EPA-821-R-01-015
                                  January 2001
            METHOD 1684

    Total, Fixed, and Volatile Solids
     in Water, Solids, and Biosolids
                 Draft

             January 2001
 U.S. Environmental Protection Agency
            Office of Water
   Office of Science and Technology
Engineering and Analysis Division (4303)
      1200 Pennsylvania Ave. NW
        Washington, DC 20460

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 Method 1684
                                  Acknowledgments

This method was prepared under the direction of William A. Telliard of the U.S. Environmental Protection
Agency's (EPA's) Office of Water (OW), Engineering and Analysis Division (EAD). The method was
prepared under EPA Contract 68-C-98-139 by DynCorp with assistance from Quality Works, Inc.
                                        Disclaimer

This draft method has been reviewed and approved for publication by the Analytical Methods Staff within
the Engineering and Analysis Division of the U.S. Environmental Protection Agency.  Mention of trade
names or commercial products does not constitute endorsement or recommendation for use. EPA plans
further validation of this draft method. The method may be revised following validation to reflect results of
the study.  This method version contains minor editorial changes to the February 1999 version.

EPA welcomes suggestions for improvement of this method.  Suggestions and questions concerning this
method or its application should be addressed to:

William A. Telliard
USEPA Office of Water
Analytical Methods Staff
Mail Code 4303
1200 Pennsylvania Ave., NW
Washington, DC 20460
Phone: 202/260-7134
Fax: 202/260-7185
Requests for additional copies of this publication should be directed to:

Water Resource Center
Mail Code RC-4100
1200 Pennsylvania Ave., NW
Washington, DC 20460
(202) 260-7786 or (202) 260-2814
                                                                               Draft-January 2001

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                                                                                      Method 1684
  Note: This method is performance based. The laboratory is permitted to modify or omit any steps or
  procedure, provided that all performance requirements in this method are met. The laboratory may not
  omit any quality control analyses. The terms "shall", "must", and "may not" indicate steps and
  procedures required for producing reliable results. The terms "should" and "may" indicate optional
  steps that may be modified or omitted if the laboratory can demonstrate that the modified method
  produces results equivalent or superior to results produced by this method.
Draft-January 2001

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                                                                                 Method 1684
                                      Method 1684

     Total, Fixed, and Volatile Solids in Water, Solids, and Biosolids

1.0   Scope and Application

1.1    This method is applicable to the determination of total solids and the fixed and volatile fractions in
       such solid and semisolid  samples as soils, sediments, biosolids (municipal sewage sludge), sludge
       separated from water and wastewater treatment processes, and sludge cakes from vacuum
       filtration, centrifugation,  or other sludge dewatering processes.

1.2    This method is for use in the United States Environmental Protection Agency's (EPA's) data
       gathering and monitoring programs under the Clean Water Act, the Resource Conservation and
       Recovery Act, the Comprehensive Environmental Response, Compensation, and Liability Act, and
       the Safe Drinking Water Act.

1.3    Method detection limits (MDLs) and minimum levels (MLs) have not been formally established for
       this draft method. These values will be determined during the validation studies.

1.4    This method is performance based. The laboratory is permitted to omit any step or modify any
       procedure (e.g. to overcome interferences, to lower the cost of measurement), provided that all
       performance requirements in this method are met. Requirements for establishing method
       equivalency are given in  Section 9.1.2.

1.5    Each laboratory that uses this method must demonstrate the ability to generate acceptable results
       using the procedure in Section 9.2.

2.0   Summary of Method

2.1    Sample aliquots of 25-50 g are dried at 103 °C to 105 °C to drive off water in the sample.

2.2    The residue from Section 2.1 is cooled, weighed, and dried again at 550°C to drive off volatile
       solids in the sample.

2.3    The total, fixed, and volatile solids are determined by comparing the mass of the sample before and
       after each drying step.

3.0   Definitions

       Definitions for terms used in this method are given in the glossary at the end of the method (Section
       18).

