Sampling Instructions - caltestlabs.com€¦ · Sampling Instructions- Cyanide Analysis 9 Sampling Instructions – Containers with Sulfuric Acid (H 2 SO 4) Sampling Instructions-

Sampling Instructions

CA-ELAP Certification 1664

NELAP/ORELAP Certification 4036

1885 North Kelly Rd • Napa, CA 94558

(707) 258-4000 - [email protected]

www.CaltestLabs.com

Caltest Analytical Laboratory—Sampling Guide 2020 (REV 5/29/20)

Page | 1

TABLE OF CONTENTS

Introduction

2

Caltest Reference Chart: Holding Time, Bottle Type, Preservation How to Fill out a Caltest chain of Custody Form (COC)

4

6

Caltest Shipping Instructions

7

Sampling Instructions- Bacteriological Analyses 8

Sampling Instructions- Cyanide Analysis

9

Sampling Instructions – Containers with Sulfuric Acid (H2SO4) Sampling Instructions- Containers with Nitric Acid (HNO3)

(200.8 metals and Hardness)

11

12

Sampling Instructions- General Industrial Stormwater Parameters

13

Sampling Instructions - Volatile Organic Compounds (EPA 624.1,524.2 and 8260)

14

Sampling instructions – Trace Mercury, Methyl Mercury and Metals (EPA 1630, 1631 and 1638)

16

Sampling Instructions – Lead and Copper Rule Caltest Overview

18

19

Additional Caltest Forms: Caltest Chain of Custody (COC) – General Caltest Chain of Custody (COC) -P/A Caltest Chain of Custody (COC) – Multiple P/A

20 21 23


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CALTEST SAMPLING GUIDE OVERVIEW

We’ve put this sampling guide together to provide guidance on the proper, method and/or permit-specified sampling protocol. Proper sampling is critically important for a variety of reasons including those noted below. This guide includes the details you’ll need to collect a variety of types of samples and analyses. If you have any questions, or if there is a method that isn’t noted in this guide, please feel free to contact our client services team to get more information. Call 707/258-4000 or email [email protected]. If you need sampling containers, request a bottle order using the online request form. If you need samples picked up, request a pickup using the online form. Proper sampling techniques, why are they important?

• Minimize/eliminate non-compliance data o Meet method requirements o Comply with permit requirements

• Reduce interferences

• Maintain integrity of the sample

Developing a sampling plan to ensure proper sample collection

✓ What analysis and method do you need?

✓ What is your matrix (e.g., stormwater, wastewater, drinking water etc.)? Who is your regulator? ✓ What containers, sample volume, preservation and holding times are noted for the method?

✓ What else? Need gloves? Need pretreatment (Chlorine or Nitrates?) ✓ Check the Bottle Preservation and Holding Time Chart included in this guide. ✓ What type of sample are you collecting?

o Grab or comp o Raw water vs distribution

✓ Do I need any specific QC – e.g., MS/D?

✓ Field blanks and trip blanks—some permits and/or methods may require field or trip blanks, some may suggest them.

✓ Location and timing ✓ Representative sample ✓ Coordinate with your Caltest Project manager to order supplies arrange for pickups and alert lab of any

analyses with short holding times ✓ Request project-specific COC and review the “How to Complete a COC” document to follow.

Reminder-- when in doubt, check your permit or check with your regulator! After sampling Deliver or ship samples to the laboratory to ensure that holding times are met. Holding time starts at sample collection and ends at preparation and/or analysis. Be sure to allow time for the laboratory to process the samples. See Shipping instructions for more specifics on shipping samples to Caltest.

mailto:[email protected]

https://caltestlabs.com/request-a-bottle-order/

https://caltestlabs.com/request-a-pickup/


Page | 3

For more information

• Visit the Caltest website to review methods and get access to a wide array or resources.

• For information specific to 40 CFR Part 136.3: https://www.epa.gov/cwa-methods/approved-cwa-chemical-test-methods

• Drinking Water Analytical Methods—EPA https://www.epa.gov/dwanalyticalmethods

https://caltestlabs.com/

https://www.epa.gov/cwa-methods/approved-cwa-chemical-test-methods

https://www.epa.gov/cwa-methods/approved-cwa-chemical-test-methods

https://www.epa.gov/dwanalyticalmethods


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REFERENCE CHART: HOLDING TIME, BOTTLE TYPE, PRESERVATION and MINIMUM VOLUME

Note: Multiple analyses may be run from the same container, provided that the bottle type, volume and preservation are appropriate.

Analytical Parameter Maximum Holding Time

Required

Container Type Required

Preservative Minimum Amount

Alkalinity (Bicarb, Carb, Hyd, and Tot); SM 2320 B 14 days Plastic / Glass 0-6°C 100 mL

Ammonia (NH3 as N); SM 4500NH3 B/C or B/G 28 days Plastic / Glass H2SO4 pH <2 +0-6°C 200 mL

Anions by EPA 300.0: Chloride (Cl-); Fluoride (F-); Nitrate (as N); Sulfate (SO4

2-) 28 days 48 hours (Nitrate)

Plastic / Glass 0-6° C 100 mL

Asbestos (TEM) 48 hours Plastic / Glass 0-6°C 1000 mL

Bioassay (Acute Tox) % survival 36 hours Plastic cubitainer 0-6°C 1-5 gal

Biochemical Oxygen Demand (BOD); SM 5210 B 48 hours Plastic / Glass 0-6°C 250 mL

Chromium, Hexavalent (CrVI); SM 3500Cr B 24 hours Plastic / Glass 0-6°C 200 mL

Chlorine, residual; SM 4500Cl B or G 15 minutes Field Measurement - - -

Chemical Oxygen Demand (COD); SM 5220 D or EPA 410.4

28 days Plastic / Glass H2SO4 pH <2 +0-6°C 50 mL

Chlorophyll A (Algal Biomass) / Pheophytin; SM 10200 H

48 Hours to filter 28 days once filtered

Amber Plastic 0-6°C, unfiltered -20°C, filtered

1 L

Coliform, Total / Fecal; SM 9221 B/E 8 hrs – wastewater/stormwater 24 hrs – drinking water

Plastic (sterile) Na2S2O3 + 0-10°C 100 mL

Coliform, Total / E.Coli; SM 9223 B (Present/Absent or Quantitray)

24 hours Plastic (sterile) Na2S2O3 + 0-10°C 100 mL

Color; SM 2120 B 48 hours Plastic / Glass 0-6°C 100 mL

Conductivity (EC/SC); SM 2510 B 28 days Plastic / Glass 0-6°C 100 mL

Cyanide Total; SM 4500CN B/C/E or B/C/I

14 days

Amber or opaque plastic with NaOH pH >10+0-6°C Pre-treatment for Total Cyanide samples with chlorine or NO3/NO2 should be done prior to preservation. Kits can be provided upon request.

