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To verify compliance for NPDES
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To determine if our processes are efficient

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Must be representative
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Consider your collection point
Consider the analysis
Sample containers must be clean and free from interference
Must be handled right to avoid degradation, contamination, compromising
Correct collection and preservation
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Low level mercury
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Biological

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Assess the potential for hazards
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Physical
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 leaning, stretching, pulling, lifting
Awkward positions
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Constituents
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Toxic, biological, pathogens
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Entry: skin, eyes, nose, mouth

General PPE
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Gloves
Eye protection
Ventilate area if vapors may be present
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Specific PPE
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Containment suits
Special gloves, boots

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Manual
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Dippers
Buckets
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Automated
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Flow based
Time based

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Grab samples or composite grab
Mix well before transfer
Proper container
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Rusty coffee cans are probably not the right container…….

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Usually 24 hour
Flow based more accurate than time based
Clean tubing
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2 sets- one cleaning, one in use
Wear on tubing could change volume pumped
Calibrate pump frequently
NPDES states to pull at least 100ml

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Dedicate containers
Clean containers well
Use detergents that are free of interference/contamination potential
Rinse with DI water 3 X
Dry completely
Container should not interfere with analysis

Organic Carbons
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Can not use plastic containers to collect
VOC, TOC, or any C’s
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It will contaminate sample

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Glass or plastic
Hard glass (pyrex) is preferred
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Silica, sodium, and boron may be leached from soft glass but not plastic
Use glass for all organics (VOC, semi VOC, pesticides, PCBs, oil and grease)
Avoid plastic when possible- phthalate esters can contaminate sample

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Use amber glass bottles to avoid photodegradation
Caps are important too!
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No paper liners
Use foil or PTFE liners
Be aware that metal liners can contaminate samples for metals

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Most methods tell you the minimum quantity needed
Give yourself some extra
For pre-preserved containers
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Make sure that the quantity collected is the right volume. Don’t fill ¼ full if the bottle needs to be full.

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Provide “snapshot”
Used for process control
Short hold time
Used when samples are not variable
Used for testing that requires immediate analysis
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Cl2, pH, temp, organic, volatiles
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Several grabs over time course to show variability

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Represent heterogeneous matrix
Can be set to represent flow based
Can result in loss or dilution of analyte
Can result in increase interferences
Can not be used on certain tests
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Cl2, pH, temp

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Field blank
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Usually DH20 transferred from one container to another while at sampling site
Usually low level contaminates
Lab blank
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Usually DH2O analyzed in tandem
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Tests for contamination/proper technique
Indicates background levels

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Pole dippers
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Secure container
Submerge container
Buckets
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Start downstream and move into flow
Direct
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Start downstream and move into flow

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Set Sampler to collect flow based or timed
Determine potential for contamination from tubing
Tubing should be clean
Tubing should be located in area that is representative
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Don’t rest on bottom
Avoid dead areas
Needs to be in center of flow

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Same location every time
TOC and some volatiles should not be put into plastic containers
Transfer quickly with minimal exposure to air
Don’t transfer multiply times
Cap container quickly
Label the container
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Time, date, location, collector

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Collection bottle should be refrigerated
Clean tubing and collection bottle
Collection bottle should be large enough to mix sample
Mix the right way
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Too little and not enough mix of settlables
Too much and incorporate air/analyte loss

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For stream sampling, make sure you enter downstream of where you will take sample
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Move upstream to gather your samples if you have multiple sites
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Change gloves frequently

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Minimize exposure to air when transferring
Don’t overfill pre-preserved bottles
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Put preserve in bottle after sample
Leave headroom for biologicals
No air bubbles for volatiles

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Handle caps with care
Setting them on the ground risks contamination
Setting them upright risks contamination
Holding them risks contamination
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Depends on the surroundings……

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Two people
Dirty hands/clean hands technique
One person only handles the sample containers
One person collects sample, pours into sample container

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NPDES states “at least” 8 grabs of at least
100 mls over periodic intervals during working hours
Collect each grab and refrigerate
Mix equal amounts of grabs together
Mix well
Example: radium in sludge

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Wear gloves
Protects you
Protects the sample
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DEET
Lotions/soap
Do you know where your hands have been?

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 pH control
Chemical addition
Amber or opaque bottles
Refrigeration
Filtration
Freezing

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Retard biological action
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Retard hydrolysis of chemical compounds
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Reduce volatility of analyte

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Depends on Analysis
Some acids can degrade plastics- be careful

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Ice or refrigerate immediately
Keep temperature from fluctuating
Preserve immediately if bottle is not prepreserved
Some samples are stored at room temp

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Begins when sample is collected
Depends on analyte
Rule of thumb:
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The quicker it’s analyzed, the better

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Labels
Seals for bottles
Facility bench sheets/ Field log books
Analysis request sheet (COC)
Record of delivery to laboratory
Receipt and logging of sample
Assignment of sample

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Traceability
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Shows who handled sample from collection, preservation, storage, and analysis.
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Allows for routine control of samples and also aides in litigation issues

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Permanent maker
Attached to container
Lists the following:
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Date and time of collection
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Facility
Location
Type of sample
Preservative
Analysis
Collector

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Usually from Lab
Fill out completely
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Sample name, date and time of sample
Type of sample
Preservative
Bottle and volume
Analysis needed

(10) Monitoring and records.
(a) Samples and measurements taken for the purpose of monitoring shall be representative of the monitored activity.
(b) The permittee shall retain records of all monitoring information, including all calibration and maintenance records, and all original strip chart recordings for continuous monitoring instrumentation, copies of all reports required by this permit, and records of all data used to complete the application for this permit, for a period of at least 3 years from the date of this permit, measurement, report or application. This period may be extended by request of the
Agency at any time.
(c) Records of monitoring information shall include:
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The date, exact place, and time of the sampling or measurements;
The individual(s) who performed the sampling or measurements;
The date(s) analysis were performed;
The individual(s) who performed the analyses;
The analytical techniques or methods used; and
The results of such analyses.
(d) Monitoring must be conducted according to test procedures approved under 40 CFR Part 136, unless other test procedures have been specified in this permit. Where no test procedure under
40 CFR Part 136 has been approved, the permittee must submit to the Agency a test method for approval. The permittee shall calibrate and perform maintenance procedures on all monitoring and analytical instrumentation at intervals to ensure accuracy of measurements.

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All calibration and maintenance Records
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Yearly maintenance of balance etc
Replacement date of probes
Thermometer calibrations
Pipettes
Original strip chart recordings
Required Reports
Keep for 3 years

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Date, exact location, collector and time of sample
Date, time, analyst, and method for each test
Record results in proper units
Include time points for analysis
 time in /time out of oven, weighing, ect
Daily temperatures and calibration of instruments need to be recorded

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EPA, IEPA are taking a closer look at paperwork.
Make sure you have it written down
Make sure you have a copy
If you don’t have SOPs, make sure you can at least support your procedure

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CFR has hold times and preservatives
Standard Methods 1-33 has hold times, preservatives and container types and size
NPDES
EPA/ IEPA
FVOA

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“Complete and unequivocal preservation of samples, whether domestic wastewater, industrial wastes, or natural waters, is a practical impossibility because complete stability for every constituent never can be achieved. At best, preservation techniques only retard chemical and biological changes that inevitably continue after sample collection”

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Doesn’t mean we shouldn’t try.
Just need to be realistic
Follow basic rules
Be consistent
Analyze as soon as possible