chapt4

4.4.1.1 Obtaining Clean Containers

Sample containers shall be cleaned or obtained by one of three protocols:

a. Purchased from commercial vendors as precleaned containers. The cleaning grades must meet EPA analyte specific requirements. All records for these containers (lot numbers, certification statements, date of receipt, etc.) and their intended uses must be documented; or

b. Obtained from a subcontracted laboratory with an approved sample cleaning and handling protocols in their Comprehensive QA Plan. The contractor must verify that the laboratory has outlined sample container cleaning protocols in its approved DER CompQAP; or

c. Cleaned and maintained by the organization following all analyte specific container cleaning procedures as follows:

4.4.1.2 Container Cleaning Procedures

Analysis/Parameter	Cleaning Protocols (in order specified)

Extractable Organics	1, 2, 4, 6, (5 and 7 optional), 12
(GC, HPLC, GC/MS and Total Phenols)

Purgeable Organics (VOCs)	1, 2, 4, (6 optional, methanol only), 7
(GC, GC/MS, TOX)

Metals (Including Cr and Hg)	1, 2, 3, 4, 8, 12

Inorganics	1, 2, 3*, 4, 8, 9, 12
(Including Cyanide, Alkalinity, Acidity, Residues, BOD, Color, Surfactants, COD, TOC, Chloride, Turbidity, Sulfate, Bromide, Sulfide, Fluoride, Nutrients and Radionuclides)	(* For nutrients, nitric acid should be replaced by hydrochloric acid, or hydrochloric acid may be used after the nitric acid rinse)

Oil & Grease (and TRPH)	1, 2, 3, 4, (5, 6, 7 optional), 12

Bacteriologicals	1, 2, 8, 10

Toxicity Tests (Bioassays)	1, 2, 11, 2, 4, 6 (10 optional)

NOTES: a) New container cleaning procedures may skip steps 1 and 2.

b) This sheet does not represent all possible cleaning procedures, and deviations may be accepted on a case by case basis.

Cleaning Procedures:

1. Wash with hot tap water and a brush using a suitable laboratory-grade detergent.

Organics- Liquinox, Alconox or equivalents

Inorganic anions- Liquinox or equivalent

Inorganic cations- Liquinox, Acationox, Micro or equivalents

Bacteriologicals- must pass an inhibitory residue test.

2. Rinse thoroughly with hot tap water.

3. Rinse with 1:1 nitric acid solution.

4. Rinse thoroughly with deionized water.

5. Rinse thoroughly with pesticide-grade methylene chloride.

6. Rinse thoroughly with pesticide grade acetone or methanol (acetone only for Bioassays).

7. Oven dry at 103 C to 125 C for at least 1 hour.*

* VOC vials and containers should remain in the oven in a contaminant-free environment until needed. They should be capped in a contaminant-free environment just prior to dispatch to the field or to field sampling consultants.

8. Invert and air-dry in contaminant-free environment.

9. Container is rinsed with sample unless container already contains preservative.

10. Autoclave containers (the tops of which are covered with aluminum foil and autoclave indicator tape is applied over the top of the container).

11. Rinse with 10% HCl followed by a sodium bicarbonate solution.

12. Cap tightly and store in a contaminant-free environment until use.

4.4.1.3 Documentation

a. Organizations that order or clean containers shall maintain records of packing slips and lot numbers (if ordered) and/or records of cleaning protocols for container lots.

b. Cleaning records shall at a minimum record the following:

1. Cleaning procedure;

2. Lot numbers of reagent solvents and acids;

3. Date of cleaning;

4. Initials of person who cleaned containers;

5. Lot number (date of cleaning may be used);

6. If performed, the results of quality control tests that were run on lot numbers; and

7. Any additional cleaning or problems that were encountered with a specific lot.

c. Records shall be maintained that link lot numbers (either vendor or internal) to projects and/or clients.

4.4.2 Sample Preservation and Holding Times

4.4.2.1 General Considerations

a. Proper sample preservation is the responsibility of the sampling team, NOT the lab providing sample containers.

b. It is the responsibility of the field team to assure that all samples are appropriately preserved.

c. "IMMEDIATELY" is defined as within 15 minutes. This pertains to preservation as well as filtration immediately followed by preservation (i.e. dissolved metals, orthophosphate, etc.).

4.4.2.2 Sample Preservation

a. Sample preservation shall be accomplished by obtaining prepreserved bottles from an acceptable source or actually adding preservative to the sample in the field:

1. Sample containers obtained from the subcontracted laboratory prepreserved.

a. It is the responsibility of the organization ACCEPTING these containers to make sure that they are provided by a lab that has a DER-approved CompQAP.

b. The laboratory shall supply additional same-source preservatives in suitable containers.

