Cryogenic Grinding of Chewable Gels

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1.0 Purpose 
 
 This document describes the procedure for the cryogenic grinding of chewable gels (gummies).
 
 2.0 Scope 
 
 This procedure applies to any sample preparation involving chewable gels where reducing
 them to powder may be desirable. Examples may include the facilitation of chemical and/or
 microbiological assessments. 
 
 3.0 Responsibility 
 
 3.1 It is the responsibility of QC and Analytical chemists who have verified their ability to
 execute this procedure to follow this procedure. 
 3.2 It is the responsibility of the QC Laboratory Management to implement this procedure
 
 and to ensure that the procedure is being followed. 
 3:3 It is the responsibility of the QC Laboratory Management and AD Personnel to keep
 
 this procedure current with the associated monographs and laboratory practices.
 4.0 Definitions 
 
 4] QC — Quality Control 
 
 4.2 AD — Analytical Development 
 43 Cryogenic — Being or relating to very low temperatures. 
 
 44 LN2 — Liquid Nitrogen 
 
 4.5 Dewar — Vacuum insulated vessel used for storing cryogenic liquids.
 
 4.6 Phase Separator — Metallic frit terminating LN2 transfer line designed to minimize
 hazardous splashing and vaporization. 
 5.0 References 
 
 Si] Liquid Nitrogen Container Handling Instructions — Chart, Inc. Ref 10468660, Rev C,
 
 2010. 
 5.2 Operating Manual for MVE Liquid Nitrogen Dewars — Chart, Inc. Ref 11624417, Rev
 T, 07/19. 
 
 
 

[SOP 

 Standard Operating Procedure SOPNo | Rev 
 
 Cryogenic Grinding of Chewable Gels D-793 0 Page 2 of 3 
 
 5.3 Operating Instructions for Waring Commercial Spice Grinder — Conair, Inc. Ref
 WSG30 IB 08WC050, Rev F IB-8373, 2009, 
 
 6.0 Supplies 
 
 6.1 Chemical — Food Grade or Better 
 
 6.1.1 LN2—180 Liter Dewar @ 22 psi (Airgas P/N NI 180LT22) 
 6.2 Supplies and Hardware 
 
 6.2.1 72” Nitrogen Hose Assembly (Transfer Line) w/ Phase Separator
 
 6.2.2 5 Liter Dewar w/ Pour Spout 
 6.2.3 1 Liter Dewar 
 
 6.3 Equipment 
 
 6.3.1 Waring Commercial Spice Grinder (Waring P/N WSG30) 
 7.0 Procedure 
 
 7.1. CAUTION 
 
 7.1.1 LN2 freezes human tissue almost instantaneously! (At atmospheric pressure,
 LN2 boils at -196°C!) When handling, always wear insulated gloves and safety
 glasses! 
 
 7.1.2 LN2 produces massive volumes of gas that do not support respiration! (1L of
 LN2 vaporizes into ~25 cubic feet of nitrogen gas!) Only use in large, well
 
 ventilated areas! 
 7.2 LN2 Storage & Use 
 
 7.2.1 In order to facilitate use, LN2 is stored / used / dispensed out of three different
 on-site dewars. A 180 liter dewar located in the warehouse provides for bulk
 storage. 
 
 7.2.2 A 5 liter dewar located in the QC Laboratory provides for convenient
 intermediate bulk storage capable of supporting multiple sample preparations.
 
 7.2.3 Individual sample preparations are performed in a 1 liter dewar located in the
 QC Laboratory. 
 
 vee; Sample Preparation 
 731 Connect the 72” Nitrogen Hose Assembly (Transfer Line) w/ Phase Separator to
 
 the 180 liter LN2 tank at the port labeled Liquid. Open the port labeled
 Pressure Building until gas can be heard exiting the safety valve, then close it.
 7.3.2 Place the end of the transfer line into the 5 Liter dewar and slowly open the
 
 Liquid valve. Do not overfill the dewar! When full, the liquid level should be
 
 
 

[SOP 

 Standard Operating Procedure SOP No | Rev 
 Cryogenic Grinding of Chewable Gels D-793 0 Page 3 of 3 
 
 2-4 inches below the shoulder of the dewar. Gently install the dewar cap, being
 
 careful not to damage the delicate Styrofoam cylinder. 
 7.3.3 When ready to powder the chewable gels, precool the removable grinder bowl
 by placing it (with lid attached) into a freezer. 
 
 7.3.4 Gently remove the cap from the 5 liter dewar and apply the pour spout. Tighten
 firmly! 
 
 1:35 Add enough LN2 to the 1 liter dewar to completely submerge the required
 number of chewable gels. Then, with the mouth of the 1 liter dewar pointed
 away from yourself, slowly introduce the gels one or two at a time.
 
 7.3.6 Confirm that the sample is totally submerged, then gently replace the 1 liter
 dewar cap and allow to freeze for 10 minutes. 
 
 13d Decant off the LN2 and transfer the frozen gummies into the cold grinder bowl
 as quickly as possible. Grind to powder and weigh the sample as quickly as
 possible into an appropriately sized beaker. 
 
 7.3.8 Dissolve the powder in the applicable diluent, being attentive (if applicable) to
 any sensitivities (e.g. exposure to light, air, heat etc.) pertinent to the analyte of
 
 interest. Quantitatively transfer the contents of the beaker into the appropriate
 volumetric glassware. 
 
 8.0 Revision History 

| Rev | Date | Description of Changes | CCR # | By |
|-----|----------|------------------------|-------|----|
| 0 | 02/10/20 | New N/A C. Perry | - | - |