NTN Bottles Leakage StudyKim Attig and Mark Rhodes

National Atmospheric Deposition Program

Central Analytical Laboratory (CAL)

Illinois State Water Survey

Institute of Natural Resource Sustainability

University of Illinois at Urbana-Champaign

Champaign, IL 61820; attig@illinois.edu

Abstract

Weekly NTN samples are decanted into 1 liter bottles and are shipped to the

Central Analytical Laboratory (CAL) for analysis. In 2009, the number of NTN

samples that leaked during shipment increased to 40%. Prior to 2009, that number

averaged 30%. Associated with bottle leaks are the potential for sample

contamination, and the potential loss of sample volume for analysis and archiving.

Additionally, samples may be lost or destroyed as the shipping container is

compromised due to water damage.

To address these concerns, the NADP is taking action to reduce and eliminate leaks

from NTN bottles during shipping. In 2010, several options were tested to address

the bottle leak problem. These options include the use of parafilm, rubber bands,

and additional packing material.

The NADP a 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 non-governmental 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. 2008-39134-19508). Any findings or conclusions in this poster do not reflect the views of the U.S. Department of Agriculture or other NADP sponsors. The Illinois State

Water Survey is a division of the Institute of Natural Resource Sustainability at the University of Illinois.

Thanks to Greg Wetherbee, Kieth Halbrook, Melissa Rury, and Jason Karlstrom for their help in testing. Thanks to Phyllis Ballard for her help in shipping the bottles. Thanks also to Pam

Bedient for poster formatting and review.

Year

NTN

# Leaks %

Leaks

2000 3633 29.9

2001 3496 27.8

2002 3258 24.3

2003 3760 27.5

2004 4328 31.2

2005 5040 36.4

2006 4550 32.9

2007 4109 29.4

2008 4681 33.8

2009 5148 40.2

Tests with Parafilm

200 mL of faux rain water was added to four 1L NTN sample bottles. Two

bottles had parafilm wrapped around the sealed bottle cap, the other two did not.

The four bottles were sonicated for one hour. Leakage was measured to be 10 –

20 mL per bottle. Two NTN 1L NTN bottles, half full of deionized water, were

sent to four participants. One bottle was the “control” as it was treated as NTN

sample bottles are normally shipped, and the second bottle was “experimental”

as it had parafilm wrapped around the neck of the closed bottle.

Two 1L NTN sample bottles were partially filled with water, and parafilm was

used to cover the bottle mouth. The lid was then screwed on over the parafilm.

The bottle was placed in the back of a pickup truck and the truck was driven 200

miles, to mimic shipment of a sample bottle. Leakage from the bottle was

measured to be more than 100 mL.

One 1L NTN sample bottle was partially filled with water, and parafilm was

wrapped around the threads on the neck of the bottle. The bottle was placed in

the back of a pickup truck and the truck was driven 200 miles, to mimic

shipment of a sample bottle. Leakage from the bottle was measured to be less

than 10 mL. The procedure for shipping to the four participants was repeated

with parafilm wrapped around the threads on the neck of the bottles.

Tests with Rubber Bands

200 mL of deionized water was added to three 1L NTN bottles. A rubber band was put around

each bottle and they were sonicated for three hours. One bottle leaked 10-20 mL of water, but the

other two bottles did not leak.

Four 1L NTN bottles were partially filled with water and wrapped with rubber bands. The bottles

were placed in the back of a pickup truck and the truck was driven 200 miles, to mimic shipment

of a sample bottle. Leakage from each bottle was measured to be less than or equal to 10 mL.

Two 1L NTN bottles, half full of deionized water, were sent to four participants. One bottle was

the “control” as it was treated as NTN sample bottles are normally shipped, and the second bottle

was “experimental” as it rubber band stretched from top to bottom of the bottle. This procedure

was then repeated using two rubber bands stretched from top to bottom of the bottom,

perpendicular to each other.

Locations of Individuals participating in the study:

Gainesville FL Seattle WA

Washington DC Denver CO

Parafilm Results

As indicated in the chart below, parafilm did not prevent or reduce bottle leaks. On

the positive side, the use of parafilm did not cause contamination of the samples.

Rubber Band Results

As indicated by the chart below, rubber bands did not prevent or reduce bottle leaks. When

samples were analyzed upon their return to the CAL, there was apparent contamination of

calcium and sulfate in the samples from the bottles that were rubber banded bottles. This

indicates cross contamination between the sample, the rubber bands and the sample bag.

Conclusions

Even though the number of samples for each test was small, no definite improvement

resulted from any of the tests. Neither parafilm nor rubber bands were shown to

eliminate or reduce leaks in a reliable, reproducible manner. Additionally, there was

apparent contamination in the water samples from the bottles wrapped with rubber

bands. Further testing is needed to determine whether cross contamination of leaking

samples is a concern. Transit of the sample bottles from the sites to the CAL may have

an effect on sample leaks. Elevation, and the associated pressure changes may impact

bottle leaks. The age and condition of the bottles may also impact bottle leakage.

Additional testing will be performed to assess cross contamination, different packing

methods, and pressure changes during transit on NTN sample bottles.

