n th e sampl e container

constitute s th e sample , tha t th e sampl e wa s collecte d an d preserved properly , andtha

t i t doe s no t contai n extraneou s contamination
. Du e t o th e sophisticatio n o f today' s measurement

techniques , an

dthei r cost , considerabl e plannin g i s necessar y to insure tha t tes t dat ai s meaningfiil
. Th e goa l i s t o collec t

a n appropriate numbe

r o f hig h qualit

y sample s tha

t represent th e environmenta

l entit y bein g tested
. Reduce dnumber s o f sample s requir

e eve n bette r plannin g t o insur e tha t gap s i n th e dat aset , caused b

y omission s o

r post-analysi s dat arejection , don' t weaken conclusion s o

r preclude decision-making
. 

### DE Q Laborator y Sampl e Acceptanc e Polic y It i s DE Q Laborator

y polic y t o accept

sample s fo

r analysis , an

d repor t analysi s results , fo

r sample s tha

t mee t th e followin g minimu mrequirement s upo n receip t a t Laboratory : 1
. Complete sampl e documentatio n including :

sampl e description , sampl e matri x (liquid , solid , sludge , sediment) , sampl e classificatio n (grab , continuous , composite) , an d date an dtime o f collection , collector' s name(s) , program/projec t

identificatio n (fun

dcode) , samplin g locatio n (includin g latitude-longitud e an d elevation) , o

r permanen t LASAR ' Station Number , an dspecia l remark s describin g th e sample , i f appropriate
. 2
. Sampl e container(s ) appropriat e fo r sampl e typ e an

d analysi s requested ; • preservation(s ) (or

lac k of preservative) , an

d

* Taylor , J.K. , Qualit

y Assuranc e o f

Chemica l Measurements , (Chelsea , MI : Lewi s Publishers , 1987)
.

' Laborator y Analytica

l Storag e An dRetrieva l

### DE Q LAB : Fiel d Samplin g Referenc e Guide Decembe r 199 8 Revisio n 6. 0 - UNCONTROLLE D DOCUMEN

T Pag e 1 6 3
. Parameter/Metho dfieco/Mmenrferf HoMi/i g rim e not

exceeded ; an

d 4
. . Adequat

e quantit y o f sampl e t o accommodat

e test s requeste dby collector , judge d appropriat e b y la b supervisor , o r stipulate d i

n Samplin g an

dAnalysi s Pla

n (SAP ) b y projec t manager . " - 5
. Minimu

mSamplin g Pla

n submitted' " whe n mor e tha n five (5 ) sample s submitted , includin g • Numbe

r o f sample s (by matrix) , iricluding Q A (dupes , matii x spike s & duplicates , blanks , etc.) , • projec t

manager , • who mt o repor t dat ato , • analyse s (tests ) requested , an d
• Detectio n limi t

neede d[qualitativ e screen , drinkin g wate r Maximu mContaminan

t Limi t (MCL) , Toxicit y Characteristi c Leachin g Procedur e (TCLP) , NPDE S permit

compliance , etc.]. , Sample(s ) failin g t o mee

t th e abov e criteri amay b e analyzed , dependin g o n th e circumstances , bu t

th e dat awil l b e unambiguously flagge dwhen reporte d a s havin g bee n compromise ddue t o deficiency i n one o r more ofth e element s liste dabove
. Releas e o f datafro mcompromise d sample s wil l b e deferred awaitin g th e necessar y documentation
. Documentatio n ofan y o f

thes e element s ma

y b e furnisheda

t an y time u p t o tha t time whe n th e flagged dat ai s release d fromth e Laboratory , preferabl y a s soon as possible
. I f

al l acceptanc e criteri aar

e consequently met , qualifying flag will b e expunge dfrpmth e report , o n conditio n tha

t dat aqualit

y i s no t affected
. 

# VIII
. Sampl e Collectio n Collectin g arepresentativ e sampl e ca n b e difficult , bu

t i t i s th e mos t

crucia l i n th e proces s o f

obtainin g vali d data
. Collec t duplicat e sample s t o measur

e variabilit y fromsample-to-sample
. Thi s Q A measur e ca n substantiate your datab y demonstratin g tha

t you r sample s are , indeed , representativ e ofth e populatio n bein g measured
. A n importan

t facto r i n collectin g arepresentativ e sampl e i s th e us e o f prope r sampl e container s an

d appropriat e preservation
. Sample s shoul dalway s b e collecte d i n container s supplie d b

y th e Lab
. Thi s insure s tha t th e containe r ha s been properly cleaned
. Whe n th e containe

r i s filled, th e La

b i s insure d they wil l hav e enoug h sampl e t o d o th e tes t requested
. Sample s submitte dt o th e la b tha t ar e not i n aLa b supplie d containe

r {e.g
. mayormaise , pickle , o r peanut butte r jars ) are likel

y t o be rejectedfo

r analysis
. Sample s mus t

als o b e properl

y preserve d o

r they ma y b e rejected
. Refe

r t o Tabl e 2
.

1 0 ^ Failur e t o submi t asamplin g pla n coul dresul t i n holdin g times bein

g exceede d du e t o prio r schedule d wor k i n th e Lab
.

### DE Q LAB : Fiel d Sampling Referenc e Guid e Decembe r 199 8 Revisio n 6. 0 - UNCONTROLLE D DOCUMENT Pag e 1 7
Notic e tha t som e "Preservatio n Codes " followin g Tabl e 2 cal l fo r addin g ')c', ' drop s o f

apreservativ e t o a"y " siz e container : I t

i s importan t

whe n container s ar e ?io

f full o f sampl e tha t

aproportiohate.quantit y of preservativ e b e adde d(e.g
. I f

a500-m l container-is.only.half-fiill , an dpreservatio n require s 1 2 drop s o f cone , sulfuri c acid/50 0 ml , us e only

- 6 drop s o f

aci dfo r thi s bottle.)
. Collectin g representativ e sample s o f liqui dmatiice s require s decidin g wha t i t i s you wan

t t o represent . Ar

e you intereste di

n th e effluen

t itself , th e impac t

ofth e effluen

t on it s receivin g wate

r a t th e point wher e they mi x {mixin

g zone) , o r th e impac t

th e effluen

t i s havin g 10

0 meter s downstrea

mfromit s poin

t of discharge ? Shoul d a "background " sampl e b e collecte dupstrea mofth e discharg e point ? Collectin g arepresentativ e sampl e o f a multiphas e waste i

n asteel dru

mpresent s differen

t problem s tha

n collectin g asampl e o f

"pure product. " Doe s a representativ e soi l sample " include rocks , vegetation , o r sticks ? Considerin g thes e and simila r question s befor

e samplin g wil l determin e wha t you r sampl e represents . It i s u p to th e sample

r t o determin e wha

t constitute s a"sample, " an d wha t i t "represents. " Unles s th e Laborator y i s tol dotherwise , whatever

i s i n th e containe

r i s "sample. " It

i s imperativ e tha

t the sample

r infor mth e La b whe n intereste donly i

n specifi c fractions o f

asample , an

d it' s als o necessar

y t o mak e certai n tha

t there i s sufficien

t quantit y ofth e fraction o f

interes t t o successfully perfor

mth e analyses
. If

you'r e no t

sure , call th e Laboratoi y an d ask
. Sample s "split " wit

h asourc e o

r suspecte dviolato r

mus t b e a s clos e t o identica

l a s i t i s possibl e t o achieve
. Ifth e sourc e o r suspecte dviolato r

intend s t o hav e th e sampl e analyze d b y their ow n la b i t woul d b e pmdent

t o hav e their la b contac t DE Q La b to agre e o

n wha t portio n eac h la

b define s a s th e "sample. " If on e la b screen s out

an d discard s th e larg e rocks , whil e th e othe r retain s them , th e concentratio n o f analyt e i n the tw o sample s wil l b e significantl y different
. 

## WATE R SAMPLE S The Water Qualit y Monitorin g (WQM ) sectio n collect s sample s fo r WQ , HSW , an

d WMC projects
. WQ

M ' samplin g procedure s ma

y b e foun di n thei r Mode o f Operatio n Manua l (MOM) , whic h include s procedure s fo r samplin g rivers , stteams , estuaries , lakes , groundwater wells , soil , shellfish , fish, an d sediment
. All long-ter

m samplin g performe db

y La b personne l require s a

n approve d SA

P and/or Qualit y Assuranc e Projec t

Pla n (QAPjP)
. 

### Groundwate r Monitorin g well s without

dedicate dpump s ma

y b e sample dusin g bailers
. Som e bailer s ar

e expensiv e an

d difficul t t o decontaminate
. Disposabl e bailer s ar e availabl e fromth e La

b Sample Tracke

r o n request . Collec t drinkin g water

o r irrigatio n well sample s by first purgin g wate

r lines
. Fill sampl e containe r directly from tap , unles s sampl e i s to b e split
. Insur e tha t spli t sample s ar

e homogeneous : fill larg e clean container , mix an d pou r int o appropriate containers
. Sample s collecte di n purg e vial s fo

r VO C analyse s canno t

b e spli t i n thi s manner . The

y mus t b e filledindividually , directly fromth e ta p o r bailer (Appendi x A)
. Groundwate

r well s mus t

b e properly "developed. " Al l sub-sample s from agive n sit e shoul d b e representative
. 

### Surfac e wate r Sample s are bes t

collecte d usin g astainles s stee l bucket
. Th e collectio n containe r shoul d first

b e rinse d wit

h sample , t o was h out

previou s sample
. Collec t

afresh sample
. Avoi d dipping bottl e into sample , i f possible ; pou

r DE Q La b ha s receive dsainples containin

g larg e roclcs , coins , unfire

d .2 2 rifle ammunition

, etc .

### DE Q LAB : Fiel d Samplin g Referenc e Guide Decembe r 199 8 Revisio n 6. 0 - UNCONTROLLE D DOCUMEN

T Pag e 1 8 fromcollectio n container , wit h minima l agitation , int

o sampl e bottle
. Residu e fromth e outside surfac e ofth e container , o

r your hands , coul dcontaminat

e sample s and/or

expos e you to hazardou s materials
. If astainles s samplin g container

i s no t available , di

p bottl e directly into sample , instal l lid , an d wip e of f outside o f containe r wit h pape r towel
. 

### AI R Th e Ai r Qualit y Monitorin g (AQM ) section collect s sample s fo r A Q Progra

mprojects
. The AQ M Procedure s Manua l contain s samplin g procedure s fo r pollutant gase s (CO , SO2 , O3 , an

d NOx) , PMi

o an d Suspende d Particulate , an

d canister ga s sampling
. Ai

r sampling/monitorin g equipmen t i s highl y specialized , require s considerabl e logisti c support , an di s not generally availabl e fo

r us e outside o f

AQM
. Anyone intereste d in proposin g amonitoring/samplin g project shoul dcontac t

AQ M Supervisor
. DE Q La b ha s samplin g capabilit

y fo r PU F an dBubble r samples , an

d subsequen

t analyse s fo

r PA H (TO-4) , volatil e toxic s (TO-14) , an

d carbonyl s (aldehyde s & ketone s usin g TO-11)
. Ai r particulate materia

l ca n b e analyze dfo

r specifi c source-relate dchemicals , woo d fiber, asbestos , etc . Technique s fo r particulat e sampliri g includ e Particl e Fallou t Sampler s an

d"Stick y Paper. " Evacuate d Stainles s Steel canister s passively sampl e ambien

t ai r which i s retume d to the La b an d subjecte d t o ga s chromatographi c analyse s fo r ttace organic s (e.g
. solvents , gasoline , BTEX , etc.)
. 

