U.S. Fish & Wildlife Service Emblem
U.S. Fish & Wildlife Service
Analytical Control Facility
A Branch of Ecological Services

Contents:
Who We Are
Services We Provide
Staff & Who to
Contact
Contract
Laboratories
How we assign Labs
Quality Control
Inorganic Lab
Statement of Work
Organic Lab
Statement of Work
Catalog Information
Pricing Guides
Analytical Methods
Contaminant Database

How to Use the Pricing Guides

 
Home
 
Links:
DOI Home Page
USFWS Home Page
DEQ Home Page
Contact us at: chemistry@fws.gov
Privacy & Disclaimer
FOIA
 

Laboratory and Environmental Testing, Inc. (LET) Laboratory Methods

Method Code

Method Title

001

Homogenization

002

L9 - Freeze drying and % Moisture

003

L1 - HNO3/HClO4 Digestion with HCl

004

L2 - HNO3 Digestion

005

L3 - Digestion for Mercury

006

L4 - HNO3/HClO4 Digestion

007

L5 - Magnesium Dry Ash

008

L6 - HNO3/H2O2 Digestion

009

L10 - Microwave Digestion

010

PARTICLE SIZE ANALYSIS HYDROMETER METHOD

011

SOIL ORGANIC MATTER Loss-On-Ignition

012

Hydride Generation AA

013

Cold Vapor AA

014

Flame AA

015

ICP - Jarrell-Ash Model 61 016 Graphite Furnace using the 5100 Zeeman
016 Graphite Furnace using the 5100 Zeeman

017

Perkin-Elmer Elan 5000 ICP/MS

018

ICP on Perkin-Elmer 4300 DV
019 L15-Pb in Blood-HGA

 

 

 

 

 

 

Lab Name: Laboratory and Environmental Testing, Inc.                     Method Code 001

Homogenization

1. Sample homogenization will depend on the sample type and size.

2. Water samples will not need to be homogenized.

3. For sampl es weighing less than 100 grams the whole sample will be freeze-dried first, and then homogenized, unless aliquots are being sent for Organic determination, then the sample would be homogenized first and an aliquot taken for freeze-drying.

4. Larger animal samples will be homogenized with a meat grinder. Then an aliquot of approximately 100 grams will be freeze-dried and then further homogenized using a blender, or if necessary, a Spex mixer mill with a Tungsten Carbide vial and ball.

5. Soil and Sediment samples will be mixed and aliquots of 100-200 grams taken for freeze-drying. After freeze-drying, soils will be sieved with a 20 mesh sieve and sediments will be sieved with a 10 mesh sieve followed by grinding with a Spex mixer mill, using a Tungsten Carbide vial and ball.

6. Plant samples will be freeze-dried and then homogenized with a blender, followed if necessary by grinding in a Spex mixer mill with a Tungsten Carbide vial and ball. If aliquots are being sent for Organic determinations, then the samples will be homogenized first, followed by freeze-drying, and further homogenization.

Back to the Top Back to the Top Arrow


Lab Name: Laboratory and Environmental Testing, Inc.                     Method Code 002

L9 - Freeze drying and % Moisture

1. Choose an appropriately sized container for the sample. Usually a Whirl-Pak works best for tissue samples. If the sample weighs less than 50 grams and is not being split for organics then use the whole sample.

2. Weigh and record the weight of the bag. If the sample weighs more than 2 grams then a three-place balance should be used. Small samples may require the use of a four or five-place balance.

3. Weight the bag, record the weight and transfer the sample to the bag. Weigh the bag and sample and record the weight. Seal the container or bag and place in a freezer at least overnight or until frozen solid.

4. After the samples are frozen, they are ready to place in the freeze-drier. Turn on the freeze-drier and start the refrigeration. When the temperature reaches -50 C open the container or Whirl-Pak and place in the chamber of the freeze-drier. Close the chamber and start the vacuum pump.

5. Depending on the number of samples and the amount of water present freeze-drying may take 1 - 5 days. When the pressure stops going lower, the samples may be done. If, upon removal, the samples are still cold, place back in the freeze-drier for a longer period of time.

6. After the samples are dry, remove them from the chamber. Then seal the container and weigh on the same balance. Record the weight of the bag and dry sample.

7. Calculate the weight of the dry sample and the weight of the wet sample. To calculate % Moisture divide the weight of the dry sample by the weight of the wet sample, subtract 1 and multiply by 100. Ignore the - sign.

Notes:

1. If the samples do not require % Moisture, then all of the weighing steps can be eliminated.

Back to the Top Back to the Top Arrow


Lab Name: Laboratory and Environmental Testing, Inc.                     Method Code 003

L1 - HNO3/HClO4 Digestion with HCl

1. Using a clean beaker or flask, write the sample number on the container in permanent black ink.

2. Weigh or measure the sample an d transfer to the container. Record the sample weight or volume on the paperwork.

3. Add 20 ml. of concentrated trace metal grade HNO3 and 2.5 ml. of concentrated trace metal grade HClO4. Then cover with a watch glass.