100 mL

Cyanide WAD; SM 4500CN B/C/E or B/C/I 14 days Amber plastic NAOH pH >10+0-6°C

Dissolved Organic Carbon (DOC); SM 5310 B Filter within 48 hours 28 days

250 mL Amber glass Filter then add HCl to pH< 2 + 0-6°C

50 mL

Dissolved Oxygen (DO); SM 4500O G 15 minutes Field Measurement or

Glass bottle/no headspace Collect in duplicate

0-6°C 500 mL

Enterococcus by Enterolert 8 hours Plastic (sterile) Na2S2O3 + 0-10°C 100 mL

Heterotrophic Plate Count (HPC/SPC); SIMPLATE 8 hours Plastic (sterile) Na2S2O3 + 0-10°C 100 mL

Hardness (by titration); SM 2340 C 180 days Plastic / Glass HNO3 pH <2 250 mL

Metals, Dissolved {2}; EPA 200.8 Filter within 15 minutes{2}, 6 months

Plastic / Glass Filter then add HNO3 100 mL

Metals, Total; EPA 200.8 Metals, Total; EPA 6010/6020

6 months

Plastic / Glass Solids in Glass SJ

HNO3 pH <2 0-6°C

100 1

mL 8oz

Mercury (Hg) EPA 245.1 Mercury (Hg) EPA 7471

28 days Plastic / Glass Solids in Glass SJ

HNO3 pH <2 0-6°C

100 1

mL 8oz

Mercury, Total; EPA 1631 (Aqueous) Mercury, Total; EPA 1631 (Sludge or Solids)

48 hours to preserve 90 days once preserved 90 days frozen

Glass, Dbl Bagged (not appropriate for samples with solids TSS>200 mg/L) Solids in Glass SJ

HCl 0-6°C

100

1

mL 8oz

Mercury, Dissolved {2}; EPA 1631 Filter within 24 hours, Preserve within 48 hours 90 days once preserved

Glass, Dbl Bagged

Filter in lab, then HCl 100 mL

Mercury, Methyl; EPA 1630 (Aqueous) Mercury, Methyl; EPA 1630 (Sludge or Solids)

Preserve {8} within 48 hrs 6 months preserved 6 months frozen

Glass, Amber Dbl Bagged Solids in Amber Poly SJ

Dark and cool + (HCl or H2SO4 {8}) Solids to be Frozen

100

1

mL 8oz

Mercury, Dissolved {2} Methyl; EPA 1630 Filter & preserve within 48 hrs 6 months once preserved

Glass, Amber Dbl Bagged

Filter in Lab, 0-6°C + HCl if < 10 ppT salinity {8}

100 mL

Nitrate (as N); EPA 300.0 48 hours Plastic / Glass 0-6°C 100 mL

Nitrite (as N); SM 4500NO2 B 48 hours Plastic / Glass 0-6°C 100 mL

Nitrate+Nitrite as N (NO3+NO2-N) EPA 353.2, or SM NO3 F


Nitrogen, Total Kjeldahl (TKN); SM 4500Norg + SM 4500NH3 B


Nitrogen, Total Organic (TON) TKN-NH3= TON calc 28 days Plastic / Glass H2SO4 pH <2 +0-6°C 200 mL

Odor; SM 2150 B 6 hours (recommended) / 24 hour regulatory

Glass only 0-6°C 250 mL

Oil & Grease, Total and/or Hydrocarbons EPA 1664 28 days Amber Glass only-in duplicate HCl pH <2 + 0-6°C 1 L {10}

Chlorinated Pesticides & PCBs EPA 625.1 (formerly EPA 608) /8081/8082

7 days, Aqueous 14 days, Sludge or Solid

Glass Amber Liter {6} Solids in Glass SJ

0-6°C {5} 0-6°C

1 1

L 8oz


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Analytical Parameter Maximum Holding Time

Required

Container Type Required

Preservative Minimum Amount

Polynuclear Aromatic Hydrocarbons (PAH’s) EPA 625.1/8270



0-6°C {5} 0-6°C

1 1

L 8oz

Organophosphorus Pesticides EPA 625.1 (formerly EPA 614) /8141


Glass Amber Liter. Collect In triplicate Solids in Glass SJ

0-6°C {5} 0-6°C

1 1

L 8oz

Semi-volatile Organics EPA 625.1/8270



0-6°C {5} 0-6°C

1 1

L 8oz

Pyrethroid Pesticides GCMS-NCI-SIM/ EPA 8270M/625.1M

7 days /3 days {9} 14 days, soil or sediment

Glass Amber Liter. Collect In triplicate Solids-Amber Glass SJ

0-6°C {5} Solids to be Frozen

1

1

L 8oz

Carbamate Pesticides EPA 632/8321


Glass Amber Liter. Collect In triplicate Solids in Glass SJ

0-6°C 1 L

Volatile Organics EPA 524.2 {4}

14 days, preserved Glass VOA vial {1} (sample in triplicate)

HCl pH <2 + 0-6°C {4}

40 mL

Volatile Organics EPA 624.1 {3}

(Includes Acrolein and Acrylonitrile)

14 days except: 3 days unpreserved for Acrolein {12} 7 days unpreserved for BTEX only {11}

Total of four 40 mL VOA Vials; Two Pres w/ HCl Two Unpreserved {1} THMS only—3 HCl VOAs

0-6°C (see holding time for additional preservation)

