Chain of custody; recommendations for acceptance and analysis of evidentiary geochemical samples

U.S. GEOLOGICAL SURVEY CIRCULAR 1138

U.S. GEOLOGICAL SURVEY CIRCULAR 1138

UNITED STATES GOVERNMENT PRINTING OFFICE, WASHINGTON : 1997

BRUCE BABBITT, Secretary

Gordon P. Eaton, Director

CONTENTS

Executive Summary Introduction Sample Control Routine Procedures

Policies Required Prior to Acceptance of Evidentiary Samples

Sample Control Evidentiary Procedures

Sample Preparation of Chain-of-Custody Samples Chain-of-Custody Sample Laboratory Analysis Chain-of-Custody Sample Neutron Activation Analysis Sample Completion and Miscellaneous Information Personnel Policy Governing Chain-of-Custody Samples General Policies Governing Physical Security of Chain-of-Custody Samples

References Appendix 1. Government Cost Estimate Appendix 2. Building 20 Map Appendix 3. Shortened Version of Chain-of-Custody Policies Acknowledgments

FIGURES

Acceptance of Samples Withdrawal of Samples

Federal Center Security Building Security Sample Control Security Sample Preparation Security Laboratory Security Backup Chain-of-Custody Sample Storage Devices Computer Security for Chain of Custody

2. Self-adhesive labels
3. Sample control 3"x5" card
4. Pre-assessment form
5. Chain-of-Custody (COC) form
6. Deliveries to sample control memorandum
7. Low-level Au analysis form

EXECUTIVE SUMMARY

This report details the procedure for handling samples submitted to the Mineral Resource Survey Program (MRSP), formerly the Branch of Geochemistry (BGC). In addition, there are rules required by law when the samples are used as evidence. This report covers both evidentiary and routine samples.

This report includes:

Acceptance of Samples (Nonevidentiary)

Personnel from the Analytical Chemistry Services Group (ACSG), Mineral Resource Survey Program (MRSP), formed a team to determine the policies for acceptance and analysis of geochemical samples. This team contacted law enforcement agencies that handle litigious samples, laboratories that work with samples of a special nature, and the Solicitor General, Department of the Interior. Using the knowledge from these agencies as well as the expertise of our personnel, the following policies have been enacted.

Sample control personnel are responsible for maintaining the chain of custody for all samples submitted to MRSP from submittal to eventual storage. Samples used in litigation are controlled by an even more rigorous set of guidelines to ensure their security. Policies for both the routine chain of custody (COC) procedures and the evidentiary COC procedures are detailed below.

All samples submitted to MRSP must be accompanied by a completed request for analysis (RFA) form (figs. 1A and 1B). The RFA accompanies the samples through the entire system as the accountable record. All important information, such as the evidentiary nature of a sample or high elemental concentration in a sample, is noted on this form along with the requested analysis. All fields noted on the RFA as mandatory must be completed prior to acceptance by sample control.

Samples accepted by sample control personnel are scanned for radioactivity. If samples are above the safe levels defined by the MRSP safety officer, samples are placed in an alternate storage area, and the safety officer is notified. If the safety officer deems the samples unacceptable, the submitter is asked to retrieve them within 30 days. Other samples that might pose a threat to the safety of personnel, such as hazardous waste material, are also referred to the safety officer.

Samples are counted and checked against the RFA. Discrepancies are resolved prior to formal acceptance. The number of samples is recorded in a sample control log book.

The samples are placed on numbered shelves in a holding area for unprepared samples. The shelf number is noted on the RFA and the RFA is forwarded for data entry into the computer.

The information from the RFA is entered in a computer and a job number is issued to each batch. Individual sample numbers are also issued (laboratory numbers). The job number and laboratory numbers are added to the RFA.

A computer printout of the requested analysis, the assigned job number, the laboratory numbers, the submitter’s identifying numbers (usually the field Front of Request for Analysis coding sheet form.

A photocopy of the RFA and computer printout are placed in a loose leaf notebook filed by job number in the sample control area.

Three, 3 "x5"cards are typed and filed (fig. 3). One card is filed in job number order and used for tracking routine samples. A second card is filed in alphabetical order by submitter name and is used to record the date each analysis is completed. The final card is filed in order by lab number as a cross reference permanent storage card.

Figure 2. Self-adhesive labels.

Pre-Assessment Meeting

Figure 3. 3"x5" sample control card.