4. Place on a hot plate and adjust the temperature to allow reflux without significant loss of the acid.

5. Allow to reflux for 4 hours or overnight. Samples for Se or samples containing high lipid will require the longer reflux time.

6. After reflux, turn up the temperature to allow the HNO3 to be driven off without severe boiling, bumping or charring of the sample. When definite HClO4 fumes are observed, remove the sample from the hot plate and allow to cool.

7. Add 1.0 ml. of concentrated trace metal grade HCl to the samples and replace on the hot plate with watch glass, at the same temperature that was used to drive off the HNO3. Swirl the containers to help drive off the HNO3 residue and the HCl. After dense HClO4 fumes are observed allow the samples to reflux for 2 - 5 minutes. Remove from the hot plate and cool.

8. Add 2.0 ml. of concentrated trace metal grade HCl to the samples and place on the hot plate at a temperature that will boil water. When the solution is hot (2-5 minutes) add approximately 20 ml. of D.I. water and heat until clear or until the solution boils.

9. Remove and allow to cool. Dilute to 50.0 ml. with D.I. water and transfer to a clean 2 oz. bottle.

Notes:

1. Steps 3 and 8: for samples diluted to other than 50.0 ml. the volumes should be adjusted in relation to the other volume.

2. Step 9: the final volume may be other than 50.0 ml. If so an appropriate size container should be used.

3. This digestion can be used for water, biological fluids, plant and animal tissues, waste, soils and sediments. For soils and sediments the digestion will not be complete, being a hot acid extraction.

4. The digestion can be used for Flame AA, Flame Emission, ICP, Hydride for Se, and some elements by HGA.

Back to the Top Back to the Top Arrow


Lab Name: Laboratory and Environmental Testing, Inc.                     Method Code 004

L2 - HNO3 Digestion

1. Weigh up to 0.5 g. of sample on a three place balance and transfer to a clean 100 ml. beaker or flask. For liquids use a calibrated pipet to transfer up to 25 ml. to the beaker or flask.

2. Add 20.0 ml. of concentrated trace metal grade HNO3 .

3. Place container on the hot plate or kjeldahl rack and turn on heat high enough to allow the HNO3 to reflux.

4. Allow samples to reflux for a minimum of two hours. Overnight may be needed for difficult samples.

5. After the reflux, turn up the heat to allow the HNO3 to evaporate to a volume of approximately 2 ml.

6. Cool, add a pproximately 20 ml. of D.I. water and heat to near boiling to allow any solids a chance to dissolve.

7. Dilute the sample to 50.0 ml. with D.I. water and transfer to a 2 oz. labeled bottle.

Notes:

1. The digestion can be used for water, biological fluids, plant and animal tissue, waste, soils and sediments. For soils and sediments the digestion is not complete, being a hot acid extraction.

2. The digests can be analyzed by Flame AA, HG A and ICP.

3. For some elements Teflon or quartz containers will give lower blanks.

Back to the Top Back to the Top Arrow


Lab Name: Laboratory and Environmental Testing, Inc.                     Method Code 005

L3 - Digestion for Mercury

1. Weigh up to 0.5 g. of sample on a three place balance and transfer to a clean 50 ml. round bottom flask. For liquids use a calibrated pipet to transfer up to 10 ml. to a clean 50 ml. round bottom flask.

2. Add 5.0 ml. of concentrated trace metal grade HNO3 .

3. Place flask under condenser, making sure water is flowing through the condenser for reflux, and turn on heat high enough to allow the HNO3 to reflux.

4. Allow sample to reflux for two hours, then turn off the heat and allow to cool.

5. Rinse condenser into the flask with 1% HCl, remove the flask and rinse condenser tip into flask.

6. Dilute the sample to 50.0 ml. with 1% HCl and transfer to a 2 oz. labeled glass bottle.

Notes:

1. The digestion can be used for water, biological fluids, plant and animal tissue, waste, soils and sediments. For soils and sediments the digestion is not complete, being a hot acid extraction.

2. Soils and sediments should be diluted at least 1/3 before analysis.

3. Sample weights can be as high as 1 g.

Back to the Top Back to the Top Arrow


Lab Name: Laboratory and Environmental Testing, Inc.                     Method Code 006

L4 - HNO3/HClO4 Digestion

1. Using a clean beaker or flask, write the sample number on the container in permanent black ink.

2. Weigh or measure the sample and transfer to the container. Record the sample weight or volume on the paperwork.

3. Add 20 ml. of concentrated trace metal grade HNO3 and 2.5 ml. of concentrated trace metal grade HClO4. Then cover with a watch glass.

4. Place on a hot plate and adjust the temperature to allow reflux without significant loss of the acid.

5. Allow to reflux for 4 hours or overnight. Samples containing high lipid will require the longer reflux time.

6. After reflux, turn up the temperature to allow the HNO3 to be driven off without severe boiling, bumping or charring of the sample. When definite HClO4 fumes are observed, allow the sample to reflux for 5 - 10 minutes. Then remove from the hot plate and allow to cool.

