How Clean is Clean?

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How Clean is Clean? Jane Rothert and Chris Lehmann National Atmospheric Deposition Program, Central Analytical Laboratory, Illinois State Water Survey 2204 Griffith Dr.; Champaign, IL 61801 Email: [email protected]; Phone: 217-244-0868; Internet: http://nadp.sws.uiuc.edu/CAL The NADP Central Analytical Laboratory (CAL) has been providing clean sampling supplies for the NTN and AIRMoN for almost 30 years. As method detection limits (MDLs) have decreased, supplies once thought to be clean now have detectable contamination. Our supplies preparation staff want to know…. When is clean, clean enough? Deionized Water Blanks One deionized water (18 MΩ-cm or better) sample is taken weekly from the CAL’s sample preparation laboratory Samples are collected in triple- rinsed 60 mL virgin high density polyethylene (HDPE) bottles Samples are not filtered before analysis Description Deionized water blanks are consistently below both old and current MDLs. The CAL’s deionized water is not a source of supply contamination. 1-Liter Shipping Bottle Blanks The NTN uses 1-L HDPE bottles for precipitation sample shipping. These bottles are washed with deionized water and reused. Four supply blanks are prepared weekly from randomly- selected bottles. Solutions include: • 50 mL deionized water (data shown at right) • 150 mL deionized water • 50 mL CAL internal standard (FR25) • 150 mL CAL internal standard (FR25) Solutions are left in the bottles for one week Samples are not filtered before analysis The majority of shipping bottle blanks are below old and current MDLs. In 2006, five shipping bottle blanks (< 10%) had elevated concentrations of calcium. There is more scatter in shipping bottle blanks as compared to deionized source water. NTN shipping bottles are not an appreciable source of potential sample contamination. Collector Bucket Blanks The majority of collector bucket blanks are below old MDLs. Unfortunately, the majority of these blanks are above current MDLs for calcium and ammonium. For nitrate and sulfate, the majority of blanks are below current MDLs. The majority of blanks are below the 10 th percentile of the 2002-2006 NTN data set for calcium, sulfate, and nitrate. From 2001 through 2003, the majority of blanks were above the 10 th percentile of the 2002-2006 NTN data set for ammonium. Since 2004, approximately 90% of blanks fell below the 10 th percentile of the NTN data set. Conclusions The CAL’s deionized water and 1-L shipping bottles are not an appreciable source of sample contamination. Since buckets are exposed to the environment, contamination levels are higher than those observed in the 1-L shipping bottles. Contamination levels in collector buckets are consistently at or below the 10 th percentile of the NTN data set as required in the CAL’s work plan. Acknowledgements The NADP is National Research Support Project-3: A Long-Term Monitoring Program in Support of Research on the Effects of Atmospheric Chemical Deposition. More than 240 sponsors support the NADP, including State Agricultural Experiment Stations; universities; private companies and other nongovernmental organizations; Canadian government agencies; state, local, and tribal government organizations; and federal agencies, including the U.S. Department of Agriculture–Cooperative State Research, Education, and Extension Service (under agreement no. 2002-39138- 11964). Any findings or conclusions in this poster do not reflect the views of the U.S. Department of Agriculture or other NADP sponsors. The authors gratefully acknowledge the wondrous creative talent of Pam Bedient and her assistance in preparing this poster and Nichole Samson for taking the photographs (and washing all those buckets). Observations The NTN & AIRMoN use 3.5 gallon HDPE buckets to collect precipitation samples. In the NTN, these buckets are exposed to field conditions for one week. Buckets are washed with deionized water at the CAL and reused. Four blanks are prepared weekly from randomly-selected buckets. Solutions include: Solutions are left in the buckets for one week Samples are not filtered before analysis • 50 mL deionized water (data shown at right) • 150 mL deionized water • 50 mL CAL internal standard (FR25) • 150 mL CAL internal standard (FR25) Concentration (mg/L) Concentration (mg/L) Concentration (mg/L) Concentration (mg/L) Calcium Nitrate Ammonium Sulfate 1% of NTN samples below 0.056 mg/L old MDL = 0.03 mg/L current MDL = 0.010 mg/L 10% of NTN samples below 0.222 mg/L 1% of NTN samples below 0.069 mg/L old MDL = 0.03 mg/L current MDL = 0.017 mg/L 10% of NTN samples below 0.270 mg/L 1% of NTN samples and old MDL = 0.009 mg/L current MDL = 0.003 mg/L 10% of NTN samples below 0.027 mg/L 1% of NTN samples below < 0.004 mg/L old MDL = 0.02 mg/L current MDL = 0.004 mg/L 10% of NTN samples below 0.035 mg/L Concentration (mg/L) Concentration (mg/L) Calcium Ammonium old MDL = 0.009 mg/L current MDL = 0.003 mg/L current MDL = 0.004 mg/L old MDL = 0.02 mg/L Concentration (mg/L) Concentration (mg/L) Calcium Ammonium old MDL = 0.009 mg/L current MDL = 0.003 mg/L current MDL = 0.004 mg/L old MDL = 0.02 mg/L

description

Jane Rothert and Chris Lehmann National Atmospheric Deposition Program, Central Analytical Laboratory, Illinois State Water Survey 2204 Griffith Dr.; Champaign, IL 61801 Email: [email protected] ; Phone: 217-244-0868; Internet: http://nadp.sws.uiuc.edu/CAL. - PowerPoint PPT Presentation

Transcript of How Clean is Clean?