### SOIUSEDIMEN T Us e astainles s steel spoo n o r disposabl e plasti c scoop to collec t soil/sediment

samples
. Th e plasti c scoop s ar e - usefu l fo r sof t soil s an d thos e contaminate dwit

h organics , whic h are difficul t t o clea n off
. It i s common practic e t o composit e severa l subsample s o f

soil to obtai n arepresentativ e sampl e of a n environmenta

l condition
. Composit

e samplin g i s achieve db

y collectin g severa

l roughl y equa l sub-sample s an

d thoroughly mixing t

o for mon e sample
. Selec t soil tha t contain s a s fe

w larg e rock s a s possible , unles s you wis h th e rock s include d i n the analysis
. Subsurfac e soil s ca

n b e collecte dwhil e well s ar e bein g drilled , durin g excavation , o r usin g ahollow-cor

e soi l drill
. The La b ha s n o specia

l equipment

to collec t subsurfac e soils , beyondusin g auger s an d cor e samplers
. 

### SUSPEC T H W CONTAINER S Us e adisposabl e bailer

o n bulk containers , suc

h a s 55-gallo n dmms , storag e tanks , etc . A t leas t one-hal f foo t dept h o f produc t i s require dfo

r th e baile r to function
. The la

b als o supplie s disposabl e glas s tube s (approximately 4 fee t long ) tha t ma y b e used t o "pipette " produc t ou t of larg e containers
. Eithe

r proces s i s messy . Tak

e a n ampl e suppl

y of clea n wate r andpape r towel s to clea

n of f sample bottles
. Wea

r disposabl e surgica

l glove s t o protec t hands
. Decontaminat

e al l samplin g equipment , except disposabl e variety , befor

e retumin g i

t to the lab
. D o no t

retur n o r transpor t an y contaminate dsamplin g equipmen t in ic e chest s wit

h samples ! Spraying wit

h wate r i s generally adequate
. Carr

y asquir t bottl e o r water-fille dpump-typ e garden spraye r to remot e sites
. Mak

e your ow n arrangement s t o dispos e o f waste s generate dduring samplin g {i.e
. disposabl e equipment , was h water , surgica

l gloves , an dpape r towels)
. Th e lab ha s n o disposal facilitie s o r resource s t o accommodat e disposa l o f waste s tha t accumulat e whe n yo u decontaminat e equipment
. Th e La b will not stor e o r dispos e o f

purg e water .

### DE Q LAB : Fiel d Samplin g Referenc e Guide Decembe r 199 8 Revisio n 6. 0 - UNCONTROLLE D DOCUMEN

T Pag e 1 9 

# IX
. SUBMITTIN G SAMPLES , Reques t fo rAnalysi s Includ e th e followin g information o n th e Reques t

fo r Analysi s form : samplin g site descriptio n an d neares t town ; dat e an dtime collected ; sampler' s name ; progra mt o b e charge d(Fun

d Code , Projec t

Billin g Code) ; purpos e fo

r sampling ; descriptio n fo

r each discrete samplin g location ; container I D number(s ) (i n space s provided) ; an d reques t analysi s fo r

aspecifi c analyt e by nam e o r tes t group , NO T metho d nuriiber
. T o insur e tha t th e correc t

perso n receive s th e dat areport , ente r one o r mor e name s i n th e uppe

r righ t han d spac e labeled : "Repor

t Dat aTo : . " On Request s fo r Analysi s without

anyone listed , dat awil l b e reporte d t o th e sampl e submitter
. 

## REQUES T FO R ANALYSI S FOR M Th e Reques t

fo r Analysi s for

mi s a n important

element fo r loggin g sample s into th e Laboratory , an d serve s a s documentatio n linkin g analytica l dat ai n LIM S wit

h th e appropriate projec t

o r monitorin g event . Certain informatio n o

n th e for mi s absolutely necessary . Suc h informatio n a s th e Samplin g Projec t Location/Sit

e should b e kep t short , bu t b e a s descriptiv e a s possible
. When asamplin g event

i s onl y on e o f several , mak

e certai n tha

t th e sam e projec t nam e i s used o n eac h Reques t fo r Analysi s fo

r each samplin g event . A s each cas e i s complete dan d reporte d ou

t adatabas e i s update d whic h link s th e projec t nam e wit h appropriat

e cas e number s an

d dat e o f reporting
. I f

severa l samplin g event s relate d t o th e sam e \ projec t ar e liste d usin g differen

t names , i t ma y b e impossibl e t o connec t themi n th e fiiture. Th e Reques t

fo r Analysi s for

musually contain s th e onl y informatio n th e La

b ha s about

sampl e origin , possibl e contaminant s andsources , condition s o f collection , etc . It

woul d b e helpful , whe

n th e field sample

r ha s kept afield notebook , i f

pertinen t informatio n wa s transcribe d ont o thes e forms
. Information , such a s "suspec t cyanide i n samples, " "diese l spill, " "sample s contai n elementa l mercury, " shoul d b e note d a s asafet y wamin g to th e Sample Tracker an d Analyst s tha

t wil l subsequenti y b e handlin g th e samples
. Staffsubihittirig.samplesfo r th e LUS T Progra mmus t hav e a n Inciden t Lo g Nuniber't o include on th e Reques t fo r AnalysisForm.-Thisinsures.thatproperresourcesareusedtopa y foranalysis
. . , , " ; ' " ' Waste Management

andCleahu p project s mus t hav e auniqu e Projec t

Billin g Co(le'assigried t o each projec t throug h the.Busines s 6ffi'ce"if

CbstlVecoveiy i s (or

ma y become ) involved. " Th e Laborator y niustb e informed wha

t thi s • - code,i s before , o

r at th e time , sample s are submitted
. . •',-. ' ,".-_,'• ' " '

### DE Q LAB : Fiel d Samplin g Referenc e Guid e Revisio n 6. 0 - UNCONTROLLE D DOCUMEN

T Decembe r 199 8 Pag e 2 0

DEPARTMEN T O F ENVIRONMENTA L QUALITy LABORATORi'DIVISIO N

REQUES T FORANALYSI S Cas e Number:
. Locatiar/SitB;
_ Collecledby:
_ DaleSanpbd:
_ FtrdCcd e ReoauedatLsb:
.

_. . DateFfeporie d
_ Ffepor l Dat a To : Ccnunsnc s

ITE M

• # 1 2 .....3...
. 4
.. . 5..
. .....P....
. : SANPLIN G POIN T :

: DESCRPTIO N SarrpbCcrtai-eraooatJr g : t o testis ] requested ' " Nutrient s Bas e D O

BO D : Metal s

Oroari c Mis c

Misc ' ' • TESTE ) REQUIRE D
.

•••—:•—-—••••••• - •--•••• • : Laboratot y Goitiinents:
_

. Contac t Saiihpl e TracKwfotpropis r

sampling container s an

dpreseivalioi i procedur

e a t 503.229-598 3

DE Q La b "Reques t

Fo r Analysis " I t i s obviou s tha

t Collecte dBy , Dat e Sampled , Purpose , an dRepor t Dat aT o are important

fields to be complete d b y th e sampler
. The La

b wil l fill in th e Dat e Sample s Received
. Fltzsefla g o

n th e Reques t

fo r Analysi s sample s know n o r suspecte d t o contai n sewage , cyanide , toxi c solvent s o r

heav y metals , etc . Thi s i s safet y informatio n for

th e Sampl e Tracke r

an d Analyst s wh o wil l subsequentl y handl e th e containe r an dsampl e material
. Alway s kee

p i n mindtha

t th e Holdin g Tim

e fo r asampl e begin s whe

n th e sampl e i s collected , not whe n i t arrive s a t th e Laboratory
. Thi s coul dlea dto problem s fo

r sample s havin g extremel

y shor t holdin g time , suc

h as BOD 5 o r Turbidit y (4 8 hours) , an

dChromium"^ ' (24 hours)
. Shoul dasampl e b e delivere d s o lat e a s to exceed the holdin g time th e tes t

wil l b e performed , but

result s wil l b e reportedas a n ''estimate " an

d th e dat aflagged. Eac h "item " shouldinclude aconcis e Samplin g Poin t Descriptio n o f

where , o r sampl e identificatio n number , an d whe n (time ) sample taken
. T

t i s helpfiil t o hav e th e sample r not e th e matrix (surfac e water , groundwater , soil , sediment , etc.)
. The complet

e (alph a+ numeric ) sampl e bottl e numbe r should b e entered unde

r Sampl e Containe r

Accordin g t o Test(s ) Requeste di

n th e appropriate colum

n to th e righ

t of "samplin g poin

t description. " If

container s aren' t

unde r

### DE Q LAB : Fiel d Samplin g Referenc e Guid e Decembe r 199 8 Revisio n 6. 0 - UNCONTROLLE D DOCUMEN

T Pag e 2 1 th e correc t

colum n it' s not abi g problem
. Fro mth e container prefix th e La

b know s wha

t analj^e s com

e ou t ofeae h bottle
. "Test(s ) Required " shoul d include each analyte , o r typ e o f analyte , yo

u are intereste d i

n havin g asampl e ite

m teste d for
. Tr

y t o b e a s specifi c a s possible
. Th e La b wil l assig n method s appropriat e t o the analyte s you ar

e lookin g for
. Eve n thoug h yo u (o r

you r contractor ) hav e provide daSamplin g & Analysi s Pla n (SAP) , dono t expec t th e Sampl e Tracke r

to'sor t ou t yoursample s an d fill outtheRequestfo r Analysis , base d on you r

SAP
. Tracke r doe s no t hav e tim e t o d o this
. . " - •,,.,_ _

• Note o n "Reques t

Fo r Analysis " whethe r

preservative s wer e added,^whic h preservative , an d th e amount. ' ' • < Th e DE Q La

b Informatio n Managemen t System(LIMS ) assign s auniqu e "Cas e Number " to each batc h o f sample s tha t are loggedin
. A cas e numbe r migh t b e assigne d t o all sample s from aspecifi c projec t o n agiven sampl e day , o

r all sample s collecte ddurin g a n ambien t monitorin g event

spaimin g mor

e tha n one day
. I

n n o even t wil l acas e numbe r be assigne dt o include sample s fromdifferen t monitorin g projects
. Cas e Number s hav e sb

c digits
. Th e first

tw o digit s represent

th e year , followed b

y fou r digit s assigne d sequentially by LIM S an

drepresentin g th e orde

r th e case s wer e logge d i

n durin g th e year . Possibl e cas e number s fo r an y yea r rang e fromYYOOO

l t o YY9999
. Eac h Cas e ha s a

t leas t one "item, " representin g adistinc t samplin g site
. A Cas e ma y hav e a n unlimite d numbe

r of "items. " I n tum , each "item " consist s o f on e o r more uniquely numbere d {e.g
. P105 , DM456 , R207 , B002459 , etc. ) sampl e containers , dependin g o n th e type(s ) o f

test(s ) th e sample s were collecte d for
. Th e container

numbers , sizes , an

dmaterial s are aresul t

ofth e variou s chemica

l preservation s an

d quantit y o f sampl e require dt o tes t

fo r differen t analytes
. Test s fo

r severa l analytes , havin g identica

l preservatio n requirements , ar e frequently performe do n asingl e bottle
. It' s obviou s that abottl e preserve d wit

h nitri c (TM-poly ) o

r sulfiiri c aci d (R-poly ) canno t

b e analyze dfo

r nitrate , sulfate , pH , alkalinity , conductivity , etc. ; however , thos e test s ca n b e performedo

n abottl e (e.g
. P-poly ) wher e th e only preservatio n i s refrigeratio n a t 4°C
. Basedon th e analyte s you request , an dyou r DQO s (when specified) , th e La b will assig n a

n appropriat

e analysi s method
. Analytica

l procedure s usedb

y DE Q La b comply wit

h requirement s ofth e applicabl e federa l regulations ; [e.g
. Nationa

l Interi mPrimar

y Drinkin g Water

Regulatio n (NIPDWR) , NPDES , RCRA ] an d ar e EP A approved' ^ methods
. Al

l procedure s ar

e reference dt o current

publishe dliterature
. I f

DQO s ar e no t specified th e La

b wil l emplo y their

default metho dfo

r th e test . DE Q La

b Method s ar

e liste d i n th e mos t recent Laborator y Qualit y Assuranc e Plan
. Occasionally non-standar

dmethod s ma

y nee dt o b e develope dwhen astandar d metho d i s not

available , o

r whe n interferin g substance s influenc e th e performanc e o f astandar dmethod
. Non-standar

d method s wil l be appropriately validated , documented , an

d note d o n the dat arecord
.