4.0   Interferences

4.1    Sampling, subsampling, and pipetting multi-phase samples may introduce serious errors.  Make
       and keep such samples homogeneous during transfer. Use special handling to ensure sample
       integrity when subsampling. Mix small samples with a magnetic stirrer.  If visible suspended


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 Method 1684
        solids are present, pipette with wide-bore pipettes. If part of a sample adheres to the sample
        container, intensive homogenization is required to ensure accurate results. When dried, some
        samples form a crust that prevents evaporation; special handling such as extended drying times are
        required to deal with this.  Avoid using a magnetic stirrer with samples containing magnetic
        particles.

4.2     The temperature and time of residue drying has an important bearing on results. Problems such as
        weight losses due to volatilization of organic matter, and evolution of gases from heat-induced
        chemical decomposition, weight gains due to oxidation, and confounding factors like mechanical
        occlusion of water and water of crystallization depend on temperature and time of heating. It is
        therefore essential that samples be dried  at a uniform temperature, and for no longer than specified
        in the method. Each sample requires close attention to desiccation after drying.  Minimize the time
        the desiccator is open because moist air may enter and be absorbed by the samples.  Some samples
        may be stronger desiccants than those used in the desiccator and may take on water. If uptake of
        water by a sample is suspected, the operator should weigh the sample to  see if it gains weight while
        in the desiccator. If the sludge is indeed taking on water, then a vacuum desiccator  should be used.
4.3    Residues dried at 103 °C to 105 °C may retain some bound water as water of crystallization or as
       water occluded in the interstices of crystals. The residues also lose CO2 in the conversion of
       bicarbonate to carbonate. The residues usually lose only slight amounts of organic matter by
       volatilization at this temperature. Because removal of occluded water is marginal at this
       temperature, attainment of constant weight may be very slow.

4.4    Results for residues high in oil or grease may be questionable because of the difficulty of drying to
       constant weight in a reasonable time.

4.5    The determination of both total and volatile solids is subject to negative error due to loss of
       ammonium carbonate and volatile organic matter during the drying step at 103 °C to 105 °C.
       Carefully observe specified drying time and temperature to control losses of volatile inorganic salts
       if these are a problem.

5.0   Safety

5.1    This method does not address all safety issues associated with its use.  The toxicity or
       carcinogenicity of reagents used in this method have not been fully established.  Each chemical and
       environmental sample should be regarded as a potential health hazard and exposure should be
       minimized.  The laboratory is responsible for maintaining a safe work environment and a current
       awareness file of OSHA regulations regarding the safe handling of the chemicals  specified in this
       method. A  reference file of material safety data sheets (MSDSs) should be available to all
       personnel involved in these analyses. Additional information on laboratory safety can be  found in
       References 5-7.

5.2    All personnel handling environmental samples known to contain or to have been in contact with
       human waste should be immunized against known disease causative agents.
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                                                                                    Method 1684
6.0   Equipment and Supplies
       NOTE: Brand names, suppliers, and part numbers are cited for illustrative purposes only.  No
       endorsement is implied. Equivalent performance may be achieved using equipment and
       materials other than those specified here, but demonstration of equivalent performance that
	meets the requirements of this method is the responsibility of the laboratory.	

6.1    Evaporating dishes-Dishes of 100-mL capacity. The dishes may be made of porcelain (90-mm
       diameter), platinum, or high-silica glass.

6.2    Watch glass-Capable of covering the  evaporating dishes (Section 6.1).

6.3    Muffle furnace-Capable of maintaining a uniform temperature of 5 5 0 ° C throughout the drying
       chamber.

6.4    Steam bath for evaporation of liquid samples.

6.5    Desiccator-Moisture concentration in the desiccator should be monitored by an instrumental
       indicator or with a color-indicator desiccant.

6.6    Drying oven-Thermostatically-controlled, capable of maintaining a uniform temperature of 103 °C
       to 105 °C throughout the drying chamber.

