D-122

Laboratory Operations

Section D — Laboratory Operations and Specifications Revision 0 16 pages

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1.0 Purpose 
 
 The objective of the Laboratory Operations process is to perform testing services meeting
 customer requirements, according to applicable test methods and in conformance with ISO 17025
 
 requirements. 
 
 The purpose of this procedure is to describe the method by which laboratory operations activities
 
 are conducted under controlled conditions to ensure that tests are completed using validated test
 methods and to ensure that customer requirements are met. This procedure also addresses the
 
 treatment of lab nonconforming work discovered before, during and after laboratory operations
 are completed. 
 
 2.0 Scope 
 This procedure applies to all ISO 17025 accredited testing activities. 
 
 3.0 Responsibility and Applicability 
 
 3.1 This procedure applies to all QC laboratory personnel, which includes QC Laboratory
 Management, QC Laboratory Analysts, QC Laboratory Technicians, and others as
 
 designated who perform accredited testing activities. 
 
 3.2 QC laboratory personnel are responsible for, and authorized to, perform their assigned
 activities and to react appropriately to those results. 
 
 3.3. QC laboratory personnel are also responsible for and authorized to stop testing when
 problems are discovered and to control further testing while management is notified for
 
 resolution. 
 
 3.4 QC Laboratory Management is responsible for authorizing specific personnel to perform
 specific types of laboratory tasks, to perform accredited testing, and to operate types of
 
 equipment. 
 
 
 

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 3.5 QC Laboratory Management is responsible for providing opinions and interpretations to
 persons external to the Lab. 
 
 3.6 QC Laboratory Management is responsible for and authorized to develop, validate, and
 approve lab developed test methods and changes to test methods if lab-developed or non-
 
 standard methods are used (refer to D-103 Analytical Method Validation and
 Verification). 
 
 3.7 Responsibilities regarding Lab nonconforming work (section 11.4 below) are as follows:
 
 3.7.1.1 Evaluate significance: QC Laboratory Management 
 
 3.7.1.2 Disposition authority: QC Laboratory Management 
 
 3.7.1.3 Authorize resumption of work: QC Laboratory Management 
 
 3.8 QC Laboratory Management is responsible for establishing lab work priorities/schedules
 and for communicating priorities to QC laboratory personnel accordingly. QC Laboratory
 
 Management is responsible for identifying infrastructure/work environment resource
 needs. 
 
 3.9 QC Laboratory Management, and QC Laboratory Analysts or Technicians are responsible
 
 for monitoring supplies and equipment to the extent they affect testing activities and
 quality. (Resource needs are fulfilled according to SOPs E-601 Vendor Qualification, D-
 
 117 Laboratory Purchasing and Receiving, or hired according to SOP A-113 Training
 
 Procedure, A-117 Personnel Qualifications, and D-120 Laboratory Management
 Structure and Position Requirements). 
 
 3.10 QC Laboratory Management is responsible for ensuring that this procedure is accurate,
 understood and implemented effectively. This procedure may not be changed without
 
 the authorization of QC Laboratory Management. 
 
 4.0 References 
 
 4.1 D-103, SOP, Analytical Method Validation and Verification 
 
 4.2 E-601, SOP, Vendor Qualification 
 
 4.3 D-117, SOP, Laboratory Purchasing and Receiving 
 
 
 

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 4.4 A-113, SOP, Training Procedure 
 A-117, SOP, Personnel Qualifications 
4.5 4.6 D-120, SOP, Laboratory Management Structure and Position Requirements
 
 4.7 G-208, SOP, Analytical Calibration and Equipment Control 
 
 4.8 QS-108, SOP, Corrective and Preventative Action (CAPA) 
 
 4.9 D-118, SOP, Laboratory Quality Assurance Activities Plan (Proficiency Testing)
 
 4.10 D-101, SOP, Laboratory Housekeeping 
 
 4.11 D-602, SOP, Labeling and Expiration Dating of Laboratory Chemicals
 
 4.12 D-105, SOP, Out of Specification / Out of Trend Investigation 
 
 4.13 C-502, SOP, Record Storage, Retention, and Destruction 
 
 4.14 D-119, SOP, Sales — Laboratory Sample Submission 
 
 5.0 General 
 
 5.1 QC Laboratory personnel handle customers’ samples, lab reference standards and
 reference materials, and equipment in such a manner as to ensure their own safety and
 
 the safety of others. QC laboratory personnel take care to handle and store customers’
 samples, lab reference standards and reference materials in such a manner as to maintain
 
 their identification and traceability and to preserve their conformity with no
 contamination, loss, or damage to the item during handling, transporting, storing/waiting,
 
 and preparation for testing. 
 