4 0 CF R136, SW-846 , Standar

dMethods , etc .

### DE Q LAB : Fiel d Sampling Referenc e Guid e Decembe r 199 8 Revisio n 6. 0 - UNCONTROLLE D DOCUMEN

T Pag e 2 2 CHAI N O F CUSTOD Y Tw o level s o f

Chain-of-Custod

y hav e been develope d to eliminat e som e ofth e paperwor

k associate d wit

h maintainin g arigorou s Chain-of-Custody
. It shoul db e notedtha

t custod y leve l ha s n o bearin g whatsoeve r on analytica l dat aquality ; i

t onl y document s wh o ha

d th e sampl e i

n thei r possessio n a

t an y particula r time
. 

### FIRS T CUSTOD Y LEVE L Intende d fo

r routine , ambien

t monitoring , an

d sample s unlikely t o becom e involve d i

n litigation
. N o forma

l custod y transfe r i s documented
. Sample s ar e treate d routinely , whic h includes : analyse s usin g EP A approve d methods ; replicat e analyses , matrix spikes , an dQC standard s usin g metho d an d EP A Q C criteri a o n a1:2 0 frequency; compariso n agains t historica l data , if i t exists ; dat arevie w fo

r consistency , completeness , precisio n an daccuracy ; Q

A review o f

duplicat e sampl e data ; an

d standardize d reportin g on th e Laborator

y LIMS
. FIRS T CUSTOD Y LEVE L sample s will b e discarde d upo n completio n o f analyse s an

drepor t o f results
. 

### SECON D CUSTOD Y LEVE L Include s everythin g i

n FIRS T LEVEL , plu s custod y i s thoroughly documente d throug h ever y transfe r from sample r t o Lab , t o an

d fromsecure storage , custod y durin g analysi s i

n laboratory , an

d retentio n o f remainin g sampl e unde

r secur e storag e a s evidence
. Sample remainin g afte

r analyse s are finished , o

r empt y containe r whe n sampl e i s exhauste d durin g analyses , wil l b e retaine d i

n secur e storag e unti l releas e i s approve di n writin g b

y progra mo r sample r (se e Appendix D)
. Sample s handle da t th e THIR D CUSTOD Y LEVE L ar e suitabl e fo

r Crimina l Actions
. 

### SAMPL E SHIPMEN T Transpor t sample s to th e La

b immediately afte

r collection
. Notif

y th e Sampl e Tracke

r (229-5983 ) prio r

t o sampl e collectio n t o allo w adequate tim e fo r schedulin g analysis , advanc e preparation , and/or technica l assistance
. Shi

p samples'^ , packe do

n ic e i n asealed ic e ches t

availabl e fromth e lab , vi aGreyhound
. Th e La b ha s prepai dGreyhoundshippin g label s available
. Fo r shipmen t o f lega l samples , refe

r to "Lega l Chain-of-Custod

y Procedures " Appendi x D
. Ship sample s to : 

### DE Q Laboratorie s 171 2 S W 11t h Avenu e Portland , O R 9720 1 I f possible , han

ddelive r sample s to th e Laboratory
. W e ar e locatedo

n th e Portlan d Stat

e Universit

y campu s i

n th e Scienc e I I Building , o

n 11t h Avenu e between Cla

y an d Montgomery
. Parkin g i

n front ofth e buildin g i s restricte d to 1 5 Minute s an d Officia

l Us e Onl y (i.e
. Stat e license dvehicles)
. Privat e car s wil l quickl

y b e cited b

y Campu s Security
. Yo

u ma y obtai n atemporar

y parkin g pas s fromth e La b receptionist , allowin g you mor e time t o conduc t business
. " ' " ^ - Sample s ONLY , vi apubli c carrier
. No

t preservativ e chemicals , deco

n solvents , o

r othe r sanctione d hazardou s materials
.

### DE Q LAB : Fiel d Sampling Referenc e Guide Decembe r 199 8 Revisio n 6. 0 - UNCONTROLLE D DOCUMEN

T , Pag e 2 3 VOLATIL E ORGANICS : T o avoi dcross-contaminatio n o f sample s durin g shipment , sea l sample s an

d"Transpor

t Blank " vial s i

n ziploc k bags
. BACTERIA L sample s {fecalcoliform , E.Coli ) mus t b e receive dn o late r

tha n 1200 hour s (Noon ) on Thursday
. Fo r Lega l bacterial/microbiologica l samples , th e maximumholdin g time o f 6 hour s mus t

b e adhere d to , wherea s routin e sample s ca

n b e hel dfo

r amaximumo f

3 0 hours
. Analysi s fo

r a"non-routin e "organis m{E.Coli , tota l coliform , feca l strep ) i s required , notif y th e La b well in advanc e s o tha

t specia l medi aca n b e prepare d fo

r th e test . Microbiologica

l testin g i s currently performe d exclusively b y th e Orego n Healt

h Divisio n Lab , i

n th e adjacen

t building
. BOD : Sample s mus t

be receive d n o late

r tha n 120 0 hour s on Friday
. ' " I f i t i s necessar

y t o sampl e between 12:00 Frida y and08:0 0 o

n Tuesday , th e La

b wil l nee d t o schedul e someone t o com e in o n th e weekend
. Specia

l notificatio n i s require dprio r to collectio n an

d shipmen t o f samples
. 

## FIEL D NOTEBOOK S A boun d fieldnoteboo k

shoul d b e maintaine d t o provid e adaily recor d of significan t events , observations , an

d measurement s durin g fieldinvestigations
. Thi s recor dshoul d include field measurements , personnel , persona l an d weather observations , an

d physica l conditions
. Al l entrie s i

n field notebook s shoul d b e made , signed , an d dated j n ink
. Fiel dnotebook s shoul db e kep t a s apermanent

record
. Thes e notebook s ar

e intende dt o provid e sufficien t data , observations , an

d documentatio n t o enabl e participant s t o reconstruc t

event s tha

t occurre d durin g a

n activity , an

dto refresh their

memor y whe n called upon to giv e testimon y durin g lega

l proceedings
. 

### CORRECTIO N T O DOCUMENTATIO N All origina l dat arecorde din fieldnotebooks , chain-of-custod y records , an d othe r form s mus t

b e writte n i

n INK
. Non e o f

thes e document s shoul d b e destroye d o r thrown away , eve

n i f they are^ecom e illegibl e o r contain inaccuracie s tha

t require areplacemen

t document
. . ' I f a n error i s mad e o n adocumen

t assigne d t o a

n individual , tha

t individua l mus t mak e correction s b

y crossin g a singl e line throug h th e error , ente r th e correc t

information , an

dinitia l th e correction
.

### DE Q LAB : Fiel d Samplin g Referenc e Guid e Decembe r 199 8 Revisio n 6. 0 - UNCONTROLLE D DOCUMEN

T Pag e 2 4

### DE Q LAB : Field Sampling Referenc e Guide Decembe r 199 8 Revisio n 6. 0 - UNCONTROLLE D DOCUMEN

T Pag e 2 5 

## Appendi x A SAIVIPLIN G FO R VOLATIL E ORGANIC S Contaminatio n Becaus e ofth e sensitivit

y ofth e analytica

l techniqu e (0. 5 part s pe

r billion) , an

d potentia l fo r sampl e contamination , volatil e organic s samplin g i s somewha t complex
. I t

i s important

tha t all step s b e followed
. Ever y effor t mus t b e mad e to avoi dcontamination , an d t o document

wher e contaminatio n migh

t originat e (e.g
. field, transport , la

b blanks)
. 

## Preparatio n Notif y th e Organi c La

b befor e collectin g an

y volatil e organi c samples
. Th e laborator y wil l prepare th e following vial s upon proper

notificatio n an

dscheduling : 1
. LA B BLAN K

Tw o vial s filled b y Sampl e Tracker

wit h purified wate

r an d kept in th e Organi c La

b fo r late r analysis
. 2
. TRANSPOR

T BLAN K Two vial s filledwit

h purifie d water

to accompan

y sample s throughou t

the sampling run . D o NO T open thes e vial s in th e field. Retu mt o th e La b wit h samples
. 3
. TRANSFE

RBLANK

Thre e vials , filled wit

h purifie dwater

by laborator

y personnel , carrie d t o th e samplin g sit e wher e th e Sample

r transfer s th e content s to tw o fresh vials
. 4
. SAMPL

E VIAL S Th e Sample r i s provide dwit

h sufficien

t duplicat e numbere d vial s fo

r DUPLICAT

E samplin g a

t each site
. Duplicate vial s ar e distinguishe db

y "-A " an d "-B " to designat

e first an dsecon d sample , respectively
. 

## Samplin g an d Documentatio n i
. Th e laborator

y will provide the Sample

r wit h pre-numbere d vial s fo

r the Samples , La

b Blanks , an

d Transpor

t Blanks
. Thes e via

l number s mus t

b e liste d on th e "Reques t

fo r Analysis"
. 2
. Transpor

t Blank s ar e NO T to b e opened , an

dare t o accompan

y th e Sample s a

t all times
. 3
. Th e Sample

r i s require dto prepar

e tw o Transfe

r Blank s a t th e samplin g site , usin g wate r supplie d b

y the laboratory
. . 4 ; Al l sample s ar e collecte di n REPLICATE , an d immediately refrigerated
. 5
. Sample s shoul d b e delivere dto th e Laborator y withou t delay
. 

## Sampl e Collectio n A
. Collec t

volatil e organi c sample s i

n paire d set s o f

40-m l glas s purg e vial s wit

h Teflon-line d (non-reactive ) septum s i n th e lids , labeled"A " an

d"B"
. Fil l tw o vials , i

n th e orde r

"A " followe d b y "B, " fromth e sam e spurc e wit h a s littl e time-lapse a s possibl e between them
. Fil l vial s all th e wa y t o th e to p an

d alittl e above , generatin g a positiv e meniscus
. N o air

bubble s shoul dpas s throug h th e sampl e a s the bottl e i s filled, o r b e trappe d i

n th e sample

### DE Q LAB : Field Sampling Referenc e Guide Decembe r 199 8 Revisio n 6. 0 - UNCONTROLLE D DOCUMEN

T Pag e 2 6 whe n th e bottl e i s sealed
. A positiv e meniscu s a t th e top ofth e bottl e wil l help ensur e tha t no ai r i s trappe d inside whe n ca p i s screwedon . Plac e th e vial s i n aplasti c bag , clos e th e top , an d pu t th e bag i n acoole r wit h ice
. Ship th e sample s t o the la

b a s soon a s possible
. 

