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ANR Analytical Lab

Quality Assurance Manual

August 25, 2006

University of California, Davis 207 Hoagland Hall One Shields Avenue Davis, CA, USA 95616-8627 Phone: 530-752-0147 Email: [email protected] Web Site: http://danranlab.ucanr.org

ANR Analytical Laboratory QA Manual

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TABLE OF CONTENTS

CHAPTER ONE - Introduction 1.1 Mission Statement 1.2 Core Values 1.3 Ethics Policy 1.4 Good Laboratory Practices 1.5 Confidentiality 1.6 Complaint Resolution CHAPTER TWO - Organization and Structure 2.1 Organization Structure 2.2 Floor Plan 2.3 Instrumental Services 2.4 Testing Services 2.5 Procedures CHAPTER THREE ­ Operational Procedures 3.1 Sample Submission 3.2 Sample Log-in 3.3 Chain-of-Custody 3.4 Client Notification of Sample Receipt 3.5 Sample Storage Prior to Analysis 3.6 Processing and Retention of Client Sampling Documents 3.7 Job Tracking 3.8 Data Reporting 3.9 Storage of Completed Samples, Reports, Data and Job Envelopes 3.10 Shipping and Receiving CHAPTER FOUR - Laboratory Quality Control 4.1 Internal Quality Control 4.2 Blind Duplicates 4.3 External Quality Control Programs 4.4 Corrective Action 4.5 Laboratory Control Standards - Reference Materials 4.6 Data Packages and Data Review 4.7 Quality Assurance Audits CHAPTER FIVE ­ Laboratory Operations 5.1 Instrument Maintenance Logs 5.2 Instrument Calibration and Standard Operating Conditions 5.3 Instrument Performance Checks 5.4 Calibration of Support Equipment

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Chapter 1: Introduction

The ANR Analytical Laboratory, established in 1950, is a high production analytical laboratory specializing in chemical analysis. The Laboratory performs analyses on selected chemical constituents of soil, plant, water, wastewater, and feed, using state-of­the-art analytical equipment. Technical staff is comprised of trained and educated chemists. The Laboratory has in place a training program to ensure that staff chemists are kept up-to-date on any method changes, SOP changes, instrument additions, and Good Lab Practices. The Laboratory has a strict Quality Assurance program. High quality of work is a prerequisite in serving clients' needs. ANR Analytical Laboratory clients are County Advisors, Extension Specialists and University of California academics. The Laboratory performs over 250,000 tests per year. The Lab also accepts samples from other educational institutions and government agencies on a limited basis. The Quality Assurance Manual describes the procedures that are followed to monitor the quality of work. Chapter 1: Introduction. Includes ANR Analytical Laboratory Mission Statement, Core Values, and Ethics Statement, Good Lab Practices, Confidentially Statement and Complaint Resolution. Organization and Services. Describes the organization, services offered, and summarizes the analytical procedures used. Included is an organizational chart and floor plan of the laboratory. Operational Procedures. Describes the procedures that are used to log, track, and store samples, analytical data and reports. Laboratory Quality Control. Describes the procedures used to monitor the precision and accuracy of data. Laboratory Operations. Lists various laboratory quality assurance procedures.

Chapter 2:

Chapter 3: Chapter 4: Chapter 5:

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1.1 Mission Statement To provide precise and accurate analyses of soil, plant, water, feed and other samples at a low cost and in a reasonable period of time.