2. Sample containers preserved in the field after sample addition. These preservation protocols shall be followed:

a. Preservatives shall be reagent grade or of a higher grade. Unless supported by equipment blanks, the acid for metals shall be suitable for trace metals analysis

b. Fresh preservatives shall be obtained from parent stocks prior to each sampling event. Any remaining preservatives that are not in sealed ampoules SHALL NOT be returned to stock, but must be appropriately discarded.

c. Preservatives shall be transported to the field in plastic or teflon containers unless sealed by the manufacturer in glass ampoules.

d. Preservatives shall be added with disposable pipettes or premeasured ampoules to each sample container

e. The same amount of preservative shall be added to the associated equipment blanks

b. The pH shall be checked on all pH preserved samples (except VOC, O&G, and TRPH) using the following protocol:

1. The effectiveness of required pH adjustment must be checked in the field.

2. Narrow range pH paper shall be used to test an ALIQUOT of the preserved sample.

a. Pour a small portion of the sample into disposable container

b. Place the pH paper into the container and compare the color with the manufacturer's color chart

c. Discard the aliquot appropriately. DO NOT POUR BACK INTO THE SAMPLE CONTAINER.

3. If the pH is acceptable (ex. greater than 10, less than 2, etc.), document acceptability in field records and prepare container for shipment to the laboratory.

4. If the pH is unacceptable:

a. Add additional preservative in measured increments, mix and test ALIQUOTS of the sample as described above.

b. Continue to add measured increments of preservatives until an acceptable pH has been reached.

c. Record the TOTAL amount of preservative that was needed.

d. Additional chemical preservatives used in the field shall be from the same source as the chemical used for original preservation. DO NOT REUSE OLD SUPPLIES OF PRESERVATIVES.

5. Alternatively, an extra "dummy sample" may be used to test pH. Contents of the containers shall be suitably discarded.

6. The same amount of additional chemical preservative shall be added to the corresponding equipment blank (or field blank, if used). NOTE: the maximum amount of preservative that was used to preserve any single sample in the sample set SHALL BE ADDED to the equipment blank.

7. Sample pH shall be checked at the following minimum frequencies:

a. during the first sampling event at a particular site, ALL samples that are pH-adjusted must be checked, and

b. during subsequent visits to a particular site, AT LEAST ONE sample per parameter group that must be pH-adjusted shall will be checked.

c. If the frequency of sample collection at a specified location is greater than once per month (i.e. weekly or daily), the pH checks shall be made on AT LEAST ONE sample per parameter group according to the following schedule:

1. Weekly sampling - 1 pH check per month

2. Daily sampling - 1 pH check per week

3. < 1 sampling episodes per day - a minimum of 1 pH check, and 1 additional check per 10 sampling episodes.

c. The organization preparing and preserving the containers must keep all documentation for preservation, consisting of:

a. the grades and lot numbers of all preservation reagents

b. the opening date and expiration date.

c. the specific preservation technique that was used with each sample.

4.4.2.3 Holding Times, Container Types and Preservation

Holding time, container type and required preservation for samples shall comply with the following tables:

a. Table 4.2 (Table II of 40 CFR Part 136) and Table 4.3 (Table 4 of Chapter 17-160, F.A.C.) for aqueous samples;

b. Table 4.4 (Table 5 of Chapter 17-160, F.A.C.) for solid samples AND

c. Table 4.5 (Table 8 of Chapter 17-160, F.A.C.) for specific drinking water holding times.

4.4.2.4 Special preservation protocols:

a. All special preservation protocols outlined in Section 4.2.2 of the surface water section shall be followed for all aqueous samples.

b. Samples for Chlorophyll shall be treated as follows:

1. samples shall be filtered in the laboratory within 24 hr. of collection,

2. magnesium carbonate shall be added to the filter while the last of the filtrate passes through the filter,

3. the sample will be either analyzed immediately or frozen for later analysis within 21 days.

4.4.3 Sample Dispatch

4.4.3.1 Documentation

Field documentation will consist of, at a minimum, field notes, sample labels and Chain of Custody forms (or sample transmittal forms). These items must contain a minimum amount of information that can be traceable back to the original sampling event. A complete discussion of the mandatory information to be completed in the field are in Chapter 5, Sample Custody and Documentation.

4.4.3.2 Sample Packing and Transport

a. Samples shall be packed such that they are segregated by site, sampling location or by sample analysis type. Sample segregation may follow this segregation scheme or any other that is sensible and well thought out. These schemes are dependent upon the levels of contamination present, the number of bottles to be transported, the size of the bottles, etc.

1. VOC samples from different locations may be placed into the same cooler to reduce the number of required trip blanks provided that the samples are wrapped or containerized (ziplock bag or metal can) separately.

2. Samples in breakable containers shall be packed with materials (i.e. bubble wrap, cans with vermiculite) to avoid breakage.