## CAUTION ! Som e purg e vial s fromthe DE Q La b ar e pre-acidifiedfo r

preservation
. Eac h via

l contain s 1 0 drop s o f concentrate dhydrochlori c acid
. Acidifie dcontainer s normally giv e of f fumes , whic

h shoul d not

be inhale d I f spille do n clothe s o r

skin , flus h immediatel

y wit h copiou s amount s o f

coo l water . I n additio n to duplicat

e sampl e vial s fromeac

h site , asampling even

t shoul d include vial s fo

r Lab , Transport , an

d Transfe r blanks
. Whe

n sample r desire s Matri x Spikes(MS ) o r Matrix Spik

e Duplicate(MSD ) samples , h e mus t collec t an dsubmi t additiona l vial s fo r analysis
. Vial s fo

r MS o r MS D analyse s mus t

b e clearly designate d a s a separate ite

mon th e Reques t

fo r Analysi s form
. Not e th e numbe

r ofeae h purg e vial o

n th e "Reques t

fo r Analysi s Form " wit

h asit e description , dat

e an d time sampl e wa s taken , a s eac

h sampl e i s collected
. B
. Whe

n samplin g from atap , open th e ta p an dallo w th e syste

mt o flush unti l th e wate

r temperatur

e ha s stabilize d(usuall

y 5-1 0 min.)
. Adjus t

flow to about

50 0 ml/min an

d collec t duplicat e sample s fromth e flowing stream . The sample

r shoul densur

e tha t th e ta p i s free o f

aerator , strainer , an

d hos e attachmen

t o r wate r purificatio n device
. C
. Whe

n sampling froma

n open bod

y o f wate r fill a1 quar

t bottl e o r clea n beake r wit h sample , an

d carefull y fill duplicate sampl e bottle s fromth e container
. D
. Whe

n sampling well s wit

h abailer th e VO C sample shoul d b e collecte d fromth e first bailer-fiill afte

r purgin g well
. Precaution s shoul d b e take n to preven t aeratio n o f

sample
. E
. Whe

n sampling achlorinate dwate r suppl y fo r volatile s i t i s necessar

y to preserv e th e sample s wit h 25-m g Ascorbi c acid , the n acidif y wit h 2 drop s 1: 1 hydrochlori c aci dto destro y an y chlorin e tha

t ma y b e present . D o no t us e 40-m l vial s tha t

alread v contai n HCl
. If

thi s i s not done th e free chlorin e ca

n reac t wit h som e volatiles , producin g chlorinate d compound s tha t did not exis t i n th e origina

l sample
. Chec k VO C vial s fo r

Ai r Bubble s Inver t via l an d ta p o n soli dsurface.".I f present , ai r

bubble s wil l ris e

### DE Q LAB : Field Samplin g Referenc e Guide Decembe r 199 8 Revisio n 6. 0 - UNCONTROLLE D DOCUMEN

T Pag e 2 7 

## Appendi x B SAMPLIN G PROCEDUR E FO R DISSOLVE D OXYGE N INTRODUCTIO N Us e thi s procedur

e fo r fieldpreservatio n o f

wate r an d wastewater

sample s fo

r dissolve d oxygen . Th e preservatio n metho d employ s dr y reagent pillow s t o "fix " th e dissolve d oxyge n fo r late r analysis
. Manganou s ion react s wit h th e dissolve d oxygen present i n th e alkalin e solutio n to for mamanganes e (IV ) oxid e hydroxid e floe
. Azid e ion i s adde d t o suppres s interferenc e b y nitrite , which react s wit

h th e free iodin e generate d durin g analysis
. Followin g acidification , reduc e th e manganes e (IV ) flo e wit h iodide ; then titrate th e free iodine produce d wit h sodiu m thiosulfat e (o r PAO ) titrant
. 

## SAMPL E COLLECTIO N Collec t wate r sample s i n aclea n 300-m l BO D bottl e to overflowin g wit h minima l aeration
. Thi s ensure s tha t there wil l b e no ai

r bubble s trappe di n th e bottle
. Replac e groundglas s stoppe r unti l yo u ar

e read y to ad d reagent pillows
. 

## SAMPL E PRESERVATIO N 1
. Remov e glas s stoppe r an dad d content s o f

one Manganou s Sulfat

e Powde r Pillow
. Replac e ca

p an d inver t severa l time s t o facilitat

e mixing
. 2
. Remov e glas s stoppe r andad dcontent s o f

one Alkalin e Iodide-Azide Reagen t Powde r Pillow
. Inser

t stoppe r an dinver t bottl e severa

l time s t o mix
. A flocculent precipitate will form
. It

wil l be brownish-orang e i f dissolve doxyge

n i s present

o r white i f oxygen i s absent
. 3
. Allo w th e sampl e t o stan dunti l th e floe ha s settled
. Agai n inver t th e bottl e severa

l time s t o mix , an

d let standunti l th e floe settles
. 4
. Transpor

t sample s immediately t o th e Lab
. Stor e in th e dar k a t 10-20° C durin g transport . Preserve d sample s ca

n b e heldfo

r u p to 8 hour s prio r

t o final titration
. NOTES : a . I f

D O i s fo r Initia l D.O
. measurement use di n BOD determination s asecond bottl e mus t b e collecte d simultaneously an

dsen t t o th e la b i n acoole r wit h ic e (d o not

ad danythin g to thi s bottle)
. The coole r mus t b e carefull y packe dt o protec t

th e sampl e containers
. b
. Whe

n collectin g fo

r La b BOD measurement , an

d BO D i s expecte d t o b e greate

r tha n 5 mg/L , collec t

a n additiona l P-pol y o f sampl e fo r BO D dilutio n setups , instea dofth e second BOD bottle
. c . Remembe

r t o schedul e DO s an

dB0D5 s wit

h laborator

y s o tha t personne l ca

n b e scheduled t o perfor

m analyse s

### DE Q LAB : Fiel d Samplin g Referenc e Guide Decembe r 199 8 Revisio n 6. 0 - UNCONTROLLE D DOCUMEN

T Pag e 2 8

### DE Q LAB : Field Sampling Referenc e Guide Decembe r 199 8 Revisio n 6. 0 - UNCONTROLLE D DOCUMEN

T Pag e 2 9 

## Appendi x C FIEL D FILTRATIO N PROCEDUR E APPARATU S Th e filtering apparatu s consist s o f awide-mout

h jar , rubbe

r stoppe r wit h filter funne l bas e an d filter inserted , an

d removabl e magneti c filter

funnel
. Us e ahand-operate dvacuumpum p t o filter th e sample
. Filter s used mus t b e 0.4 5 micro n cellulos e membrane (4 7 m mdiameter)
. OPERATIO N 1
. Remov e ca

p fromclea

n 25 0 m l "DP" , o r "DM" , poly bottle ; plac e i n cente r of filtering jar
. 2
. Plac e rubbe

r stoppe r (wit h filter base ) firmly i

n ja r opening , wit

h filter ste minside pol

y sampl e bottle
. (Vacuu mcanno t b e produce dunles s ja r

i s securel y sealed)
. 3
. Plac e filter

membrane on filter

bas e grid
. (Mak

e certai n that

blu e separator

disk i s not attache d t o membrane)
. 4
. Plac e fiinnel ove

r filter. 5
. Pou

r approximately 25 0 m

l o f sampl e into th e fiinnel
. Evacuate th e filtering ja r (usin g han

d vacuumpump ) until sampl e begin s t o pas s throug h filter. If sampl e i s ver

y turbid , filter

severa l smal l volumes , replacin g filter membrane a s i

t become s plugged , unti l container i s frill. 6
. Remov e poly sampl e bottl e fi-o mth e Maso n filtering

jar
. Rins e filter

gri d an d funne l betwee n sample s wit

h distille dwater .

### DE Q LAB : Field Samplin g Referenc e Guid e Decembe r 199 8 Revisio n 6. 0 - UNCONTROLLE D DOCUMEN

T Pag e 3 0

### DE Q LAB : Fiel d Samplin g Referenc e Guide Decembe r 199 8 Revisio n 6. 0 - UNCONTROLLE D DOCUMEN

T Pag e 3 1 

## Appendi x D LEGA L SAMPL E CHAIN-OF-CUSTOD Y PROCEDUR E Purpos e T o provide appropriate suppor t t o litigatio n th e Departmen t mus t demonstrat

e th e integrit

y of sample s submitte d fo

r analysis , an

dtes t results , b y documentin g chain o f

possessio n o r

custody
. Written procedure s mus t

b e availabl e an

dfollowe d wheneve

r sample s destine d to becom e evidenc e are collected , transferred , stored , analyzed , o r discarded
. Their

primar y objectiv e i s t o creat

e a n appropriat

e an d accurate recor

d tha t ca n b e use dt o trac e th e possessio n o f asampl e fromit s collection , through analysis , until it s infroduction a s evidence
. A sampl e i s considere d t o b e i « ctw/oii v if i t is : a . I n actua l physica l possession
. b
. I n view , afte

r bein g i n physica l possession
. c . I n physica l possession , an

dthen place di

n secur e storage . d
. In asecure d are awhere acces s i s resfricte dt o authorize dpersonnel
. 

## Pre-samplin g Prior t o an y "Legal " sampl e collectio n th e Inorganic , Organic , an dQ A Mafiager

s a t th e Laborator

y shoul d b e appraise d ofth e project' s regulator y objectives , propose dsamplin g location s an d procedures , matrices , analytica l requirements , an

dchain-of-custod

y procedure s t o b e followed
. Thi s i s especially tru e fo r an y projec t collectin g LEGA L samples , o

r whe n non-routin e samplin g procedure s are employed
. Whe n crimina l actio n i s contemplate dth e potentia l litigant als o mus t b e informed tha

t sample s ar

e t o b e collected
. Sinc e analytica

l result s ma

y b e use d a s evidence , th e potentia l litigan t i s entitie d t o collec t

duplicat e sample s an

d hav e the manalyze dby someon e else , o r observ e th e analysi s bein g don e b y th e DE Q Laboratory
. 

## Sampl e Collectio n Th e minimu

mnumbe r o f person s shoul db e involved , an deac h shoul d b e traine d i

n prope r collectio n an

d handlin g o f samples
. Written procedure s fo

r collection , preservation , an dhandling , specifi c fo

r each sampl e typ e an

d analysi s mus t

b e followed , an

d an y deviation s documented
. Fiel drecord s mus t

b e complete , dated , an

d initiale d at

th e tim e th e sampl e i s collected
. Fil l ou t th e Reques t

fo r Analysi s form , providin g a t leas t th e followin g information : a . Specifi c samplin g locatio n b
. Date an

d tim e sampl e collecte d c . Purpos e d
. Sampl e container

numbe r e . Preservative s adde dan

dquantit y f
. Analyse s require d g . Pertinent

fielddat a(e.g. , pH , temperature ) h
. Nameo f

collector(s) : A separate , boun dfiel dlo g boo k i s highly desirable
. Th

e necessity , an d the specifi c information to b e recorde d therei n must

b e determine dprio r

t o sampling , h

y th e projec t manage r

### DEQ LAB : Fiel d Samplin g Referenc e Guide Decembe r 199 8 Revisio n 6. 0 - UNCONTROLLE D DOCUMEN

T Pag e 3 2 Th e sampl e collector

i s responsibl e fo

r th e care an

d custod y ofth e sample s (includin g documentation ) unti l th e sample s are properly shippe dt o th e Laboratory , o r custod y i s transferre d to anothe

r person . Color slide s o r photograph s ofth e samplin g locatio n are recommende d to facilitat e identificatio n and subsequen t recollectio n b

y th e sampl e collector(s)
. Sign an dwrite date , time, an

d location o

n th e bac k ofeae h photo
. Handl e photograph s accordin g t o chain-of-custod y procedures
. Keep ari

d protec t negative s (i f

appropriate ) a s par

t ofth e documentation
. 

### Transfe ro f Custod y Whe n transferrin g possession/custod y o f sample s th e dat

e an dtime o f fransfer mus t b e recorded , an

d al l person s involve dmus t

sign th e record
. Th e sampl e collecto r i s responsibl e fo

r prope r packaging , security , and fransport of sample s t o th e Laborator

y fo r analysis , a s wel l a s providin g al l necessar y sampl e documentation
. Sample s shippe dt o th e Laboratory , eithe r by mai l o r private carrier , mus t

b e i n ashippin g containe

r seale d wit h security tap e o

r aNumbere dSecurit

y Seal
. Th e numbe r

embosse do n th e securit y sea l mus t b e recorde d o

n th e Reques t

for Analysi s form , whic h accompanie s th e samples
. - ^ Onc e locked , awire cutter

i s require dt o remov e th e seal , assurin g th e integrit y ofth e samples
. Th e sampl e collector shoul d retai n acopy ofth e Reques t fo r Analysi s form
. Th e Laborator y as par t ofth e permanen

t chain-of-custod

y documentatio n wil l retai n copie s o f receipt s frompos t

offices , o r bill s of lading
. Adhesive-backe d"securit y seals" , whic h theoretically^sustai n damag e when removed , canno t alway s b e relie dupon . Experienc e ha s show n thes e seal s d o no t adher e t o som e plasti c ic e chest s (e.g
. the y can b e remove d withou t

damage!)
. A n effectiv e securit

y tap e i s filament

packin g tap e wrappe d severa l time s completel

y around th e cooler
. Th e tap e shouldb e signedo

r initiale d an

ddated usin g apermanent

marke r pe n acros s the tail-en d o f

the'tape
. Shipmen t o f asecur e cooler/ic e ches t

vi abu s doe s no t

requir e signatur e b y th e bu s compan

y agen t t o documen

t custod y transfe r fo r eithe r SECON D CUSTOD Y LEVEL
. Th e sampl e collector

mus t complet e aChain-of-Custod

y for mfo r SECOND CUSTOD Y LEVE L sample s (Criminal ) tha

t ar e delivere d directly t o th e Laiboratory
. Th e sampl e collector wil l receiv e acop

y to acknowledg e receip t ofth e sample s b

y th e Sampl e Tracker
. 