1.2 Core Values At the ANR Analytical Lab we hold the following principles and values to be the most important, and we consider these values in making decisions: · honesty · safety of our employees and community · good science · fairness · quality 1.3 Ethics Policy Ethics is a set of moral principles, a code for right and wrong, or behavior which conforms to accepted professional practices. All employees at all times shall conduct themselves in an honest and ethical manner. Examples of unethical behavior include, but are not limited to the following: · Improper manipulation of data or software · Improper handling of data errors, non-compliant data, or QC outliers · Lack of reporting unethical behavior by others · Artificially fabricating results · Misrepresenting data such as peak integration, calibration, tuning, or system suitability · Improper clock setting to meet holding times · Intentional deletion of non-compliant data An employee must report any suspected unethical behavior or fraudulent activities to a supervisor. An employee has the right to remain anonymous. 1.4 Good Laboratory Practices (GLP) While GLP regulations under FDA and EPA refer to specific regulated activities, the ANR Analytical Laboratory follows many of the GLP practices as standard procedures. Quality Control (QC) refers to steps taken by the analysts to ensure and monitor precision and accuracy. Quality Assurance (QA) is a completely separate and independent monitor of the study and QC activities. The ANR Analytical Laboratory provides independent QC and QA functions. This manual provides a brief description of both.

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1.5 Confidentiality Client information is confidential and will not be discussed with anyone, even those affiliated with the client not designated as a contact, without permission from the client. Confidential information includes test results, origin of samples, business relationship with the client, any procedures and testing that they conduct or investigate, and information about their research. 1.6 Complaint Resolution Anytime a serious complaint is received, it is brought to the attention of Laboratory Director, recorded for a permanent record, tracked to ensure resolution. A serious complaint is one that questions the validity of results. The nature of the complaint is documented following the procedure for a nonconforming QC result. After resolution, the client is contacted for final comments. A permanent record is kept by the Quality Assurance Officer.

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Chapter 2: Organization and Services

2.1 Organization Structure The laboratory is divided into four (4) groups in the following manner: Group Laboratory Administrative Information Technology Lab Support Components Analytical Testing Administrative Management and Support IT Support Sample Receiving and Preparation

An organizational chart appears in Figure 1. Group leaders are responsible for administrative management, assigning work to individual members of the group, organizing the work efforts, reviewing data, and helping solve analytical problems.

Director / Acting QA Officer Dirk Holstege

Management Services Officer Nikki Schwab

Programmer YanPing Zuo

Programmer / Analyst Gail Nishimoto

Lab Supervisor Traci Francis

QA Officer Open

Administrative Assistant Leah Montez

Student Assistants 1.0 FTE

Receiving Area Manager Gary Chan

Supervising Chemist Open

Chemist Irenee Ramirez

Chemist J. Marcos Jimenez

Student Assistants 0.5 FTE

Lab Assistant Sarah Tran

Lab Assistant Olga Kovaleva

Chemist Kelly Gardner

Chemist Rani Singh

Student Assistants 3.0 FTE

Figure 1 ­ Organizational Chart

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2.2 Floor plan A floor plan is provided in Figure 2. The ANR Analytical Laboratory space is approximately 5250 square feet. The floor space is assigned in the following manner: Application Wet Chemistry Instrument Lab Sample Storage Administrative Offices IT Office Sample Preparation/Storage Rooms 213, 208, 252, 206 222 205X, 205Y 207 227 Annex 110 Space (sq ft) 2660 245 330 303 143 780

