draft quality assurance project plan (qapp) supplements erm

Environmental Resources Management

99 Boylston Street 6th Floor 13 August 2001 oston Massachusetts 02116

Reference 215-20 (617) 267-8377 (617) 267-6447 (fax)

Mr David Lederer http wwwerm com

United States Environmental Protection Agency - Region I One Congress Street Boston MA 02114-2023

RE Phase IB Remedial Investigation Draft Quality Assurance Project Plan (QAPP) Supplements Shpack Superfund Site ERM NortonAttleboro MA

Dear Dave

Please find the supplemental laboratory information (1 copy) for inclusion in the Shpack QAPP submitted to EPA on 8 August 2001 Please insert this information into Appendix C of volume 2

Should you have any questions please feel free to contact me at 617-267shy8377

Sincerely

Steven P Sacco PG Project Manager

cc Ed Conroy Metcalf amp Eddy (2 copies) File (2 copies)

SOP No STL-RC-0003 Revision No

Revision Date 3 42801 S E V E R N

PageImplementation Date

1 of 43001

12 T R E N T

-ED COPY SERVICES

STL St Louts

OPERATION-SPECIFIC STANDARD OPERATING PROCEDURE

TITLE Drying and Grinding

of Soil and Solid Samples (STL-RC-0003 Rev 2)

Prepared by

Approved by Technical Specialist

Approved by Quality Assurance Manager

Approved by fajbufav~- EnvironmentapoundHealth and Safety Coordinator

Approved by Laboratory Director

Proprietary Information Statement

This document has been prepared by Severn Trent Laboratories (STL) solely for STLs own use and the use of STLs customers in evaluating its qualifications and capabilities in connection with a particular project The user of this document agrees by its acceptance to return it to STL upon request and not to reproduce copy lend or otherwise disclose its contents directly or indirectly and not to use it for any other purpose other than that for which it was specifically provided The user also agrees that where consultants or other outside parties are involved in the evaluation process access to these documents shall not be given to said parties unless those parties specifically agree to these conditions

THIS DOCUMENT CONTAINS VALUABLE CONFIDENTIAL AND PROPRIETARY INFORMATION DISCLOSURE USE OR REPRODUCTION OF THESE MATERIALS WITHOUT THE WRITTEN AUTHORIZATION OF SEVERN TRENT LABORATORIES IS STRICTLY PROHIBITED THIS UNPUBLISHED WORK BY STL IS PROTECTED BY STATE AND FEDERAL LAW OF THE UNITED STATES IF PUBLICATION OF THIS WORK SHOULD OCCUR THE FOLLOWING NOTICE SHALL APPLY

bullpoundCOPYRIGHT 2000 SEVERN TRENT LABORATORIES INC ALL RIGHTS RESERVED STL St Louis is a part of Severn Trent Laboratories Inc

SOP No STL-RC-0003 Revision No 3

Revision Date 042801 Page 2 of 12

Implementation Date 043001

SUMMARY OF METHOD

11 This SOP describes the method for drying and grinding samples to a uniform particle size so that radiochemical analyses can be performed

SCOPE AND APPLICATION

21 This SOP provides detailed instructions for the preparation of soil and solid samples by grinding and pulverization to achieve a uniform matrix

22 This method is applicable to solid samples including sediment and soil This method is likely to evaporate volatile radionuclides and should not be used for samples that must be analyzed for volatile chemicals such as iodine (I29I) and tritium (3H)

23 Responsibilities

231 It is the responsibility of Associates in the Radiochemistry Group to schedule and order samples requiring analysis

232 It is the responsibility of the analyst to follow this procedure and to report any abnormal results to the Radiochemistry Group Leader

233 It is the responsibility of the Radiochemistry Group Leader or designee to review data prior to release from the lab

DEFINITIONS

31 See policy QA-003 for definitions

INTERFERENCES

41 This method is likely to evaporate volatile radionuclides such as iodine (1291) and tritium (3H) This method should not be used for samples that must be analyzed for volatile chemicals

SAFETY

51 Procedures shall be carried out in a manner that protects the health and safety of all associates

52 The Chemical Hygiene Plan (CHP) gives details about the specific health and safety practices which are to be followed in the laboratory area Personnel must receive training in the CHP including the written Hazard Communication plan prior to working in the laboratory Consult the CHP the Health and Safety Policies and Procedures