One 40mL of each

container type described

Volatile Organics; EPA 8260 {3}

14 days (aqueous) 14 days Sludge/solid

Glass VOA vial {1} (in triplicate) Solids in separate glass jar filled to top

HCl pH <2 + 0-6°C

0-6°C

40

1

mL

8oz

TPH Diesel/Motor Oil; EPA 8015 7 days Glass Amber Liter {6} 0-6°C 1 L

Tributyltin (TBT) 7 days (recommended) Glass Amber Liter {6} 0-6°C 1 L

TPH Gas/ BTEX/ MTBE; EPA 8260 14 days preserved Glass VOA vial {1} HCl pH <2 + 0-6°C 40 mL

Dioxin; EPA 1613 1 year Glass Amber Liter {6} 0-6°C {5} 1 L

Perchlorate; EPA 314.0 28 days Plastic/Glass 0-6°C 100 mL

pH; SM 4500 H+ B 15 minutes Plastic / Glass 0-6°C 100 mL

Phenols, EPA 420.1 28 days Glass Amber 250 mL H2SO4 pH <2 +0-6°C 200 mL

Phosphate, Ortho (as P); SM 4500P E 48 hours Plastic / Glass 0-6°C 100 mL

Phosphate, Ortho, Dissolved (as P); SM 4500P E 15 minutes to filter / 48 hrs once filtered

Plastic / Glass 0-6°C 100 mL

Phosphorus, Total (PO4 as P); SM 4500P B/F or B/E 28 days Plastic / Glass H2SO4 pH <2+0-6°C 100 mL

Solids, Settleable (SS); SM 2540 F 48 hours Plastic / Glass 0-6°C 1000 mL

Solids, Total (mg/L or %); SM 2540 B, or SM 2540 G 7 days Plastic / Glass 0-6°C 100 mL

Solids, Total Dissolved (TDS); SM 2540 C 7 days Plastic / Glass 0-6°C 100 mL

Solids, Total Suspended (TSS); SM 2540 D 7 days Plastic / Glass 0-6°C 200 mL

Solids, Volatile Suspended (VSS); SM 2540 E 7 days Plastic / Glass 0-6°C 200 mL

Sulfate (SO42-), EPA 300.0 28 days Plastic / Glass 0-6°C 100 mL

Sulfide, Dissolved; SM 4500 S2- B/D 7 days Glass 250 mL AlCl3 + NaOH +0-6°C 250 mL

Sulfide, Total; SM 4500 S2- C/D 7 days Glass (preferred)/plastic (no headspace)

NaOH + ZnAC pH >9 + 0-6°C

250 mL

Sulfite (SO3) 7 days Glass Amber 500 mL EDTA + 0-6°C 250 mL

Surfactants (MBAS); SM 5540 C 48 hours Plastic / Glass 0-6°C 250 mL

Suspended Sediment Conc. (SSC); ASTM D3977 7 days Plastic / Glass 0-6°C {7} 100 mL

Total Organic Carbon (TOC); SM 5310 B 28 days Amber Glass VOA (3 vials) HCl pH <2 + 0-6°C 40 mL

Turbidity; SM 2130 B, or EPA 180.1 48 hours Plastic / Glass 0-6°C 100 mL

Ultraviolet Absorption (UVA at 254nm); SM 5910 B 48 hours Glass Amber 125mL 0-6°C 125 mL

{1} Volatile organic samples need to be filled in multiple VOA vials without air bubbles/headspace. {2} Dissolved metals require field or lab filtration through 0.45-micron filter prior to preservation. 40 CFR 136.3 requires filtration within 15 minutes. {3} Volatile organic methods EPA 624.1 and 8260 require dechlorination using Sodium Thiosulfate (Na2S2O3) at time of sampling if chlorine is present. (Thiosulfate dechlorination bottles are available at the laboratory upon request.) Dechlorination is to occur before transferring to the appropriate VOA. {4} Volatile organic method EPA 524.2 requires de-chlorination using ascorbic acid at time of sampling if chlorine is present. Ascorbic acid dechlorination kits are available at the laboratory upon request. If analyzing for THMs only, Sodium Thiosulfate (Na2S2O3) may be used, and acidification can be omitted. Otherwise, dechlorinate with Ascorbic acid, then preserve with HCl. If the sample foams vigorously upon addition of HCl, discard and collect unpreserved dechlorinated sample, and notify the laboratory as the samples must be analyzed within 24 hours of collection if they are to be analyzed for any compounds other than THMs. Method 524.2 requires a travel/trip blank with each sample set collected. {5} If sampling from a chlorinated location, add 80 mg/L Sodium Thiosulfate (Na2S2O3) per liter and mix well. Any method suitable for field use may be employed to test for residual chlorine (Reference 16). Add more sodium sulfate if 80 mg/L is insufficient but do not add excess sodium thiosulfate. {6} Semi Volatile Organics Amber Liters (AL) should be collected in duplicate, to ensure volume for re-extraction if necessary. When possible, please collect 4 AL per method to allow the laboratory to perform matrix Quality Control (MS/MSD). {7} Suspended Sediment Conc.(SSC) requires its own container and the entire contents are used for the analysis. {8} Preserve with HCl if less than 10 ppT Salinity, or Preserve with H2SO4 if greater than 10 ppT Salinity. {9} Cyhalothrin in water has a 3-day hold time in reagent water per USGS study. Permethrin in water has a 3-day hold time per Storage Stability Study by CA Dept. of Food and Agriculture. {10} 1000 mL required for RL of 5 mg/L; 250 mL bottle recommended for samples with expected concentrations of 20 mg/L or higher. {11} If unpreserved, must be analyzed within 7 days of sampling {12} Hold time can be extended to 14 days if preserved to pH 4-5 at time of collection. REV 06/11//20


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HOW TO FILL OUT A CALTEST CHAIN OF CUSTODY (COC) FORM

The Caltest Chain of Custody form (COC) acts as a chain of custody of the sample(s), legally documenting

possession or custody from the time of sample collection to the time of sample drop off at the lab. It also acts as

an official order form to the lab, indicating what analyses should be performed on what samples, date/time of

sample collection, and reporting/invoicing instructions. Below are descriptions of the required parameters on the

form.

Client: The name of the company to which the report and/or invoice will be made out. For homeowners, the

name of the person the account will be under.

Report Attn: The name of the person the report will be addressed to. For homeowners, may be same as client

name.