Figure 2 - ANR Analytical Laboratory Space

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2.3 Instrument Services The Laboratory maintains state-of-the-art analytical equipment. Major pieces of equipment include: · Thermo Iris inductively coupled plasma emission spectrometer (ICP-AES) · Perkin-Elmer/Sciex API 2000 HPLC/MS/MS · Perkin-Elmer AAnalyst 800 flame/graphite furnace atomic absorption spectrometer · Perkin-Elmer AAnayst 200 flame atomic absorption spectrometer (AA) · CEM microwave sample digestion system · Lachat Flow Injection Analyzers (FIA) · Timberline Flow Injection Ammonium Analyzer · Leco-FP528 Nitrogen Analyzer · Thermo-Finnegan Series 1112 carbon/nitrogen analyzer · Dionex ICS-2000 Ion Chromatograph The ICP-AES instrument can be used for an hourly charge by UC researchers. The LC/MS/MS can be used for a daily fee by UC researchers. 2.4 Testing Services Soils Testing · Salinity/Alkalinity/Toxicity (saturation extract): SP, pH, EC, SAR, ESP, HCO3, CO3, Ca, Mg, Na, Cl, B, K, SO4-S. · Fertility (nutrient status): DTPA Extractables: Zn, Mn, Fe, Cu, N, TKN, NH4N, NO3N Exchangeables: X-K, X-Ca, X-Mg, X-Na Olsen-P, Bray-P, SO4S (CaPO4 extract) · Characteristics: Cation Exchange Capacity, Organic Matter, Particle Size Analysis (Sand/Silt/Clay), CaCO3, Lime Requirement, Bulk Density · Moisture Retention Analysis (1/3, 1, 5, 10 and 15 atm) · Elements (Totals): As, C, Cd, Cr, Cu, Fe, Mn, Ni, Pb, Se, Zn Plant and Feed Testing · Total C and N · Total Nutrients: B, Ca, Cu, Fe, Mg, Mn, Mo, Na, P, S, Zn · Extractable Nutrients: Cl, K, NH4-N, NO3-N, PO4-P, SO4-S · Elements (Totals): Al, As, Ba, Cd, Co, Cr, Hg, Ni, Pb Se, Si, V · Acid Detergent Fiber, Neutral Detergent Fiber, Lignin

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· · · ·

Ash Content, Dry Matter Carbohydrates (Fructose, Glucose, Sucrose, Sorbitol) Starch Crude Protein

Water and Wastewater Testing · Salinity, alkalinity and toxicity characteristics: Alkalinity, NH4-N, NO3-N HCO3, CO3, Cl, pH, SO4-S, Electrical Conductivity Exchangeable Sodium Percent, Sodium Adsorption Ratio, Hardness TKN Total Solids, Total Dissolved Solids, Total Suspended Solids. · Elements (Solubles): Al, B, Ca, Cu, Fe, Mg, Mn, P, K, Na, Zn · Elements (Totals): Al, B, Cd, Ca, Cr, Cu, Fe, Pb, Mg, Mn, Mo, Ni, P, K, Se, Si, Na, S, Zn

2.5 Procedures Routine methods are documented in the ANR Analytical Laboratory Standard Operating Procedures (SOP) manual. SOPs are reviewed annually and revised periodically as needed; revision dates and summary of changes are documented in each SOP. Original copies and computer files are kept in a secure place. Copies are controlled and kept in each staff member's individual SOP Manual. The references used for each method are documented in the SOPs.

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Chapter 3: Operational Procedures

3.1 Sample Submission Typically, samples are collected by the Client in the Field. When samples are shipped to the Laboratory, a Laboratory Work Request Form is provided by the Client with each sample batch up to 100 samples. The Work Request Form documents the sampling, holding, and shipment of samples from the Client to the Laboratory. At the Laboratory, the Work Request Form also serves as the Client's request/order to perform specific tests requested by the customer. 3.2 Sample Log-In Samples are received in the Sample Receiving area (110 Hoagland Annex) where the Receiving Manager or trained personnel are responsible for logging in the samples in accordance with the Sample Receiving SOP (SOP 2010). At login, each client uses a customized work request form that has the following information: · Client ID (assigned by the Lab) · Client Name / phone number / E-mail / Alternate Contact information · Billing information · Number of samples · Sample information and descriptions · Desired sample disposition on completion of the testing · Required sample preparation · Tests requested · Signature of the Client or responsible party · Delivery method or name of person delivering samples A sequential number is assigned to each Work Request. 3.3 Chain of Custody The location of the samples are tracked internally using a bar-coding system. Internal tracking of sample location is followed for all samples. External Chain-ofCustody (CoC) procedures are followed for samples received with CoC forms. The CoC record is used to document the change in possession from sampling to delivery to receipt by the laboratory. Each sample must be clearly identifiable. The condition of the sample is noted upon receipt. Signatures of parties relinquishing custody as well as the date are documented on the form Work Request Form and any external CoC form. 3.4 Client Notification of Sample Receipt The Laboratory Information Management Software (LIMS) organizes the above data in such a manner that log-in entries can be verified, sample progress can be tracked, analytical data can be appended to the record, and final reports can be created. When log-in has been reviewed, a Sample Receipt Confirmation is sent electronically to the Client.

