Pharmco Product, Inc. SOP # : 7-5-1-E & 8-2-4-A Rev 2.4 3/31/06 Subject: Sample Collection EF -1- SOP 7-5-1-E & 8-2-4-A Created by Paul DiMarco Approval/Effective Date: 01/01/2002 1.) Scope: This procedure provides general instructions for collecting samples of all shipments and finished products at Pharmco Products, Inc. 2.) Normative References: SOP 4-2-2 Quality Manual SOP 4-2-3-F MSDS’s SOP 6-2-2-A Hazardous Communication Program SOP 6-2-2-C Chemical Hygiene Plan SOP 6-2-2-D Personal Protective Equipment Program SOP 6-2-2-I OSHA Formaldehyde and Methylene Chloride Rule SOP 7-4-3-A Testing of Incoming Chemicals SOP 7-4-3-B Testing of Incoming Denaturant Raw Materials SOP 7-5-1-G cGMP Procedures SOP 7-5-3-A Lot, Batch & Serial Numbering System SOP 7-5-3-B Retain Sample Program WI 040601 QC Sample Collection 3.) Terms and Definitions: Bulk Chemical: Raw material supplied to Pharmco by railcar or tank truck. This could include tote shipments. Finished Products: Products that ship with a Pharmco Label or in bulk to a customer with a Pharmco BOL. Batch Record: Document that details the materials and production processes for a particular production run. Pure Ethanol: Any ethanol product that consists of pure ethanol or a mixture of pure ethanol and water. Denatured Ethanol: Ethanol that is rendered unfit for drinking purposes as designated by the Bureau of Alcohol Tobacco and Firearms (BATF) Specially Denatured Alcohol: Specially denatured alcohol (SDA) is a type of denatured alcohol. SDA is often used in industry. If a customer wants to purchase more than 5 gallons of SDA in one year, that customer must obtain a permit from the BATF. Pharmco Product, Inc. SOP # : 7-5-1-E & 8-2-4-A Rev 2.4 3/31/06 Subject: Sample Collection EF -2- SOP 7-5-1-E & 8-2-4-A Created by Paul DiMarco Approval/Effective Date: 01/01/2002 Completely Denatured Alcohol: Completely denatured alcohol (CDA) is a type of denatured alcohol. Due to its odor and other properties, the use of CDA is limited. A customer does not need a permit to purchase this type of alcohol. Cut Alcohol: Pure Ethanol that has been blended with water to reduce the proof of the finished product. Ethanol Solvents: Ethanol based formulas approved by the Bureau of Alcohol, Tobacco and Firearms for use as a solvent. Reagent Solvents: Non Ethanol Based Solvents which are single component chemical liquids, i.e. Acetone, IPA, Methanol. COA: Certificate of analysis. The actual chemical analysis for that particular lot of chemicals. COA Template: The original or master document for COA’s for each chemical. The template lists each specification required in the chemical product monograph, i.e. the product “Grade” designation. The template also lists the product limits (maximum and minimum requirements) for each specification. Currently the template lists a set of data for these specification (results) from some previous testing review. For new chemicals, the template is created from the original testing review. When the validation study is complete on a particular chemical, these results will be coded to tell the reviewer which results came from the validation study, which came from in-house testing and which came from the vendor certificate of analysis. The COA Template in most cases should (but does not necessarily have to) match the specifications on the product label. Product File: Product documentation verifying origin of manufacturing site, receipt, source, quality review and ultimate disposition for each lot of chemicals moving through our facility. Product files are used for all chemicals raw materials. Individual package sessions of a particular lot is controlled through the use of batch records. Example: chemicals packaged on our high speed, automated filling equipment or otherwise processed through our bulk terminal. This file contains information for each lot of every Reagent and Specialty chemical purchased. The information in each product file is as listed on FormQA100. Product files are also the vehicles by which the correct labels are produced for finished product manufactured from in-bound raw material. Product files are also the vehicles by which labels are generated for all manufacturing done off premises. Release Label: A label applied to inbound raw material to release it for use by Pharmco Product, Inc. SOP # : 7-5-1-E & 8-2-4-A Rev 2.4 3/31/06 Subject: Sample Collection EF -3- SOP 7-5-1-E & 8-2-4-A Created by Paul DiMarco Approval/Effective Date: 01/01/2002 production. This label also meets the HMIS requirements for chemicals stored in our warehouse. The release label states product name, primary hazard, CAS number, lot number, purchase order #, the NFPA rating and diamond for the product, and is signed and dated by the person receiving the product. Testing Review: Process by which the certification requirements are reviewed for a particular lot of chemicals. A testing review is conducted for all product files. 