Project Name: Will be the title of the report/project (no wrong answer). Examples include, “Water Testing” or

“Annual Compliance.” We recommend titling the report something that someone else can look at 5+ years from

now and understand what the project was about.

Mailing Address: The mailing address for the report. The address of the sample is not needed.

Billing Address: The mailing address for the invoice. Can simply write “same” if same as mailing address.

Phone Number: Best number to reach someone if there’s a need to call for any reason.

Email Address: Email address of primary contact person.

Regulatory Drinking Water? If the sample is a drinking water regulatory sample that needs to be reported to the

state, select the “Y” box and add the 10-digit PS Code(s); otherwise select the “N” box.

Date/Time Sampled: When the sample was collected.

Sample ID: The name of the sample. Again, no wrong answer. Examples include “Kitchen Sink” or “Pre-Filtered.”

We suggest naming the sample something that someone else can look back on years from now and understand

where the sample was collected.

Analyses Requested: This is where to request the analyses needed for each sample. The COC is designed with

rows and columns so that multiple analyses can be requested on the same sample, or the same analysis can be

requested on multiple samples.

Comments: This is a great place to request an email distribution list (“Please email to: __”) should you want the

report to be sent to multiple recipients. Listing contacts here will also give us authorization to speak with those

individuals about this project.

Relinquished By: Please sign and date/time whenever the sample changes custody to show who possesses the

sample at all times. When the sample is turned in to the lab, the last signature will be the sample receiving

employee at Caltest.

Reporting Options: By default we email reports and invoices to the client. Hard copies are only available upon

request.

Please contact Caltest Client Services with any questions: 707/258-4000 or [email protected]



Page | 7

CALTEST SHIPPING INSTRUCTIONS

1. Please ship samples overnight to arrive to the lab Monday- Friday, as soon as possible after sample

collection.

2. Place containers in plastic bags (secondary containment for preserved samples).

3. Fill cooler with ice and put sample upright in the middle of the ice. Note: for Metals (EPA 200.8) ice and

overnight shipping is not required

4. Ensure that the cooler is completely full so that the sample won’t move around during shipping.

5. Put completed Chain of Custody (COC) form in a Ziplock bag and place on top of ice, inside cooler.

6. Ship overnight to:

Caltest Environmental Laboratory

Sample Receiving

1885 North Kelly Road

Napa, Ca 94558

Note on outside of cooler: “Sample Enclosed, Open Upon Receipt”


Page | 8

CALTEST SAMPLING INSTRUCTIONS- BACTERIOLOGICAL

Analyses and holding times

Analysis Method Holding time

Coliform (Total/E.Coli) SM 9223 B 8 hours Wastewater/stormwater; 24 hours drinking water

Coliform (Total/Fecal) SM 9221 B/E 8 hours Wastewater/stormwater; 24 hours drinking water

Enterococcus Enterolert 8 hours

Heterotrophic Plate Count (HPC/SPC) SM 9215C 8 hours

Container: 125 or 250 mL plastic sterile container with Sodium Thiosulfate (NA2S2O3)

Coliform is an indicator bacteria which is not found naturally below

the ground or in ground water, but it is abundant above ground

and found on the surface of nearly everything. This is why the

steps below should be followed in order to avoid any potential

contamination.

The bottle received from Caltest is sterile and has a clear plastic

seal around the lid. Request a new container if the seal is

broken or missing. Each bottle contains a dechlorination

reagent that looks like a white powder – DO NOT RINSE.

Do not open bottle prior to step 7 (below).

Sampling Drinking Water Sources: Pick a cold water tap that is commonly used. Do not use a swivel faucet.

1. Remove any tap attachments (filters, aerators, etc.).

2. Let the water run for 5 to 10 minutes.

3. Turn water off, and clean opening of faucet with rubbing alcohol, inside and outside.

4. Turn water on, but limit flow of water to a ‘pencil-size’ stream. If possible, avoid any spraying or splashing.

5. Label the bottle (with a waterproof marker): Name, sample location, and sample date/time.

6. Hold the sample container near the bottom.

7. Remove and discard seal around lid. Remove lid without touching the neck of the bottle or inside of lid. Note

that the bottle has a 100 mL line and a 120 mL fill line.

8. Carefully insert opening of bottle into the ‘pencil-size’ stream. Avoid splashing or over-filling. Fill the bottle

between the two lines. Try not to fill beyond the 120 mL line. The analysis cannot be performed without a

minimum of 100 mL.

10. Recap container and tighten. Please store/transport on ice or in a refrigerator (<10°C) and return to lab within

12 hours of sample collection (drinking water); stormwater or wastewater return to lab within 6 hours of

sampling.

11. Fill in Chain of Custody (COC) form and sample bottle label with dates, times, and locations of sampling.


Page | 9

CALTEST SAMPLING INSTRUCTIONS-CYANIDE

Analyses and holding times- Cyanide

Analysis Method Container/Preservation Holding time

Cyanide, standard (RL= 3 ug/L) SM 4500 – CN C/E Amber Plastic with Sodium Hydroxide (NaOH) pH >10+0-6°C

14 days

Cyanide, low-level (RL= 1 ug/L) SM 4500 – CN C/E 14 days

Cyanide, WAD SM 4500 – CN I/E 14 days

Note: Pretreatment for Total Cyanide samples with chlorine or NO3/NO2 should be done prior to preservation—request

needed kit and see notes below.

Sampling instructions (for Sources with Nitrate/Nitrite)

Treat for nitrate/nitrite per the instructions below at the time of sample collection (i.e. within 15 minutes of

sample collection).

1. Nitrate/nitrite treatment: Fill clear pint bottle labeled for sulfamic acid with source water—do not

overfill. Allow sulfamic acid to dissolve.

2. Pour water from the bottle labeled for nitrate/nitrite into the amber pint bottle with 3x NaOH, the final

sample container.

o For samples that are treated with sulfamic acid, 3x the standard amount of NaOH is needed.

3. Keep sample cool (0–6°C / 32–43°F).

Sampling instructions (for Sources with Chlorine)

Treat for chlorine per the instructions below at the time of sample collection (i.e. within 15 minutes of sample

collection).

1. De-chlorination: Collect sample into the clear pint bottle labeled for sodium thiosulfate. Allow sodium

thiosulfate to dissolve.