3. Shipping transport containers shall be insulated (if cooling is required).

4. Shipping containers shall be sealed with strapping tape or locked to avoid tampering. Tamper-proof seals may also be placed over cooler lid.

5. All samples that require thermal preservation shall be packed in thermally insulated coolers with wet ice. Only wet ice shall be used in cooling samples to 4 C. BLUE ICE OR CHEMICAL COOLING PACKS ARE NOT ACCEPTABLE.

Table 4.2

40 CFR Part 136 TABLE II: REQUIRED CONTAINERS, PRESERVATION TECHNIQUES, AND HOLDING TIMES

(WATER/WASTEWATER SAMPLES)

PARAMETER #	PARAMETER NAME	CONTAINER[i]	PRESERVATION[ii],[iii]	MAX HOLD TIME[iv]
Table 1A-Bacterial Tests:
1-4.	Coliform, fecal and total	P, G	Cool 4C, 0.008% Na₂S₂O₃[v]	6 hours
5.	Fecal streptococci	P, G	Cool 4C, 0.008% Na²S₂O_3v	6 hours

Table 1B-Inorganic Tests:
1.	Acidity	P, G	Cool 4C	14 days
2.	Alkalinity	P, G	Cool 4C	14 days
4.	Ammonia	P, G	Cool 4C, H₂SO₄ to pH<2	28 days
9.	Biochemical oxygen demand	P, G	Cool 4C	48 hours
11.	Bromide	P, G	None required	28 days
14.	Biochemical oxygen demand carbonaceous	P, G	Cool 4C	48 hours
15.	Chemical oxygen demand	P, G	Cool 4C, H₂SO₄ to pH<2	28 days
16.	Chloride	P, G	None required	28 days
17.	Chlorine, total residual	P, G	None required	Analyze immediately
21.	Color	P, G	Cool 4C	48 hours
23-24.	Cyanide, total and amenable to chlorination	P, G	Cool 4C, NaOH to pH>12, 0.6g ascorbic acid ^v	14 days[vi]
25.	Fluoride	P	None required	28 days
27.	Hardness	P, G	HNO₃ to pH<2, H₂SO₄ to pH<2	6 months
28.	Hydrogen ion (pH)	P, G	None required	Analyze immediately
31, 43.	Kjeldahl and organic nitrogen	P, G	Cool 4C, H₂SO₄ to pH<2	28 days

Metals[vii]
18.	Chromium VI	P, G	Cool 4C	24 hours
35.	Mercury	P, G	HNO₃ to pH<2	28 days
3. 5-8, 10, 12, 13, 19, 20, 22, 26, 29, 30, 32-34, 36, 37, 45, 47, 51, 52 58-60, 62, 63, 70-72, 74, 75	Metals, except chromium VI and mercury	P, G	HNO₃ to pH<2	6 months
38.	Nitrate	P, G	Cool 4C	48 hours
39.	Nitrate-nitrite	P, G	Cool 4C, H₂SO₄ to pH<2	28 days
40.	Nitrite	P, G	Cool 4C	48 hours
41.	Oil and grease	G	Cool 4C, H₂SO₄ to pH<2	28 days
42.	Organic carbon	P, G	Cool 4C, HCl or H₂SO₄ to pH<2	28 days
44.	Orthophosphate	P, G	Filter immediately, Cool 4C	48 hours

Table 4.2, cont.

PARAMETER #	PARAMETER NAME	CONTAINERⁱ	PRESERVATION^ii,iii	MAX HOLD TIME^iv
47.	Oxygen, Winkler	G (Bottle & top)	Fix on site and store in dark	8 hours
48.	Phenols	G only	Cool 4C, H₂SO₄ to pH<2	28 days
49.	Phosphorus (elemental)	G	Cool 4C	48 hours
50.	Phosphorus, total	P, G	Cool 4C, H₂SO₄ to pH<2	28 days
53.	Residue, total	P, G	Cool 4C	7 days
54.	Residue, Filterable	P, G	Cool 4C	7 days
55.	Residue, Nonfilterable (TSS)	P, G	Cool 4C	7 days
56.	Residue, Settleable	P, G	Cool 4C	48 hours
57.	Residue, volatile	P, G	Cool 4C	7 days
61.	Silica	P	Cool 4C	28 days
64.	Specific conductance	P, G	Cool 4C	28 days
65.	Sulfate	P, G	Cool 4C	28 days
66.	Sulfide	P, G	Cool 4C add zinc acetate plus sodium hydroxide to pH>9	7 days
67.	Sulfite	P, G	None required	Analyze immediately
68.	Surfactants	P, G	Cool 4C	48 hours
69.	Temperature	P, G	None required	Analyze immediately
73.	Turbidity	P, G	Cool 4C	48 hours