### Laborator y Custod y The Sample Tracke

r i s th e principa

l custodia n o f sample s i n th e Laboratory
. Th

e Q A Chemist , Inorgani c an

d Organi c Laborator

y Managers , an

d Laborator

y Divisio n Administrator

ar e als o designate d to act

a s sampl e custodians
. Sample s shoul db e handle d b y a^minimu

mnumbe r of persons . Th e Laborator

y maintain s locke d refrigerator s exclusively fo r storin g SECON

D CUSTOD Y LEVE L samples
. A log book i n which t o recor

dsampl e transfers , an

dasecur e plac e t o kee

p Chain-of-Custod

y forms accompanie s eac

h refrigerator
.

### D E Q LAB : Fiel d Samplin g Referenc e Guid e Decembe r 199 8 Revisio n 6. 0 - UNCONTROLLE D DOCUMEN

T Pag e 3 3 Th e Sample Tracker , o r

designate d altemate , receive s incomin g sample s an d document s receip t

o f SECON D CUSTOD Y LEVE L sample s wit h amulti-par

t NC RChain-of-Custod

y form
. Information require d b y th e form : a . Dat

e an dtime receive d b
. Number

o f sampl e container s receive d c . Dat

e sample s wer

e collecte d d
. Name o f

collecto r e . Name o f

perso n deliverin g sample s f
. Descriptio n an

didentificatio n numbe

r o f sampl e container s g . Signatur

e ofth e perso n deliverin g andperso n receivin g the samples
. 

## / / i s alway s appropriat e t o make writte n comment s o n th e Reques t fo r Analysi s o r Chain-of-Custod y for mconcemin g th e integrit y o r conditio n o f

samples
. Th e perso n deliverin g sample s get s the Pin k copy , th e Whit e cop y goe s to the Laborator y Offic e Manage

r fo r filing, an d th e Yello w cop y remain s wit h the samples
. Ifth e sample s hav e been maile do r shippe d t o th e Laboratory , th e Padloc k Securit y Sea l numbe r mus t b e recorde do

n th e Chain-of-Custod

y form
. Transportatio n receipt s ar e attache d t o th e Whit

e copy fo r filing, an d th e Pin k cop y given to th e sampl e collecto r t o acknowledg e receipt
. SECON D CUSTOD Y LEVE L sample s ar e distribute d fo

r analysi s o

r secured i n alocke d refrigerator , a s ' appropriate
. Th e Yello w cop y ofth e Chain-of-Custod

y for mmus t b e kep t wit h samples
. Al l laborator

y documentatio n an

dlog s ar e filledout

a s usual , but

th e sample s ar

e identified a s "LEGAL " to aler t the

. analys t ofth e nee dt o follo w custod y procedures
. Th e laborator

y are ai s designate dasecur e area , an d acces s i s resfricted t o authorized personnel only
. Laborator y personne l ar

e responsibl e fo

r th e care an

dcustod y ofth e sample , onc e i

t i s i n their possession
. The

y shoul db e prepare dt o testif y tha t th e sampl e wa s i

n thei r view , o r secure d i n th e Laboratory , a

t al l time s whil e i

n their custody
. Approve dmethod s fo

r laborator y analysi s will b e used an

ddocumented
. Al

l analytica l result s ar e recorde d ir

f boundnotebooks , retaine da s apermanen t recor di n th e Laboratory , a s wel

l as o n LIMS
. Whe n sampl e analyse s ar

e complet e th e unuse d portio n o f

sampl e mus t

b e returned to secur

e storag e unti l datai s reporte dou

t ofth e Laboratory
. Unuse dportio n o f

sample s loggedinto th e Laborator y under FIRS T CUSTOD Y LEVE L wil l b e discarde da s soon a s th e analytica l dat ai s reported
. SECON D CUSTOD Y LEVE L (Criminal ) sample s wil l b e discarded/destroye d onl y b y order ofth e Divisio n Administrato r

afte r consultatio n wit

h enforcemen

t officials , whe

n i t i s verified tha

t sample s ar

e n o longe r required
. The dat

e an dtim e o f destructio n i s recorde d o

n the Yello w cop

y ofth e Chain-of-Custod

y form , whic h i s initiale d an

dfiledwit h th e Whit

e copy .

### DE Q LAB : Fiel d Samplin g Referenc e Guide Decembe r 199 8 Revisio n 6. 0 - UNCONTROLLE D DOCUMEN

T Pag e 3 4

### DE Q LAB : Fiel d Samplin g Referenc e Guide Decembe r 199 8 Revisio n 6. 0 - UNCONTROLLE D DOCUMEN

T - Pag e 3 5



## Reference s NPDE S Complianc e Sampling Manual
. U.S
. EPA 0-241-037/44 , Enforcemen t Division , Offic e of

Wate r Enforcement , 197 7 Handboo k fo r Analytica l Qualit y Confro l in Water an dWastewate

r Laboratories
. U .S
. E

P A 600/4-79-019 , EMS L - Cincinnati , Office of Research an

dDevelopment , March , 1979.SPIKES , SPIK E DUPLICATES ? Wha t i s meant by Matri x Spike l Matri x Spik e Duplicate ? Th e concep t ca n b e ver y conflising
. Matri x Spike s (MSs ) are usefu l fo r assessin g th e analytica l bia s of amethod , i.e
. systemati c error s arisin g fromunstabl e calibratio n standards , matrix effects , interferences , elevate d blanks , instrumen t shifts , analys t

bias , etc . Matri x Spik e Duplicate s (MSDs ) ar e jus t a s th e name describes : aduplicat e ofth e Matri x Spike
. MSD s are usefii l fo r assessin g analytica l precision , i.e
. rando merror s arisin g frominstrumen t instability , fault

y technique , tolerances , etc. . Analytical precisio n ca n als o b e determine d b y analysi s o f tw o portion s ofth e sam

e sample , e.g . duplicate samples , withou t spiking
. Analysi s offiel d duplicate sample s ca n b e used t o asses s field samplin g precision
. Variou s method s developed unde r differen t program s (CWA , SDWA , & RCRA) requir e MS s an d MSD s a t afrequency from 5 t o 10 % ofth e sample s collected
. Mos t analytical method s ar

e develope dusin g relativel y clea n sample s unde

r wel l confrolle d conditions
. Whe n th e metho di s applie d by areal-worl danalys t t o areal-worl d sampl e matri x containin g chemica l compound s tha t interfer e wit h th e method , b

y eithe r reducin g o r

enhancin g th e recover

y ofth e analyt

e o f interest , w e ar

e said t o hav e abias
. Althoug h i t

ma y no t appea r logical , i t i s no t uncommo n to ad

d a n accurately know

n quantit y o f analyt e to asample , analyz e it , an

dget bac k considerably les s o

r mor e tha n 100 % of wha t wa s added
. I

n mos t case s bia s i s characterize d by occurrin g i n th e sam e direction , e.g . fo

r agiven analyst-matrix-metho d combination the result s ar e nearly alway s biase d in th e same direction , eithe r hig h o r low
. Th e degre e o f

bia s an dprecisio n i

n tes t dat ai s aresul t

o f bot h systemati c an

d rando merro r i n bot h the samplin g an

d analytical phase s ofth e project
. Assessin g whic h uncertaint y i s attributabl e t o which activit y i s not a precis e science , give n th e limite d amoun t o f dat aassociate d wit

h each individua

l projec t an d uniqu e matrix
. Theoreticall y th e sample , MS , an d MS D analyse s are performe do n identica l 'portion s o f

homogeneou s sampl e materia

l originatin g i

n asingl e sampl e container
. Thi s i s doabl e fo r som e type s o f sample , e.g . aqueous , o

r ver y finely divided , dr

y soli d(e.g
. powderedsand) , bu t i t i s no t possibl e fo

r ever y sampl e matrix o

r method
. Th e ke y t o thi s admonitio n i s tha

t th e sampledmateria

l mus t b e homogeneous , an

d ther e mus t b e enough sampl e quantit

y t o prepar e an danalyz e severa

l portion s ofth e sam

e sample
. Th e basi s fo

r thi s techniqu e i s tha

t b y analyzin g aportio n ofth e origina l sample , a s i

t come s fromth e field, w e determin e th e concentratio n of thos e analyte s in a

U portion s o f

tha t sample , includin g thos e portion s w e subsequently spike (M S an d MSD ) wit

h aknown concenfratio n o f analyte
. It i s necessar

y to find th e analyt

e concentratio n i

n th e un-spiked , origina

l sampl e materia

l befor e i t i s possibl e to calculate th e recover

y ofth e added(spiked ) concentration
. Matri x spik e recover y i s calculate d as follows :



### „ ., ' ^„ „ Observe d Concentratio n Percen t Spik e Recover y = lOOx - (Spik e Concentration)-I-(Initia l Concentration )

### DE Q LAB : Field Sampling Referenc e Guide

Revisio n 6. 0 - UNCONTROLLE D DOCUMEN

T Decembe r 199 8 Pag e 3 6 Where : Observe dConcentratio n = concentratio n of analyt e foun di n spike d sampl e Spike Concentratio n = concenfration o f analyt e spik e added Initia l Concentratio n = concenfration o f analyt e i n un-spike d sampl e Uncertaint y ma y b e create dwhen sample , MS , an d MS D ar e collecte d a s separate , discreet samples ; a questio n o f

homogeneit

y arises , particularl y fo

r soil s o r solids , raisin g concem s about th e relevanc e o f

MS & MS D analyses
. Th e probabilit

y o f collectin g tw o o

r mor e soil gra b samples , eve

n out ofth e same hole , an

d hav e the mb e identica l i s practically non-existent
. For vali dsample s fo

r spiking collec t

multipl e gra

b samples , mi

x the mtogethe r t o produc e ahomogeneou s composite , an dthe n sub-sampl e th e composite
. Althoug h i t woul d b e bes t

to sen d a single , bul k sampl e t o th e Lab , ifth e composit e i s thoroughly mixed i

t could b e package d in multipl e containers
. Thi s approac h shoul dwor

k fo r semi-volatiles , pesticides , TPH , herbicides , PAH , an d PCB s i n soil
. Ideally th e diagra

mbelo w i s th e wa

y M S & MS D sample s should originate , no t by collectin g separat

e gra b sample s fo r eac h entity
.
Fiel d Activit

y Composit e Initia l Sampl e

Analyz e a s Matri x Spik e Duplicat e

Concentratio n "y " Concentratio n « x " 4 - "v" : Concentratio n «._ M t a„, , . Mixin g acomposit

e o f soil gra b sample s i s generally not

avali dapproach fo

r Volatil e Organi c samples ; sample s fo r VOC s shouldb e disturbe da s littl e a s possibl e t o preclude los s of volatiles
. Instead i t

i s bette r t o collec t severa l smalle r gra b sample s Ein

d plac e the min th e containe r undisturbed
. A t th e presen

t tim e there i s alogisti c issu e a

t th e Lab : making certain tha t thos e organi c sample s wher e a MS & MS D ar

e requestedar

e spike dan

d analyzed
. It

arise s fromth e wa

y the Laborator

y Information Managemen

t Syste m(LIMS ) identifie s samples , assign s tests , andgenerate s wor k list s fo r the analysts
. T o minimiz e thi s difficult y we hav e requeste d tha

t samples , M S samples , an

dMS D sample s eac

h b e logge d int

o LIM S as aseparat

e ite mi n separat e containers
. Although thi s work s fo r us , it' s not

rigorousl y producin g M S o

r MS D data
. W

e assum e tha t materia l in^l l the container s i s homogeneous ; The quantit

y of sampl e submitte dca

n hampe r doing M S an

d MS D analyses
. Wit

h soil s i t i s les s of a concem , becaus e relatively small quantitie s o f sampl e ar e necessar y fo r analyses
. Howeve

r fo r aqueou s sample s th e metho d require s tha

t "...aroun d 1 lite

r o f sample... " b e exfracted
. A n "X " o r "L " glas s ja r

contain s aquar

t o r pin t of

### DE Q LAB : Fiel d Samplin g Referenc e Guid e Decembe r 199 8 Revisio n 6. 0 - UNCONTROLLE D DOCUMEN

T Pag e 3 7 ' sample , respectively
. Thi s doe s no t allo w performin g muhipl e analyse s o n asingl e containe

r o f liqui d fo r semivolatiles , pesticides , herbicides , etc. , becaus e i t take s on e fiill container

fo r eac h analysis
. 