As laboratory personnel request work, sample control personnel note on the tracking card the location and the date each job is moved. When the samples are returned, the last entry is crossed out with a single line indicating that the samples have been returned to sample control. The samples are then filed numerically by job number on the sample control pending shelves.

The card filed by the submitter name is the record of the chain of analysis. As each requested analysis is completed, the date is noted on the card. Three months after all requested work for a job has been completed, the card is filed in the card permanent storage.

When all work on a job has been completed, sample control personnel file all of the original paperwork in loose leaf computer notebooks by job number. Six months after the completion of analysis, samples of completed jobs are moved to the permanent storage facility.

Prior to sample submittal the project leader(s) requiring strict chain of custody (COC) must meet with all relevant laboratory personnel to discuss details of the project, including the handling, analysis, and final disposition of samples. At this meeting, any concerns, such as the capability of the laboratory to meet the submitters’ needs, are discussed and resolved.

The meeting should include representatives from sample control, computer group, sample preparation laboratory, analytical laboratories, and quality assurance (QA). Items to be discussed include the following: the exact number of samples to be analyzed, the anticipated submittal dates, required data delivery date, necessary sample preparation, laboratory techniques, and a plan to notify the MRSP when litigation is complete. The project leader should discuss the possible hazardous nature of the samples when applicable and any special precautions laboratory personnel should follow when handling the samples. Any desired modifications of the laboratory’s established QA guidelines or data reporting protocols should be clarified. Any changes in the QA guidelines require approval by the laboratory’s QA coordinator. Costs of the routine laboratory work and sample disposal are calculated by the MRSP and the project leader and are presented at this meeting. All meeting information is reported on the pre-assessment meeting form (fig. 4). If the project is a multi-phase or multi-year study, pre-assessment meetings are convened prior to the submittal of samples for each phase or year of the study. The pre-assessment form must be signed by the chief scientist prior to acceptance of COC samples.

Pre-assessment meetings for all projects originating from other Federal agencies (OFA) are conducted by a representative from the requesting agency and a designated MRSP liaison. If an MRSP liaison is the meeting leader, it is his/her responsibility to provide all pertinent information, especially that which relates to the hazardous nature of the samples. The laboratory reserves the right at any time to refuse any sample that exceeds laboratory safety guidelines.

If it is determined at the pre-assessment meeting that the numbers of samples being submitted for COC analysis exceeds the current laboratory capacity, the meeting information is forwarded to a panel convened by the MRSP laboratory manager to resolve the problem. Project leaders and laboratory management incorporate panel recommendations in the final plan.

SAMPLE CONTROL EVIDENTIARY PROCEDURES

Samples that might involve litigation are handled as evidence. A specific set of COC procedures are maintained on all such samples. These samples are subject to the following rules:

• The sample control custodian (SCC) is the designated custodian of evi-
• The SCC is responsible for the primary keys for this area and keeps an
• If emergency personnel, janitorial personnel, or others require access to

dentiary samples and maintains all COC samples, forms, and tracking cards. These are located in a specially designated, locked evidentiary area in the sample control area.

extra set of keys locked in a cabinet in the sample control area. The sample control area is entered using a key card; entry is monitored by the Federal Protective Service (FPS). If the custodian is unavailable, a sample control employee will be authorized to maintain custody and will be given the keys. The security of this area is detailed later in this document.

the sample control area, a visitors log is signed with date, time, and reason for entry. Analysts withdrawing COC samples, who enter the sample control office, also sign the visitors log.

Est. total number of COC samples______________________________

Techniques # COC required samples

Hazardous material Yes_____

(If yes, identify suspected hazardous compounds or items)

reg. samples present

Estimated Cost $_____________ Project ID__________________

Initials of rep. Estimated completion date

Acceptance of Samples

control personnel count and check the samples against the RFA. Any discrepancies are resolved prior to official acceptance of the samples. The SCC has the right to refuse samples as evidentiary, if the sample containers are improperly sealed, damaged, leaking, or the samples themselves are above the levels of toxicity or radioactivity predetermined by the MRSP safety officer. Samples that arrive with incomplete or incorrect paperwork may also be refused. The identifying numbers are recorded on the sample control COC Form (fig. 5), which is maintained in a bound book. Information required includes the number of samples, the type of sample media, the submitter name, and the date and time of acceptance. Both the submitter and the receiver (or the receiver in the presence of the submitter) sign this form. The submitter signs on the line indicating the release of samples; the SCC signs on the line indicating the acceptance of samples. Special notes such as the condition of seals are added to the form prior to both parties signing.

chains and a padlock. Samples that require refrigeration are placed in the refrigerator, which is located in a secured sample preparation laboratory.

control evidentiary holding area. Formally accepted samples are entered into the system as described in the routine section above. The exceptions to the routine procedures are that laboratory and job numbers are added to the COC form, and a fourth 3"x5" card is created. All four cards indicate that these samples are evidentiary. Three of the cards are filed and kept as in the routine procedure. The fourth card is filed in a small file that is kept in the COC area. This card is identical to the other tracking card held in sample control except that individuals requesting custody of samples must sign the COC tracking card with name and date.