Table 1C-Organic Tests:[viii]
13, 18-20, 22, 24-28, 34-37, 39-43, 45-47, 56, 66, 88, 89, 92-95, 97.	Purgeable Halocarbons	G, Teflon- lined septum	Cool 4C, 0.008% Na₂S₂O₃ ^v	14 days
6, 57, 90	Purgeable aromatic hydrocarbons	"	Cool 4C, 0.008% Na₂S₂O₃ ^v HCl to pH2[ix]	14 days
3, 4,	Acrolein and acrylonitrile	“	Cool 4C, 0.008% Na₂S₂O₃ ^v Adjust pH to 4-5[x]	14 days
23, 30, 44, 49, 53, 67, 70, 71, 83, 85, 96.	Phenols[xi]	G, Teflon lined cap	Cool 4C, 0.008% Na₂S₂O₃ ^v	7 days until extraction, 40 days after extraction
7, 38.	Benzidines^,xi,[xii]	"	Cool 4C, 0.008% Na₂S₂O₃ ^v	7 days until extraction, 40 days after extraction[xiii]
14, 17, 48, 50-52.	Phthalate esters ^xi	"	Cool 4C	7 days until extraction, 40 days after extraction
72-74.	Nitrosamines ^xi,[xiv]	"	Cool 4C, store in dark, 0.008% Na₂S₂O₃ ^v	"
76-82.	PCBs ^xi acrylonitrile	"	Cool 4C	"
54, 55, 65, 69.	Nitroaromatics and isophorone ^xi	"	Cool 4C, 0.008% Na₂S₂O₃ ^v store in dark	"
1, 2, 5, 8-12, 32, 33, 58, 59, 64, 68, 84, 86.	Polynuclear aromatic hydrocarbons ^xi	"	"	"

Table 4.2, cont.

PARAMETER #	PARAMETER NAME	CONTAINERⁱ	PRESERVATION^ii,iii	MAX HOLD TIME^iv
15, 16, 21, 31, 75.	Haloethers ^xi	"	Cool 4C, 0.008% Na₂S₂O₃ ^v	"

29, 35-37, 60-63, 91.	Chlorinated hydrocarbons ^xi	"	Cool 4C	"
87.	TCDD ^xi	"	Cool 4C, 0.008% Na₂S₂O₃ ^v	"

Table 1D-Pesticides Tests:
1-70.	Pesticides ^xi	"	Cool 4C, pH 5-9 [xv]	"

Table 1E-Radiological Tests:
1-5.	Alpha, beta and radium	P, G	HNO3 TO pH<2	6 months

Reference: This table is reprinted from 40 CFR Chapter I, Revised as of July 1, 1988. According to Federal Register of Thursday, September 3, 1987, preservation for Oil and Grease may also be performed with HCl

Table 4.3

APPROVED WATER AND WASTEWATER PROCEDURES, CONTAINERS, PRESERVATION AND HOLDING TIMES

FOR PARAMETERS NOT FOUND IN 40 CFR 136 **

PARAMETER	METHOD	REFERENCE[xvi]	CONTAINER [xvii]	PRESERVATION[xviii]	MAXIMUM HOLDING TIME[xix]

Bromine	DPD Colorimetric[xx]	SM 408E	P, G	None required	Analyze immediately
		SM 4500-Cl-G

Bromates	Ion Chromatography	EPA-300.0 B [xxi]	P, G	Cool, 4C	30 days

Chlorophylls	Spectrophotometric	SM 1002G	P, G [xxii]	14d in dark	30 days ^g
		SM 10200H

Corrosivity	Calculated	SM 203	P, G	Cool, 4C [xxiii]	7 days ^h
	(CaCO3 Stability,	SM 2330
	Langelier Index)	ASTM D513-82

Odor	Human Panel	SM 207	G only	Cool, 4C	6 hours
		SM 2150

Salinity	Electrometric ⁱ	SM 210 A	G, wax seal	Analyze	30 days [xxiv]
		SM 2420 B		immediately or
	Hydrometric	SM 210 B		use wax seal
		SM 2520 C
	Argentometric	SM 210C

Taste	Human Panel	SM 211 A,B	G only	Cool, 4C	24 hours
		SM 2160 B
		SM 2160 C
		SM 2160 D
		ASTM 1292-86

Total Dissolved Gases	Direct-Sensing Membrane-Diffusion Method	SM 2810	---	---	Analyze in-situ

Transparency	Irradiometric [xxv]	17-3.021(6), FAC	---	---	Analyze in-situ

Un-ionized Ammonia	Calculated [xxvi]	DER-SOP [xxvii]	P, G	Cool, 4C	8 hours unpreserved
				Na2S2O3 ^k	28 days preserved^k

Organic Pesticides[xxviii]	GC and HPLC	EPA (600-series) ^m	[xxix]	ⁿ	ⁿ

**Reference: 17-160.700, F.A.C., Table 4

b. Packed samples shall be delivered to the analyzing laboratory by the sampling team or via common carrier.