6.7    Analytical balance-Capable of weighing to 0.1 mg for samples having a mass up to 200 g.

6.8    Reference weights-2 mg, 1000 mg, and 50g class "S" weights.

6.9    Container handling apparatus-Gloves, tongs, or a suitable holder for moving and handling hot
       containers after drying.

6.10  Sample handling apparatus-Spatulas, spoonulas, funnels, or other equipment for transfer and
       manipulation of sample.

6.11  Bottles-Glass or plastic bottles of a suitable size for sample collection.

6.12  Rubber gloves (Optional)

6.13  No. 7 Cork borer (Optional)

6.14  Dessicant (Optional)

7.0    Reagents and Standards

7.1    Reagent water-Deionized, distilled, or otherwise purified water.

7.2    Quality control spiking solution- If a  commercially available standard can be purchased that
       contains standard fixed and volatile solids, the laboratory may use that standard.  The laboratory
       may also prepare a spiking solution.  One possible recipe is given below for a NaCl-KHP solution.

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 Method 1684
       7.2.1   Dissolve 0.10 g sodium chloride (NaCl) in 500 mL reagent water. Mix to dissolve.

       7.2.2  Add 0.10 g potassium hydrogen phthalate (KHP) to the NaCl solution (Section 7.2.1) and
               mix. If the KHP does not dissolve readily, warm the solution while mixing. Dilute to 1 L
               with reagent water. Store at 4°C.  Assuming 100% volatility of the acid phthalate ion, this
               solution contains 200 mg/L total solids, 81.0 mg/L volatile solids, and 119 mg/L fixed
               solids.

8.0   Sample  Collection, Preservation,  and  Storage

8.1    Use resistant-glass or plastic bottles to collect sample for solids analysis, provided that the material
       in suspension does not adhere to container walls. Sampling should be done in accordance with
       Reference 16.10. Begin analysis as soon as possible after collection because of the impracticality
       of preserving the sample.  Refrigerate sample at 4 °C up to the time of analysis to minimize
       microbiological decomposition of solids. Preferably do not hold samples more than 24 hours.
       Under no circumstances should the sample be held more than seven days.  Bring samples to room
       temperature before analysis.

9.0   Quality Control

9.1    Each laboratory using this method is required to operate  a formal quality control (QC) program.
       The minimum requirements of this program consist of an initial demonstration of laboratory
       capability, and the ongoing analysis of laboratory reagent blanks, precision and recovery
       standards, and matrix-spiked samples as a continuing check on performance.  The laboratory is
       required to maintain performance records that define the  quality of data thus generated.
       Laboratory performance is compared to established performance criteria to determine if the results
       of analyses meet the performance characteristics of the method.

       9.1.1   The analyst shall make an initial demonstration of the ability to generate acceptable
               accuracy and precision with this method.  This ability is established as described in
               Section 9.2.

       9.1.2  In recognition of advances that are occurring in analytical technology, the analyst is
               permitted certain options to improve separations  or lower the costs of measurements,
               provided that all performance specifications are met. If an analytical technique other than
               the techniques specified in this method is used, that technique must have a specificity equal
               to or better than the specificity of the techniques  in this method for total, fixed, and volatile
               solids in the sample of interest.  Specificity is defined as producing results equivalent to the
               results produced by this method for laboratory-prepared solutions (Section 7.2) that meet
               all of the QC criteria stated in this method.

               9.1.2.1       Each time a modification is made to this method, the  analyst is required to
                             repeat the Initial Precision and Recovery (IPR) test in Section 9.2.2 to
                             demonstrate that the modification produces results equivalent to or better
                             than results produced by this method. If the detection limit of the method
                             will be affected by the modification, the analyst must demonstrate that the
                             MDL (40 CFR part 136, appendix B) is less than or equal to the MDL in
                             this method or one-third the regulatory compliance level, whichever is
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                                                                                       Method 1684
                              higher.  The tests required for this equivalency demonstration are given in
                              Section 9.2.