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3.5 Sample Storage Prior to Analysis Samples are logged within one working day of receipt of the samples and a completed Work Request Form. Samples are stored appropriately after receipt. Samples requiring immediate processing such as drying are processed immediately following log-in. Samples that have been logged and processed are stored by Work Request Number. Separate storage is maintained to segregate sample types where cross-contamination is a possibility. 3.6 Processing and Retention of Client Sampling Documents When samples are received from a Client, the Work Request Form and any other chain-of-custody documents provided by the Client are reviewed by the Administrative Group and filed together. Any other written or electronic communications, including the Sample Receipt E-mail are added to this Work Request file. 3.7 Job Tracking A list of outstanding work is prepared daily by the LIMS. An automatic report is generated daily that lists Work Requests for which all work is completed but the final report has not been generated. An automated report listing Rush tests is also printed daily. 3.8 Data Reporting After work is complete, the results are transferred to the LIMS by the chemist. A report is assembled by the chemist and checked by the Lab Supervisor or designated chemist. This report is added to the Work Request file for storage until completion of all work. After all work on a Work Request is completed, the Lab Supervisor or designated chemist checks the complete data package, and submits it to the Administrative Group. The final report and invoice are prepared by the Administrative Group. Completed reports are reviewed and signed by the Lab Supervisor or a Senior Chemist and the Quality Assurance Officer/Lab Director before being sent to the client. The report is compiled in Excel format and delivered by email. 3.9 Storage of Completed Samples, Reports, Data and Work Request Files Approximately four weeks after invoicing, samples are either discarded or returned to the customer per the client selection on the Work Request form. Samples are disposed of following all State and Federal regulations governing disposal. A copy of the signed final report is filed in the Work Request file. Data packages are also filed in the Work Request file. Hard copies of the Work Request files are retained for three years. Computer data files, including scanned data packets, are retained for seven years.

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3.10 Shipping and Receiving The Lab is open for sample receiving from 8:00 a.m. to 5:00 p.m., Monday through Friday, excluding University of California holidays. A drop box is available for after-hours sample drop-off. Late night, weekend, or holiday sample receipt can be arranged. For employee safety, any known sample hazards must be explained in the paperwork sent with samples. All items shipped from the ANR Analytical Laboratory meet DOT regulations.

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Chapter 4: Laboratory Quality Control

The quality control program consists of both internal and external checks on precision and accuracy of analytical results. The responsibility for maintaining the program rests with the Quality Assurance Officer. Independent oversight and monitoring is performed by the Quality Assurance Unit (QAU) composed of the Quality Assurance Officer (QAO) and others as assigned. Employees are trained in quality control and GLP during bimonthly training sessions. 4.1 Internal Quality Control The following QC samples are analyzed with client samples: Blanks A reagent blank is analyzed with every set of samples that are extracted or digested. This reagent blank includes any and all reagents that are used in the analytical process and is carried through the entire process, including extraction and filtering or digestion. Duplicates At least ten percent of samples are analyzed in duplicate to yield data on the precision of the analysis. Duplicate values should typically fall within 8% of each other for all samples unless sample homogeneity is a problem. This information is included in the report. Standard Reference Materials At least one standard reference material is analyzed with each set of samples. The values for the standard reference materials are included in the final report. Samples run with a standard reference material that falls outside the control limit are reanalyzed, including digestion or extraction if necessary. The use of data outside of warning limits is at the discretion of the Lab Supervisor or reviewing analyst. The use of data outside control limits shall be at the discretion of the QAU depending on the needs of the client. Spike Samples Sample fortifications or spikes are used to verify accuracy of tests requiring extensive sample manipulation (such as acid digestion) or for non-standard sample types.

4.2 Blind Duplicates A sub-set of samples that have been analyzed are re-submitted to the Laboratory as new samples, and the results of testing compared to the original analyses.