Withdrawal of Samples

request withdrawal of COC samples prior to arriving in the sample control area. The analyst meets the SCC in the sample control area and signs the visitors log. The analyst inspects the evidence seals to check that the samples meet standard evidence rules. Samples, either individually sealed or sealed in trays by job, are given to the analyst after the analyst signs the tracking card and the bottom section of the COC form with name, date, time, reason for withdrawal, amount to be used in analysis, and where the samples are to be moved. Samples may then be moved to another secured area. Samples must be returned to sample control as soon as the amount required for analysis has been removed and weighed. Samples are never left unattended or unsecured. The analyst adds any additional notes, such as increased amount of sample withdrawn, to the COC form when the samples are returned to sample control. While the submitter or designated agent of the submitter is present, sample

Samples that require drying in an oven are placed in the oven secured with

Samples that require no refrigeration or drying are locked in the sample

Analysts authorized to work with COC samples must contact the SCC to ______ of ______Pages

Submitted By: Received By: Date/Time Received:

Received By:

(Time and Date)

Mineral Resource Survey Program Chain-of-Custody Form

Job Number:

List Sample Identification Numbers

Custodial Locations Purpose: Location: Number of Samples: Sample Media:

Lab Numbers:

Returned To: (Time and Date)

CHAIN-OF-CUSTODY SAMPLE LABORATORY ANALYSIS

If it is necessary to complete analysis in an area that has been secured with a padlock or dead bolt lock, the analyst signs the tracking card for both the samples and the key for the secured lock. The SCC is the only other individual who has a key to these locks. The analyst must return the key to the SCC as soon as the analysis is complete. When COC samples are in a laboratory, no other samples are permitted in that laboratory to eliminate any possibility of cross-contamination with COC samples. Anyone entering a secured area while COC samples are present must sign a log book with name, date, time, and reason for entry.

COC sample preparation protocol only differs from the standard operating procedure for sample preparation by the additional security and documentation. Physical sample preparation of COC samples is performed in accordance with the quality assurance manual for the Branch of Geochemistry (Arbogast, 1990). Any special preparation instructions, the amount of sample to be prepared, the disposal of excess material and the cost for disposal of any hazardous materials is agreed upon at the pre-assessment meeting.

If any excess sample is being returned to the submitter, a 3-oz unaltered split of the sample is maintained in the locked sample control area until the litigation is completed. All other excess sample is either returned to the submitter or discarded. If hazardous materials/waste disposal costs are incurred, the submitter is responsible.

A trained and certified sample preparation technician accepts the sample(s) from the SCC. The samples are taken to the COC sample preparation laboratory and prepared for analysis. Upon completion of preparation the technician notes on the RFA any problems such as broken seals. The sample preparer’s log book details all steps taken in the processing of samples to allow for recall of these specific samples. The samples and excess bulk, if any, are secured with evidence tape, initialed and dated. They are then returned to the SCC. The SCC checks to ensure all samples are present and sealed properly and signs the bottom section of the COC form, next to the analyst’s name, to indicate the resumption of custody.

After the prepared samples are returned to sample control, laboratory analysts withdraw samples following the procedure discussed above. Samples are moved to secured laboratory areas. Any sample removed from the custodial sample (for example, 10 g for Au analysis) is documented on the COC form. If analysis requires formation of solutions, the solution may be kept in the secured area, but the original sample is returned to sample control as soon as the amount needed for analysis has been weighed and removed.

Routine techniques validated in the quality assurance manual for the Branch of Geochemistry (Arbogast, 1990) are used for the majority of analyses of COC samples. Nonroutine techniques may also be used for the analysis of COC samples, but it then becomes the responsibility of the research scientist to provide the necessary QA/QC information and method references for validation of the research technique to the SCC to be filed with the samples on which the analysis is performed.

