Tri-State Laboratories, Inc

Cardinal Laboratories, LLC Standard Operating Procedure

Procedure No.: 2020 Revision Date: 09/05

Subject: (EPA Method 160.2) Total Suspended Solids (TSS):

Revision #/Date: Approved By: Date:

Procedure 2020 Revised 09/05 Total Suspended Solids (TSS) EPA Method: 160.2 Scope and Application

This method determines non-filterable residue in drinking, surface, and saline waters; domestic and industrial wastes.

Matrix

Aqueous

Description

This method is used to determine the amount of non-filterable materials contained in aqueous samples. This method is applicable to samples with greater than 4 mg/L total suspended solids.

Definitions

Residue, non-filterable, is defined as those solids, which are retained by a glass fiber filter and dried to a constant weight at 103-105°C.

Method Blank: aliquot of reagent water treated exactly as a sample including exposure to all glassware, equipment, solvents, reagents, internal standards, and surrogates used. Used to determine if interferences or analytes are present in the lab environment.

Duplicate Sample: sample analyzed second time exactly the same way as the first analysis. Used to calculate precision expressed as Relative Percent Difference (RPD).

Matrix Spike (MS) and Matrix Spike Duplicate (MSD): aliquots of sample to which known quantities of the analyte of interest is added in the laboratory. The MS and MSD are prepared and analyzed exactly as a field sample. The purpose is to quantify any bias or imprecision caused by the sample matrix. The background concentrations of the analyte(s) in the sample matrix must be determined in a separate aliquot and the measured values in the MS and MSD corrected for background concentrations.

QCS Quality Control Sample: A sample containing analyte(s) of interest at known concentrations. The QCS is obtained from a source different than the calibration standards. Purpose is to check performance using materials prepared independently from normal preparation procedures.

Precautions

Standard laboratory practices must be followed (see procedure 0010)

Sample Preservation

Procedure 2020 Revised 09/05 Samples may be collected in either glass or plastic containers. Samples to be analyzed for TSS are unpreserved and cooled to 4°C. Samples must be analyzed within seven (7) days of sampling.

Interferences

Waters with a significant concentration of calcium, Magnesium, Chloride and/or Sulfate may be hygroscopic & require prolonged drying, proper desiccation & rapid weighing. Excessive residue on the filter may form a water entrapping crust. The sample size should be limited to a volume that yields no more than 200 mg residue. For samples high in dissolved solids, rinse the filter thoroughly to ensure removal of the dissolved material prolonged filtration times resulting from clogging of the filter may produce results that are high, because increased colloidal materials are captured on the clogged filter.

Sample Preservation

Preservation of this sample is not practical; analysis should begin as soon as possible. Refrigeration or icing to 4°C, to minimize microbiological decomposition of solid, is recommended.

Apparatus

- Glass fiber filters (Pre-weighed) - Vacuum flask - Vacuum funnel and support - Vacuum pump - Drying oven, set at 103° - 105°C - Desiccator - Analytical balance - 500 mL Graduated cylinder

Reagents

- Kaolin

- Potassium Bromide (KBr)

- Standard:

Into a 1 liter volumetric flask, add 900ml ultra pure water. Add 5g of Kaolin and 50g of potassium bromide. Kaolin must be moistened with ultra pure water before transfer to avoid weight loss. Bring to volume using ultra pure water. TSS = 50mg/10ml of standard. Procedure

1.0 Filter Preparation

1.1 Filters used for this procedure are factory rinsed and weighed. No addition preparation is required.

Procedure 2020 Revised 09/05 2.0 Sample Preparation

2.1 Record initial weight and serial number of each filter paper used. Label filter tray with laboratory number of the sample to be filtered.

2.2 Assemble filtration apparatus.

2.3 Determine an appropriate sample volume to be filtered, usually 500mls. For samples with a high concentration of suspended material, reduce the sample size so that the residue weighs no more than 200 mg.

2.4 Transfer sample, after mixing, to a graduated cylinder to selected volume.

2.5 Turn on vacuum pump and wet filter with approximately 10ml ultra pure water.

2.6 Begin to transfer sample from the flask. Do not allow filter to go dry during this transfer.

2.7 Rinse volumetric flask with approximately 10ml ultra pure water. Allow filter vacuum to dry disk for 1-2 minutes.

2.8 Remove filter from support, place in labeled filter tin. Place tin and filter in drying oven for at least 1 hour. Remove to desiccator to cool.

2.9 After sufficient drying and cooling time, reweigh the filter and record weight in notebook. Return filter to desiccator.

2.10 Reweigh filter and record weight in notebook, continue reweighing until a stable weight is shown. ( ± 4% or ± 1.0mg )

Calculation

mg/L Total Suspended Solids (TSS) = (A-B) X 1000 C Where: A = Final weight of filter in grams B = Tare weight of filter in grams C = Volume of sample in liters

Report results <100 mg/L to 2 significant figures. Example; 56.7 mg/L would be reported as 57 mg/L. Report results >100 mg/L to 3 significant figures. Example; 123.4 mg/L sould be 123 mg/L.

Pollution Prevention/Waste Disposal

Dispose of used filters in solid waste drum. The filtrate should be disposed of down the drain with running water.

Procedure 2020 Revised 09/05 Quality Control

* Each analytical batch analyzed for TSS must be accompanied by a method blank consisting of 1000ml ultra pure water and a standard of 50mg Kaolin.

* All weights, volumes, comments etc. for each batch must be entered in notebook form for data review.

* Every tenth sample shall be run in duplicate and %RPD calculated . Every fifteenth sample shall be run as a duplicate spike and % recoveries and % RPD calculated. (see procedure 0110 for calculations).

* Required recoveries for duplicates and Spike duplicates shall be determined using historical data. The current acceptable limits for these parameters are listed in procedure 0120.

* Failure to meet quality control acceptable limits requires corrective action (see procedure 0150).

Method Performance

See QAPP section 5.2 Aqueous Precision = 20%, Aqueous Accuracy = 93-108%

References

Methods for Chemical Analysis of Water and Wastes EPA 600/4-79-020 March 1983 Method 160.2 pp. 160.2 - 1 through 160.2 - 2

Standard Methods for The Examination of Water and Waste Water 18th Edition 1992 Method 2540D pp. 2-56

National Environmental Methods Index. April 1994. Method 160.2. 5 April 2004.

Procedure 2020 Revised 09/05