7. Place on the hot plate at a temperature that will boil water. Add approximately 20 ml. of D.I. water and heat until clear or until the solution boils.

8. Remove and allow to cool. Dilute to 50.0 ml. with D.I. water and transfer to a clean 2 oz. bottle.

Notes:

1. Step 3: for samples diluted to other than 50.0 ml. the volumes can be adjusted appropriately for the other volumes.

2. Step 8: the final volume may be other than 50.0 ml. If so an appropriately sized container should be used.

3. This digestion can be used for water, biological fluids, plant and animal tissues, waste, soils and sediments. For soils
and sediments the digestion will not be complete, being a hot acid extraction.

4. The digestion can be used for Flame AA, Flame Emission, ICP, Hydride for As and Se, and some elements by HGA.

Back to the Top Back to the Top Arrow


Lab Name: Laboratory and Environmental Testing, Inc.                     Method Code 007

L5 - Magnesium Dry Ash

1. Weigh 0.5 g. of sample on a three-place balance and transfer to a cleaned 100 ml. glass beaker with etched numbers. Record the beaker number as well as the sample weight.

2. Wet with 3 ml. of methanol. Then add 5 drops of anti-foam agent, 10 ml. of 40% (W/V) Magnesium Nitrate Hexahydrate, 10 ml. of concentrated trace metal grade HNO3 and 2 ml. of concentrated trace metal grade HCl.

3. Cover with a watch glass and reflux on a hot plate overnight (8-12 hours) at low heat (70-80 C).

4. After reflux increase temperature to 200 C. Slide the watch glass to the side to allow for faster evaporation and cook to complete dryness. This may take 8-12 hours.

5. When no moisture is visible, cover fully with the watch glass and allow to cool.

6. Transfer samples to the cold muffle furnace and use the following program: Start at 250 C and ramp to 500 C at a rate of 1 degree per minute. When 500 C is reached hold for 3 hours then turn off and allow samples to cool to room temperature.

7. Place the cooled samples on a hot plate and add 20 ml. of 50% trace metal grade HCl. Allow the samples to gently boil for 1 hour. After 1 hour readjust volume to 20 ml. with 50 % HCl. Do not allow the samples to go dry. If necessary add more 50 % HCl during the heating.

8. Allow the samples to cool. Then dilute to 50.0 ml. with D.I. water and transfer to a clean 2 oz. labeled bottle.

Notes:

1. This digestion can be used for As or Se by Hydride Generation AA.

2. This digestion must be used on fish for As by Hydride Generation AA.

Back to the Top Back to the Top Arrow


Lab Name: Laboratory and Environmental Testing, Inc.                     Method Code 008

L6 - HNO3/H2O2 Digestion

1. Weigh up to 0.5 g. of sample on a three-place balance and transfer to a clean 100 ml. beaker or flask. For liquids use a calibrated pipet to transfer up to 25 ml. to the beaker or flask.

2. Add 20.0 ml. of concentrated trace metal grade HNO3.

3. Place container on the hot plate or Kjeldahl rack and turn on heat high enough to allow the HNO3 to reflux.

4. Allow samples to reflux for a minimum of two hours. Overnight may be needed for difficult samples.

5. After the reflux turn up the heat to allow the HNO3 to evaporate to a volume of approximately 2 ml.

6. After cooling add 1 ml. aliquots of high purity H2O2 and heat. Do this until the liquid is colorless or pale yellow. Use a maximum of 20 ml. of H2O2.

7. Cool, add approximately 20 ml. of D.I. water and heat to near boiling to allow any solids a chance to dissolve.

8. Dilute the sample to 50.0 ml. with D.I. water and transfer to a 2 oz. labeled bottle.

Notes:

1. The digestion can be used for water, biological fluids, plant and animal tissue, waste, soils and sediments. For soils and sediments the digestion is not complete, being a hot acid extraction.

2. The digests can be analyzed by Flame AA, HGA and ICP.

3. For some elements Teflon or quartz containers will give lower blanks.

Back to the Top Back to the Top Arrow


Lab Name: Laboratory and Environmental Testing, Inc.                     Method Code 009

L10 - Microwave Digestion

1. Weigh 0.5 g of dry sample into a clean Teflon digestion vessel. Record the weight to three decimal places.

2. Add 5.0 ml. of concent rated trace metal grade HNO3.

3. Loosely seal to allow release of pressure from the initial acid reaction with the sample.

4. After a few minutes open the vessel and add 1.0 ml of high purity H2O2.

5. Loosely seal the vessel to allow release of pressure.

6. Cap the vessel at the recommended pressure and place in the microwave. Run the program set up for this type of sample.

7. After the microwave heating is complete and the samples have cooled to room temperature, open the vessels and dilute the sample to 50.0 ml. with D.I. water and transfer to a clean 2 oz. plastic bottle. Any vessels that vented during the digestion will need to have the sample redigested and either use less sample or a longer ramp at the lower temperatures.