Manual and available Material Safety Data Sheets (MSDS) prior to using the chemicals in the method

53 Consult the Health and Safety Policies and Procedures Manual for information on Personal Protective Equipment Eye protection that satisfies ANSI Z871 (as per the Chemical Hygiene Plan) laboratory coat and appropriate gloves must be worn while samples standards solvents and reagents are being handled Disposable gloves that have become contaminated will be removed and discarded other gloves will be cleaned immediately VITON gloves may be worn when halogenated solvents are used for extractions or sample preparation Nitrile gloves may be used when other solvents are handled [Note VITON is readily degraded by acetone all solvents will readily pass through disposable latex rubber gloves]

54 The health and safety hazards of many of the chemicals used in this procedure have not been fully defined Additional health and safety information can be obtained from the MSDS files maintained in the laboratory The following specific hazards are known

541 No hazardous chemicals are used to implement this procedure

55 Exposure to chemicals will be maintained as low as reasonably achievable therefore unless they are known to be non-hazardous all samples will be opened transferred and prepared in a fume hood or under other means of mechanical ventilation Solvent and waste containers will be kept closed unless transfers are being made

56 Samples should be screened or surveyed (with a GM 44-9 betagamma probe) before being handled by the associate Controls shall be implemented to limit exposures to Category HI and Category IV samples as defined by the Radiation Safety Officer

57 The analyst should practice effective contamination control methods in order to minimize the spread of radioactive contamination from the prepared sample to ones hands or other surfaces

58 Hearing protection is required when using the pulverizer or ball mill in the event that noise levels exceed 90 dB(A) within 3 feet of the grinder Contact the EHampS Coordinator to determine the results of the noise surveys

59 All work must be stopped in the event of a known or potential compromise to the health or safety of any associate The situation must be reported immediately to a laboratory supervisor

510 Laboratory personnel assigned to perform hazardous waste disposal procedures must have a working knowledge of the established procedures and practices outlined in the Health and Safety Manual These employees must have training on the hazardous waste disposal practices initially upon assignment of these tasks followed by annual refresher training




EQUIPMENT AND SUPPLIES

61 Equipment and supplies for this procedure consist of the following

611 Drying Oven

612 Pulverizer

613 Ball mill

614 Paint cans

615 Assorted tools and routine laboratory glassware

616 Tumbling cylinders or steel balls

REAGENTS

71 Reagents

711 Quartz sand

72 Standards

721 No standards are used in this procedure

SAMPLE COLLECTION PRESERVATION AND STORAGE

81 Refer to the appropriate analytical SOP

QUALITY CONTROL

91 QC requirements

911 A decontamination blank is processed and analyzed prior to use of the pulverizer or ball mill The decontamination blank consists of quartz sand which is processed for a minimum of 10 minutes in the pulverizer or 30 minutes in the ball mill with grinding media The blanks are then analyzed by gamma spectroscopy Results of the analysis will indicate whether typical decontamination efforts are sufficient in removing potential carryover from previous samples

92 All quality control data shall be maintained and available for easy reference

93 Procedural Variations

10




931 One time procedural variations are allowed only if deemed necessary in the professional judgment of the analyst to accommodate variation in sample matrix radioactivity chemistry sample size or other parameters Any variation shall be completely documented using a Nonconformance Memo and approved by the Supervisor and QA Manager

932 Any unauthorized deviations from this procedure must also be documented as a nonconformance with a cause and corrective action described

94 Nonconformance and Corrective Action

941 Any deviations from QC procedures must be documented as a nonconformance with applicable cause and corrective action approved by the facility QA Manager

95 QC Program

951 Further details of QC and corrective action guidelines are presented in the QC Program policy document (QA-003)

CALIBRATION AND STANDARDIZATION

101 None

1 1 PROCEDURE

111 Sizing of Sample

1111 For solid samples with various particle sizes including pebbles or small rocks processing by ball milling may be adequate to achieve a uniform particle size

1112 For solid samples that must be reduced to a fine mesh size (ie 200 mesh) a pulverizer will be necessary A ball mill may be used if it is necessary to homogenize the pulverized sample

1113 In addition solid samples that are composed of large particles such as rock cement stone etc it may be necessary to fracture or reduce the size of the sample before pulverizing