–continued on next page

Special handling instructions for containers with preservatives

1. Use gloves and safety glasses whenever handling bottles.

2. Inspect containers to confirm that they are intact, with lids

secured.

3. With lid secured, inspect that there is solid preservative in the

containers.

Sampling instructions- General

1. When sampling, use gloves and safety glasses. Open the lid

carefully and away from face. Use care not to spill and

avoid inhaling. Fill to allow a little headspace at the top of

the bottle.

2. Fill in Chain of Custody (COC) form and sample bottle label

with dates, times, and locations of sampling.


Page | 10

2. Pour water from the bottle labeled for sodium thiosulfate into the amber pint bottle with NaOH, the final

sample container.


Sampling instructions (for Sources with Nitrate/Nitrite and

Chlorine)

Treat for nitrate/nitrite and chlorine per the instructions below

at the time of sample collection (i.e. within 15 minutes of

sample collection).

1. Nitrate/nitrite treatment: Fill clear pint bottle labeled

for sulfamic acid with source water, do not overfill.

Allow sulfamic acid to dissolve.

2. De-chlorination: Pour water from the bottle with

sulfamic acid into the clear pint bottle labeled for

sodium thiosulfate. Allow sodium thiosulfate to

dissolve.

3. Pour water from the bottle labeled for sodium

thiosulfate into the amber pint bottle with 3x NaOH,

the final sample container. For samples that are treated with sulfamic acid, 3x the standard amount of

NaOH is needed.



Page | 11

CALTEST SAMPLING INSTRUCTIONS- CONTAINERS with SULFURIC ACID (H2SO4)

Analyses and holding times-- frequently requested parameters collected in H2SO4 containers


Ammonia (NH3 as N) SM 4500-NH3 B,C 28 days

Chemical Oxygen Demand (COD) EPA 410.4 / SM 5220 D 28 days

Nitrate+Nitrite (as N) EPA 353.2 / SM 4500-NO3 F 28 days

Phosphorus, Total (PO4 as P) SM 4500-P B/F 28 days

Total Kjeldahl Nitrogen (TKN) SM 4500-Norg C/NH3 B,C 28 days

Special handling instructions for containers with Sulfuric Acid

(H2SO4):


2. Inspect containers upon receipt to confirm that they are

intact, with lids secured.

3. With lid secured, inspect that there is liquid preservative in

the bottle. You should see an approximately nickel to quarter

size drop in the bottom.

4. When sampling, use gloves and safety glasses. Open the lid

carefully and away from face. Use care not to spill and avoid

inhaling. Try not to overfill as that will deplete the

preservative. Fill to allow a little headspace at the top of the

bottle.

5. Fill in Chain of Custody (COC) form and sample bottle label

with dates, times, and locations of sampling.

6. Keep the samples refrigerated or on ice between 0 - 6°C/32-

43°F.


Page | 12

CALTEST SAMPLING INSTRUCTIONS- CONTAINERS with NITRIC ACID (HNO3)

Metals and Hardness Analyses

Analyses and holding times- Commonly requested analyses with Nitric acid-preserved containers


Metals EPA 200.8 6 months

Mercury EPA 245.1 28 days

Hardness (by titration) SM 2340 C 180 days

Special handling instructions for containers with HNO3:

1. Use gloves and safety glasses whenever handling

bottles.

2. Inspect containers upon receipt to confirm that they

are intact, with lids secured.

3. With lid secured, inspect that there is liquid

preservative in the bottle. You should see an

approximately nickel to quarter size drop in the

bottom.

4. When sampling, use gloves and safety glasses. Open

the lid carefully and away from face. Use care not to

spill and avoid inhaling. Try not to overfill as that will

deplete the preservative. Fill to allow a little

headspace at the top of the bottle.

5. Fill in Chain of Custody (COC) form and sample bottle

label with dates, times, and locations of sampling.


Page | 13

CALTEST SAMPLING INSTRUCTIONS- GENERAL INDUSTRIAL STORMWATER PARAMETERS

Analyses and holding times for General Stormwater permit analyses. Refer to your permit to confirm your required parameters.

Analysis Container Type Holding time

Oil & Grease (EPA 1664 A) (1) HCl-preserved Amber Glass Liter 28 days

Total Suspended Solids (TSS) SM 2540 D (1) Unpreserved Poly Pint 7 days

pH—to be collected/recorded in the field Use pH meter or pH strips 15 minutes

Special handling instructions for containers with Hydrochloric Acid (HCl):


2. Inspect containers upon receipt to confirm that they are intact, with lids secured.

3. With lid secured, inspect that there is liquid preservative in the bottle. You should see an approximately

nickel to quarter size drop in the HCl- preserved container.

4. When sampling, use gloves and safety glasses. Open the lid carefully and away from face. Use care not to

spill and avoid inhaling. Try not to overfill as that will deplete the preservative. Fill to allow a little

headspace at the top of the bottle.

5. Fill in Chain of Custody (COC) form and sample bottle label with dates, times, and locations of sampling.

6. Keep the samples refrigerated or on ice between 0 - 6°C/32-43°F.


Page | 14

CALTEST SAMPLING INSTRUCTIONS- Volatile Organics (VOCs)

EPA 8260, EPA624.1 and EPA 524.2

Analyses and holding times for Volatile Organic Compounds (VOCs).

Analysis Required Container Type Holding time

EPA 8260 (3) HCl-Preserved VOAS 14 days

EPA 624.1 (with Acrolein & Acrylonitrile) (4) VOAs [(2) HCl-Preserved, (2) unpreserved]

3 days unpreserved for Acrolein only1

14 days preserved. See 40 CFR 136.3 for more details.

EPA 524.2 (drinking water)- full list EPA 524.2 (drinking water) – THMs only

(3) HCl-Preserved VOAS (3) VOAs w/Na2S2O3

14 days 14 days

Note 1: Hold time can be extended to 14 days if preserved to pH 4-5 at time of collection. Request 6-pack (Total of Six 40 mL VOA Vials; Two Pres w/ HCl, Two Unpreserved, Two Client preserved to pH 4-5). General Note: Chlorinated sources require field dechlorination prior to preservation—request dechlorination kit and see notes below.