Notes:

1. Different sample types will require different heating programs to prevent losses due to exceeding the maximum vessel pressure.

2. To keep the same sample dilution, as little as 0.25 g of sample can be weighed and diluted to a final volume of 25.0 ml. using 1/2 of the HNO3 and H2O2.

3. This digestion can be used for Flame AA, HGA, CV, and ICP.

4. If Mercury is to be run, remove a 10 ml aliquot immediately after dilution and place in a plastic tube and add 100 microliters of concentrated Trace Metal grade Hydrochloric Acid.

Back to the Top Back to the Top Arrow


Lab Name: Laboratory and Environmental Testing, Inc.                     Method Code 010

PARTICLE SIZE ANALYSIS HYDROMETER METHOD

Principle of the Method

1.1 This method quantitatively determines the proportions of sand, silt and clay soil particles based on their settling rates in aqueous solution using a hydrometer. Settling rates are based on the principle of sedimentation as described by Stokes' Law.

1.2 The use of an ASTM 152H-type hydrometer is based on a temperature of 20oC and a particle size density of 2.65 g cm-3.

1.3 Dispersion is achieved with a 5% solution of sodium hexametaphosphate.

Range and Sensitivity

2.1 The method has a detection limit of 2% sand, silt and clay on a dry basis.

Interferences

3.1 Soluble salts, organic matter, carbonates and iron oxides may need to be removed by pretreatment.

Precision and Accuracy

4.1 The method is reproducible to + 8%.

Equipment

5.1 Balance.

5.2 Mixer.

5.3 Sodium hexametaphosphate (Calgonä).

5.4 Settling cylinder with a one liter mark that is 36 + 2 cm from the bottom.

5.5 Hydro meter (Bouyoucus).

5.6 Plunger.

5.7 Timer.

5.8 Thermometer.

5.9 Watch glass.

Preparation

6.1 Prepare the sodium hexametaphosphate solution by dissolving 50 g in 1000 mL of deionized water.

Procedure

6.1 Weigh 40.0 g of air-dried soil.

6.2 Transfer soil into mixer. Add 100 mL of sodium hexametaphosphate solution and 300 mL of deionized water.

6.3 Mix 1 minute in the mixer on the low speed setting.

6.4 Transfer the suspension quantitatively into settling cylinder.

6.5 Add deionized water to bring volume to 1000 mL

6.6 Fill a cylinder with 100 mL of 5% hexametaphosphate and 900 mL of deionized water. This will be the blank sample.

6.7 Allow suspensions to come to room temperature (22 to 27oC)—approximately two hours.

6.8 Insert plunger into the cylinder and carefully move up and down to thoroughly mix the contents of the cylinder. Be sure to displace sediment on the bottom of the cylinder. Finish mixing with two to three smooth strokes.

6.9 Remove the plunger and lower the hydrometer into the suspension.

6.10 After 30 seconds from the plunger removal, record the hydrometer reading as hydrometer #1 reading. Record a reading on the blank.

6.11 Remove the hydrometer carefully, rinse the surface and wipe it dry.

6.12 Cover cylinders with watch glasses to prevent foreign material from entering solutions during the settling period.

6.13 After 6 hours record temperature and refer to the temperature correction table (taken from the Western States Laboratory Proficiency Testing Program (9.3). Do not move the cylinder or reshake the suspension during the standing period.

6.14 Reread hydrometer at the prescribed time. Record as hydrometer #2 reading. Repeat a reading on the blank.

Calculations

Table 1. Suspension temperature effect on time of hydrometer reading for clay determination

Temperature Settling time for clay

oC
hours and minutes
18
8:09
19
7:57
20
7:45
21
7:35
22
7:24
23
7:13
24
7:03
25
6:53
26
6:44
27
6:35
28
6:27

Classification of soil texture

Soil texture can be classified by the guide for textural classification from the USDA Natural Resource Conservation Service. In the USDA textural triangle below, the corners represent 100 percent sand, silt, or clay (gravel and organic soils are not included). The triangle is divided into 10 percent portions of clay, silt, and sand. Heavy lines show the divisions between the12 basic soil textural classes. If the percentage for any two of the soil separates is known, the correct textural class can be determined. However, the summation of the three percentages must total 100 percent. Sometimes the point representing the texture of a soil sample falls exactly on the line between two texture names. It is customary to use the finer texture class when this happens. For example, a sample containing 40 percent clay, 30 percent silt, and 30 percent sand is called clay rather than clay loam.

References

8.1 McElreath, D. L. and Johnson, G.V. 1990. Soil texture–hydrometer method. In Laboratory Procedures Manual. Oklahoma State University Soil, Water, and Forage Analytical Laboratory.

8.2 Michigan State University. Manual of Laboratory Procedures. Soil and Plant Nutrient Laboratory. Michigan State University. Dept. of Crop and Soil Sci. East Lansing, MI 48824.

8.3 Miller, R. O., J. Kotuby-Amacher, and J. B. Rodriguez. 1998. Western States Laboratory Proficiency Testing Program-Soil Plant and Analytical Methods. Ver. 4.10.