5.2 Competent QC laboratory personnel conduct testing service activities according to test

 methods, written instructions, or according to good laboratory practices and procedures
 to which they have been trained. QC laboratory personnel have access to equipment
 (including, but not limited to, instruments, software, measurement standards, reference
 
 materials, reference data, reagents, consumables, or auxiliary apparatus) that is required
 
 for the correct performance of laboratory activities and that can influence the results.
 
 
 

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 5.3 All internal or external personnel working in the QC laboratory and/or affiliated with lab
 testing services, that can influence the QC laboratory’s activities shall act impartially, be
 
 competent and work in accordance with LMS. 
 5.4 QC laboratory personnel are trained in the handling and use of calibrated equipment to
 
 ensure continued accuracy of measurements and continued fitness of the instruments. All
 
 equipment used for lab testing, including equipment for subsidiary measurements (e.g.,
 for environmental conditions) having a significant effect on the accuracy or validity of
 
 the testing results are calibrated before being put into service. This equipment is
 controlled according to the G-208 Analytical Calibration and Equipment Control.
 
 5.5 Records of the relevant authorizations are maintained in job descriptions and this
 
 procedure. The competence, educational and professional qualifications, training, skills,
 and experience of the QC laboratory personnel, including contracted personnel, are
 
 maintained in the training records in accordance with SOP A-113 Training Procedure, A-
 117 Personnel Qualifications, and D-120 Laboratory Management Structure and Position
 
 Requirements. Roles and responsibilities are also identified in this procedure.
 
 5.6 Any customer property that is in the facility and becomes lost or unintentionally damaged
 will be brought to the attention of Quality Management, or QC Laboratory Management
 
 who will ensure the incident is recorded on the Quality Events Log and reported to the
 customer. As appropriate, Quality Management or QC Laboratory Management will
 
 initiate a corrective action and inform the customer of the problem as well as any actions
 taken to avoid its recurrence in accordance with SOP QS-108 Corrective and Preventative
 
 Action (CAPA). 
 
 5.7. Reports are not released for distribution to the customer until all requirements are fulfilled
 (the test results have been reviewed and approved) unless otherwise approved by the
 
 customer. 
 5.8 Testing and/or reports which result in laboratory nonconforming work are recorded and
 
 dispositioned according to section 5.4 of this procedure. 
 5.9 Laboratory testing validity and accuracy are monitored by various means as described in
 
 the D-118 Laboratory Quality Assurance Activities Plan (Proficiency Testing).
 
 
 

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 6.0 Laboratory Accommodation and Environmental Conditions 
 
 6.1 Management ensures that energy sources, lighting and environmental conditions are
 
 adequate to facilitate correct performance of the testing services performed.
 
 6.2 Laboratory personnel performing testing activities ensure that the environmental
 conditions at the time of the testing do not invalidate the results or adversely affect the
 
 quality of any measurement, reference material, reference standard or testing procedure.
 
 Lab testing is not performed at sites other than Ion Labs. 
 
 6.3 The technical requirements for accommodation and environmental conditions that can
 affect the results of the test are documented in test methods (see SOP D-103 Analytical
 
 Method Validation and Verification). 
 
 6.4 Due attention is paid to dust, electromagnetic disturbances, humidity, electrical supply,
 temperature, and vibration levels, as appropriate to the technical activities concerned.
 
 Tests are stopped when the environmental conditions jeopardize the results of the tests.
 
 (It should be noted that radiation and sound levels are not likely present or not likely to
 influence or jeopardize the results of the accredited testing). 
 
 6.5 Should there be a neighboring area in which there are incompatible activities, an effective
 
 separation will be implemented. Measures will be taken to prevent cross-contamination
 if necessary. 
 
 6.6 Top management has determined that the circumstances of the testing activities in the
 
 laboratory and use of areas affecting the quality of the test results do not require controlled
 
 access beyond the current access in place. 
 