Special handling instructions for containers with Hydrochloric Acid (HCl)


2. Inspect containers upon receipt to confirm that they are in a Ziplock bag, intact, with lids secured and that

there is liquid preservative in the vials as noted above.

3. For Chlorinated sources only: please note, you will also be receiving a 250 mL amber bottle for

dechlorination in addition to the VOAs. Inspect that there is a white dechlorination powder in the amber

bottle. Note special dechlorination instructions below.

4. When sampling, use gloves and safety glasses. Open the lid carefully and away from face. Use care not to

spill and avoid inhaling.

-continued on next page


Page | 15

Sampling instructions

Since the analysis is for gases, it is important that samples be as free of air as possible.

Chlorinated sources only:

1. Fill 250 mL amber bottle with source water; do not overfill and do not shake. Allow dechlorination

powder to dissolve (approximately 1-2 minutes).

2. Using the 250 mL amber bottle, fill VOAs slowly to avoid aerating; fill to the top without overflowing.

3. Carefully set the container on a level surface.

All sources:

1. Fill sample bottles slowly to avoid aerating; fill to the top without overflowing.

2. Carefully set the container on a level surface.

3. Fill the septum (cap) with sample, place on the crown of water formed and tighten lid.

4. Turn container upside down and tap to check for air bubbles. If there is air, remove cap carefully, and add

more water. DO NOT DUMP AND START OVER.

5. Repeat with rest of VOAs.

6. Place containers back into Ziploc bag and keep cool (0–6°C / 32–43°F).

7. Please fill in Chain of Custody form and sample bottle label with dates, times, and locations of sampling.

Please note on Chain of Custody whether there were bubbles left in the container after sampling.

8. Return samples to laboratory within 24 hours.


Page | 16

CALTEST SAMPLING INSTRUCTIONS- For Trace Mercury, Methyl Mercury and Metals by

EPA 1630, 1631 and 1638

Analyses and holding times

Analysis Container type Holding time

Mercury, Total (Hg) EPA 1631 500 mL glass preserved with hydrochloric acid (HCl), double-bagged

90 days

Mercury Methyl, Total (Hg) EPA 1630 500 mL amber glass preserved with hydrochloric acid (HCl), double-bagged

6 months (cold storage required)

Mercury, Dissolved (Hg) EPA 1631 500 mL glass, Unpreserved, double-bagged

Filter within 24 hours, preserve within 48 hours. 90 days once preserved.

Mercury, Methyl, Dissolved (Hg) EPA 1630 500 mL amber glass, Unpreserved, double-bagged

Filter and preserve within 48 hours. 6 months once preserved. (cold storage required)

Field Blank for 1630 and 1631 —see sampling instructions below

(1) HCl-preserved glass container (amber if 1630), double-bagged plus (1) unpreserved glass container with mercury- free blank water.

Travel Blank for EPA 1630 and 1631 —see sampling instructions below

(1) HCl-preserved glass container (amber if 1630) filled with mercury-free water double-bagged.

Metals by EPA 1638 500 mL Poly with nitric acid (HNO3), double bagged

6 months (cold storage required)

Field Blank for 1638—see sampling instructions below

(1) HNO3-preserved poly container, double-bagged plus (1) unpreserved, container with metals- free blank water.

Special handling instructions for containers with Hydrochloric

Acid (HCl) or Nitric Acid (HNO3):

1. Without opening bags, inspect containers to confirm that

they are intact, with lids secured and that there is liquid

preservative in the bottle. You should see an

approximately nickel to quarter size drop in the bottom of

the HCl-preserved containers and in the HNO3 container.

2. When sampling, use mercury-free gloves and safety

glasses. Open the lid carefully and away from face. Use

care not to spill and avoid inhaling fumes. Try not to

overfill as that will deplete the preservative. Fill to allow a

little headspace at the top of the bottle using the “Clean

Hands-Dirty Hands” technique noted below.

-continued next page


Page | 17

Sampling technique utilizing “Clean Hands-Dirty Hands” sampling protocol:

(Excerpt from EPA Method 1669 - see page 17 here)

To avoid sample contamination, we recommend using the set of gloves provided by the laboratory.

If only one person is sampling, two pairs of gloves should be worn. The outer pair of gloves (“dirty hands”) are

used to open the cooler, operate sampling equipment, etc, and then to open the outer bag on the glass container.

The inner gloves (“clean hands”) are used to open the inner bag, open the lid, fill the sample bottle, replace lid,

and reseal both bags.

If there are two samplers, one person is designated “clean hands” and the other person is designated “dirty

hands.”

Field Blank Preparation (Clean Hands/Dirty Hands Method):

1. While at the site, before collecting samples, the “dirty hands” opens both the outer bags of the empty

bottle and the mercury-free water

bottle.

2. The “clean hands” opens the inner bags and lids and pours the mercury-free water into the empty HCl-

preserved bottle labeled "Field Blank." Replace lids on bottles and reseal both bags around field blank.

Discard or return emptied blank water bottle to lab.

Keep samples refrigerated or on ice between 0 - 6°C/32-43°F (not required for EPA 1631 analysis).

Travel Blank:

Please keep the Travel Blank with the other sample containers. Do not open bags or bottle.

https://www.epa.gov/sites/production/files/2015-10/documents/method_1669_1996.pdf


Page | 18

CALTEST SAMPLING INSTRUCTIONS- LEAD & COPPER RULE

Container needed: (1) Unpreserved plastic liter

1. A minimum 6-hour period during which there is no water use throughout the house must be achieved

prior to sampling. It is recommended that either early mornings or evenings upon returning home are the

best sampling times to ensure the necessary stagnant water conditions exist.

2. Use a kitchen or bathroom cold-water faucet to collect the sample. Place the clean plastic one-liter

sample bottle provided by the laboratory below the faucet and gently open the cold-water tap. Fill the

sample bottle and turn off the water. No preservative is needed at the time of collection.

3. Label the sample with sample identification/location, date and time of collection.

4. Complete the Chain-of-Custody (COC) form including mailing/email address, name of sample collector,

description of sample point, date and time of collection, and test ordered (i.e. "Lead & Copper").