Instrument calibration and maintenance are performed according to quality assurance manual (Arbogast, 1990). Instrument calibrations are documented in log books or on computer printouts. The laboratory chief maintains a log of localities for all paperwork not filed with COC samples.

Lab books and log books are bound, and entries are recorded in permanent ink. Lab books contain pertinent information such as job number, name of submitter, sample number, weight of sample, date of preparation, and method of dissolution. A visitor’s log book is kept at the entrance to each COC laboratory to record any entry and departure of non-COC personnel into the secured areas during preparation and (or) analysis of COC samples. The analyst is responsible for placing all data in a secured area during sample analysis (for example, strip charts or graphs). When the analysis is complete, all original data not contained in a notebook is given to the SCC for storage.

CHAIN-OF-CUSTODY SAMPLE NEUTRON ACTIVATION ANALYSIS

Samples are checked out from the SCC in the manner previously described. The samples are then taken directly to Building 15 at the Denver Federal Center, which is a controlled access building where the outside doors are locked at all times. The samples are prepared by heat-sealing the sample split in a polyethylene vial, which protects the integrity of the sample. The sample vials are also imprinted with a sample and irradiation code using a permanent marker. The prepared sample splits are placed in a locked cabinet in the analyst’s office, and any sample beyond the amount needed for this analysis is returned to the SCC. The key for the cabinet is in the possession of the analyst.

Prior to irradiation, the samples are given to the reactor staff for loading in the reactor. The samples remain in the reactor overnight and then are placed in a locked, lead-shielded container in the reactor bay area. This container remains locked until the analyst, who has the only key, removes the samples. The samples are allowed to decay in this container for about 5 or 6 days. After signing the appropriate forms required by the Nuclear Regulatory Commission (NRC), the samples are taken by the analyst to the laboratory in Building 15 and analyzed by routine procedures described in Baedeker and McKown (1987). NRC security procedures are similar to standard evidentiary regulations.

During the analysis, unprocessed spectral data of the samples are transferred from the analyzer to a VAX 750 computer. This spectral data is also copied to a floppy disk. The data disks are locked in the COC cabinet in the analyst office. All of the principal data reduction is performed using the spectral data residing on the VAX computer. Selected data reduction routines are performed on a computer using the spectral data stored on the floppy disks and independent software to verify the primary results. The laboratory and office of the analyst is locked after business hours, and the keys to these areas are held by the analyst.

SAMPLE COMPLETION AND MISCELLANEOUS INFORMATION

Samples that are insufficient for all requested analyses are noted on the RFA and the COC form when they become insufficient. All requested splits are kept in the secured areas with the original samples. Should a portion of the sample be requested for litigation, a split can be made available after permission has been granted by the Solicitor General. The amount of sample removed and the date and time is noted on the COC form.

When all requested analyses are complete, computer printouts of the results are filed in a loose leaf book in the secured sample control area. The samples and all related paperwork are secured until all litigation is complete.

Sample submitters are contacted annually to ascertain the status of the litigation process. When litigation is complete, the submitter is notified to retrieve the samples. A split of the original sample is maintained by MRSP for permanent archive but as a nonevidentiary sample. The evidentiary samples and a copy of all RFA documentation, computer printouts, and results are returned to the submitter who signs the COC card and the COC form, which is filed in sample control.

A room in the preparation area has been provided for sorting large batches of samples which are COC. As this room is shared, there is a limited time available for its use.

Samples that have a short viability (such as water samples) will be held for 6 weeks. At that time they will be returned to the submitter along with a copy of all documentation. The submitter will be required to sign for the samples on the COC card and form.

Samples that are sent through the mail room with evidence tape will not be released by the mail room personnel to anyone but the SCC or designated backup individual (fig. 6).

If the litigation is not completed, the samples and all related documents continue to be held as evidence with all appropriate safe guards. Storage charges may be assessed if storage of more than two years is anticipated or incurred. Figure 6. Deliveries to sample control.

Figure 6. Deliveries to sample control.

Federal Center Security

Information regarding the samples may be released to the submitter only. Any requests for information from anyone other than the submitter are referred to the Solicitor General.

Employee conduct is governed by the Ethics Reform Act of 1989. Details of this act are available in the local personnel office of the U.S. Geological Survey. The guidelines set forth in this act are to be followed by all private (contract) and government employees working on COC samples in this laboratory.

The supervisory sample control specialist serves as the principal COC custodian for the laboratory and is responsible for the coordination of sample submittal, retrieval and storage (short and long term) of samples. A designated individual from sample control serves as a backup COC custodian.