 6.7 QC laboratory personnel practice good housekeeping and organization in the lab.
 Established policies such as SOP D-101 Laboratory Housekeeping and D-602 Labeling
 
 and Expiration Dating of Laboratory Chemicals identify requirements and evidence of
 QC laboratory personnel’s awareness is in their training records in accordance with SOP
 
 A-113 Training Procedure and A-117 Personnel Qualifications. 
 
 6.8 The laboratory does not perform sampling, therefore Reports of Sampling” are not
 
 provided. 
 
 
 

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 7.0 Metrological Traceability 
 
 7.1. Equipment used for accredited testing, including equipment for subsidiary measurements
 
 (e.g., for environmental conditions) having a significant effect on the accuracy or validity
 of the testing result is controlled in accordance with SOP G-208 Analytical Calibration
 
 and Equipment Control. 
 
 7.2 Certified reference materials are purchased from accredited reference material producers.
 Measurements are calibrated at appropriate intervals to ensure they maintain validity (see
 
 SOP G-208 Analytical Calibration and Equipment Control). Reference materials are used
 
 prior to their expiration date. 
 
 7.2.1 External calibration services and external certified reference material
 providers are approved in accordance with SOP E-601 Vendor Qualification
 
 and D-117 Laboratory Purchasing and Receiving based on their accreditation
 to ISO 17025 or ISO 17034 as appropriate, which ensures they can
 
 demonstrate competence, measurement capability, and traceability.
 
 7.2.2 The calibration certificates provided by external calibration service providers
 
 for each calibrated or verified measurement equipment and reference standard
 used during calibrations contain the measurement results, including the
 
 measurement uncertainty and a statement of conformity with an identified
 metrological specification, including the decision rule applied.
 
 7.2.3 The certificates for reference materials provided by external reference
 
 material producers contain the standards used, measurement results, including
 
 the measurement uncertainty, and the decision rule applied.
 
 7.3 Currently, there are no testing results that cannot be made or traceable to the International
 System of Units (SI). Direct or indirect comparison to national or international standards
 
 are confirmed. 
 
 8.0 Control of Data 
 
 8.1 Upon completion of any calculations or data transfers, QC laboratory personnel verify
 
 the calculations or transfers are accurate and consistent. 
 
 
 

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 8.2 When mistakes occur in electronic records, measures are taken to avoid loss or change of
 
 original electronic data and may include saving files by other filenames or in locations
 
 that preclude data from being overwritten, thereby allowing original mistaken data to be
 retrieved, or by electronic versioning and dating. 
 
 8.3. Records are revised in accordance with SOP C-502 Record Storage, Retention and
 
 Destruction. 
 
 9.0 Equipment and Maintenance 
 
 9.1 Equipment maintenance requirements are planned and completed in accordance with
 
 SOP G-208 Analytical Calibration and Equipment Control. 
 
 10.0 Process Inputs 
 
 10.1. Inputs to the Laboratory Operations process include, but are not limited to:
 
 10.1.1 Projects generated as the result of the Sales-Laboratory Sample Submissions
 
 process (refer to SOP D-119 Sales — Laboratory Sample Submission).
 
 10.1.2 Existing work priorities established by the current schedule.
 
 11.0 Process Activities 
 
 11.1 Laboratory Operations Planning 
 
 11.1.1 Required testing is planned when samples are received from a customer.
 
 11.1.2 The laboratory’s schedule is derived from pending orders. General planning
 for the laboratory is performed by Laboratory Management. 
 
 11.2 Laboratory Operations and Testing 
 
 11.2.1 According to the order assigned, QC laboratory personnel retrieve the sample
 
 from the sample area and begin to set up the equipment, retrieve the required
 standards and reagents, prepare blanks, etc. Identification and lot traceability,
 
 expiration dates, etc., are recorded as required in the test data.
 
 11.2.2 Abnormalities or departures from normal or specified conditions, as described
 in the test method, are also recorded in the test data. All concerns regarding
 
 
 

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 the suitability of the sample are resolved with Laboratory Management and
 customer, as necessary. 
 
 11.2.3 QC laboratory personnel complete the final adjustments and setups in
 
 accordance with the designated test methods recording actions taken in their
 lab notebook or designated prep sheets. 
 