Back to the Top Back to the Top Arrow


Lab Name: Laboratory and Environmental Testing, Inc.                     Method Code 011

SOIL ORGANIC MATTER Loss-On-Ignition

Principle of Method

1.1 This method estimates organic matter by measuring weight loss that results from the ignition of organic matter (Loss On Ignition, LOI) in a high temperature oven. It requires that soil is adequately dried before ignition, and then organic matter is quantitatively destroyed without altering other soil constituents such that soil weight is changed.

1.2 Various methods using different heating times and temperatures have been investigated. These are noted in the references 8.1, 8.2 and 8.4. A minimum heating temperature of 105o C for 24 hours is necessary to eliminate hygroscopic water and water of hydration from minerals such as gypsum. Excessive heating may result in weight loss associated with carbonates, structural water of silicate clays, oxidation of Fe+2 and dehydration of salts. The method noted here is adapted from Storer (8.7).

Range and Sensitivity

2.1 This method has been used with soils ranging in organic matter content from <1 to 45%. It has a sensitivity of 0.2 to 0.5% organic matter.

Sources of Error

2.1 Loss of water from incomplete preheating dehydration can result in over-estimation of organic matter. The problem is particularly likely in high clay soils with low organic matter, such as with subsoils. The method is not considered suitable for calcareous soils.

Precision and Accuracy

3.1 This method directly estimates organic matter, and it correlates well with organic carbon determinations. Yet it results in greater estimates of organic matter than with methods previously used. So organic matter is estimated from this method by regression of data with other established methods.

3.2 Mineral composition and soil horizons may affect LOI results.

3.3 Consistent analytical results are possible with a range of sample sizes, ashing vessels, ashing temperatures and length of ashing times.

3.4 Repeated analyses should provide results with a maximum coefficient of variability of 1 to 4%.

Equipment

5.1 NCR-13 2-g scoop.

5.2 10 mL glass beakers

5.3 Oven capable of heating to approximately 360o C.

5.4 Stainless steel racks for holding beakers.

5.5 Balance sensitive to ± 1 mg in draft-free environment.

Procedure

6.1 Scoop or weigh 2 g of air-dried soil into tared 10-mL glass beakers.

6.2 Dry for at least 2 hours at 150o C.

6.3 Record pre-weight to + 1 mg.

6.4 Heat at 360oC for 2 hours after oven temperature reaches 360o C.

6.5 Move the beakers from the oven to a lab bench; allow cooling approximately 15 minutes to cool. NOTE: if samples can not be weighted immediately then they should be re- dried in an oven at 150o C for 2 hours prior to recording post-weight.

6.6 Record post-weight to + 1 mg.

Calculations

7.1 Calculate loss of weight on ignition (LOI)

7.2 Estimate soil organic matter

Estimation of organic matter from LOI is done by regression analysis. Sixty soils were selected at random from those submitted to the lab. LECO-C was determined on these samples as well as % LOI. Percent organic matter was determined from LECO-C by multiplying % C by 1.79. LOI was regressed on LECO-OM forcing the intercept through the origin. The resulting equation is used to convert % LOI values into % organic matter. The equation is:

References

7.1 Ball, D. F. 1964. Loss-on-ignition as an estimate of organic matter and organic carbon in non-calcareous soils. J. Soil Sci. 15:84-92.

7.2 Combs, M. and M. V. Nathan. 1998. Soil Organic Matter. Ch. 12. In J. R. Brown (ed.). Recommended Chemical Soil Test Procedures for the North Central Region, N.C. Reg. Res. Pub. 221 (Revised). (Mo. Agric. Exp. Stn. SB 1001).

7.3 Goldin, A. 1987. Reassessing the use of loss-on-ignition for estimating organic matter content in non-calcareous soils. Commun. Soil Sci. Plant Anal. 18:1111-1116.

7.4 Handbook on reference methods for soil analysis. 1992. Soil and Plant Analysis Council, Inc. Georgia University Station, Athens, GA 30612-0007.

7.5 Michigan State University. Manual of Laboratory Procedures. Soil and Plant Nutrient Laboratory. Michigan State University. Dept. of Crop and Soil Sci. East Lansing, MI 48824.

7.6 Nelson, D. W. and L. E. Sommers, 1996. Total carbon, organic carbon, and organic matter. In D. L. Sparks (ed.). Methods of Soil Analysis, Chemical Methods, Part 3. Soil Science Soc. Am. Madison, WI.

7.7 Storer, D. A. 1984. A simple high sample volume ashing procedure for determining soil organic matter. Commun. Soil Sci. Plant Anal. 15:759-772.

7.8 Western States Laboratory Proficiency Testing Program, Soil and Plant Analytical Methods. 1998. Version 4.10.

Back to the Top Back to the Top Arrow


Lab Name: Laboratory and Environmental Testing, Inc.                     Method Code 012

Hydride Generation AA

Turn on the computer, printer, 3100, FIAS 200.and Argon. Place the appropriate lamp in the instrument and if an EDL turn to its required power. Place the furnace in the burner compartment if it is not already present.