Analytical results of the DI water shipped in the bottles

Analytical results of the DI water shipped in the bottles

Rubber Band Around Bottle

Location Bottle, No Rubber Band Bottle, with Rubber Band

Shipped Received Shipped Received

Gainesville, FL N N A A

Seattle, WA B B B B

Washington, D.C. A A A A

Denver, CO B A B A

Two Rubber Bands Around Bottle

Location Bottle, No Rubber Band

Bottle, with 2 Rubber

Bands

Shipped Received Shipped Received

Gainesville, FL B B B A

Seattle, WA B A B N

Washington, D.C. A A B A

Denver, CO B A A A

Parafilm Wrapped Around Bottle and Lid

Location Bottle, No Parafilm Bottle, with Parafilm

Shipped Received Shipped Received

Gainesville, FL A N A B

Seattle, WA B A C C

Washington, D.C. N N N A

Denver, CO B N A N

Parafilm Wrapped Around Bottle Threads

Location Bottle, No Parafilm Bottle, with Parafilm

Shipped Received Shipped Received

Gainesville, FL B A A A

Seattle, WA N/A C N/A C

Washington, D.C. B B N N

Denver, CO C N C A

Leak Categories:

C is > 100mL

B is 10 to 100mL

A is ≤ 10mL

none

Number Description pH Cond Ca K Mg Na Cl NO3 SO4 NH4 PO4

RD100033 DI from no rubber band bottle from Gainsville FL 5.54 1.4 0.007 0.003 0.003 0.004 0.022 0 0 -0.003 0.001

RD100034 DI from rubber banded bottle from Gainsville FL 5.56 1.2 0.024 0.001 0.001 0.001 0 0 0.014 -0.002 0.001

RD100035 DI from no rubber band bottle from Washington DC 5.58 1.2 0 0 0.001 0 0 0 0 0 0.001

RD100036 DI from rubber banded bottle from Washington DC 5.73 1.2 0.045 0.01 0.003 0.006 0.01 0 0.027 -0.004 0.002

RD100037 DI from no rubber band bottle from Denver CO 5.61 1.2 0.003 0.003 0.002 0.003 0.013 0 0 0.003 0.004

RD100038 DI from rubber banded bottle from Denver CO 5.59 1.3 0 0 0.001 0 0 0 0 0.002 -0.002

RD100039 DI from no rubber band bottle from Seattle WA 5.67 1.4 0.013 0.004 0.003 0.043 0.033 0 0.018 0.004 0.003

RD100040 DI from rubber banded bottle from Seattle WA 5.61 1.4 0.007 0.002 0.001 0.001 0 0 0 -0.001 0.004

Number Description pH Cond Ca K Mg Na Cl NO3 SO4 NH4 PO4

RD100013 DI from untaped bottle from Denver CO 5.62 1.2 0 0.001 0 0 0 0 0 0.002 0.002

RD100014 DI from taped bottle from Denver CO 5.62 1.3 0 0.001 0 0.001 0 0 0 0.004 -0.001

RD100015 DI from untaped bottle from Seattle WA 5.69 1.3 0.001 0.002 0 0.002 0.004 0 0 0.004 0.002

RD100016 DI from taped bottle from Seattle WA 5.74 1.4 0.001 0.005 0 0.005 0.007 0 0 0.005 0.003

RD100017 DI from untaped bottle from Washington DC 5.64 1.3 0 0.001 0 0 0.003 0 0 0 -0.002

RD100018 DI from taped bottle from Washington DC 5.62 1.2 0 0.002 0 0.001 0.003 0 0 0.005 -0.002

RD100019 DI from untaped bottle from Gainesville FL 5.63 1.4 0 0 0 0 0 0 0 0.001 0.002

RD100020 DI from taped bottle from Gainesville FL 5.63 1.4 0 0.004 0 0.003 0.008 0 0 0 0.001

RD100021 DI from untaped bottle from Gainesville FL 5.6 1.2 0 0 0.001 0 0 0 0 -0.001 0.004

RD100022 DI from taped bottle from Gainesville FL 5.6 1.3 0 0 0.001 0 0 0 0 0 0.002

RD100023 DI from untaped bottle from Washington DC 5.66 1.2 0 0.001 0 0.001 0 0 0 0 0.002

RD100024 DI from taped bottle from Washington DC 5.66 1.2 0 0 0 0 0 0 0 0.001 0.002

RD100025 DI from untaped bottle from Denver CO 5.68 1.3 0 0.003 0 0.002 0.005 0.017 0 -0.001 0.002

RD100026 DI from taped bottle from Denver CO 5.66 1.3 0 0.003 0 0.002 0.004 0 0 0 0.003

RD100027 DI from untaped bottle returned from UPS 5.72 1.5 0.01 0.077 0.003 0.057 0.079 0.01 0 0.049 -0.001

RD100028 DI from taped bottle returned from UPS 5.75 1.4 0.006 0.045 0.002 0.036 0.046 0.009 0.009 0.039 0.001

Bottle in the sonicator

Bottles in the back of a pickup truck

Percentage of Leak Size for all Samples from each NTN Site