## Surrogat e Spike s I n man y organi c analytica

l methods
. Surrogat e Spikes' ^ are adde d t o eac h sampl e analyzed , a s aqualit y contro l measure . Percent

recover y o f thes e surrogate s mus t

fal l withi n aspecifi c rang e fo r th e analysi s t o b e considere d"acceptable. " A Surrogat e i s astabl e compoundtha t i s chemically simila

r t o th e analyte s bein g analyze d for , bu t either isotopicall y labele d o r

els e doe s no t

occur a s anatural o r

manmade substanc e normally observe d i n envirbnmenta

l samples
. Example s include D6-Benzen e (benzen e wit h al l si x hydrogen s replace d b y deuterium) , bromofluorobenzene , variou s di

- o r tri-substitute dfluorobenzenes, etc. . Problem s ca

n occur wit h surrogat e recoverie s on sample s containin g elevate d concenfration s o f on e o r more analytes
. Surrogat

e spike s are prepare d a

t aconcentratio n t o function withi n th e norma l calibratio n rang e o f th e analytica

l instrument
. Observatio n o f ver y high concentration s o f

on e o r mor e analyte s require s th e sampl e b e dilute dto brin g thes e elevate dconcentration s within th e vali dconcenfratio n range . Substantia l sampl e dilutio n ofte

n result s i n dilutio n ofth e surrogate concentratio n t o alevel tha t i s belo w thei r

detectio n limit
. Although surrogat e recover y ma y appea r bad , i t ma y no t b e whe n all th e fact s are known
.

Anywher e fromon e t o thre e surrogat e compound

s pe r method , dependin g o n th e method
.

## Tabl e 2 Analyte/Containe r

ANALYT E Acidit y Alcohol s i Alkalinit y > Asbesto s (bulk ) | As h fre e dry weigh t BT U BOD S (Sfrea mBOD 5 initia l D O performe di n field) BOD 5 (DO<5mg/ L and/o r initia l D O performe d i n lab ) CBO D NBOD ^ Chlorid e Chlorin e Chlorophyl l a Chlorinate dPesticides/PCB s CO D 1 E
. Coli
. ; Feca l coliform , non-chlorinate d Feca l coliform , chlorinate d Tota l coliform , chlorinate d Colo r Conductivit y Coppe r 8 Quinolinat e Corrosivit y • Cyanid e Dissolve d Oxyge n (DO ) Ethylen e Dibromid e (EDB ) Flas h Poin t Fluorescei n Fluorid e Formaldehyd e Glyco l Hardnes s (calc. ) Herbicide s Hydrocarbo n I D Iodin e CONTAINE R P, T X P, T Z L, Z BO D bottl e P BO D bottle , P 2 X BO D bottle , P DP , D T BO D bottl e Chlorophyl l Tub e X, L R, V Plasti c Bac- T Narro w mout h bottl e Wid e mout h bottl e Wid e mout h bottl e P, T P, T X, L P BO D bottle , P 3 x 2 L X D P X X DP,D T X, L X, L D P MIN
. QUANTIT Y 10 0 m l 5 0 m l 10 0 m l 20 0 g 20 0 g 30 0 m l 50 0 m l 30 0 m l 60 0 m l 10 0 m l 30 0 m l 8 m l 80 0 m l 5 0 m l 7 5 m l 7 5 m l 7 5 m l 7 5 m l 5 0 m l 5 0 m l 80 0 m l 50 0 m l 30 0 m l 2 X 4 0 m l 20 0 g 80 0 m l 5 0 m l 80 0 m l 80 0 m l 20 0 m l 80 0 m l 80 0 m l 20 0 m l PRESERVATIO N 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 HOLDIN G TIME '

1 4 day s 1 4 day s 7 2 hour s N/ A 3 0 day s 4 8 hour s 4 8 hour s 4 8 hour s 4 8 hour s 2 8 day s Immediate ^ 3. 5 week s 7 day s t o extract * 2 8 day s 6 hour s Legal , 3 0 hour s routin e 6 hour s Legal , 3 0 hour s routin e 6 hour s Legal , 3 0 hour s routin e 6 hour s Legal , 3 0 hour s routin e 4 8 hour s 2 8 day s 7 day s t o extract' ' 1 4 day s 0. 5 h , 8h" * 1 4 day s 3 0 day s 3 0 day s 2 8 day s 3 0 day s 3 0 day s 2 8 day s 7 day s t o extract * 7 day s t o extract * 1 4 day sANALYTE

Ketones-Aldehyde s Lignin-Tanni n MBA S METALS ' •• . •.,-. • Chromium+ 6 Mercur y Boron , Silica , Commo

n Cation s Othe r Metal s Dissolve dMetal s Metal s i n solid s Methan e ga s Nitrogen : Ammoni anitrogen Nitrogen : Nitrite nitrogen Nitrogen : Nitrate+Nitrite nitrogen Nifrogen ; Tota

l Kjeldah l Nitroge n Oil & Greas e Organotin s (TBT , etc. ) Orth o Phosphat

e Polynuclea

r Aromati c Hydrocarbon s (PAH) PC B Pentachloropheno l Percen t Fa t Percent Sulfii r P H Phenolic s Pheophyti n a Phthalate s Propane i n wate r Sedimen t moistur e Sedimen t Partica l Sizin g Sedimen t Oxygen Deman

d(SOD ) Semivolatil e Organic s (PPOE , BNA) Sulfat e Sulfide s Percent Solid s Solvent s Suspende d Solid s CONTAINE R Cartridg e P P T M T H DP , DT T M D M L, Z Tedla r ba g R, V P,R, V R, V .R, V X, L Polycarbonat

e DP X, L X, L X, L Foi l L P,T, 0 X, L Chlorophyll tub e X, L B S S S X, L
. DP,D T BOD Bottl e Z B P, 0 MIN
. QUANTIT Y

Ai r sample s 5 0 m l 25 0 m l 10 0 m l 300 m l 10 0 m l 10 0 m l 10 0 m l 10 0 g 500 m l 5 0 m l 5 0 m l 5 0 m l 5 0 m l 800 m l 800 ml ' 10 0 m l 800 m l 800 m l 800 m l 5 gram s o f

tissu e 20 0 m l 10 0 m l 500 m l 8 m l 1 0 g , 800 m

l 4 0 m l 100 0 g I L 100 0 g 800 ml , 1 0 g 10 0 m l 30 0 m l 20 0 g 4 0 m l 20 0 m l PRESERVATIO N N A A A F C E C, E A D A D D D(cwA ) o r E(RCRA i M C A A A N A A L H A G A A A A C K B G A HOLDIN G TIME "

7 day s to extract * N/ A 4 8 hour s 2 4 hour s 1 4 day s 6 month s 6 month s 6 month s 6 month s 1 4 day s 2 8 day s 4 8 hour s 2 8 day s 2 8 day s 2 8 day s 180 day s to extract * 4 8 hour s 7 day s t o extract * 7 day s t o extract * 7 day s to extract * 6 month s 1 4 day s Immediate^ ^ 2 8 day s 3. 5 week s 7 day s to extract * 1 4 day s @N A 6 month s 7 day s t o extract * 2 8 day s 7 day s @N A 1 4 day s 7 day sANALYTE

Thiocyanat

e \ TCL P Tota l Dissolve d Solid s Tota l Organi c Carbo n Tota l Organi c Carbon (Soil ) Tota l Organi c Halide s Tota l Phosphat e Tota l Solid s Tota l Volatil e Solid s Turbidit y i Volatil e Aromatic s ' Volatil e Organic s ! Woodstov e Catalys t

, CONTAINE R P TM , A , X , L , S P R, V L Amber , TO

X bottl e R P P P Bx2, L Bx2, L TS P Filte r MIN
. QUANTIT Y

5 0 m l 200 g " 20 0 m l
. 2 0 m l 10 0 g 1 0 g , 200 m

l 10 0 m l 10 0 m l 200 m l 5 0 m l 2 X 4 0 ml , 5 g 2 x 4 0 ml , 5 g PRESERVATIO N A A A D A DfRCRA i o r E(cwA > D A A A G G B HOLDIN G TIME *

7 day s to extract * 7 day s 2 8 day s 2 8 day s 1 4 day s to extract * 2 8 day s 7 day s 7 day s 4 8 hour s 1 4 day s 1 4 day s Holdin g times les s tha

n o r equa l t o 7 2 hour s ar

e printe di n bol d text . ^ Nifrogenou s BOD determine db y differenc e betwee

n BO D & CBOD
. ' Chlorin e sample s analyze dwithi n 0. 5 t o 2 4 hour s afte r sampl e collectio n are reporte d a s estimates
. Sample s olde r tha n 2 4 hour s ar

e rejected
. * Sample s hel du

p to 4 0 day s afte

r extraction
. Analyz e immediately
. Winkler allow s stabilizatio n & holdin g fo r 8 hour s unti l titration. ^ ^ p H sample s olde

r tha n 3 6 hour s ar

e reporte d a s estimates
. ' ^ Ifth e sampl e contain s filterable solids , collec t sufficien t volum e to contain 200 g o f

solids
. Refe

r to DEQ' s field samplin g referenc e guide
.

## Preservatio n Code s A = Refrigerat

e o n ic e a t 4oC
. B = N o preservatio n required , bu t shoul db e kep t

on ic e a t 4oC
. C = Filter

in Fiel d(0.4 5 | i filter), an

d refrigerat

e a t 4oC
. D = Ad

d1 2 drop s cone . H2S0 4 to 50 0 m l bottl e an d refrigerate
. [H2S0 4 = Sulftiric Acid ] E = Ad

d2 5 drop s cone . HN0 3 t o 25 0 m l bottl e an drefrigerate
. [HN0 3 = Nitt-i c Acid ] F = Ad

d 5 0 drop s cone . HN0 3 to 500 m l bottl e an drefrigerate
. G = N o ai

r spac e i n container ; refrigerat

e a t 4oC
. H = Filte r

in field; store i

n aceton e wit

h MagnesiumCarbonate ; freeze wit h dr y ice ; avoi d light ! I = Ad

d alkalin e Potassiumiodide an dManganou s sulfate ; refrigerate! , (Se e samplin g procedur e fo r Dissolve d Oxygen ) J = Ad

d4- 5 pellet s o f

soli dpotassiumo r

sodiumhydroxid e t o 1000 m l bottle ; pH > 10 ; refrigerate
. K = Ad d Zin c acetate . Potassiumhydroxide t o pH > 9 ; exclude air ; refrigerate
. L = Addcone . H3P0 4 to pH < 4 ; Methyl orang e and 1 g Coppe r sulfate ; refrigerate
. [H3P04=Phosphori c acid]
. M = Ship o n dr

y ic e (freeze) ; allo w 1 inch headspac e fo r expansio n o f

sample
. N = Wra

p in clea n aluminumfoi

l an d freeze. 