Training documents identify the qualified analysts who can perform a particular procedure or parts of a procedure. Only qualified analysts will perform the requested analyses. Training documentation (fig. 7) is kept and maintained by the quality assurance (QA) coordinator. Analyst performance is routinely checked using quality control (QC) results to demonstrate that the analyst performs under the guidelines set forth under the QA Manual for the MRSP.

COC analysis personnel have work plans that include a critical element governing compliance with COC guidelines. These individuals are all certified by the laboratory chief to handle COC samples.

The chief scientist or the MRSP laboratory manager represent the lab in all court cases where routine procedures are used to analyze COC samples. When nonroutine techniques are used in the analysis of samples it is the research scientist’s responsibility to provide all necessary documentation, QA/QC information, and testimony at any legal proceedings.

The MRSP COC protocol includes three levels of security. The first level controls passage onto the Denver Federal Center (DFC) with a fenced enclosure and entrance guards who record all access of nongovernment employees and all access of government employees after normal business hours. A second level of security is provided by regular police patrols of the DFC by the Federal Protective Service (FPS). The final level is provided by our building security, which is described in detail below. Low-level Au Analysis

Name______________________________________________________________ Job title/Grade_______________________________________________________ Supervisor__________________________________________________________ Date of training initiation______________________________________________

TRAINER MUST INITIAL AND DATE

Not yet In Proficient PROCEDURE trained process

1. Sample weighing

a. Cleaning crucibles and sample weighing

2. Sample digestion

b. Dissolution of samples

3. Au Extractions
4. Flame AA
5. GFAA
6. Cleanup
7. QC paperwork
8. Data sheets

Building Security

oratory facility. These include sample control/sample storage, sample preparation, and a portion of the analytical laboratories. In all three areas, access is controlled through card readers, motion detectors, or deadbolt locks. Only designated personnel that have been approved by management have access to these secured areas. The security system in all three areas can be modified to accommodate approved changes in laboratory personnel. All security measures that have been installed in this facility have been approved by the FPS, who will monitor the installation.

Sample Control Security

and a one-way alarm door. In addition to these security measures, MRSP restricts access to this area to authorized sample control personnel and those authorized by the SCC.

Sample Preparation Security

include a special preparation/sorting and drying room used by sample submitters, a room designed for sample crushing and grinding, and a room used for preparation of biologic materials. These rooms are equipped with special combination locks and (or) card readers. A motion detector is in place in the plant laboratory providing additional security.

Laboratory Security

include ICP-AES, ICP-MS, CV-AAS for mercury determination, and AAhydride generation for determination of arsenic, antimony, and selenium (app. 2). Because these laboratories were constructed with solid walls that run from floor to ceiling, securing them for COC work required monitoring only the entry to the laboratory. This was accomplished by the installation of card reader monitors and (or) special door combination locks. These security measures provide adequate electronic monitoring while providing reasonable access for an approved analyst. In addition, they can be deactivated when noncustodial samples are being analyzed. The easy installation of these door security systems allows for a “phased” installation. Thus laboratories can be secured as other techniques are added to the suite of approved COC work.

Backup Chain-of-Custody Sample Storage Devices

as temporary sample storage units. These lockers can be used by analysts or sample submitters if samples cannot be secured in the sample control area by Security for COC samples restricts access to three distinct areas in the lab-

The sample control area (app. 2) is secured by three card-reader monitors

Three rooms are designated for sample preparation (app. 2). The rooms

Four laboratories are used for COC analytical work. These laboratories

A set of three storage lockers are located outside of sample control to serve

REFERENCES

Arbogast, B.F., editor, 1990, Quality assurance manual for the Branch of

Baedecker, P.A., and McKown, D.M., 1987, Instrumental neutron activation analysis the close of business. After these lockers have been closed, only the SCC can reopen them.

Computer access to the COC information stored in MRSP computers requires a valid user identification and a password. Authorized computer access is limited to selected personnel. When a COC job is entered into the laboratory information management system (LIMS), the assigned job number and laboratory numbers are sent to personnel who work with these samples. No one has authority to access this data without special permission. Analytical data are printed as they are generated. This hard copy is considered the original (primary) document. The analytical results are also stored in the computer as a backup to the primary document. Data storage is a design feature of LIMS. A password is required to access the system. Additional precautions may be taken such as storing data on separate electronic storage devices, if it becomes apparent that the computer security that is currently in place has been breached.