Shipping instructions

7. Please ship samples to arrive to the lab Monday–Friday, as soon as possible after sample collection.

8. Place containers in plastic bags.

9. Place sample upright in the middle of a cooler; ice is not required.

10. Ensure that the cooler is completely full with packing material so that the sample won’t move around

during shipping.

11. Put completed Chain of Custody (COC) form in a Ziplock bag and place on top, inside cooler.

12. Ship to:

Caltest Environmental Laboratory Sample Receiving 1885 North Kelly Road Napa, Ca 94558 Note on outside of cooler: “Sample Enclosed, Open Upon Receipt”

Please contact Caltest Client Services with any questions: 707/258-4000 or [email protected]


About Caltest

Caltest has been delivering high-quality, customer-focused and responsive service to clients throughout California since

1982. Our model is to provide the trust, transparency, integrity and personal touch that you would expect from your

own in-house lab.

As a Caltest client, it is our goal to make the process easier for you by providing:

• A dedicated project manager who understands the requirements of your project and a team that can respond

quickly to your questions and requests.

• Project-specific quotes, sampling kits, LIMS set-up, reporting and electronic deliverables.

• Client and regulatory-specific exceedance alert set up upon request to provide immediate notification in the

event of exceedances.

• A field services team available for container delivery and sample pickup throughout the Bay Area and in the

Sacramento & Central Valley communities.

• Reports designed with you in mind; find the data you need quickly knowing it is backed by our commitment to

transparency, thorough documentation and full access to our lab team.

• Data Level II reports as our default; Level III and IV data packages available upon request.

Online Resources:

Please visit our website for pickup requests, bottle order requests, Caltest forms and resources

➢ For sample container requests, click here to go to our online bottle order request form-- please provide 2-3 day

notice for local delivery; 1 week for shipments outside our delivery area.

➢ For pickup requests, click here to go to our online pickup request form-- please provide 2-3 day notice for local

delivery; 1 week for shipments outside our delivery area.

➢ Download our holding time & preservation reference chart

➢ Online payments: click here to pay easily and securely online by credit card.

Questions? Call your project manager, (707)258-4000 or reach out to the client services team at: [email protected]

https://caltestlabs.com/

https://caltestlabs.com/request-a-bottle-order/

https://caltestlabs.com/request-a-pickup/

http://3cp1hp1be6xw3gh24m2wvbul-wpengine.netdna-ssl.com/wp-content/uploads/2019/06/Caltest_Bottle_Preservative_Holding_Time_Reference_Chart_rev12132018.pdf

https://caltestlabs.com/pay-an-invoice/

PAGE OF

CALTEST SAMPLE #

CLIENT LAB #

COMP. or GRAB

Samples: WC MICRO BIO MET SV VOA

SIL: HP PT QT VOA

W/HNO3 H2SO4 NaOH

PIL: HNO3

1885 N. KELLY ROAD NAPA, CA 94558 (707) 258-4000 [email protected] www.CaltestLabs.comSAMPLE CHAIN OF CUSTODY

PROJECT NAME / PROJECT NUMBER: P.O. NUMBER LAB ORDER #

CLIENT: REPORT ATTN:ANALYSES REQUESTED

MAILING ADDRESS: STATE: ZIP

EMAIL ADDRESS:

RUSH

DUE DATE:

TURN-AROUND TIMEBILLING ADDRESS: ATTN:

STANDARD

SAMPLER (PRINT & SIGN NAME):PHONE NUMBER:

DATE SAMPLED TIME SAMPLED SAMPLE

MATRIX*CONTAINER

TYPE/ AMOUNT** PRESERVATIVE SAMPLE IDENTIFICATION / SITE

RELINQUISHED BY DATE/TIME RECEIVED BY RELINQUISHED BY DATE/TIME RECEIVED BY

*MATRIX: W = Aqueous Non-drinking Water,Digested Metals; ML = Final Effluent, Minimum-Level / Low-Level R.L.; DW = Drinking Water; SL = Soil, Sludge, Solid; FP = Free Product

**CONTAINER TYPES: AL = Amber Liter; AHL = 500 ml Amber; PT = Pint (Plastic); QT = Quart (Plastic); HG = Half Gallon (Plastic); SJ = Soil Jar; B4 = 4oz. BACT; BT = Brass Tube; VOA = 40mL VOA; OTC = Other Type Container

H2SO4 NaOH HCl

FOR

LAB

USE

ONL

Y

TEMP: SEALED: Y / N INTACT: Y / N

COMMENTS:

BD: BIO WC MET

C C ON ICE: Y / N REPORTING OPTIONS (Choose One): EMAIL MAIL BOTH

REGULATORY DRINKING WATER?Y N

If Y, write 10-digit PS Code(s) below:

Rev. 02/15/20

ONLY THE STATEMENT 'TOTAL COLIFORM ABSENT ' MEANS THAT THE WATER MEETS THE BACTERIAL REQUIREMENTS OF THE STATE HEALTH AND SAFETY CODES FOR POTABLE WATER.

7.8.9.

3.2.1.

4.5.6. Check here for RUSH Turnaround

CLIENT INFORMATION:

$50.00

add $20.00*Sample must be received by 3 PM and paid in full inorder to receive results by end of the next business day.

CARE MUST BE TAKEN IN THE FOLLOWING STEPS TO AVOID SPLASHINGReduce the flow of water to a 'pencil' stream.Remove cap without touching the neck or inside of cap.Open the sample container - carefully insert opening into the water stream. Fill the container to between the 100mL and 120mL lines (not less than 100mL, but not more than 120mL). Recap container and tighten. RETURN TO THE LAB WITHIN 12 HOURS.

Pick a water tap that is commonly used. Do not use a swivel faucet. Remove any tap attachments (filters, aerators, etc).Let the water run for a full 5 to 10 minutes.Clean faucet with rubbing alcohol, inside and outside.Open the cold water valve to a full steady stream.Hold the sample container near the bottom.