               9.1.2.2       The laboratory is required to maintain records of modifications made to
                              this method. These records include the following, at a minimum:

                       9.1.2.2.1      The names, titles, addresses, and telephone numbers of the
                                      analyst(s) who performed the analyses and modification, and of
                                      the quality control officer who witnessed and will verify the
                                      analyses and modification.

                       9.1.2.2.2      A listing of pollutant(s) measured (total, fixed, and volatile
                                      solids).

                       9.1.2.2.3      A narrative stating reason(s) for the modification.

                       9.1.2.2.4      Results from all quality control (QC) tests comparing the
                                      modified method to this method, including:

                                      (a)     Initial precision and recovery (Section 9.2.2).
                                      (b)     Analysis of blanks (Section 9.3).
                                      (c)     Accuracy assessment (Section 9.5).
                                      (d)     Ongoing precision and recovery (Section 9.4).

                       9.1.2.2.5      Data that will allow an independent reviewer to validate each
                                      determination by tracing  the instrument output (weight,
                                      absorbance, or other signal) to the final result. These data are to
                                      include:
                                      (a)     Sample numbers and other identifiers.
                                      (b)     Sample preparation dates.
                                      (c)     Analysis dates and times.
                                      (d)     Analysis sequence/run chronology.
                                      (e)     Sample weights.
                                      (f)     Make and model of analytical balance and weights
                                             traceable to NIST.
                                      (g)     Copies of logbooks, printer tapes, and other recordings of
                                             raw data.
                                      (h)     Data system outputs, and other data to link the raw data
                                             to the results reported.

        9.1.3  Analyses of laboratory blanks are required to demonstrate freedom from contamination.
               The procedure and criteria for blank analyses are  described in Section 9.3.

        9.1.4  Analyses of ongoing precision and recovery (OPR) samples are required to demonstrate
               that the sample preparation and analysis are in control. The procedure and criteria for
               OPR samples are described in Section 9.4.

9.2     Initial demonstration of laboratory capability - The initial  demonstration of laboratory capability is
        used to characterize laboratory performance and method detection limits.

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 Method 1684
        9.2.1  Method detection limit (MDL) - The method detection limit must be established for the
               analyte, using the QC spiking solution (Section 7.2). To determine MDL values, take
               seven replicate aliquots of the diluted QC spiking solution and process each aliquot
               through each step of the analytical method.  Perform all calculations and report the
               concentration values in the appropriate units. MDLs should be determined every year or
               whenever a modification to the method or analytical system is made that will affect the
               method detection limit.

        9.2.2  Initial Precision and Recovery (IPR) - To establish the ability to generate acceptable preci-
               sion and accuracy, the analyst shall perform the following operations:

               9.2.2.1        Prepare four samples by diluting the QC spiking solution (Section 7.2) to
                               1-5 times the ML. Using the procedures in Section 11, analyze these
                              samples for total, fixed, and volatile solids.

               9.2.2.2       Using the results of the four analyses, compute the average percent recov-
                              ery (x) and the standard deviation (s, Equation 1) of the percent recovery
                              for total, fixed, and volatile solids.

                                            Equation 1
                                    .=
                                                 n-
               Where:
                       n = number of samples
                       x = % recovery in each sample
                       s = standard deviation
               9.2.2.3       Compare s and x with the corresponding limits for initial precision and
                              recovery in Table 1.  If s and x meet the acceptance criteria, system
                              performance is acceptable and analysis of samples may begin. If,
                              however, s exceeds the precision limit or x falls outside the range for
                              recovery, system performance is unacceptable. In this event, correct the
                              problem, and repeat the test.

9.3    Laboratory blanks

       9.3.1  Prepare and analyze a laboratory blank initially (i.e. with the tests in Section 9.2) and with
               each analytical batch. The blank must be subjected to the same procedural steps as a
               sample, and will consist of approximately 25 g of reagent water.