## Containe rCode s ORGANIC S I N W

A TER : X = New , 100

0 m l ambe r glas s ja r wit h Teflon line d lid
. B = New , 4 0 m

l glas s via l wit h Teflon septum ; o

r Amber , 4 oz . TOX bottle
. METAL S I N WATER : T M = New , 25 0 m

l polyethylen e bottle
. D M = New , 25 0 m

l polyethylen e bottle
. T H = New , 500 m

l polyethylen e bottle
. SURFAC E WATER : P = Reused , 1000 m

l polyethylen e bottle
. D P = Reused , 25 0 m

l polyethylen e bottl e fo

r filtered sample
. R= Reused , 50 0 m

l polyethylen e bottl e fo

r sample s preserve d wit

h H2SO4
. LANDFILLS : T = D T = V = Reused , 1000 m

l polyethylen e bottle
. Reused , 25 0 m

l polyethylen e bottl e fo

r filtered sample
. Reused , 50 0 m

l polyethylen e bottl e fo

r sample s preserve d wit

h H2SO4
. SOLIDS : Z S L = "Zip-Loc " baggies
. = New , 1000 m

l polyethylen e bottle
. = Ne w 500 m

l ( 1 pint) Mason jar
. WAST E WATER : ST P = Reused , 100

0 m l polyethylen e bottle
. 5 = Reused , 25 0 m

l steril e polycarbonat

e bottle
. R= Reused , 50 0 m

l polyethylen e bottl e fo

r sample s preserve d wit

h H2SO4
. MIXE D PHASE : T L = Reused , 200 0 m

l o r 400 0 m l polyethylen e bottle
. T S = Reused , 50 0 m

l clea r glas s jar
. 5 = New , 1000 m

l polyethylen e wid

e mout h bottle
.

## Tabl e 3 CHEMICA L GROUPS , B Y ORGANI C ANALYT E

ALCOHOL S Methano l 1-Propano l iso-Propano l Ethano l n-Butano l 2-Propano l 

### CHEMICA

L OXYGE

N DEMAN

D (COD ) Nonspecifi c tes t

t o measur e oxygen depletio n potentia l o f awater sampl e assumin g al l material s are chemicall y oxidize d t o thei r

highes t oxidatio n state : reporte d a s m g oxyge n pe r liter
. 

### CHEMICA

L MAS S BALANCE CARBO N (CMB ) Nonspecifi c tes t

tha t measure s elementa

l carbo n an

dorgani c carbon o

n suspende d particulate samples , alon g wit h variou s metal s andchemica l species
. 

### CYANIDE Tota l Cyanide * Mus t reques t Cyanid e Amenabl e to Chlorinatio n whe n seekin g t o determin e characteristi c waste criteri a unde r RCRA
. 

### HERBICIDE S 2,4- D Dicamb a 2,4-D B MCP P 

### Hydrocarbo n I D (HCID ) Kerosen e Stoddar d Solven t Thinne r Gasolin e Minera l Spirit s 

### N- P PESTICIDE S Guthion Demeton- S Coumapho s Dimethoat e Fensulfothio n Phosdrin Disulfoton Fenthio n Dibrom Tetrachlorvinpho s Sulfote p 

### Oi l AND GREAS E Dichlorprop Dalapo n Dinose b 2,4,5- T
Fuel Oil # 1 Fuel Oil #2 (Diesel ) Fuel Gil # 4 Fuel Oil s #5 , #6 (Bunker

)
Sulprofo s Diazino n '

" Phorat e Fenchloropho s EP N Malathio n Parathion-ethy l Tokuthio n Tefraethylpyrophosphat

e Silvex

MCP A Piclora m

Chlorpyrifo s Dichlorvo s
Propho s Merpho s Parathion-methy l Trichloronat

e
Non-specifi c tes t

fo r hydrocarbon-lik

e compound s containin g -CH2

- linkage s (infra-re d techniqu e looking fo r C- H stretch)
.

### CHLORINATE D PESTICIDE S a-BH C P-BHC 5-BH C r-BH C (Lindane ) Heptachlor Aldri n Heptachlo r

epoxide p,p'-DD E Dieldri n Endri n p,p'-DD D Endosulfa n I I p,p'-DD T Endri n Aldehyd e 

### POLYNUCLEA

RAROMATI C HYDROCARBONS (PAHs ) Acenaphthen e Acenaphthylen e Anthracen e Benzo(a)anthracen e Benzo(a)pyren e Chrysen e Fluoranthen e Fluoren e Heptacosan e Naphthalen e Azulen e Dibenzofura

n Dibenzothiophen e Phenanthren e Pyren e Acridin e Carbazol e Benzo(b)fluoranthen e p,p'-Methoxychlo r Endri n keton e Chlordan e Toxaphen e Endosulfa n sulfat e Endosulfa n 1
Benzo(k)fluoranthen e Perylen e Dibenzo(a,h)anthracen e Indeno ( 1,2,3-c,d)pyren

e Benzo(g,h,i)perylen e



### POLYCHLORINATED BIPHENYL s (PCBs ) Aroclo r 101 6 Aroclo r 124 8 Aroclo r 122 1 Aroclor 125 4 Aroclo r 123 2 Aroclo r 1260 Aroclo r 1242 Aroclo r 126 2 

### PHENOLIC S Non-specifi c tes t

fo r phenolic-lik

e compound s (colorimefri c procedur e in whic h sensitivit

y i s inversel

y relate d t o th e numbe

r o f substitution s o

n th e aromati c ring)
. I f

specifi c phenol s ar

e required , se e semi-volatil e organi c exfractables
. Wil l no t

measur e pentachlorophenol
. 

### SEMIVOL

A TIL E ORGANIC s (Priorit y Pollutant s Organi c Extractables ) Acenaphthen e Acenaphthylen e Aldri n a-BH C Anthracen e Endosulfa n sulfat e Benzo(a)anthracen e Benzo(a)pyren e Benzo(b)fluoranthen e b-BH C bis(2-chloroethoxy)methan e bis(2-chloroethyl)ether bis(2-chloroisopropyl)ether bis(2-Etiiylhexyl)phthalate 4-bromopheny l Pheny l Ethe r Butylbenzylphthalate 4-Chloro-3-methylpheno l 2-Chloronaphthalen e 2-Chloropheno l 4-Chlorophenylpheny l Ethe r 2,4-Dinittotoluen e 2,6-Dinitrotoluen e di-n-octy l phthalate Endosulfa n I Endosulfa n II Benzo(g,h,i)perylen e Endri n Endrin aldehyd e Fluoranthen e Fluoren e Y-BH C Heptachlor Heptachlo r

epoxide Hexachlorobenzen e Hexachlorobutadien e Hexachlorocyclopentadien e Hexachloroethan e Isophoron e 2-Methyl-4,6-dinifropheno l 2-Methylpheno l Indeno ( 1,2,3-c,d)pyren e Dibenzo(a,h)anthracen e 1,2,4,5-Tetrachlorobenzene Dibenzofura

n Diethylphthalate Pyren e Endosulfa n cycli c sulfat

e bis(2-ethylhexyl)adipat

e Benzo(k)fluoranthene 2,4,5-Trichloropheno I trans-Nonachlo r 2,4,6-Trichloropheno l 2,4-Dinitropheno l 1,2,4-Trichlorobenzene Dimethy l phthalat

e 2,3,4,6-Tetrachloropheno l 2,4-Dimethypheno l 2,3,5,6-Tetrachloropheno l DieldrinChrysen e

4,4'-DD D 4,4'-DD E 4,4,-DD T 6-BH C Dibuty l phthalate 1,2-Dichlorobenzene 1,3-Dichlorobenzen e 1,4-Dichlorobenzene 3,3'-DichIorobenziden e 2,4-Dichloropheno l 4-Methylpheno l Naphthalen e Nitrobenzen e 2-Nifrophenol 4-Nifropheno l N-Nitrosodimethylamin e N-Nifroso-di-(n-propyI)amine N-Nifrosodiphenylamin e Pentachloropheno l Phenanthren e Pheno l Plu s Tentatively Identifie d Component s (TICs ) i n th e Sampl e Extr a 

### SOLVENT S Aceton e 2-Propano l Methy l isobuty l keton e (MIBK ) 

### VOL A TIL E AROM

A TIC s ( B Benzene , o-Xylen e 

### VOLATIL

E ORGANIC s (VO Chloromethan e Viny l chlorid e Bromomethan e ^ Chloroethan e N Trichlorofiuoromethan e Acrolei n (2-Propenal ) 1,1-Dichloroeth

y Ien e Methylen e chloride trans-1,2-Dichloroethylen e 1,1-Dichloroethane 2,2-Dichloropropan e cis-1,2-Dichloroethylen e 2-Butanon e (MEK

) Bromochloromethan e Chlorofor m 1,1,1-Trichloroethane Carbo n tetrachlorid e ^ Benzen e 1,2-Dichloroethane Trichloroethylen e 1,2-Dichloropropane Bromodichloromethan e 2-Chloroethy l vinyl ethe

r cis-1,3-Dichloropropen e 4-Methyl-2-pentanon e (MIBK ) Hexachloro-1,3-Butadien e ¥* l Methy l ethy l keton e (MEK ) Ethyl acetate

. 

### TEX ) Toluen e m-Xylene 

### Q Toluen e frans-1,3-Dichloropropene 1,1,2-Trichlorethane 1,1,2,2-Tefrachloroethylene 1,3-Dichloropropane Dibromochloromethan e 1,2-Dibromoethan

e (EDB ) Chlorobenzen e Ethyl benzen e 1,4-/1,3-Dimethylbenzene 1,2-Dimethylbenzene Styrene Bromofor m Bromobenzen e 1,1,2,2-Tefrachloroethane n-Propy l benzene 2-Chlorotoluen e 4-Chlorotoluen e 1,2,4-Trimethylbenzene 1,3-Dichlorobenzene 4-Isopropyltoluen e 1,4-Dichlorobenzene 1,2-Dichlorobenzene n-Butylbenzen e 1,2,4-Trichlorobenzene
T

- A_A ; i_
. ¥ j ^:r:-. j /" " ] » Ethylbenzen e p-Xylen e

/T^T/~'« \ Plu s Tentativel y Identifie dCompound s (TICs ) 

### TOTA L ORGANI C CARBON (TOC ) Nonspecifi c tes t

tha t measure s organi c carbo

n conten t o f awate r sampl e a s milligram s of

Carbo n pe r liter
.

### TOTA L ORGANI C HALIDE S (TOX ) Nonspecifi c tes t

that measure s tota

l halid e (fluorine , chlorine , bromine , iodine ) content o f a n organi c exfract
. 

### TOTA L PETROLEU M HYDROCARBON (TPH ) Hydrocarbo n I D analysi s performedon soi l sample
. Base do n ID result , analysi s ma y b e followed u p wit

h TPH-G , TPH-D , and/or

amodifie dversio n o f

metho d 418.1
.

