AEROSOL TRAINING

Off-the-Top and Total Exhaustion

Before we start…

METHOD OVERVIEW

SOP ABSTRACT

Off-The-Top (OTT)Shake can well and use a tubing adaptor to

spray into a volumetric flask Total Exhaustion (TE)

Freeze can to allow puncturingBring to temperature and transfer to jarMulti-phase needs to be dissolved into a single

phase

OFF THE TOP

Read label directions Some cans aren’t worth the trouble Some cans spray upside-down Some cans need to be shaken throughout spraying

Weigh intact can before starting Shake aerosol can well, as specified on label Test spray into a beaker with a shallow layer of desired

solvent Weigh between sprays Get a “feel” for the product Never use first spray for extraction

When ready, spray into desired flask in solvent

COMPRESSED AIR PROPELLANT

TARGET CONCENTRATIONS

OTT and TE 0.2 . . % Level 3 for Picaridin

Spray between 2 and 10g of sample into a 50mL volumetric flask to be on the calibration curve.

6.7g is ideal.

SINGLE-PHASE WEIGHTEXAMPLE: SPORTSMEN GEAR SMART INSECT REPELLENT

Weight of unopened can (Wun) 263.70g Weight of can after release of propellant (Wex) 247.11g Weight of empty storage jar (WJ) 281.65g Weight of jar + sample (WJ+S) 455.27g Weight of jar + sample post sonication (WSon) 453.41g Sample in jar: (WSon – WJ) 171.77g Weight of propellant: Wprop = (Wun – Wex) + (WJ+S – Wson) 18.44g Weight of empty can: (Wcan) 72.86g Total sample weight: Wts = (Wun – Wcan) 190.84g % Propellent: (Wprop/Wts) x 100 9.66%

16.59g

1.86g

MULTI-PHASE WEIGHTEXAMPLE: CUTTER SKINSATIONS ULTRA LIGHT

Weight of unopened can (Wun) 147.12g Weight of can after release of propellant (Wex) 129.58g Weight of empty storage jar (WJ) 309.95g Weight of jar + sample (WJ+S) 399.83g Sample in jar = (WJ+S – WJ) 89.88g Empty aerosol can = Wcan 38.78g Total sample weight in can: Wts = (Wun – Wcan) 108.34g

MULTI-PHASE CONT.

Dilute multi-phase into single phase solution Use THF, IPA, and Hexane in varying quantities

Each product is different, there are no hard and fast rules for diluting

THF and IPA have different, but overlapping, solubility ranges

Hexane can be used to clarify solution After merging of phases, analysis must be

performed within 24 hours!

MULTI-PHASE CONT.

Theo. Concentration (mg/mL) = (Wts)(% Label Claim Picaridin)

Final Dilution

Total weight already has propellant factored in.

HORWITZ

SampleSportsmen Gear

Smart

Analyte Picaridin Uniform Samples Nonuniform Samples

Claim % HCV % HSD Claim-3HSD Claim+6HSD Claim-4HSD Claim+8HSD

15.0 2.661 0.39915 13.8026 17.3949 13.4034 18.1932

Limits

Upper LowerConc. Range

PICARIDIN

PICARIDIN GC/FIDArea Ratio

 

 Processing

 Method:

 Tuesday Date Calibrated:

 5/1/2013 6:41:20 AM EDT

Processing Method ID: 1456 System: 6890_01 Channel:   HP6890 Ch2 Calibration ID: 1457

 

Slope: 4.228918 Intercept: -0.015629

R: 0.999941 R^2 0.999881

 Calibration Plot

   

1.40   

1.20   

1.00   

0.80   

0.60   

0.40   

0.20   

0.00 0.00 0.05 0.10 0.15 0.20 0.25 0.30

Amount

GROUP 1 RESULTS

Sample ID Weight (mg) Final Du % Picaridin Claimed

% Picaridin Found % of Claim

OTT CMD 5120.00 5000 15.0 9.506 63.37OTT DCB 6500.00 5000 15.0 9.184 61.23OTT TS 6400.00 5000 15.0 8.222 54.81OTT VG 6610.00 5000 15.0 4.944 32.96

Sample ID Weight (mg) Final Du % PicaridinClaimed

% PicaridinFound % Propellant % Picaridin

Corrected % of Claim

TE CMD 5120.00 5000 15.0 18.754 7.78 17.29 115.30TE DCB 6500.00 5000 15.0 13.557 7.29 12.57 83.79TE TS 6400.00 5000 15.0 15.061 8.94 13.71 91.43TE VG 6610.00 5000 15.0 15.315 8.00 14.09 93.93

Sample ID Weight (mg) Final Du % PicaridinClaimed

% PicaridinFound % Propellant % Picaridin

Corrected % of Claim

QC05-0734 14984.02 5000 7.0 6.901 n/a n/a 98.59TE NCW 6704.41 5000 15.0 15.113 9.66 13.65 91.02

GROUP II

Sample ID Weight (mg) Final Du % Picaridin Claimed

% PicaridinFound % of Claim

OTT MV 6380.00 5000 15.0 9.926 66.17

OTT MB 6080.00 5000 15.0 10.129 67.53

OTT JS 4240.00 5000 15.0 12.398 82.65

Sample ID Weight (mg) Final Du % PicaridinClaimed

% PicaridinFound % Propellant % Picaridin

Corrected % of Claim

TE MV 6650.00 5000 15.0 18.168 8.17 16.68 111.22

TE MB 6660.00 5000 15.0 17.438 8.56 15.95 106.30

TE JS 6720.00 5000 15.0 17.926 8.54 16.40 109.30

Sample ID Weight (mg) Final Du % PicaridinClaimed

% PicaridinFound % Propellant % Picaridin

Corrected % of Claim

QC05-0734 14984.02 5000 7.0 6.933 n/a n/a 99.04

TE NCW 6704.41 5000 15.0 15.181 9.66 13.71 91.43