1. If sent by common carrier, all documentation (transmittal form, bill of lading, analyses order, etc.) shall be sealed and placed inside the shipping container prior to sealing it closed. The QA Section recommends that all records be placed in a plastic bag and taped to the underside of the cooler lid.

All reagents, cleaning materials and preservatives that are maintained by the field consultant shall be stored, transported and handled in such a way to prevent and/or minimize contamination.

The following storage and use protocols shall be observed. Those that are double bracketed ([[ ]]) are RECOMMENDED protocols that should be considered when storing various chemicals:

[[a. All chemicals that are maintained in-house and transported to the field shall be segregated according to reactivity (i.e. acids, bases, etc.).]]

[[b. If possible, acids should be stored in an acid storage cabinet and solvents should be stored in a vented solvent storage cabinet. If specialized storage is unavailable, all chemicals shall be stored in a well-ventilated area.]]

c. All chemicals transported to the field shall be stored in bottles which will be packed to avoid breakage.

d. If quantities of reagent chemicals are transferred from the original container, the transport container shall be appropriately precleaned and must be of similar construction type as the original container (e.g. acids and bases may be transported in plastic or teflon containers).

e. Chemicals shall be segregated from sample containers so as to avoid reaction and accidental contamination.

g. Analyte-free water shall be segregated from solvents to prevent contamination.

Field-generated wastes may require segregation and containerization for proper disposal by a commercial contractor. This decision is highly dependent upon which DER program the site work is being conducted and the nature of the waste. If there is a DER technical Project Manager that is in an oversight position, they should be consulted regarding the fate of all wastes. In general, these wastes can be categorized as: (1) decontamination wastes, especially waste solvents, (2) waste acids and bases, (3) contaminated purge waters, and (4) calibration standards from field meters.

a. All field investigations will generate some amount of waste material, especially groundwater investigations. Boring, developing, purging, and sampling monitor wells will generate soils, waters, and spent reagents that must be handled in a way that will not spread or increase contamination at the site. Activities from other sampling matrices will generate similar wastes.

b. These wastes are normally categorized into hazardous and non-hazardous wastes.

1. Hazardous wastes must be disposed of according to any and all applicable Federal (RCRA, CERCLA, etc.), State, County, or municipal regulations.

c. Proper handling and disposal of all waste materials should be addressed prior to initiating site work. The following are a list of some materials that will require proper treatment, storage, and disposal. Additionally, these must be segregated by their hazardous or non-hazardous nature:

2. disposable equipment: ground covers, equipment covers (aluminum foil, plastic garbage bags, etc.), disposable bailers or tubing, broken or unused sample containers, shipping containers, etc.,

7. spent calibration standards for field analytical equipment (field GC, conductance, pH, etc.).

a. Decontamination and calibration wastes must be segregated and disposed of properly.

b. Soap solutions and waste tap/DI/analyte-free water can be disposed of on site.

c. Calibration standards (pH and conductance) may be diluted with spent detergent solution and wash waters and disposed of in sanitary sewer.

e. Waste solvents shall be handled as hazardous waste and must be collected and transported back to the office or lab to be handled by commercial disposal or recycling contractor. DISCHARGE OR EVAPORATION OF WASTE SOLVENTS ON-SITE, IN ANY AMOUNT, IS NOT ACCEPTABLE. See discussion below on hazardous waste handling.

f. Concentrated, reagent grade preservative acids and bases shall be transported back to the office, laboratory, or disposed of by commercial contractor.

a. Contaminated purge waters must be handled prudently. Recommendations from an DER Project Manager should be used and will supersede guidance defined in this document.

b. If wastewater generated from well development or purging of monitor wells is likely to contain contaminants in excess of the MCL (maximum contaminant level) as listed in Florida Administrative Code (e.g. Chapter 17-302, 17-550 or 17-770), the water shall be contained on-site in temporary storage (e.g., lined pit, drum, tank or tanker truck) until the waters can be characterized by the appropriate approved analytical method(s).

c. In many cases it may be possible to directly discharge contaminated purged water on-site, but only if the purged water will infiltrate into the SAME aquifer zone from which it was purged from or into a more contaminated aquifer zone.

d. Additionally, exposure of such purged water must not pose a health risk and the purged water shall not be discharged into any surface water body, unless permitted.

e. Purged water must be adequately treated (contaminants should not exceed established standards) prior to discharge on-site if the above conditions cannot be met.

f. Alternatively, purged water may be transported to an off-site facility such as sewage treatment plant/sewer system (some wastewater treatment systems are capable of treating water with total VOC concentrations up to 500 ppm). THE WASTEWATER TREATMENT PLANT OPERATOR MUST BE NOTIFIED AND MUST GIVE APPROVAL BEFORE DISCHARGE CAN OCCUR.

g. The QA Section strongly recommends contacting the overseeing regulatory authority concerning criteria for discharge of moderately contaminated purge water. By contacting the DER (District or headquarters), county, or municipal authority that is in charge of a particular program, local ordinances or procedures may be obtained that relate to collection and transportation of purge water.

