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6.0              ANALYTICAL PROCEDURES

6.1              LABORATORY GLASSWARE CLEANING PROCEDURES

      In the analysis of samples the preparation of scrupulously clean glassware is mandatory.  Lab glassware cleaning procedures must follow specific written method requirements.  If procedures are not listed then the method of cleaning should be adapted to both the substances that are to be removed, and the determinations (tests) to be performed.  Recommendations for such cleaning procedures are listed below.

      If documentation through an active quality control program using spiked samples and reagent blanks can demonstrate that certain steps in the cleaning procedure are not required for routine samples, then those steps may be eliminated from the procedure.

Lab Glassware Cleaning Procedures

Cleaning Procedures:

1.   Remove all labels using sponge or acetone.

2.   Wash with hot tap water and a brush to scrub inside of glassware, stopcocks, and other small pieces, if possible, using a suitable laboratory-grade detergent.

Organics- Liquinox, Alconox or equivalents

Inorganic anions- Liquinox or equivalent

Inorganic cations- Liquinox, Acationox, Micro or equivalents

Microbiology- must pass inhibitory residue test

3.   Rinse thoroughly with hot tap water.

4.   Rinse thoroughly with deionized water.

5.   Rinse thoroughly with pesticide grade Acetone.

6.   Rinse thoroughly with pesticide grade Methanol.

7.   Rinse thoroughly with pesticide grade Hexane.

8.   Rinse or soak with 1:1 HCl (Hydrochloric Acid).

9.   Rinse or soak with >10% HNO3 (Nitric Acid).

10.  Bake at 105 C for 1 hour.

11.  Bake at 180 C (prior to use as per method).

12.  Drain, then heat in muffle furnace for 30-60 minutes at 400 C.

13.  Clean, dry glassware should be sealed and stored in dust-free environment.

14.  Soak in oxidizing agent (Chromic acid or equivalent); preferably hot (40-50 C).

15.  Last step (prior to use) should be a rinse with the solvent used in analysis.

16.  Drain, then heat in muffle furnace for 1 hour at 550 C.

17.  Heat 1 hour in EDTA solution at 90-100 C.

18.  New glassware must be soaked overnight in 10% HNO3 or HCl.

19.  New glassware must be soaked overnight in seawater.

20.  Rinse thoroughly with dilution water.

CLASS A VOLUMETRIC GLASSWARE SHOULD NOT BE BAKED

6.2              LABORATORY REAGENT STORAGE

      1.      Laboratory reagents and chemicals must be stored according to method guidance and the manufacturer's instructions.  All solvents used for VOC analyses shall be stored separately.

      [[2.      Reagents should be segregated according to compatibility groups (e.g. Solvents {flamm/nonflamm}, bases, acids, reactive chemicals, etc.).  Storage should follow all OSHA requirements.]]

      3.   A permanent record of reagent storage and preparation shall be maintained for all chemicals.  At a minimum, these records shall document:

a.            storage conditions and location for reagents (implemented internal laboratory SOPs and/or safety plans that outline storage conditions and location may be used in lieu of specific reagent container records)

b.            vendor name

c.            date received/date opened

d.            expiration dates

e.            lot numbers

f.            preparation dates

g.            amounts and concentration of all source reagents and compounds used

h.            signature or initials of preparer.

I.            pH of microbiological culturing medias before and after sterilization

      4.      Documentation shall be maintained on all sources of analyte-free water.  This documentation shall include records on all maintenance, cartridge-changing and miscellaneous tasks performed to upkeep or repair the system and all routine QC analysis protocols specifically scheduled and performed to monitor the system.  Records must be maintained which identify the source and the specific use of analyte-free water that is obtained from commercial vendors.

6.3              LABORATORY WASTE DISPOSAL

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

      It is the responsibility of the laboratory to store, package, label, ship and dispose of hazardous wastes in a manner which ensures compliance with all Federal, State and local laws, regulations and ordinances.

      A waste is considered hazardous if:

      1.            The waste material is listed as hazardous in 40 CFR Part 261.30-261.33.

      2.            The material exhibits any of the characteristics of hazardous waste:  (ignitability, corrosivity, reactivity or TC toxicity).

      3.            The waste is listed in 1 or 2 above and is not excluded by any provisions under the Resource Conservation and Recovery Act.

      A waste is considered an acute hazardous waste if it is identified in 40 CFR Part 261.31, 261.32 or 261.33 (e) as an acute hazardous waste.

      Laboratories 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:

1.            Conditionally Exempt Small Quantity Generator

A generator who generates no more than 100 kilograms of hazardous waste or 1 kilogram of acute hazardous waste in a calendar month and accumulates no greater than 1000 kilograms of hazardous wastes (40 CFR Part 261.5).

2.            Small Quantity Generator

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

3.            Full Generator

A generator who generates hazardous 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).

      It is the responsibility of the laboratory to know which category their organization falls under.  Since most laboratories will fall into the conditionally exempt small quantity generator category these disposal requirements are listed below.

      Facilities falling into the small quantity generator and full generator categories must adhere to all regulations pertaining to waste, transport, storage and disposal in the Resource Conservation and Recovery Act.

      Conditionally exempt small quantity generators must dispose of hazardous waste in an on-site facility or ensure delivery to a treatment, storage or disposal facility, which is:

      1.      Permitted under 40 CFR Part 270;

      2.   In interim status under 40 CFR Parts 270 & 265;

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

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

6.3.1            General Disposal/Treatment Considerations

      1.      Hazardous waste solvents, as identified in the 40 CFR Part 261 may not be evaporated off in a fume hood.  Solvents evaporated off during the extraction/testing process are exempt.

      2.   Acidic & 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).

      3.   Heavy metals may be precipitated out and the liquid portion disposed of via the sanitary sewer*.  (*subject to local regulations).

6.3.2            Storage and Accumulation

      Hazardous waste storage is limited to quantity and/or accumulation time and must comply with RCRA regulations as specified in the 40 CFR.  These wastes should be packaged and separated according to compatible groups (e.g. solvents, acids, etc.)

6.3.3     Sample Disposal

      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, are being analyzed, are being held for analysis or are being maintained in custody for legal reasons.  However, once a decision is made to dispose of laboratory samples, the exclusion provisions of 40 CFR Part 261.4(d) no longer apply.  Samples that have been identified as hazardous may either be:  1) returned to the generator; or 2) disposed of according to applicable RCRA regulations summarized in this document.  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.

      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.