When the computer is ready double click on the WinLab Analyst icon. If the technique is not already FI-Hydride then click on technique and change to FI-Hydride. After the computer has confirmed the IEEE connections are OK, click on Workspace and double click fias.fms. When the screens come up double click on the method and double click on either the Se-Fias or As-Fias method. Click on FIAS and turn on the cell.

When the lamp has had time to warm up click on lamps and enter the element and click on EDL. Check lamp alignment and wavelength to give the maximum signal. Close lamps.

Prepare the 10% HCl, 0.2% NaBH4-0.05% NaOH, Calibration standards, and check standards. Change the FIAS tubing and mixing cell if it is not already the set for this element. Change the position of the tubing or new tubes, if both positions have been used.

Check the alignment of the furnace in the light path by clicking on Tools and Continuous graphics. Autozero, then check all three positional knobs to get the lowest reading. Autozero whenever necessary.

Start the pumps and place the tubes in the HCl and Borohydride. Run a 5 or 10 PPB standard until the
sensitivity has stabilized and consecutive readings vary by less than 2%.

Enter the samples to be run into the Sample Information File. Enter a name for the Data file, and make sure that print log and store data are checked. When the instrument is ready click on Analyze All.

Calibration is done with 0, 1.0, 5.0, 15.0 PPB. QC checks are 10.0 and a known Reference sample (Usually ERA). The 5.00 PPB standard is checked every 10 tubes and if is more than 5% from 5.00 the instrument is recalibrated. If the value is more than 10% from 5.00, then the last 10 samples must be rerun.

After the analysis is finished, rinse system with D.I. water, turn off the pumps (release the pressure), turn off the EDL lamp, the Argon, FIAS and 3100. Click on File then Exit to close the WinLabs Analyst.

Click on WinLab Reformat Icon. Click on Open Design. Pick the design for As or Se FIAS. Then Browse and find the file name given the data. Place a 3.5" disk in the computer and click on Save Results.

Transfer disk to computer and using Excel calculate the results.

Back to the Top Back to the Top Arrow


Lab Name: Laboratory and Environmental Testing, Inc.                     Method Code 013

Cold Vapor AA

Turn on the computer, printer, 3100, FIAS 200,and Argon. Place the appropriate lamp in the instrument and if an EDL turn to its required power. Place the furnace in the burner compartment if it is not already present.

When the computer is ready double click on the WinLab Analyst icon. If the technique is not already FI-Hydride then click on technique and change to FI-Hydride. After the computer has confirmed the IEEE connections are OK, click on Workspace and double click fias.fms. When the screens come up double click on the method and double click on the Hg-CV method. Click on FIAS and turn on the cell.

When the lamp has had time to warm up click on lamps and enter the Hg and click on EDL. Check lamp alignment and wavelength to give the maximum signal. Close lamps.

Prepare the 10% HCl, 5% Stanous Chloride-10% HCl, Calibration standards, and check standards. Change the FIAS tubing and mixing cell if it is not already the set for Mercury. Change the position of the tubing or new tubes, if both positions have been used or determining a different element.

Check the alignment of the furnace in the light path by clicking on Tools and Continuous graphics. Autozero, then check all three positional knobs to get the lowest reading. Autozero whenever necessary.

Start the pumps and place the tubes in the HCl and Stanous Chloride. Run a 10 or 20 PPB standard until the sensitivity has stabilized and consecutive readings vary by less the 2%.

Enter the samples to be run into the Sample Information File. Enter a name for the Data file, and make sure that print log and store data are checked. When the instrument is ready click on Analyze All.

Calibration is done with 0, 1.0, 5.0, 30.0 PPB. QC checks are 10.0, 20.0 and a known Reference Sample(Usually ERA). The 5.00 PPB standard is checked every 10 tubes and if is more than 5% from 5.00 the instrument is recalibrated. If the value is more than 10% from 5.00, then the last 10 samples must be rerun.

After the analysis is finished, rinse system with D.I. water, turn off the pumps (release the pressure), turn off the EDL lamp, the
Argon, FIAS and 3100. Click on File then Exit to close the WinLabs Analyst.

Click on WinLab Reformat Icon. Click on Open Design. Pick the design for Hg-CV. Then Browse and find the file name given the data. Place a 3.5" disk in the computer and click on Save Results.

Transfer disk to computer and using Excel calculate the results.

Back to the Top Back to the Top Arrow


Lab Name: Laboratory and Environmental Testing, Inc.                     Method Code 014

Flame AA

Turn on the computer, printer, 3100, FIAS 200, Acetylene and Compressed Air. Place the appropriate lamp in the 3100 and if an EDL turn to its required power. Place the burner head in the burner compartment if it is not already present.

When the computer is ready double click on the WinLab Analyst icon. If the technique is not already Flame then click on technique and change to Flame. After the computer has confirmed the IEEE connections are OK, click on Workspace and double click Manual.fms. When the screens come up double click on the method and double click on the Method for the element you are going to run.