Geochemistry, U.S. Geological Survey: U.S. Geological Survey Open-File Report 90-668, 184 p.

of geochemical samples, in Baedecker, P.A. (ed.), Methods for geochemical analysis: U.S. Geological Survey Bulletin 1770, p. H1–H14.

Prox 941 Strike Xmfr Special I/F Micro 4 8RP board 6000 ID cap Modem PIR Balanced Contact Exit switch Power Supply Moose MPI-775 Siren

APPENDIX 1 Government Cost Estimate

40.00 0.00 Labor Cost

35.00 35.00 35.00 35.00 35.00 35.00 35.00 35.00 35.00 35.00 35.00 35.00 35.00 35.00 Rev Alt Rev Alt 1 Rev Rev

280.00 70.00 70.00 140.00 630.00 735.00 210.00 140.00 70.00 70.00 0.00 4/22/94 4/22/94 4/22/94 4/26/94 Grand Total

APPENDIX 2 Building 20 Street Plan Map INTRODUCTION

ACCEPTANCE OF ROUTINE SAMPLES (NONEVIDENTIARY)

The Mineral Resource Survey Program (MRSP), formerly the Branch of Geochemistry (BGC), provides support expertise for geologic/analytical products. This includes the following:

• Development and application of single element and multi-element methods
• Development and application of geochemical techniques for environmental
• Expert testimony on sample handling and on the methods used.
• Maintenance of an up-to-date quality assurance program.

To ensure the integrity of evidentiary samples, policies have been established and are outlined below.

Sample control personnel are responsible for maintaining the chain of custody for all samples submitted to MRSP. Samples involved in litigation are controlled more rigorously to ensure their admissibility as evidence in court.

All samples submitted to MRSP must be accompanied by a completed request for analysis (RFA) form. This form is the record of accountability. Information, such as the evidentiary nature of a sample or high elemental concentrations in a sample, are noted on this form along with the requested analysis.

Samples are counted and checked against the RFA. Discrepancies are resolved prior to formal acceptance. The information from the RFA is entered in the computer and numbers are issued for each batch (job number) and each individual sample numbers (laboratory numbers).

A computer printout of the information from the RFA and the information generated by the computer is sent to the submitter for verification. The samples and paperwork remain in a sample control holding area until requested by the sample preparation laboratory personnel.

The policies used in processing routine samples are documented and maintained in the sample control office. Copies of this information are available upon request.

When all work on a job has been completed, sample control personnel file all of the original paperwork in loose leaf computer notebooks by job number. Six

Shortened Version of Chain-of-Custody Policies

used in geochemical investigations.

programs.

Withdrawal of Evidentiary Samples

months after the completion of analysis, samples from completed jobs are then moved to the permanent storage facility.

Prior to sample submittal, the project leader(s) requesting strict chain of custody (COC) conducts a meeting with all relevant laboratory personnel to discuss details of the project relating to the handling, analysis, and final disposition of samples.

The laboratory reserves the right to refuse any sample that exceeds laboratory safety guidelines.

Samples that might involve litigation are handled as evidence. A specific set of COC procedures are maintained on all such samples. The process for handling these samples requires additional precautions. Specific rules are detailed below.

The sample control specialist (SCC) or designated representative is the custodian of evidentiary samples and maintains all COC samples, forms, and tracking cards in a secured area.

While the submitter is present, sample control personnel count and check the samples against the RFA. Any discrepancies are resolved prior to official acceptance of the samples. The SCC has the right to refuse samples as evidentiary, if the sample containers are improperly sealed, damaged, leaking, above the levels of toxicity or radioactivity pre-determined by the MRSP safety officer or arrive with incomplete or incorrect paperwork. The identifying numbers are recorded on the sample control COC Form, which is maintained in a bound book. The samples are photographed, and this photograph is preserved with the RFA.

Samples are locked in the sample control evidentiary holding area. Formally accepted samples are entered into the system according to the documentation in the sample control office. The exceptions to the routine procedure are that laboratory and job numbers are added to the COC form, and a tracking card is created for evidence. This card is filed in a small file that is kept in the COC area. This card must be signed by individuals with name and date before samples will be released by the SCC.