 11.2.4 All steps in the test method are completed in the order prescribed.
 
 11.2.5 At the completion of the test, the following occurs: 
 
 11.2.5.1 Where applicable, the instrument data files are downloaded and
 stored electronically in the proper folder for the instrument. This
 
 is where the raw data and report are stored for that date.
 
 11.2.5.2 The test area and equipment are cleaned up. 
 
 11.2.5.3. Thesamples are discarded, any sample vessels or pans are cleaned,
 
 and are placed in the designated storage area. 
 
 11.2.5.4 Any issues found during the cleanup are included in the report.
 
 11.2.6 QC laboratory personnel review the resulting data and determine if the results
 indicate retesting is required (where feasible) in accordance with SOP D-105
 
 Out of Specification / Out of Trend Investigation procedure.
 
 11.2.6.1 Ifthe data is acceptable, the report is written. The report is saved
 in the folder as the raw data. 
 
 11.3. Internal Certificate of Analysis 
 
 11.3.1 QC laboratory management has implemented lab notebooks, and data
 collection forms as well as equipment software data collection that ensure
 
 each test or series of tests carried out by laboratory personnel are reported
 accurately, clearly, unambiguously, and objectively, and in accordance with
 
 any specific instructions in the test methods. These documentation methods
 facilitate the identification of factors affecting the measurement result and its
 
 associated measurement uncertainty and enable the repetition of the
 laboratory’s activities under conditions as close as possible to the original.
 
 
 

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 The documentation identifies the laboratory personnel for each lab activity in
 the test. 
 
 1.332 The results are reported in the lab notebooks, data collection forms and
 
 equipment software data collection which includes all information requested
 
 by the customer and necessary for the interpretation of the test results and all
 information required by the method used. 
 
 11,333 The format of the lab notebooks, data collection forms and equipment
 
 software data collection designed to accommodate the testing carried out
 ensuring that the possibility of misunderstanding or misuse is minimized.
 
 11.3.4 The information from the lab notebooks, data collection forms and equipment
 
 software data collection are documented onto the appropriate Certificate of
 
 Analysis by laboratory personnel (see attachment | as an example format).
 
 11.3.5 Quality reviews the records to release. The reviewer verifies the test results
 are provided accurately, clearly, unambiguously, and objectively, and include
 
 all the information agreed upon with the customer and necessary for the
 interpretation of the results and all information required by the method used.
 
 11.3.5.1 Ifthe results are acceptable, the certificate of analysis is released
 
 to the customer. 
 
 11.3.5.2 If the results are not acceptable, Laboratory Management will
 
 initiate the OOS process in accordance with SOP D-105 Out of
 Specification / Out of Trend Investigation. 
 
 11.3.6 Internal Certificates of analysis are provided only to customers. As such, less
 
 formal or simplified reports for test results are permitted. However, if any
 information is not reported to the customer, it will be readily available if
 
 necessary. All issued reports are retained as technical records.
 
 11.3.7 Quality sends the approved Certificate of Analysis to the customer via hard
 
 copy or email. 
 
 11.3.8 If requested by customers, formal Certificate of Analysis include, but are not
 
 
 

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 limited to, the following information (but not necessarily in the order
 indicated) unless Laboratory Management has valid reasons for not doing so,
 
 thereby minimizing any possibility of misunderstanding or misuse):
 
 11.3.8.1 The title (Internal Certificate of Analysis), 
 
 11.3.8.2 Our address which is the location of the where the testing was
 
 carried out, 
 
 11.3.8.3 Unique Identification by Batch# and on each page, the Batch # is
 listed in order to ensure that the page is recognized as a part of the
 
 Certificate of Analysis, and a clear identification of the end of the
 Certificate of Analysis, 
 
 11.3.8.4 Identification of the methods used, 
 
 11.3.8.5 A description of the condition of, and the unambiguous
 identification of the samples by Batch #, 
 
 11.3.8.6 The date(s) of performance of the Lab activities, 
 
 11.3.8.7. The date of issue of the report (QC Reviewed By/Date)
 
 11.3.8.8 The test results with, where appropriate, the units of measure,
 
 11.3.8.9 The identification of the person(s) authorizing the test report (QC
 
 Reviewed By/Date), 
 
 11.3.8.10 Where relevant, a statement to the effect that the results relate only
 
 to the sample tested, 
 
 11.3.8.11 Where necessary, deviations from, additions to, or exclusions from
 the test method, 
 
 11.3.8.12 Information on specific test conditions, such as environmental
 
 conditions, 
 
 11.3.8.13 When customer required, the measurement uncertainty presented
 in the same unit as that of the measured or ina term relative to the
 
 measured (e.g., percent) when: it is relevant to the validity or
 
 
 