Click on lamps and enter the element and click on EDL or HCL depending on which is being used. Check lamp alignment and wavelength to give the maximum signal. Close lamps.

Prepare the Calibration standards and check standards. The acid matrix should match for samples, standards and check standards.

Light the flame and check the alignment of the burner in the light path by clicking on Tools and Continuous graphics. Autozero, then check all three positional knobs to get the highest reading while aspirating a standard.

Start the pumps and place the tubes in the HCl and Borohydride. Run a 5 or 10 PPB standard until the sensitivity has stabilized and consecutive readings vary by less the 2%.

Enter a name for the Data file, and make sure that print log and store data are checked. Calibration is done with 0,and 1 – 3 standards depending on the element and the range of concentration of the samples. After calibration, read the 0 and three to five standards covering the range of the calibration. Analyze the check standard. If this is acceptable then read the zero standard 10 times to determine the detection limit. Run a check standard every 10-12 samples and if it is more than 5% from its true value, then recalibrate. If it is more than 10% from its true value then recalibrate and rerun the samples since the last standard.

After the analysis is finished, rinse the system with D.I. water and turn off the flame. If using an EDL lamp turn it off. Turn off the the FIAS, 3100, Compressed Air and Acetylene.

Click on File then Exit to close the WinLabs Analyst.

Click on WinLab Reformat Icon. Click on Open Design. Pick the design for the element run. Then Browse and find the file name given the data. Place a 3.5" disk in the computer and click on Save Results.

Transfer disk to computer and using Excel calculate the results.

Back to the Top Back to the Top Arrow


Lab Name: Laboratory and Environmental Testing, Inc.                     Method Code 015

ICP - Jarrell-Ash Model 61

Turn on the Instrument power, PM Tubes switch and hit reset. Turn on the Line and Control on the RF Generator. Turn on the Water and Argon. Turn on the computer and double click on the JAICP Icon.

Place fresh D.I. water in the rinse beaker and start the peristaltic pump. After a few minutes, light the Plasma. Allow the instrument to warm up for 1 hour after the Plasma is lit.

Prepare standards and check standards in the same acid type and concentration as the samples.

After warm up is complete, check the profile with the Mercury light and adjust the alignment to +/- 0.1 spectrum shifter units of zero. Load the method to be run and calibrate. After calibration run the detection limit by changing to 10 integrations and running the zero standard. Run the check standard(s). If everything is acceptable start the analysis.

Run the Standards every 10-12 samples and check the profile after each set. If the profile is off from zero by more than 0.1 readjust the profile. If the standards are off more than 10% recalibrate and rerun the last set of samples.

If any samples have high concentrations of Fe, Al or unusual levels for other elements then run a high purity sample for those elements to allow Spectral Interferences to be checked.

After the analysis is completed turn off the Plasma, Argon, Water, and Pump. Convert the data to Excel using Enable and place on a 3.5" disk. Calculate the data using Excel, being sure to correct for Blank and Spectral Interferences.

Back to the Top Back to the Top Arrow


Lab Name: Laboratory and Environmental Testing, Inc.                     Method Code 016

Graphite Furnace using the 5100 Zeeman

Turn on the Furnace Coolant, Argon, Computer, Furnace, Zeeman Power Supply and 5100 in that order. Make sure the lamp is in the right position in the turret, and if using an EDL turn on the lamp to the proper power.

Double click on the AA WinLab Analyst icon. After the ZHGA-600 and 5100 icons have a green check by them, click on workspace. Double click on LET.fm, then double click on the method. Choose the method to be run and double click on the name. Click on Browse by the Sample Information File, and then pick one for standards. (Example: Pbstds.sif) Click on sample information icon to edit the file with sample names, dilutions, etc. Click Browse for the Results Data Set and enter the name of the file to store data. (Example: Pb010101) Click on Analyze. When samples have been prepared and ready for analysis, click on Analyze All if doing calibration or Analyze Samples if just running samples. The instrument is usually calibrated with a zero and one standard. Then a zero and 3-5 standards are run to check the calibration, followed by an instrument check standard and detection limit. If this is acceptable then the samples are run. Be sure to check that the correct modifier is being used for the element being run. Some samples may require the method of Standard Additions.

After the analysis is completed, close AA WinLab Analyst, turn off furnace coolant, Argon, 5100, Zeeman Power supply, Furnace and EDL power supply. Double click on the WinLab Reformat icon. Click on Open Design and choose the design for your element and double click on the name. Click on Browse and find the data file you want to reformat. Double click on the name. Make sure there is a floppy disk in the disk drive and click on Save Results. Transfer to another computer and calculate using Excel.

Back to the Top Back to the Top Arrow


Lab Name: Laboratory and Environmental Testing, Inc.                     Method Code 017

Perkin-Elmer Elan 5000 ICP/MS

Turn on the instrument control computer. Enter elan at login.

Turn on the instrument and set up with RF power 1.0 kw, Ar floe 15 l/min plasma, 0.75 l/min nebulizer, 0.90 l/min auxilary flow, Ion lens P, 50, B 58, S2 17, E1 28, Read Delay 45 second and Method USDI 2A.

