# Study Plan

Solubility Determination of
CASRN 78-11-5 (Pentaerythritol tetranitrate )
In Hard Water

Dyno Nobel Inc 2795 East Cottonwood Parkway

Suite 500 Salt Lake City, UT 84121

July 11, 2014

## Solubility of CASRN 78-11-5 (PETN) in Hard Water

Purpose The purpose of this study is to determine the solub ility of PETN in the hard water test medium used fo r acute toxicity testing to fish and Daphnia.
Background During acute toxicity testing, the concentration of PETN in the testing medium could not attain the reported solubility limit of 2130 μg/L – the actual report provides a reported limit of 2130 μg/L for the 48 hour sample, and a reported limit of 1950 μg/L f or the 72 hour sample. The reported solubility limi t was determined in accordance with 40 CFR 799.6784 w hich uses double distilled water as the test medium.
Acute toxicity testing performed in accordance with ASTM E 729-96 provides specifications on the hard water to be used during the testing. A PETN concen tration at or near the reported solubility limit in hard water was not achieved during the acute toxici ty testing.
In correspondence from the U.S. Environmental Prote ction Agency to Dyno Nobel dated April 22, 2014, it was recommended that the solubility of PETN in t he fish and Daphnia test medium be determined. Such testing should be performed under similar cond itions (e.g., temperature, test medium, concentration of organic solvent, etc.) to those us ed in the aquatic toxicity tests.
Hard Water for the Acute Toxicity Testing to Fish a nd Daphnia The hard water to be used in this solubility testin g is to be the same as that which was used during t he previously performed acute aquatic toxicity testing to fish and Daphnia. In accordance with ASTM E 729-96, and as used by the laboratory that performe d the acute aquatic toxicity testing, the reconstituted hard water consists of the following (based on a 15 Liter quantity):

• NaHCO3 - 2280 mg (to attain 192 mg/L)

• CaSO4 - 2H2O - 1800 mg (to attain 120 mg/L)

• MgSO4 - 1800 mg (to attain 120 mg/L)

• KCl - 120 mg (to attain 8 mg/L)

• Selenium added to obtain nominal concentration of 2 μg/L

• Target Chemistry is pH 7.6 - 8.0; Hardness 160 - 18 0; Alkalinity 110 - 120

PETN Supplied to Aquatic Toxicity Laboratory PETN is a highly sensitive explosive compound. Lab oratories that perform aquatic toxicity testing can not manage and handle PETN unless it has been diluted t o render the material non-explosive. To facilitate the aquatic toxicity testing, acetone was used as a solvent to dissolve PETN to a nominal concentratio n of 5000 mg PETN/L acetone. The source of the PETN w as the Dyno Nobel facility in Graham, KY. It was provided to the U.S. Army Center for Health Promoti on and Preventative Medicine (CHPPM) for useduring the HPV1 test studies. At the request of Dy no Nobel, the CHPPM provided the test material to

the aquatic toxicity laboratory at the concentratio n of 5000 mg PETN/L acetone. The PETN to be used a t the Dyno Nobel Lehi, UT facility will be sourced fr om the Graham, KY facility, and will be accompanied by an analytical specification sheet providing informa tion on the material’s purity. The Lehi, UT facili ty will dissolve the PETN into acetone to establish a nomin al concentration of 5000 mg PETN/L acetone.
Methodology The reported solubility limit for PETN was derived by testing performed by CHPPM, and was subsequently submitted as part of the HPV1 testing rule. The same methodology for solubility testing (40 CFR 799.6784) will be utilized for the hard wat er solubility testing of PETN, except for the modifications needed to implement the recommendatio ns provided in the April 22, 2014 correspondence from the U.S. EPA.
In email correspondence dated June 3, 2014, the U.S . EPA confirmed that it would be acceptable for Dyno Nobel’s laboratory to conduct the solubility t esting for PETN as described in the earlier correspondence dated April 22, 2014.

Modifications include:

• Reconstituted hard water will be used as the test m edium

• PETN at a nominal concentration of 5000 mg PETN/L a cetone at the test material

• Temperatures of 20°C (Daphnia magna) and 25°C (Pime phales promelas)

Test Report The report is to include the following information: a) The individual analytical determinations and the av erage where more than one value was determined for each flask. b) The average of the value for the different flasks w hich were in agreement. c) The test temperature. d) The analytical method employed