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 application of the test results, when a customer’s instructions so
 require, or when the uncertainty affects conformity to a
 
 specification limit, 
 
 11.3.8.14 Where appropriate, opinions and interpretations. 
 
 11.3.9 The Laboratory is not responsible for the sampling activity:
 
 11.3.10 When a statement of conformity to a specification or standard is requested and
 
 provided, the lab documents the decision rule employed, taking into account
 the level of risk (such as a false accept and false reject and statistical
 
 assumptions) associated with the decision rule employed, and apply the design
 
 rule. 
 
 11.3.10.1 The decision rule describes how measurement uncertainty is
 accounted for when stating conformity with a specified
 
 requirement. 
 
 11.3.10.2 If the decision rule is prescribed by the customer, regulations, or
 normative documents, a further consideration of the level of risk is
 
 not necessary. 
 
 11.3.1] The statement of conformity on the Certificate of Analysis clearly identifies:
 
 11.3.11.1 To which results the statement of conformity applies,
 
 11.3.11.2 Which specifications, standards or parts of standards are met or not
 
 met, 
 
 11.3.11.3 The decision rule applied (unless it is inherent in the requested
 specification or standard). 
 
 11.3.12 When opinions and interpretations are included, Laboratory Management,
 
 who are authorized to provide opinions and interpretations, will document the
 basis upon which the opinions and interpretations have been made. Opinions
 
 and interpretations are clearly marked as such on the informal or formal
 
 Certificate of Analysis. 
 
 11.3.12.1 Opinions and interpretations included in a certificate of analysis
 
 
 

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 may comprise, but not be limited to the following: 
 
 11.3.12.2 An opinion on the statement of compliance/noncompliance of the
 results with requirements, 
 
 11.3.12.3 Fulfillment of contractual requirements, 
 
 11.3.12.4 Recommendations on how to use the results, 
 
 11.3.12.5 Guidance to be used for improvements. 
 
 11.3.12.6 When opinions and interpretations by direct dialogue with the
 customer occur, the dialogue is recorded. 
 
 11.3.12.7 Opinions and interpretations are distinguished from statements of
 
 conformity as described above. 
 
 11.3.13 Subcontractors are typically not used for any accredited testing; however, if
 subcontractors are procured to perform testing, Test Reports containing results
 
 of tests performed by subcontractors will clearly identify the subcontractor’s
 
 test results. Laboratory Management ensures subcontractors’ reports are
 provided in writing or electronically. 
 
 11.3.14 |The Laboratory is responsible for all the information provided in the report,
 
 except when information is provided by the customer. Data provided by a
 customer is clearly identified. In addition, a disclaimer is put on the report
 
 when the information is supplied by the customer and can affect the validity
 
 of results. Where the Laboratory has not been responsible for the sampling
 stage (the sample has been provided by the customer, the report states that the
 
 results apply to the sample as received.) 
 
 11.3.15 Issued reports that need to be changed, amended, or re-issued clearly identify
 any change of information and where appropriate, the reason for the change
 
 is included in the report. 
 
 11.3.16 Amendments to an issued Certificate of Analysis, are made only in the form
 of a further document, or data transfer, which includes the statement:
 
 “Supplement to Certificate of Analysis, Batch #,...” or an equivalent form of
 
 
 

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 wording. Such amendments also meet the requirements of this procedure and
 ISO 17025. 
 
 11.3.17 Ifitis necessary to issue a complete, new Certificate of Analysis the document
 
 is uniquely identified and contains a reference to the original Certificate of
 Analysis that it replaces. 
 