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4.3 External Quality Control Programs The ANR Analytical Laboratory participates in a number of sample exchange and certification programs. The Laboratory participates in the International Plant Exchange for plants materials and the North American Proficiency Testing Programs for plant materials, soils, water and manure. The Laboratory is certified by the National Forage Testing for the analysis of moisture, crude protein and acid detergent fiber in feed. 4.4 Corrective Action SOP 4200 describes corrective action steps and policies. Whenever a nonconforming result has occurred, the analyst should notify his supervisor and together try to resolve the problem which caused the situation. After resolution, the analyst will continue with the corrective action to bring the analysis back in control. 4.5 Laboratory Control Standards (Reference Materials) The ANR Analytical Laboratory uses standard reference materials from NIST, National Research Council Canada, EPA certified standards, the North American Proficiency Testing program and other sources to check the accuracy of analysis. External reference materials are used whenever possible. If external reference materials are not available for a test, the laboratory uses in-house reference materials. These materials are used to routinely check analysis using control limits from previous data. 4.6 Data Packages and Data Review Raw data is assembled with QC summaries into data packages by the analysts. The data packet includes the Data Transfer Sheet which is produced when the data is transferred into the LIMS. Analyst comments are written on the raw data or Data Transfer Sheet. The data package includes summaries of QC sample performance, such as duplicate, SRM, blank and spike results. Calibration data and QA action forms are included. The data packet is reviewed by the Administrative Group, the Laboratory Supervisor or designated chemist and the QA Officer or Lab Director. The Quality Assurance system of QC procedures, preset QC limits, review of data packages, and approval of reports is designed to catch errors and problems prior to data being reported to clients. However, when corrective action affects previously reported data, the client is notified in writing describing the problem and resolution. 4.7 Quality Assurance Audits A Quality Assurance Audit is performed once per year. The SOPs are reviewed by the Laboratory Supervisor and QA Officer. Results of proficiency and QC tests are examined and control and warning limits for QC samples are reviewed and modified as necessary. The non-conforming QC results are examined. Action plans for SOP improvement are created based on the findings of the audit.

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Chapter 5: Laboratory Operations

5.1 Instrument Maintenance Logs A Log for each listed Instrument, uniquely named, is located in the Laboratory next to the Instrument. Operators are to include in each Instrument Log a continuous record of its life in the lab including problems, repairs, and maintenance actions. 5.2 Instrument Calibration and Standard Operating Conditions Standard Operating Conditions including specifications and settings and instructions for calibrating are contained in specific Analytical Method SOPs. 5.3 Instrument Performance Checks A description of how to evaluate instrument performance by performance checks is contained in the individual Analytical Method SOPs including analysis of Calibration Curves, Check Standards, and Laboratory Control Samples. If an analysis fails to meet performance criteria, the cause is investigated. 5.4 Calibration of Support Equipment Analytical Balances are checked by placing in-house weights on the balance once per month. If a balance does not produce a reading within 0.1% of the labeled value of the weight, the balance is taken out of service for repair. Balances are cleaned and calibrated against NIST traceable weights once per year. Pipettes and Pipettors are calibrated and checked, at least semi-annually, by delivering the exact amount and type of solvent corresponding to their planned use and weighing the amount of solvent delivered on a NIST-traceable balance. Any pipette or pipettor which can not be adjusted to deliver a weight of solvent within 2% of the required weight (based on the solvent density and desired volume) is taken out of service for repair or replacement. The nominal temperature for each laboratory refrigerator is 2°-8° C and each freezer is <-5° C. Temperatures are recorded on the log attached to each unit on a weekly basis or as needed. All exhaust or fume hoods are checked annually for average face velocity with the sash open to the indicated mark. Test records are maintained on a card located at the hood along with the test date and the initials of the individual performing the test. Target face velocity is 100 linear feet per minute (fpm).

Revision History

· · Origination Date: April 1, 2005 by Dirk Holstege Updated : May 22, 2006 by Dirk Holstege

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ANR Analytical Laboratory QA Manual

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