Handling, storage and disposal of field-related hazardous wastes are subject to the regulations contained in the Resource Conservation and Recovery Act.

All of the procedures listed in this subsection pertain to the company, field consultant, primary contractor, etc. whomever is performing and is responsible for the field sampling event. For brevity, we will refer to this organization as the field consultant.

1. The field consultant is responsible for all wastes generated on-site as a result of the sampling event, excluding those waste materials already present on-site (contaminated drill cuttings, purge water, etc.).

2. It is the responsibility of the field consultant to store, package, label, ship and dispose of the hazardous wastes which are generated during the sampling event or project in a manner which ensures compliance with all Federal, State and local laws, regulations and ordinances.

3. Responsibility may also be assumed by the property owner. These requirements will not specify who is ultimately responsible. This decision will be made by the property owner and the primary contractor with regard to ALL of the RCRA requirements.

4. The field consultant is responsible for the waste if it contaminates the environment; therefore, precautions should be taken to secure all reagents (acids, bases, solvents, etc.) that, if spilled, would be characterized as a hazardous waste (listed in 40 CFR Part 261.30-.33 or if a characteristic waste).

b. The material exhibits any of the specified characteristics: ignitability; corrosivity; reactivity or TC toxicity.

a. Field consultants that generate hazardous waste are put into 3 categories based on the amount of hazardous waste generated monthly. These categories are; 1) conditionally exempt small quantity generator, 2) small quantity generator and 3) full generator.

b. Conditionally Exempt Small Quantity Generator: A generator who generates no more than 100 kilograms of hazardous waste in a calendar month. (40 CFR Part 261.5)

A generator who generates more than 100 kilograms but no more than 1000 kilograms of hazardous waste per calendar month or generates less than 1 kilogram of acute hazardous waste and accumulates no greater than 6000 kilograms of hazardous waste. (40 CFR Part 262.34)

A generator who generates wastes in excess of 1000 kilograms per calendar month or more than 1 kilogram per month of acute hazardous waste. (40 CFR Part 262.34).

3. It is the responsibility of the field consultant to know which category their organization falls under. Since most field consultants will fall into the conditionally exempt small quantity generator category, these requirements are listed below.

c. Hazardous waste Handling Protocols for Conditionally Exempt Small Quantity Generators

1. These generators may either treat or dispose of hazardous waste in an on-site facility or ensure delivery to an off-site treatment, storage or disposal facility, either of which, if located in the U.S., is:

c. Authorized to manage hazardous waste by a state with a hazardous waste management program approved under Part 271.

d. Permitted, licensed, or registered by a state to manage municipal or industrial solid waste. *(subject to local regulations).

d. Hazardous Waste Handling Protocols for Facilities falling into the Small Quantity Generator and Full Generator

1. These organizations must adhere to all regulations pertaining to waste disposal in the Resource Conservation and Recovery Act.

1. Hazardous waste solvents, as identified in the 40 CFR Part 261, shall not be evaporated on-site by pouring onto pervious or impervious surfaces.

a. These solvents shall also not be evaporated at the office or lab with or without a fume hood.

b. Solvents that evaporate during the actual decontamination process are exempt.

2. Acidic and Basic wastes may be neutralized and disposed of via the sanitary sewer if they are not hazardous due to the presence of other constituents*. (*subject to local regulations).

1. There are no special handling requirements for transportation of these wastes back to the office or laboratory.

2. There are no requirements for manifesting the waste nor placarding the vehicle (if for small quantities).

3. A sample collector shipping samples to a laboratory and a laboratory returning samples to a sample collector must comply with U.S. Department of Transportation (DOT), U.S. Postal Service (USPS), or any other applicable shipping requirements.

1. Hazardous waste storage is limited by quantity and/or accumulation time and must comply with RCRA regulations as specified in the 40 CFR.

2. These wastes shall be packaged and separated according to compatible groups (e.g. solvents, acids, etc.).

1. Samples submitted to a laboratory for analysis are excluded from regulation as hazardous waste under 40 CFR Part 261.4(d) provided the samples are being transported to or from the laboratory, or are being analyzed, are being held for analysis, or are being maintained in custody for legal reasons.

2. Once a decision is made to dispose of laboratory samples, the exclusion provisions of 40 CFR Part 261.4(d) no longer apply.