4.) Application: All raw materials and finished product requiring samples. All personnel involved in sample collection. 5.) Text: All chemical raw materials receive a full quality review according to SOP 7-5-1-A. All work done on the raw material is documented in the product file. Denaturant raw materials are sampled by production and then sent to QC for analysis. Reagent and specialty chemicals received in drums are sampled by production staff under the supervision of QC personnel. Composite sample compiled of aliquots pulled at random from the representative number of drums (√n +1) is sent to QC for analysis. Bulk Raw Materials and Finished Products are sampled by production staff. If materials are received in a multi-compartment tanker, it is the responsibility of the Quality Control staff to oversee sampling of the tanker. It is Pharmco’s policy to take one sample from each compartment of the bulk load. Pharmco accepts this sample of each compartment as being representative of the compartment of the bulk load. All samples of inbound raw materials in bulk and outbound bulk shipments are to be handled according to the following procedure: 1. All samples are to be taken using clean stainless steel sampler with the chain by submerging sampler completely into the material. 2. Sample is transferred into new pint size bottle and capped immediately with the new cap. Pharmco Product, Inc. SOP # : 7-5-1-E & 8-2-4-A Rev 2.4 3/31/06 Subject: Sample Collection EF -4- SOP 7-5-1-E & 8-2-4-A Created by Paul DiMarco Approval/Effective Date: 01/01/2002 3. Bottle and cap must be checked for cleanliness before sample transfer. 4. Bottle must be rinsed with product from vessel before sample transfer. 5. Bottle must be clearly marked with the product name and lot number, vendor’s name, vehicle information (e.g. tank car number and compartment number, if applicable), and the date. 6. Sample is taken to QC for quality review. The following procedure is used for sampling finished product or in-process samples. 1. The beaker to be used for sample collection must be clean. Samplers may be used to take a sample from the finished product container or samples can be taken directly from the filling hose. 2. If the sample is taken directly from the bottling line, the bottle must be capped. 3. The sample container must be appropriately identified. It must be delivered to the lab with the appropriate paperwork. If the sample is a filled product package (e.g. pint bottle, gallon bottle), the first filled product package must be sent to the laboratory for analysis. This sample is accepted as a representative sample for the entire run. If the sample is to be taken directly from the line, the product is filled directly into a sample beaker. This sample is accepted as a representative sample for the entire run. One container of production run is sampled. It is Pharmco’s policy to accept this as a representative sample of all of the containers filled in the specific production run. General Information: All Pharmco employees taking samples must read the MSDS for the product prior to sampling or at some point in the past. See SOP 4-2-3-F MSDS Generation and Training and SOP 6-2-2-A Hazardous Communication Program for additional information. All Pharmco employees taking samples must read and follow SOP 6-2-2-C Chemical Hygiene Plan. Pharmco Product, Inc. SOP # : 7-5-1-E & 8-2-4-A Rev 2.4 3/31/06 Subject: Sample Collection EF -5- SOP 7-5-1-E & 8-2-4-A Created by Paul DiMarco Approval/Effective Date: 01/01/2002 All Pharmco employees taking samples must wear appropriate protective gear. Refer to SOP 6-2-2-D Personal Protective Equipment Program for additional information. Any employee taking a sample of Methylene Chloride must read SOP 6-2-2-I OSHA Formaldehyde and Methylene Chloride Rule. See Work Instruction WI040601 - QC Sample Collection for more information. Revision History Revision # Revision Date Revision History started on 2.4 3/31/06 3/31/06 Revised by Reason for Revision EF EF Clarify procedure for sampling bulk materials using stainless steel sampler. This printed document was printed on: 3/12/2007. This printed document is valid for 5 days after the print date. All obsolete documents must be appropriately marked or discarded.