       9.3.2  If material is detected in the blank at a concentration greater than the MDL (Section 1.3),
               analysis of samples must be halted until the source of contamination is eliminated and a
               new blank shows no evidence of contamination.  All samples must be associated with an
               uncontaminated laboratory blank before the results may be reported for regulatory compli-
               ance purposes. Sample results are also acceptable for regulatory compliance purposes if

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                                                                                     Method 1684
               they are associated with a blank that contains less than 1/10 the concentration of the
               analyte(s) of interest in the associated samples.

9.4    Ongoing Precision and Recovery (OPR).

       9.4.1   Prepare an OPR solution identical to the IPR solution described in Section 9.2.2.1.

       9.4.2   An aliquot of the OPR solution must be analyzed with each preparation batch (samples of
               the same matrix started through the sample preparation process (Section 11) on the same
               12-hour shift, to a maximum of 10 samples).

       9.4.3   Compute the percent recovery of total, fixed, and volatile solids in the OPR sample.

       9.4.4   For each analyte, compare the results to the limits for ongoing recovery in Table 1. If all
               analytes meet the acceptance criteria, system performance is acceptable and analysis of
               blanks and samples may proceed. If, however, the recovery of an analyte falls outside of
               the range given, the analytical processes are not being performed properly for that analyte.
               Correct the problem, reprepare the sample batch, and repeat the OPR test. All samples
               must be associated with an OPR analysis that passes acceptance criteria before the sample
               results can be reported for regulatory compliance purposes.

       9.4.5   Add results that pass the specifications in Section 9.4.4 to IPR and previous OPR data.
               Update QC charts to form a graphic representation of continued laboratory performance.
               Develop a statement of laboratory accuracy for each analyte by calculating the average
               percent recovery (R) and the standard deviation of percent recovery (SR). Express the
               accuracy as a recovery interval from R-2SR to R+2SR. For example, if R=95% and
               SR=5%, the accuracy is 85-105%.

9.5    Duplicate analyses

       9.5.1   Ten percent of samples must be analyzed in duplicate. The duplicate analyses must be
               performed within the same sample batch (samples whose analysis is started within the
               same 12-hour period).

       9.5.2   The results of duplicate samples analyzed for total, fixed, and volatile solids must be
               within 10% of the solids determination.

10.0  Calibration and Standardization

10.1   Calibrate the analytical balance at 2 mg and 1000 mg using class "S" weights.

10.2   Calibration shall be within ± 10% (i.e. ±0.2 mg) at 2 mg and ± 0.5% (i.e. ±5 mg) at 1000 mg. If
       values  are not within these limits, recalibrate the balance.

10.3   Place a 50 g weight and a 2 mg on the balance. Verify that the balance reads 50.002  ±10  %
       (i.e. ± 0.2 mg).
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 Method 1684
11.0   Procedure

11.1    Total Solids

        11.1.1 Preparation of evaporating dishes-If volatile solids are to be measured, ignite clean
               evaporating dishes and watch glasses at 550°C for 1 hour in a muffle furnace.  If only
               total solids are to be measured, heat dishes and watch glasses at 103 °C to 105 °C for  1
               hour in an oven.  Cool and store the dried equipment in a desiccator. Weigh each dish and
               watch glass prior to use (record combined weight as "Wdlsh").

        11.1.2 Preparation of samples.

               11.1.2.1       Fluid samples-If the sample contains enough moisture to flow readily, stir
                              to homogenize, place a 25 to 50 g sample aliquot on a prepared
                              evaporating dish. If the sample is to be  analyzed in duplicate, the mass of
                              the two aliquots may not differ by more than 10%.  Cover each sample
                              with a watch glass, and weigh to the nearest 0.01 g (record weight as
                              "Wsample"). Spread each sample so that it is evenly distributed over the
                              evaporating dish. Evaporate the  samples to dryness on a steam bath.