3. Samples that have been identified as hazardous may either be: 1) returned safely to the generator; or 2) disposed of according to applicable RCRA regulations summarized in this document.

4. Samples which are determined to be non-hazardous may be subject to local environmental regulations. It will be the responsibility of the laboratory to be familiar with any such local regulations.

[i] Polyethylene (P) or Glass (G).

[ii] Sample preservation should be performed immediately upon sample collection. For composite chemical samples each aliquot should be preserved at the time of collection. When use of an automated sampler makes it impossible to preserve each aliquot, then chemical samples may be preserved by maintaining at 4 C until compositing and sample splitting is completed.

[iii] When any sample is to be shipped by common carrier or sent through the United States Mails, it must comply with the Department of Transportation Hazardous Materials Regulations (49 CFR Part 172). The person offering such material for transportation is responsible for ensuring such compliance. For the preservation requirements of Table II, the Office of Hazardous Materials, Materials Transportation Bureau, Department of Transportation has determined that the Hazardous Materials Regulations do not apply to the following materials: Hydrochloric acid (HCl) in water solutions at concentrations of 0.04% by weight or less (pH about 1.96 or greater); Nitric acid (HNO3) in water solutions at concentrations 0.15% by weight or less (pH about 1.62 or greater); Sulfuric acid (H2SO4) in water solutions at concentrations of 0.35% by weight or less (pH about 1.15 or greater); and Sodium hydroxide (NaOH) in solutions at concentrations of 0.080% by weight or less (pH about 12.30 or less).

[iv] Samples should be analyzed as soon as possible after collection. The times listed are the maximum times that samples may be held before analysis and still be considered valid. Samples may be held for longer periods only if the permittee, or monitoring laboratory, has data on file to show that the specific types of samples under study are stable for the longer time, and has received a variance from the Regional Administrator under Part 136.3(e). Some samples may not be stable for the maximum time period given in the table. A permittee, or monitoring laboratory, is obligated to hold the sample for shorter time if knowledge exists to show that this is necessary to maintain sample stability. See Part 136.3(e) for details.

[v] Should only be used in the presence of residual chlorine.

[vi] Maximum time is 24 hours when sulfide is present. Optionally all samples may be tested with lead acetate paper before pH adjustments in order to determine if sulfide is present. If sulfide is present, it can be removed by the addition of cadmium nitrate powder until a negative spot test is obtained. The sample is filtered and then NaOH is added to pH 12.

[vii] Samples should be filtered immediately on-site before adding preservative for dissolved metals.

[viii] Guidance applies to samples to be analyzed by GC, LC, or GC/MS for specific compounds.

[ix] Sample receiving no pH adjustment must be analyzed within seven days of sampling.

[x] The pH adjustment is not required if acrolein will not be measured. Samples for acrolein receiving no pH adjustment must be analyzed within 3 days of sampling.

[xi] When the extractable analytes of concern fall within a single chemical category, the specified preservative and maximum holding times should be observed for optimum safeguard of sample integrity. When the analytes of concern fall within two or more chemical categories, the sample may be preserved by cooling to 4 C, reducing residual chlorine with 0.008% sodium thiosulfate, storing in the dark, and adjusting the pH to 6-9; samples preserved in this manner may be held for seven days before extraction and for forty days after extraction. Exceptions to this optional preservation and holding time procedure are noted in footnote 5 (re the requirement for thiosulfate reduction of residual chlorine), and footnotes 12, 13 (re the analysis of benzidine).

[xii] If 1,2-dephenyl hydrazine is likely to be present, adjust the pH of the sample to 4.0 "0.2 to prevent rearrangement to benzidine.

[xiii] Extracts may be stored up to 7 days before analysis if storage is conducted under an inert (oxidant-free) atmosphere.

[xiv] For the analysis of diphenylnitrosamine, add 0.008% Na2S2O3 and adjust pH to 7-10 with NaOH within 24 hours of sampling.

[xv] The pH adjustment may be performed upon receipt at the laboratory and may be omitted if the samples are extracted within 72 hours of collection. For the analysis of aldrin, add 0.008% Na2S2O3.

[xvi] SM XXX = procedures from "Standard Methods for the Examination of Water and Wastewater", APHA-AWWA-WPCF, 16th Edition, 1985 (except Chlorophylls, SM 1002G).

SM XXXX = procedures from Standard Methods for the Examination of Water and Wastewater", APHA-AWWA-WPCF, 17th Edition, 1989 (Except Chlorophylls, SM 10200H).

ASTM XXXX-YY= procedure from "Annual Book of ASTM Standards", Volumes 11.01 and 11.02 (Water I and II), 1988.

[xvii] P= plastic, G= glass.

[xviii] When specified, sample preservation should be performed immediately upon sample collection.

[xix] The times listed are the maximum times that samples may be held before analysis and still be considered valid.

