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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