        NOTE:  Weigh wet samples  quickly because wet samples tend to lose weight by evaporation.
	Samples should be weighed immediately after aliquots are prepared.	


               11.1.2.2      Solid samples-If the sample consists of discrete pieces of solid material
                              (dewatered sludge, for example), take cores from each piece with a No. 7
                              cork borer or pulverize the entire sample coarsely on a clean surface by
                              hand, using rubber gloves. Place a 25 to 50 g aliquot of the pulverized
                              sample on a prepared evaporating dish.  If the sample is to be analyzed in
                              duplicate, the mass of the two aliquots may not differ by more than 10%.
                              Cover each  sample with a watch glass, and weigh (record weight as
                              "Wsample"). Spread each sample so that it is evenly distributed over the
                              evaporating dish.

        11.1.3 Dry the samples at  103 °C to 105 °C for 12 hours, minimum, cool to balance temperature
               in an individual  desiccator containing fresh desiccant, and weigh.

        NOTE: It is imperative that dried samples be weighed quickly since residues often are very
        hygroscopic and rapidly absorb moisture from the air. Samples must remain in the dessicator
	until the analyst is ready to weigh them.	

        11.1.4 Heat the residue for 1 hour, cool it to balance temperature in a desiccator, and weigh.
               Repeat this heating, cooling, desiccating, and weighing procedure until the weight change
               is less than 4% or 50 mg, whichever is less. Record the final weight as "Wtotal."

11.2    Fixed and volatile solids.

        11.2.1 Transfer the evaporating dishes containing the dried residues (Section 11.1.4) to a cool
               muffle furnace. Heat the furnace to 550°C and ignite it for 2 hours.
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                                                                                     Method 1684
       NOTE: If the residue contains large amounts of organic matter, first ignite it over a gas
       burner and under an exhaust hood in the presence of adequate air to lessen losses due to
	reducing conditions and to avoid odors in the laboratory.	

       11.2.2 Cool the residue in a desiccator to balance the temperature. Weigh the residues. Repeat
               igniting (30 min), cooling, desiccating, and weighing steps until the weight change is less
               than 4% or 50 mg, whichever is less.  Record the final weight as "Wvolatlle."

12.0  Data Analysis  and Calculations

12.1   Calculate the % solids or the mg solids/kg sludge for total solids (Equation 2), fixed solids,
       (Equation 3), and volatile solids (Equation 4).

                                           Equation 2
                              % total solids = —^	— * 100
                                            "sample ~ "dish
                              or
                              mg total solids   W. ., - W,.,
                                 ,—71,	= u      u   * 1,000,000
                                kg sludge     Wsample - Wdish

                      Where:
                              Wdlsh=Weightofdish (mg)
                              Wsample=Weight of wet sample and dish  (mg)
                      	Wtotai=Weight of dried residue and dish (mg)
                     Equation 3


                      W    -W
    % fixed solids =   vo atl e	^— *
                      "total ~ "dish
    or
    mg fixed solids _ Wvolatlle - Wdlsh
        kg sludge       Wtotal-Wdlsh

Where:
                                                           * 1,000,000
                              Wdish=Weightofdish (mg)
                              Wtotal=Weight of dried residue and dish (mg)
                              Wvolatile=Weight of residue and dish after ignition (mg)
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 Method 1684
                                           Equation 4

                                             W, ,-W,  .,
                            % volatile solids = -^	v-2^ * 100
                                              vv   — vv
                                              "'total  "'dish
                            or
                            mg volatile solids _ Wtotal - Wvolatile ^
                                kg sludge       Wtotal - Wdish
                      Where:
                              Wdlsh=Weightofdish (mg)
                              Wtotal=Weight of dried residue and dish (mg)
	Wvoiatile=Weight of residue and dish after ignition (mg)	

12.2  Sample results should be reported as % solids or mg/kg to three significant figures. Report results
       below the ML as < ML,  or as required by the permitting authority or in the permit. Duplicate
       determinations must agree within 10% of their average.