SAMPLING INSTRUCTIONS:

BOTTLE IS STERILE - DO NOT OPEN OR RINSE BEFORE SAMPLINGFEES:For Coliform Analysis OnlyStandard Turnaround (results in 5-7 days)

RUSH Turnaround (results sent next day)*

COLIFORM BACTERIA ANALYSIS

1885 North Kelly Road Napa, CA 94558

Phone: (707) 258-4000 Fax: (707) 226-1001

[email protected] www.caltestlabs.com

LAB ORDER #:

FieldChlorineResidual

LAB USE ONLY

SAMPLE LOCATION DESCRIPTION AbsentTotal Coliform Present Absent Present

SAMPLETIME

SAMPLEDATE

Date/Time Set:

Analyst(s):

Date/Time Read Out:

Analyst(s):

Client__________________________________________________________

Mailing Address __________________________ Phone_________________

City _____________________________________ St _____ Zip ___________

Project Name____________________________________________________

Sampler Name __________________________________________________

Reporting Options:

Received By:DateSubmitted By: (Print & Sign)

TimeReceived By:DateSubmitted By: (Print & Sign)

Time

E. Coli

Check here if this sample is used for regulatory purposes.

Check below to have lab send copy to a regulatory office

CDPH.RICH

Routine Repeat Raw Special

CDPH System #:(required)

NCEH CDPH.SR

Other (county/agency):

Sample Type (circle one - required) Mail Hardcopy (default) - Please fill-in complete address on reverse side of page

Email (please print): _________________________________________

Email cc (please print): _______________________________________

Regulator Email (if applicable):

Date/Time:Notification Req? Y N

Contact:

Initials:

Entered By: Reviewed By:

Temp:

Sealed:

Intact:

On ice:

Y / N

Y / N

°C

Y / N

Lab Certification (ELAP) #1664

If sample results indicate the presence of coliform bacteria, the following decontamination procedures have been recommended by County Environmental Health Departments:

1. If water is cloudy, pump the well until the water appears to be clear.2. Mix one gallon household bleach containing 5.25% sodium hypochlorite to three gallons of water. Greater amounts or

stronger chlorine solutions should be used for wells of more than 100 feet deep.3. The chlorine solution is then poured into the well. It may be necessary to lift the pump, but some wells have openings which

can be used for this purpose.4. Do not operate the pump for 30 minutes. After the 30 minute period, with the taps, faucets and hydrants open or closed,

surge the well by starting and stopping the pump several times.5. Open every tap, faucet or hydrant in the water piping system, start the pump and let the water flow until clean water with

a strong odor of chlorine comes out.6. Stop the pump and close all the taps, faucets and hydrants. Do not operate the pump for 24 hours.7. After 24 hours, open all outside taps, faucets and hydrants and let the water flow until the odor of chlorine is gone. Do not

discharge heavily chlorinated water into an individual sewage disposal system.8. A water sample for bacteriological analysis should be obtained one week or more after disinfecting the well.

NOTE: Make sure that your well is tightly sealed to keep out rodents, insects, dirt and surface water seepage.For storage tanks, use of 4 ounces of household bleach per 1000 gallons should provide 5ppm of free residual chlorine.

For additional information contact your County Health Department.

1885 North Kelly RoadNapa, CA 94558

Rev 02.20.2020

Check here if this sample is used for regulatory purposes.

Check below to have lab send copy to a regulatory office

CDPH.RICH

:yB devieceR

Routine Repeat Raw Special

CDPH System #:

ONLY THE STATEMENT 'TOTAL COLIFORM ABSENT ' MEANS THAT THE WATER MEETS THE BACTERIAL REQUIREMENTS OF THE STATE HEALTH AND SAFETY CODES FOR POTABLE WATER.

etaD)ngiS & tnirP( :yB dettimbuS

Time

Fill the container to BETWEEN the 100mL and 120mL LINES AND RETURN TO LAB WITHIN 12 HOURS.

(required)

Lab Certification (ELAP) #1664

1885 North Kelly Road Napa, CA 94558

Phone: (707) 258-4000 Fax: (707) 226-1001

[email protected]

LAB ORDER #:

Y N Date/Time:Notification Req?

Contact:

LAB USE ONLY

Absent

Total Coliform E. ColiPresent Absent

Initials:

PresentSAMPLE LOCATION DESCRIPTION

FieldChlorineResidual

SAMPLE#

SAMPLEDATE

SAMPLETIME

Date/Time Set:

Analyst(s):

Date/Time Read Out:

Analyst(s):

Mail Hardcopy (default) - Please fill-in complete address on reverse side of page

Email (please print): _________________________________________

Email cc (please print): _______________________________________

Temp:

Sealed:

Intact:

On ice:

NCEH CDPH.SR

COLIFORM BACTERIA ANALYSISCLIENT INFORMATION: Client__________________________________________________________

Mailing Address __________________________ Phone_________________

City _____________________________________ St _____ Zip ___________

Project Name____________________________________________________

Sampler Name __________________________________________________

Reporting Options:

Received By:DateSubmitted By: (Print & Sign)

Time

Y / N

Y / N

°C

Check here for RUSH Turnaround*

*Sample must be received by 3 PM and paid in full in order to receive results by end of the next business day.

Entered By: Reviewed By:

Other (county/agency):

Sample Type (circle one - required)

Regulator Email (if applicable):

Y / N

SAMPLING INSTRUCTIONS:BOTTLE IS STERILE - DO NOT OPEN OR RINSE BEFORE SAMPLING

1. Pick a water tap that is commonly used. Do not use a swivel faucet.2. Remove any tap attachments (filters, aerators, etc).3. Let the water run for a full 5 to 10 minutes.4. Clean faucet with rubbing alcohol, inside and outside.5. Open the cold water valve to a full steady stream.6. Hold the sample container near the bottom.

7. Reduce the flow of water to a 'pencil' stream.8. Remove cap without touching the neck or inside of cap.9. Open the sample container - carefully insert opening into the water stream. Fill the container to between the 100mL and

120mL lines (not less than 100mL, but not more than 120mL). Recap container and tighten. RETURN TO THE LABWITHIN 12 HOURS.

For additional information contact your County Health Department.

1885 North Kelly RoadNapa, CA 94558

Rev 02.20.2020

CARE MUST BE TAKEN IN THE FOLLOWING STEPS TO AVOID SPLASHING

Sampling Instructions - caltestlabs.com€¦ · Sampling Instructions- Cyanide Analysis 9 Sampling Instructions – Containers with Sulfuric Acid (H 2 SO 4) Sampling Instructions-

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