Analysts authorized to work with COC samples must contact the SCC for withdrawal of COC samples prior to arriving in the sample control area. The analyst comes to the sample control area and inspects the evidence seals to assure

CHAIN-OF-CUSTODY SAMPLE LABORATORY ANALYSIS

that the samples meet standard evidence rules. Samples are given to the analyst after the analyst signs the tracking card and the bottom section of the COC form with name, date, time, reason for withdrawal, amount to be used in analysis, and location to where the samples are to be moved. Samples may then be moved to another secured area. Samples are returned to sample control as soon as the amount required for analysis has been weighed and removed. Samples are not left unattended and (or) unsecured. The analyst adds any additional notes, such as increased amount of sample withdrawn, to the COC form when the samples are returned to sample control.

When COC samples are in a laboratory, no other samples are permitted in that laboratory to eliminate any possibility of cross-contamination of COC samples.

COC sample preparation protocol differs from the standard operating procedure for the ACSG sample preparation only by the additional security and documentation involved. Physical sample preparation of COC samples is performed in accordance with the quality assurance manual (Arbogast, 1990).

Any special preparation instructions, the amount of sample to be prepared, the disposal of excess material, and the cost for disposal of any hazardous materials is agreed upon at the pre-assessment meeting.

If excess sample is being returned to the submitter, a 3-oz unaltered split of the sample is retained and safeguarded until the litigation is completed. This prepared sample is maintained by the ACSG and used for analytical work. All other excess sample is either returned to the submitter or discarded. If hazardous materials/waste disposal costs are incurred, the submitter is held responsible as agreed upon at the pre-assessment meeting.

A trained and certified sample preparation technician accepts the sample(s) from the sample custodian. The samples are taken to the ACSG’s COC sample preparation laboratory and prepared for analysis. Upon completion, the technician notes on the RFA any problems such as broken seals. The samples and excess bulk, if any, are secured with evidence tape, initialed and dated. They are then returned to the sample custodian. The sample custodian checks to ensure all samples are present and sealed properly and signs the bottom section of the COC form next to the analyst’s name to indicate the resumption of custody.

After the prepared samples are returned to sample control, laboratory analysts withdraw samples following the same rules. Samples can be only moved to secured areas of the building. Any sample removed from the custodial sample (for example, 10 g for Au analysis) is documented on the COC form. If analysis requires formation of solutions, the solution may be kept in the secured area, but the original sample is returned to sample control as soon as the amount needed for analysis has been weighed and removed.

Routine techniques validated in Arbogast (1990) are used for the majority of analyses of COC samples. Nonroutine techniques may also be used for the analysis of COC samples, but it then becomes the responsibility of the research scientist to provide the necessary QA/QC information and method references for validation of the research technique.

Instrument calibration and maintenance are performed according to Arbogast (1990). Instrument calibrations are documented in log books or on computer printouts. Lab books and log books are bound with entries recorded in permanent ink. Lab books contain pertinent information such as job number, name of submitter, sample numbers, weight of sample, date of preparation, and method of dissolution. The analyst is responsible for placing all data in a secured area during sample analysis (such as strip chart and graphs). When the analysis is complete, all original data are given to the COC custodian, who is responsible for the storage of the information.

SAMPLE COMPLETION AND MISCELLANEOUS INFORMATION

Samples that are insufficient for all requested analyses are noted on the RFA and the COC form when they become insufficient. All requested splits are kept in the secured areas with the original samples. Should a portion of the sample be requested for litigation, a split is made available upon request and permission of the Solicitor General. The amount of sample removed and the date and time is noted on the COC form.

When all requested analyses are complete, computer printouts of the results are filed in a sample control loose leaf book in the sample control secured area. The samples and all related paperwork are secured until all litigation is complete.

Sample submitters are contacted on an annual basis to ascertain the status of the litigation process. When the litigation is complete, the submitter is notified to retrieve the samples. A split of the original sample is maintained by the MRSP for permanent archive but on a nonevidentiary basis. The evidentiary samples and a copy of all RFA documentation, computer printouts, and results are returned to the submitter who signs the COC card and the COC form, which is filed in sample control.

Samples that have a short viability (such as water samples) will be held for 6 weeks. At that time, they will be returned to the submitter along with a copy of all documentation. The submitter will be required to sign for the samples on the COC card and form.

Samples that are sent through the mail room with evidence tape will not be released by the mail room personnel to anyone but the SCC or the designated backup individual.

Federal Center Security

If the litigation is not completed, the samples and all related documents continue to be held as evidence with all appropriate safeguards.

Storage charges may be assessed if storage times of more than 2 years are anticipated or incurred.

Information regarding the samples may only be released to the submitter. Any requests for information from anyone other than the submitter are referred to the Solicitor General.