## Tabl e 4 ICA P TES T GROUP S

Th e Inductivel y Couple dArgo n Plasma(ICAP ) instrument i s capabl e of

simultaneously scannin g asingl e sampl e fo r multipl e trac e metals
. T o simplif y loggin g i

n sample s t o LIM S fo

r multipl e trac e metal s anumbe r o f Tes t Group s hav e been designate dt o mee t th e need s o f

differen t progra mobjective s {e.g
. landfill monitorin g wells , groundwater , surfac e water , drinkin g water , etc.)
. It i s frequently mor

e cost-effectiv e t o analyz e fo r aTes t Group , tha

n to analyz e fo

r asingl e metal
. Th e variou s "tes t Groups " are liste dbelow : Elemen t Aluminu m Antimon y Arseni c Bariu m Berylliu m Boro n Cadmiu m Calciu m Chromiu m Cobal t Coppe r Hardnes s a s CaC0 3 Iro n Lanthanu m Lea d Lithiu m Magnesiu m Manganes e Molybdenu m Nicke l Phosphoru s Potassiu m Rubidiu m Seleniu m Silic a Silve r Sodiu m Strontiu m Sulfu r Thalliu m Ti n Titaniu m Tungste n Vanadiu m Zin c Zirconiu m INDM l • '

y ^

- • • •
• • ^ V '

• "

• INDM 2

•

•

i ^ PPM l

• • V
• • V

V V

^

• V PPM 2
• V

V

V

V TPM l
/ 

### • V
•

•

•
• SCA

N y ' • • • V • V V • • V V V V ^ • • V • • ^ • • • • • • y ^ • / • V
• ' • V •

## Tabl e 5 UNIT S & CONVERSION S

Metri c System Th e basi c unit s o f

measuremen

t i n th e metri c systemare th e meter , gram , an d Uter , all ofth e res t ar e multiple s o f

thes e quantitie s usin g a n exponent

o f 10
. Prefix Symbol Multipl e Decima l Name 10' ^ 10' ' 10'

- 10 ' 10 ^ 10 ^ 10 ^ 10 ^ 10

- 10- ' 10- ^ 10- ' 10- ' 10- ' 1 liter = 100 0 milliliter s = 1,000,00

0 microliter s = 100

0 cm ^ 1 kilogra m= 1000 gram s = 1,000,000 milligram s = 1,000,000,000 microgram s 1 cm ' H2 O = 1 c c H2

O = 1 milliliter

H2 O = 1 gra mH2 O 

### Conversion s Ex a Pet a Tera Gig a Meg a Kil o Hecto Basi c unit : Cent ! Milli Micr o Nan a Pic o Femt o Att o E

P T G M k h
c m | i n P f a 1,000,000,000,000,000,00 0 1,000,000,000,000,00 0 1,000,000,000,000 1,000,000,000 1,000,00 0 1,00 0 10 0 meter , gram

^ lite r - 0.0 1 0.00 1 0.000,00 1 0.000,000,00 1 0.000,000,000,00 1 0.000,000,000,000,00 1 0.000,000,000,000,000,00 1 Quintillio n Quadrillio n Trillio n Billio n millio n thousan d hundre d hundredt h thousandt h milliont h billiont h ^ trilliont h quadrilliont

h quintilliont

h

Uni t Acre Acre Acre Barre l (petroleum) Bushe l Chai n (surveyor's ) Cor d (wood ) Cu p Degre e (temperature ) Fatho m Foo t Foo t Foot " Foot ' Foot ' Gallon , liq
. (US ) Grai n Gra m Hectare Inc h inch ^ inch ' Kilogra m Kilometer Kilometer ^ kno t (nautical ) leagu e (nautical ) Lite r Liter Meter Meter ^ Meter ' Metri c Equivalent 0.4046856 4 hectare s 4046856 4 meter s 0.004046856 4 sq . kilometer s 158.9872 9 liter s 35.2390 7 liter s 20.116 8 meter s 3.62455 6 cubi c meter s 0.236588 2 liter s ° C =(5/9)(°F-32 ) 1.828 8 meter s 30.4 8 centimeter s 0.304 8 meter s 929.030 4 cm ' 28.31684 6 liter s 0.02831684 6 meter ' 3.78541178 4 liter s 64.7989 1 milligram s 1000 milligram s 10000 meters ' 2.5 4 centimeter s 6.451 6 centimeters ' 16.387064 cm ' (or

milliliters ) 0.00 1 metri c to n . 1000 meter s 10 0 hectare s 1.85 2 kilometers/h

r 5.55955 2 kilometer s 0.00 1 meter ' 100 0 milliliter s (o

r cm' ) 10 0 centimeter s 1000 0 cm ' 1000 liter s Englis h Equivalent 4356 0 square fee

t 484 0 yard s 0.001562 5 sq . mile s .4 2 gallon s 4 peck s 6 6 fee t 12 8 cubi c fee

t 8 ounce s liqui d (US ) ° F = ° C (9/5)+3 2 6 fee t 1 2 inche s 0.33333 3 yard s 14 4 in ' 7.48051 9 gallon s (US ) 172 8 in ' 4 quarts , liq.(US ) 0.0022857 1 ounce s (advp ) 0.0352739 6 ounce s (advp ) 2.471053 8 acre s 0.0833333 3 fee

t 0.0069444 4 feet ' 0.034632 0 pints , liq
. 2.20462 3 pound s 0.6213711 9 mile s 247.1053 8 acre s 1.15 1 miles/h

r 3 nautica l mile s 1.05668 8 quarts , liq
. 1.09361 3 yard s 1.19599 0 yards ' 1.30795 1 yards 'Uni t

Micro n Mi l mile , nautica l mile , statut e ounce , adv p ounce , liqui d Pac e pint , liqui d poin t (typographical ) pound , adv p quart, , liqui d Ro d sectio n (US ) Tablespoo n Teaspoo n ton , metri c ton , shor t yar d yard ' yard ' Metri c Equivalen t 0.00000 1 mete r 0.025 4 millimeter s 1.85 2 kilometer s 1.60934 4 kilometer s 28.34952312 5 gram s 29.5735 3 milliliter s 76. 2 centimeter s 0.47317647 3 lite r 0.351459 8 millimete r 453.5923 7 gram s 0.94635294 6 lite r 5.029 2 mete r 2.589988 1 kilometer ' 14.7867 6 milliliter s 4.92892 2 milliliter s 100 0 kilogram s 907.1847 4 kilogram s 0.914 4 mete r 0.8361273 6 meters ' 764.55485798 4 liter s Englis h Equivalen t 0.000039 4 inc h 0.00 1 inc h 1.150779 4 mile s 528 0 fee t o r 8 fiirlongs 437. 5 grain s 0.062 5 pint , liqui d 3 0 inche s 0. 5 quart , liqui d 0.01383 7 inc h 1 6 ounces , adv p 2 pints , liqui d 5. 5 yard s Imile '
. 3 teaspoon s 0.3333333 3 tablespoon s 2204.62 3 pound s 200 0 pound s 3 fee t 9 feet ' 2 7 ft'or 201.97 4 gallon s 

### Perspectiv e part-per-millio n part-per-billio n part-per-trillio n pp m pp b ppt 1 mg/kg
. 1 UgAcg , Ipg/kg , 1 mg/ L \\iP/ L Ipg/L

1,000,00 0 pp t = 1,00 0 pp b = 1 pp m One ppm : 1 inc

h i n 15.78 2 mile s o

r 1 second i

n 11.5 7 day s One ppb : 1 inch i n 1578 2 mile s o

r 1 secon d i

n 31.7 1 year s On e ppt : 1 inch i n 15,782,82 8 mile s o

r 1 second i

n 31,71 0 year s 

### Percentag e .Percen t mean s parts-per-hundred
. Seldomuse d a s auni t o f environmenta

l analytica

l measurement , becaus e i t i s to o large
. Percent , % 1 0. 1 0.0 1 0.00 1 0.000 1 0.0000 1 pp m

10,00 0 100 0 10 0 1 0 1 0. 1For m I 

# DEPARTMEN T Intar-Laboira ' 

# 8TA L QUALB P

Sourc e Name : _ Contac t Person : Address : DE Q Cas e Number : Sampl e Date : Phone : Collecte d By : Region/Division : Analyt e

CBOD * BO D Suspende d Solid s Feca l Coliform * Chlorin e Residua l p H FIEL D MEASUREMENTS *

Influen t

- .'• '

.

•'• • Effluen t

gra b Effluen t

composit e

Othe rParameter s (Fil l i n test )

- ' • / -

- • _ ; 1 '

, ' -. ^ •

, -

. ^ SOURC E SAMPL E RESULT S

Influen t

M F MP N

' Effluen t gra b

M F MP N Effluen t composit e

M F MP N

- DE Q LA B RESULT S Influen t

M F

,

- ^ -

'

' ~

• " Effluen t gra b

M F

, -

- , Effluen t

composit e

. M F

Shade d are a fo r DE Q use . •DE Q sample r ente r you r fiel d measurements , i f taken ; indicat e whethe r the yar e estimates . •CBO D i s whe n nitrificatio n inhibito r i s use d i n th e BO D test . •Indicat e i f analysi s i s b yMP No r MF . Date/Tim e BOD' s se t u p a t sourc e lab : Date/Tim e FC s se t u p a t sourc e lab : Date/Tim e BOD' s se t u p a t DE Q lab : Date/Tim e FC s se t u p a t DE Q lab : Fil l i n you r spli t sampl e result s an d mai l to : DE Q La b 171 2 S W 11t h Ave
. Portland , O

R9720 1 Attn : Q

A Chemis tFor m I I

Sourc e Name : _ Contac t Person : Address : 

# OREQO M DEPART S TO P ENVDRON I -Laborator y Spli t Compariso n Sampl e Date : 

# 8TA L QUALB P DE Q Cas e Number :

Collecte d By : Phone:
_ Region/Division : Analysi s FIEL D MEASUREMENTS *

Sampl e A

- ,' " ' 1

Sampl e

f <



## ' i ! '

, t

•

c Sampl e

C

-

' ' SOURC E SAMPL E RESULT S Sampl e A Sampl e

B

' • Sampl e

C Sampl e

D Date/Tim e

Analysi s se t u p DE Q LA B RESULT S

Sampl e A :'^^.:':^''^:-!^i^^!-:'^;i:-:'i-ii i w^ww:::^:::'^: : 

## ;lii?il|l |
5 %•:;: : •;•?;&:-?»; , 

# W;§ M llllll l 1111111 1 Sampl e

B 

# liiii i liiiiii i :^^i:^^i-^"-::'-vS-;;i'::;^:- ^ ;:f;-:;::;;f.v:;:sfft,;ii:: : W:^':}^x'' h •M::ii<-':i:&\ : 

# iiiiill i 

# Iiiii l Sampl e

C 

### :iilii;p;|f |

:":>!•: - ': • r^^^-::.:- ^ •;;;i;^.r':.•; , ••^'x:v:.:;^ y *:lS;S?:E4;;f;iJK:y:: ; 

# iiiliili S Sampl e

D 

# liiiiii i liiiiii i 

# ii-'ii v^v;'
. :--';';*-\'-v- '

iiii:;,vW|i;i : : ? Date/Tim e

Analysi s se t u p 

# iiiiiliili-^ i

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

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h

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

A B C D Sampl e poin t descriptio n •

(ie
. Effluen t comp.)
. $:'''^':.-,:y:M::'WiMX m ii::S::|-:ffil:;!l®:^liillil£|i:i^ ^ 

# |i||||iii|||ii|||i i iliiiliiil i iiliiiiBiiiil i Containe rnumbe r SOURC E DEQ *

'
. Fil l i n you r spli t sampl e result s an d mai l to :
171 2 DE

Q S W Portland , Att n La b

11t h O R 

### ^•^ ^ Ave
. 9720 1 Q A Chemis t

|

Shade d are a fo rDE Q use . •DE Q sample rente ryou rfiel d measurements
. I f taken ; indicat e whethe rthe y ar e estimates
. •DE Q sample ri s responsibl e fo rcompletin g thi s column
. Nee d assistanc e wit h tlii s form ? Contac t tli e Q A chemis t a t (503 1 229-5983
.Location/Site :

Collecte dby : _ Purpose : Comments : DEPARTMEN T O F ENVIRONMENTA

L QUALIT

Y Reques t fo r Analysi s Dat e Sampled:
. Fund Code : Cas e No
. Dat e Receive di

n Lab : Dat e Reported : Repor t Datato ;
ltem #
1

2

3

4

5

6 Samplin g Poin t Descriptio n (includ e time )

•

- PF O Bucke t # :

~ - - =^-= ^ 5ii:i;_ : =i : Test(s ) Require d Lead , TPART , TASK , % VOL , PFOUP , PFOD N

Lead , TPART , TASH , % VOL , PFOUP , PFOD N

Lead , TPART , TASH , % VOL , PFOUP , PFOD N

Lead , TPART , TASH , % VOL , PFOUP , PFOD N

y Lead , TPART , TASH , % VOL , PFOUP , PFOD N

Lead , TPART , TASH , % VOL , PFOUP , PFOD N

Laborator y Comments :

Contac t Sampl e Tracke r fo r prope r samplin g containers an

d preservatio

n procedure
. (503 ) 229-598 3