 11.4 Laboratory Nonconforming Work 
 
 11.4.1 Nonconforming work is any laboratory activity or the results of lab work that
 do not conform to the Lab’s own procedures or the agreed requirements of the
 
 customer (e.g., equipment or environmental conditions are out of specified
 limits, results of monitoring fail to meet specified criteria). | Lab
 
 nonconforming work consist of, but is not limited to: 
 
 11.4.1.1 a Test Method was not followed properly 
 
 11.4.1.2 incorrect equipment setup 
 
 11.4.1.3 faulty equipment 
 
 11.4.1.4 the incorrect test method was used 
 
 11.4.1.5 measurement equipment with an expired calibration status was
 
 used 
 
 11.4.1.6 inaccurate or incomplete reports 
 
 11.4.1.7 report issued to wrong customer 
 
 11.4.1.8 wrong samples used 
 
 11.4.1.9 sample not stored or identified correctly 
 
 11.4.1.10 actual or potential partiality 
 
 11.4.2 Laboratory nonconforming work information and related disposition
 
 information is captured on the Quality Events Log or in accordance with D-
 105 Out of Specification / Out of Trend Investigation. Laboratory
 
 nonconforming work reporting is entered by either the Laboratory
 Management or the Laboratory Analysts and Technicians. The significance of
 
 

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 the nonconforming work is evaluated to determine if the effect of the incident
 infers the lab’s activities are not in compliance with ISO 17025 or the validity
 
 of the test results are questionable or invalid. 
 
 11.4.3 Actions may include halting or repeating of work and withholding reports
 
 from the customer, as necessary. 
 
 11.4.4 If, upon further evaluation by Laboratory Management, it is determined that
 the testing and/or documentation is conforming after all and therefore the
 
 situation is not nonconforming, the entry on the Quality Events Log is noted
 as such and the testing and documentation is processed accordingly.
 
 12.0 Process Outputs 
 
 12.1 Outputs from the Laboratory Operations process include, but are not limited to:
 
 12.1.1 Completed testing meeting customer requirements, 
 
 12.1.2 The associated records including test reports sent to the customer,
 
 12.1.3 Laboratory nonconforming work and the records of identification and
 
 disposition, which are recorded on the Quality Events Log. 
 
 13.0 Revision History 

| Rev | Date | Description of Changes | CCR # | By |
|-----|----------|------------------------|-------|----|
| 0 | 11/05/21 | New procedure. N/A J. Sassman | - | - |

 14.0 Attachments 
 14.1 Attachment 1 — Internal Certificate of Analysis Example 
 
 
 

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 Attachment 1 — Internal Certificate of Analysis 
 
 IANLABS 
 
 Testing Location: 8031 114" Ave, Suite 4000, Largo, FL 33773 Date Received:
 PHONE: 727.527.1072 Date Started: 
 FAX: 727.527.6758 Condition Received: 
 Product Name: Customer Lot Number: 
 Customer: Report Issued Date/ Revision:
 
 INTERNAL CERTIFICATE OF ANALYSIS 
 IDENTITY 
 Date Performed Results Calculated Measurement of
 Test Method Release Specification Uncertainty (if applicable)
 Organoleptic — Appearance D-722 Round tablet with SC&F embossed on one side
 Organoleptic — Color D-722 Off-purple to off-grey with specks 
 Organoleptic — Aroma D-722 Berry 
 Organoleptic - Taste D-722 Sweet 
 COMPOSITION 
 Date Performed Results Calculated Measurement of
 Test Method Release Specification Uncertainty (if applicable)
 Disintegration D-703 NMT 60 Minutes 
 FTIR D-823 NLT 0.90 when compared to the standard 
 
 1 
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 Attachment 1 — Internal Certificate of Analysis (cont'd) 
 
 Testing Location: 8031 114" Ave, Suite 4000, Largo, FL 33773 Date Received:
 PHONE: 727.527.1072 Date Started: 
 FAX: 727.527.6758 Condition Received: 
 Product Name: Customer Lot Number: 
 Customer: Report Issued Date/ Revision:
 
 PURITY 
 Date Performed Results Calculated Measurement of
 Test Method Release Specification Uncertainty (if applicable)
 Total Aerobic Plate Count D-715.0 NMT 1,000 CFU/g 
 Total Yeast and Mold D-715.0 NMT 100 CFU/g 
 E, Coli D-715.0 Absent 
 Salmonella D-715.0 Absent 
 S.aureus D-715.0 Absent 
 P. aeruginosa D-715.0 Absent 
 Coliforms D-715.0 Absent 
 
 QC Reviewed By: Date: 
 
 Note: Sample results apply as received. 
 END OF REPORT 
 
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 Confidential