Employee conduct is governed by the Ethics Reform Act of 1989. Details of this act are available in the local personnel office of The U.S. Geological Survey. The guidelines set forth in this act are to be followed by all private (contract) and government employees working on COC samples in this laboratory.

The supervisory sample control specialist serves as the principal sample COC custodian for the laboratory and is responsible for the coordination of sample submittal, retrieval and storage (short and long term). A designated individual from sample control acts as a backup COC custodian.

Training documents identify those analysts who are qualified to perform a particular procedure or parts of a procedure. Only analysts who are documented as qualified will perform the requested analyses. Training documents are kept and maintained by the quality assurance coordinator.

The analyst’s performance is routinely checked using Quality Control (QC) results to demonstrate that the analyst performs under the guidelines set forth under the Quality Assurance (QA) Manual for Branch of Geochemistry (Arbogast, 1990).

Individuals involved with COC analyses have work plans that include a critical element governing compliance with COC guidelines. These individuals are all certified by the laboratory chief as qualified to handle COC samples.

The chief scientist or the MRSP laboratory manager represent the lab in all court cases where routine procedures are used to analyze COC samples.

When nonroutine techniques are used in the analysis of samples, it is the research scientist’s responsibility to provide all necessary documentation, QA/QC information, and testimony at any legal proceedings.

The COC protocol includes three levels of security. The first level controls of entrance and exit of the Denver Federal Center (DFC) with a fenced enclosure and guards who record all access after normal business hours. A second level of security is provided by regular police patrols of the DFC by the Federal Protective Service (FPS), and a final level is provided by our building security system.

Building Security

ratory facility. In all areas, security equipment was recommended, installed, and is monitored by the FPS. Only designated individuals who have been approved by MRSP management have access to these secured areas. The security system in all three areas can be modified to accommodate changes in laboratory personnel without endangering the security of COC samples.

Sample Control Security

FPS and installed under their supervision. In addition to these security improvements, MRSP restricts access to this area to authorized sample control personnel and those authorized by the SCC.

Sample Preparation Security

cial preparation/sorting and drying room used by sample submitters, a room designed for sample crushing and grinding, and a room used for preparation of biologic materials. The security of these rooms was also installed under the supervision of FPS.

Laboratory Security

sures provide complete monitoring but still provide reasonable access for an approved analyst. In addition, the security can be deactivated when noncustodial samples are being analyzed. Access is monitored by FPS anytime COC samples are being analyzed.

Backup Chain-of-Custody Sample Storage Devices

as temporary sample storage units. These lockers are used by analysts or sample submitters if samples cannot be secured in the sample control area by the close of business. After these lockers have been closed, only the sample custodian can reopen them.

Computer Security for Chain of Custody

valid user identification and a password. Authorized computer access is limited to selected MRSP personnel. Security for COC samples restricts access to three distinct areas in the labo-

The sample control area is secured by various methods recommended by the

Three rooms are designated for sample preparation. The rooms include a spe-

Four laboratories are used for COC analytical work. Electronic security mea-

A set of three storage lockers are located outside of sample control to serve

Computer access to the COC information stored in computers requires a When a COC job is entered into the laboratory information management system (LIMS), the assigned job number and laboratory numbers are sent to the personnel who work with these samples. No one has authority to access this data without special permission.

Analytical data are printed as they are generated from laboratory instruments. This hard copy is considered the original (primary) document. The analytical results are also stored in the computer as a backup to the primary document. Data storage is a design feature of LIMS. A password is required to access the system. Additional precautions may be taken such as storing data on separate electronic storage devises, if it becomes apparent that the computer security that is currently in place has been breached.

REFERENCE

Arbogast, B.F., editor, 1990, Quality assurance manual for the Branch of Geochemistry, U.S. Geological Survey: U.S. Geological Survey Open-File Report 90-668, 184 p.

ACKNOWLEDGMENTS

We especially want to thank the following people for sharing their expertise: Belinda Arbogast Jim Budahn Paul Lamothe Steve McDanal

Vince Marino Jon Werkmeister

Peter Mang Jackie Bailey

Anthony Palizzi Jerry Porr

Bruce Binkley Eric Nottingham Mineral Resource Survey Program Mineral Resource Survey Program Mineral Resource Survey Program Mineral Resource Survey Program

Federal Protective Service Federal Protective Service

Colorado Bureau of Investigation Colorado Bureau of Investigation

Office of the Solicitor General, Department of the Interior

Environmental Protection Agency Environmental Protection Agency

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