[xx] The approved procedure is for residual chlorine. However, in the absence of chlorine, the DPD colorimetric procedure can be adapted to measure bromine content of the sample. In such case, the validity of this assumption must be verified by using another procedure for chlorine which is not affected by the presence of bromine (i.e. negligible interference).

[xxi] "The Determination of Inorganic Anions in Water Ion Chromatography", EPA Method 300.0 B, Revised August 1991, by John D. Pfaff, Carol A. Brockoff and James W. O'Dell, U.S. EPA, Cincinnati, Ohio 45268.

[xxii] Collect samples in opaque bottles and process under reduced light. Samples on filter taken from water having pH 7 or higher may be placed in airtight plastic bags and stored frozen for up to three weeks. Samples from acidic water must be processed promptly to prevent chlorophyll degradation.

[xxiii] Temperature and pH must be measured on site at the time of sample collection. 7 days is the maximum time for laboratory analysis of total alkalinity, calcium ion and total solids.

[xxiv] The electrometric and hydrometric analytical methods are suited for field use. The argentometric method is suited for laboratory use. Samples collected for laboratory analysis, when properly sealed with paraffin waxed stopper, may be held indefinitely. The maximum holding time of 30 days is recommended as a practical regulatory limit.

[xxv] Transparency in surface waters is defined as a compensation point for photosynthetic activity, i.e. the depth at which one percent of the light intensity entering at the water surface remains unabsorbed. The DER Rule 17-3 FAC requires that the light intensities at the surface and subsurface be measured simultaneously by irradiance meters such as the Kahlsico Underwater Irradiometer, Model No. 268 WA 310, or an equivalent device having a comparable spectral response.

[xxvi] The results of the measurements of pH, temperature, salinity (if applicable) and the ammonium ion concentration in the sample are used to calculate the concentration of ammonia in the unionized state. Temperature, pH and salinity must be measured on site at the time of sample collection. Laboratory analysis of the ammonium ion concentration should be conducted within eight hours of sample collection. If prompt analysis of ammonia is impossible, preserve samples with H2SO4 to pH between 1.5 and 2. Acid-preserved samples, stored at 4C, may be held up to 28 days for ammonia determination. Sodium thiosulfate should only be used if fresh samples contain residual chlorine.

[xxvii] DER Central Analytical Laboratory, Tallahassee, FL, Revision No. 1, October 3, 1983. The 1983 draft is available from the DER QA Section.

[xxviii] Other pesticides listed in approved EPA methods (608.1, 608.2, 614, 614.1, 615, 617, 618, 619, 622, 622.1, 627, 629, 631, 632, 632.1, 633, 642, 643, 644 and 645) which are not included in Table ID of 40 CFR Part 136 (July 1989).

[xxix] Container, preservation and holding time as specified in each individual method shall be followed.

[xxx] Adapted from tables 3-1 and 4-1 in Test Methods for Evaluating Solid Waste, SW-846, EPA, Third Edition, 1986, and First Update in 1987. The term residuals includes: (i) concentrated waste samples and (ii) sludges of domestic or industrial origin.

[xxxi] Sample shall not be homogenized (mixed) prior to filling container. Container must be filled by packing as much sample into it leaving minimal headspace. Field samples can not be composited for analysis.

[xxxii] Soils, sediments and sludges shall be kept cool at 4 C from collection time until analysis. No preservation is required for concentrated waste samples.

[xxxiii] Preservation, when required must be done upon sample collection.

[xxxiv] Stated values are the maximum regulatory holding times.

[xxxv] Parameters included are: Fecal Coliform, Total Coliform and Fecal Streptococci.

[xxxvi] If samples are analyzed after 30 hours, but within 48 hours of collection, the laboratory is to indicate in the analytical report that the data may be invalid because of excessive delay in sample processing. No samples received after 48 hours are to be accepted or analyzed for compliance with the regulations of the Department of Environmental Regulation or the Department of Health and Rehabilitative Services.

[xxxvii] Addition of sodium thiosulfate is only required if the sample has a detectable amount of residual chlorine, as indicated by a field test using EPA Method 330.4 or 330.2 or equivalent.

[xxxviii] Group A parameters are: Gross Alpha, Gross Beta, Strontium-90, Radium-226, Radium-228, Uranium and Photon Emitters.

[xxxix] Group B parameters are: Cesium-134, Iodine-131, and Tritium.

[xl] Chlorinated means that the source water has a detectable amount of residual chlorine, as indicated by a field test using EPA Method 330.4 or 330.2 or equivalent. Non-chlorinated means that the source water contains no detectable amount of residual chlorine (i.e. is below the method detection limit of the above-mentioned methods).

[xli] Ion chromatographic methods using conductivity as the detector cannot be used to analyze for nitrate in such samples.