13.0  Method Performance

13.1  Method performance (MDL and quality control acceptance criteria) will be determined during the
       multi-lab validation of this method.

13.2  Total, fixed, and volatile solids duplicate determinations must agree within 10% to be reported for
       permitting purposes.  If duplicate samples do not meet this criteria, the problem must be discovered
       and the sample must be run over.

14.0  Pollution Prevention

14.1  Pollution prevention encompasses any technique that reduces or eliminates the quantity or toxicity
       of waste at the point of generation. Numerous opportunities for pollution prevention exist in
       laboratory operation. The Environmental Protection Agency has established a preferred hierarchy
       of environmental management techniques that places pollution prevention as the management
       option of first choice. Whenever feasible, laboratory personnel should use pollution prevention
       techniques to address their waste generation.  When wastes cannot be feasibly reduced at the
       source, the Agency recommends recycling as the next best option.

14.2  For information about pollution prevention that may be applicable to laboratories and research
       institutions, consult "Less is Better:  Laboratory Chemical Management for Waste Reduction",
       available from the American Chemical Society's Department of Government Relations and Science
       Policy, 1155 16th Street N.W., Washington D.C. 20036, (202)872-4477.

15.0  Waste  Management

15.1  The Environmental Protection Agency requires that laboratory waste management practices
       conducted be consistent with all applicable rules and regulations. The Agency urges laboratories
       to protect the air, water, and land by minimizing and controlling all releases from hoods and bench

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                                                                                  Method 1684
       operations, complying with the letter and spirit of any sewer discharge permits and regulations, and
       by complying with all solid and hazardous waste regulations, particularly the hazardous waste
       identification rules and land disposal restrictions. For further information on waste management
       consult "The Waste Management Manual for Laboratory Personnel", available from the American
       Chemical Society at the address listed in the Section 14.2.

16.0  References

16.1   Goodman, B.L. 1964. Processing thickened sludge with chemical conditioners.  Pages 78 et seq. in
       Sludge Concentration, Filtration and Incineration. Univ. Michigan Continued Education Ser. No.
       113, Ann Arbor.

16.2   Gratteau, J.C. & R.I. Dick. 1968. Activated sludge suspended solids determinations.  Water
       Sewage Works 115:468.

16.3   Theriault, E.J. & H.H. Wagenhals.  1923.  Studies of representative sewage plants. Pub. Health
       Bulletin. No. 132.

16.4   U.S. Environmental Protection Agency, 1979. Methods for Chemical Analysis of Water and
       Wastes. Publ. 600/4-79-020, rev. March 1983.  Environmental Monitoring and Support Lab., U.S.
       Environmental Protection Agency, Cincinnati, Ohio.

16.5   "OSHA Safety and Health Standards, General Industry", (29CFR 1910), Occupational Safety and
       Health Administration, OSHA 2206, revised January, 1976.

16.6   "Safety in Academic Chemistry Laboratories", American Chemical Society Publication,
       Committee on Chemical Safety, 3rd Edition,  1979.

16.7   "Standard Methods for the Examination of Water and Wastewater,"  18th ed. and later revisions,
       American Public Health Association, 1015 15th Street NW, Washington, DC 20005.  1-35:
       Section 1090 (Safety), 1992.

16.8   U.S. Environmental Protection Agency, 1992. Control of Pathogens and Vector Attraction in
       Sewage Sludge. Publ 625/R-92/013. Office of Research and Development, Washington, DC.

16.9   "Handbook of Analytical Quality Control in Water and Wastewater Laboratories," USEPA,
       EMSL-Ci, Cincinnati, OH 45268,  EPA-600/4-79-019, March 1979.

16.10 "Environmental Regulations and Technology: Control of Pathogens and Vector Attraction in
       Biosolid, " 1992. EPA/625/R-92/013. Office of Research and Development. USEPA.