Set up peristaltic pump for 2-channel IS operation using Rh. Turn on the plasma and turn on peristaltic pump as soon
as plasma is on. Allow plasma to warm up at least 30 minutes before starting analysis. Fill out ICP-MS Data Log.

Under the Applications menu select Quantitative Analysis, load method USDI 2A.

Run 1% HNO3 as a blank. The Rh should read more than 20,000 c.s. If not adjust the x-y position and nebulizer flow or perform CEM optimization. Record the Rh count rate on the ICP-MS data log sheet.

Prepare the sample table for the samples to be run. Standards should be the same acid and concentration as the samples. Calibrate the instrument. Then run Detection Limit and Check samples. Run Standards after every 10-12 samples.

After analysis is complete, select "Report" on the screen. Choose "Computer Format to File". Click on "To File". Give a file name using the convention dmmddyy.txt, mmddyy being month day and year.

Reprocess the data. When finished, select "Report". De-select by clicking on "Computer Format to File". Then click on "Report" again.

Select a new screen by pressing Alt-F1. Enter "vipx". Then change directory by typing "cd elan", "cd data", or "cd reports".

Insert a 3.5 " disk into the drive and then enter "Copy" DMMDDYY.TXT, A:.

Return to Elan window by pressing Alt-F1. Select :File" the Close Application". Select "Shutdown" under ‘Application Menu. Wait for "Safe to power off" message to appear. Then turn off the power to the computer. Turn off RF power supply to the Elan 500.

Back to the Top Back to the Top Arrow


Lab Name: Laboratory and Environmental Testing, Inc.                     Method Code 018

ICP on Perkin-Elmer 4300 DV

Make sure the instrument, Chiller, Air compressor, and gases are on, and at the proper temperatures and pressures. Turn on the computer and double click on the WinLAb32 icon.

Prepare standards and check samples to match the acid matrix of the samples to be analyzed. Change the pump tubing.

Click on "file", then "Open", and then "Method". Click on the method to be used and then click "OK", TO start the ICP program and call up the Method with the elements to be determined.

Click on the Plasma icon, and click on pump to start the pump and make sure the tubes are in the pump properly. Start the plasma by clicking the "On" icon. Click on the X in the upper right corner to close the Plasma Control. Allow the instrument to warm-up while the samples and standards are loaded into the auto-sampler racks. If the Sample Info table was not filled out previously, then fill in the sample information and save the table using the Batch ID.

Before starting the run, check the Hg wavelength by clicking on "Tools", and then "Spectrometer Control". Click on Hg Realign. When that is complete, aspirate a 10.0 Mn Standard and click on "Align View". After Align View is completed, close the box.

When ready to start analysis, click on the "Auto" icon, make sure that the data is being stored in a file with the correct name for the Batch, and that the right method is being used. Click the "Analyze" icon and click on "Analyze All".

When the run is completed, click on "File", then "Utilities", then "Data Manager". Highlight the file, and then click on "Export" icon. Click "Use Existing Design". Click "Browse" and choose the appropriate template (usually LET-ICP). Click "Open", place a disk in the "A" drive, and click "Finish". Click on "Export Data" to transfer data to disk in Drive "A".

Transfer data to the main computer and calculate the final Concentrations.

Back to the Top Back to the Top Arrow


Lab Name: Laboratory and Environmental Testing, Inc.                     Method Code 019

L15-Pb in Blood-HGA

METHOD/PROCEDURE

1. Prepare an adequate volume of matrix modifier to dilute the samples and perform the analysis. The matrix modifier is 0.2% HNO3, 0.5% Triton-X 100 and 0.2% NH4H2PO4. Samples are diluted 1 part Blood and 9 parts Modifier.

2. Set up Perkin-Elmer 5100 Zeeman for Lead. Wavelength 283.3 with an EDL lamp. Furnace program is dry 110 C with 25 second ramp and 25 second hold. Char step is 800 C with a 15 second ramp and 25 second hold. A cool down to 20 C is next with a 1 second ramp and 9 second hold. Atomization is 1900 C with a 0 second ramp and 5 second hold, followed by a clean out at 2600 C with a 1 second ramp and a 5 second hold.

3. The Instrument is calibrated with a 25 or 50 ppb standard, followed by running a standard curve of 5 to 6 values between 2.5 and 100 ppb.

4. Lead is determined in the samples with a 14 ul injection. The detection limit is determined by injecting the 2.5 ppb standard 7 times and taking 3 times the standard deviation of the mean.

5. Blanks are the Triton-X Modifier and Duplicates are separate dilutions of the blood. Spikes are diluted separately and an aliquot of a Lead standard added to give 25 ppb spike. Reference material is a BLLRS Blood supplied by CDC, also diluted 1:10 like the bloods.

6. If sample concentration is above 50 ppb, further dilution of the blood is made with the riton-X Modifier.

Back to the Top Back to the Top Arrow