Page 1: How Clean is Clean?

How Clean is Clean?Jane Rothert and Chris Lehmann

National Atmospheric Deposition Program, Central Analytical Laboratory, Illinois State Water Survey2204 Griffith Dr.; Champaign, IL 61801

Email: [email protected]; Phone: 217-244-0868; Internet: http://nadp.sws.uiuc.edu/CAL

The NADP Central Analytical Laboratory (CAL) has been providing clean sampling supplies for the NTN and AIRMoN for almost 30 years. As method detection limits (MDLs) have decreased, supplies once thought to be clean now have detectable contamination. Our supplies preparation staff want to know…. When is clean, clean enough?

Dei

oniz

ed W

ater

Bla

nks

One deionized water (18 MΩ-cm or better) sample is taken weekly from the CAL’s sample preparation laboratorySamples are collected in triple-rinsed 60 mL virgin high density polyethylene (HDPE) bottlesSamples are not filtered before analysis

Description

Deionized water blanks are consistently below both old and current MDLs.The CAL’s deionized water is not a source of supply contamination.

1-Li

ter S

hipp

ing

Bot

tle

Bla

nks

The NTN uses 1-L HDPE bottles for precipitation sample shipping. These bottles are washed with deionized water and reused.Four supply blanks are prepared weekly from randomly-selected bottles. Solutions include:

• 50 mL deionized water (data shown at right)• 150 mL deionized water• 50 mL CAL internal standard (FR25)• 150 mL CAL internal standard (FR25)

Solutions are left in the bottles for one weekSamples are not filtered before analysis

The majority of shipping bottle blanks are below old and current MDLs.In 2006, five shipping bottle blanks (< 10%) had elevated concentrations of calcium.There is more scatter in shipping bottle blanks as compared to deionized source water.NTN shipping bottles are not an appreciable source of potential sample contamination.

Col

lect

or B

ucke

t Bla

nks

The majority of collector bucket blanks are below old MDLs.Unfortunately, the majority of these blanks are above current MDLs for calcium and ammonium.For nitrate and sulfate, the majority of blanks are below current MDLs.The majority of blanks are below the 10th percentile of the 2002-2006 NTN data set for calcium, sulfate, and nitrate.From 2001 through 2003, the majority of blanks were above the 10th percentile of the 2002-2006 NTN data set for ammonium. Since 2004, approximately 90% of blanks fell below the 10th percentile of the NTN data set.

ConclusionsThe CAL’s deionized water and 1-L shipping bottles are not an appreciable source of sample contamination.Since buckets are exposed to the environment, contamination levels are higher than those observed in the 1-L shipping bottles.Contamination levels in collector buckets are consistently at or below the 10th percentile of the NTN data set as required in the CAL’s work plan.

AcknowledgementsThe NADP is National Research Support Project-3: A Long-Term Monitoring Program in Support of Research on the Effects of Atmospheric Chemical Deposition. More than 240 sponsors support the NADP, including State Agricultural Experiment Stations; universities; private companies and other nongovernmental organizations; Canadian government agencies; state, local, and tribal government organizations; and federal agencies, including the U.S. Department of Agriculture–Cooperative State Research, Education, and Extension Service (under agreement no. 2002-39138-11964). Any findings or conclusions in this poster do not reflect the views of the U.S. Department of Agriculture or other NADP sponsors. The authors gratefully acknowledge the wondrous creative talent of Pam Bedient and her assistance in preparing this poster and Nichole Samson for taking the photographs (and washing all those buckets).

Observations

The NTN & AIRMoN use 3.5 gallon HDPE buckets to collect precipitation samples. In the NTN, these buckets are exposed to field conditions for one week. Buckets are washed with deionized water at the CAL and reused.Four blanks are prepared weekly from randomly-selected buckets. Solutions include:

Solutions are left in the buckets for one weekSamples are not filtered before analysis

• 50 mL deionized water (data shown at right)• 150 mL deionized water• 50 mL CAL internal standard (FR25)• 150 mL CAL internal standard (FR25)

Con

cent

ratio

n (m

g/L)

Con

cent

ratio

n (m

g/L)

Con

cent

ratio

n (m

g/L)

Con

cent

ratio

n (m

g/L)

Calcium

Nitrate

Ammonium

Sulfate

1% of NTN samples below 0.056 mg/L

old MDL = 0.03 mg/L

current MDL = 0.010 mg/L

10% of NTN samples below 0.222 mg/L

1% of NTN samples below 0.069 mg/L

old MDL = 0.03 mg/Lcurrent MDL = 0.017 mg/L

10% of NTN samples below 0.270 mg/L

1% of NTN samples and old MDL = 0.009 mg/L

current MDL = 0.003 mg/L

10% of NTN samples below 0.027 mg/L

1% of NTN samples below < 0.004 mg/L

old MDL = 0.02 mg/Lcurrent MDL = 0.004 mg/L

10% of NTN samples below 0.035 mg/L

Con

cent

ratio

n (m

g/L)

Con

cent

ratio

n (m

g/L)

Calcium Ammonium

old MDL = 0.009 mg/L

current MDL = 0.003 mg/Lcurrent MDL = 0.004 mg/L

old MDL = 0.02 mg/L

Con

cent

ratio

n (m

g/L)

Con

cent

ratio

n (m

g/L)

Calcium Ammonium

old MDL = 0.009 mg/L

current MDL = 0.003 mg/Lcurrent MDL = 0.004 mg/L

old MDL = 0.02 mg/L