17.0  Tables, Diagrams, Flowcharts, and Validation Data

17.1   Table 1 - Quality Control Acceptance Criteria for Method 1684.
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Method 1684
18.0  Definitions

18.1   Analytical batch-The set of samples analyzed at the same time, to a maximum of 10 samples.
       Each analytical batch of 10 or fewer samples must be accompanied by a laboratory blank (Section
       9.3), an ongoing precision and recovery sample (OPR, Section 9.6), and a set of duplicate samples,
       resulting in a minimum of five analyses (1 sample, 1 blank, 1 OPR, 2 duplicates) and a maximum
       of 14 analyses.

18.2   Fixed solids-The residue left in the vessel after a sample is ignited (heated to dryness at 550°C).

18.3   Initial precision and recovery (IPR)-Four aliquots of the diluted PAR analyzed to establish the
       ability to generate acceptable precision and accuracy. An IPR is performed the first time this
       method is used and any time the method or instrumentation is modified.

18.4   IPR-See initial precision and recovery.

18.5   Laboratory blank (method blank)-An aliquot of reagent water that is treated exactly as a sample
       including exposure to all glassware, equipment and reagents that are used with samples.  The
       laboratory blank is used to determine if analytes or interferences are present in the laboratory
       environment, the reagents, or the apparatus.

18.6   Laboratory control sample (LCS)-See Ongoing precision and recovery standard (OPR).

18.7   May-This action, activity, or procedural step is neither required nor prohibited.

18.8   May not-This action, activity, or procedural step is prohibited.

18.9   Method detection limit (MDL)-The lowest level at which an analyte can be detected with 99 %
       confidence that the analyte concentration is greater than zero.

18.10 Must-This action, activity, or procedural step is required.

18.11 Ongoing precision and recovery standard (OPR, also called a laboratory control  sample)-A
       laboratory blank spiked with known quantities of analytes. The OPR is analyzed exactly like a
       sample. Its purpose is to assure that the results produced by the laboratory remain within the
       limits specified in this method for precision and accuracy.

18.12 OPR-See Ongoing precision and recovery standard.

18.13 PAR-See Precision and recovery standard.

18.14 Precision and recovery standard-Secondary standard that is diluted and spiked to form the IPR and
       OPR.

18.15 Quality control sample (QCS):-A sediment sample containing analytes of interest at known
       concentrations. The QCS  is obtained from a source external to the laboratory or is prepared from
       standards obtained from a different source than the calibration standards. The purpose is to check
       laboratory performance using test materials that have been prepared independently from the normal
       preparation process.

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                                                                                        Method 1684
18.16  Reagent Water- Water that should be free of substances that interfere with analytical methods.


18.17  Sediment sample-A fluvial, sand and/or humic sample matrix exposed to a marine, brackish or
        fresh water environment.  It is limited by this method to that portion which may be passed through
        a number 10 sieve or a 2 mm mesh sieve.

18.18  Shall-This action, activity or procedural step is required.

18.19  Should-This action, activity, or procedural step is suggested but not required.

18.20  Total solids-The residue left in the vessel after evaporation of liquid from a sample and subsequent
        drying in an oven at 103°C to 105 °C.

18.21  Volatile solids-The weight loss after a sample is ignited (heated to dryness at 550°C).
        Determinations of fixed and volatile solids do not distinguish precisely between inorganic and
        organic matter because the loss on ignition is not confined to organic matter. It includes losses due
        to decomposition or volatilization of some mineral salts.
Table 1 - Quality Control Acceptance Criteria for Method 16841
Analyte

total solids
fixed solids
volatile solids
MDL

3mg/L
7mg/L
7mg/L
IPR
X
85-110%
75-110%
75-110%
s
10%Rsd
20% Rsd
30% Rsd
OPR
X
80-110%
70-110%
70-110%
1 Performance criteria are initial estimates. These estimates serve as data quality objectives for the single laboratory validation
of this method.
Draft-January 2001
13

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