1114 Refer to the appropriate Client Requirement Checklist to determine if there are client specific sizing requirements

1115 In an effort to avoid cross contamination the order of the samples processed should be from low activity to high radiological activity if this sample activty is




known Screening results or surveying with a GM 44-9 betagamma probe may be used for this purpose

1116 Proceed to step 114 for sample pulverization directions

112 Drying and Grinding of Samples - Non-volatile Isotopes

1121 Place sample in labeled heat-proof container

1122 If the sample has not been dried perform the following steps Otherwise proceed to step 1143

11221 Place sample in a drying oven for approximately 4-12 hours at approximately 105degC Record the oven temperature date time and analyst initials in the Oven Temperature Logbook

11222 Visually inspect the sample at the end of the drying period If the sample does not appear to be dry return sample to oven to continue drying

11223 When the sample is dry remove the sample from the oven Record the oven temperature date time and analyst initials in the Oven Temperature Logbook

11224 Allow the sample to cool to room temperature

113 Size reduction of solid sample in the ball mill

1131 Confirm that the sample has been dried If not perform steps 1122 through 11224

NOTE Confirm the sample number and select the correct sample paint bull can before adding sample to the paint can

1132 Load the sample into paint cans

1133 Place several tumbling cylinders or steel balls into the paint can Seal the lid onto the paint can

1134 Document the sample ID number on the paint can lid and side

1135 Repeat steps 1131 through 1134 for all samples

1136 Load each can onto the ball mill




Caution Ensure all personnel within the room are wearing hearing protection before starting the ball mill

1137 Energize the ball mill

1138 The sample should tumble for at least 1 hour to confirm adequate mixing to ensure adequate grinding the sample should roll for 6 to 14 hours

1139 Turn off the ball mill and remove the paint cans from the ball mill at the end of the processing cycle

11310 Under adequate ventilation visually sample has been ground transfer the sample to an appropriate container

11311 Label the container with the laboratory sample number

11312 Store for further analysis

114 Pulverize large solid samples such as rocks and cement samples or samples which must be reduced to 200 mesh

1141 Ensure that the pulverizer dish and puck have been cleaned and not contaminated to prevent cross contamination

1142 Fragment the sample to a size that appears acceptable to the pulverizer dish

1143 Separate the larger particles that are not acceptable to the pulverizer Continue to fracture or fragment the larger portions until the entire sample can be added to the pulverizer

1144 Confirm that the ventilation system is working

1143 Fill the dish and puck with the soil sample making sure not to overfill and prevent proper lid sealing on the dish

1146 Place the dish securely in the pulverizer holder and close the cover on the machine

1147 Open the air cylinder valve and regulate outgoing pressure to 80 psi for operation of the pulverizer

1148 Press and hold the green start burton on the pulverizer until it begins to operate at the 80 psi level

1149 To achieve 200 mesh run pulverizer for 10 minutes




11410 After pulverizing the sample for the required length of time press the red stop button to stop the pulverizer

11411 Lift the cover and remove the dish from the pulverizer

11412 In the hood carefully empty the crushed soil sample from the dish into a labelled secondary sample container

11413 Decontaminate the dish and puck by filling it with an approximately 4 oz jar of quartz sand and replacing the lid then place it in the pulverizer and operate the machine approximately 10 minutes Empty the sand and wipe the dish puck and lid Frisk with a GM 44-9 betagamma probe to scan for decontamination The dish and puck must be decontaminated before pulverizing the next soil sample to prevent cross contamination

11414 Place the pulverized samples into a paint can and homogenize the samples on the roller See section 1138

12 DATA ANALYSIS AND CALCULATIONS

121 None

13 DATA ASSESSMENT AND ACCEPTANCE CRITERIA

The following represent data assessment for samples and acceptance criteria for QC measures

131 QC sample acceptance criteria

1311 Decontamination Blank

13111 No activty above the Minimum Detectable Activity (MDA) should be observed in the decontamination blank

14 CORRECTIVE ACTIONS FOR OUT OF CONTROL DATA


1411 The samples processed prior to the defective decontamination blank are evaluated

14111 If the radionuclide found in the decontamination blank is confirmed to not be present in any of the associated samples at any level the contamination did not affect those samples This represents a non-impact situation and no specific corrective action is taken A nonconformance memo is written to notify project management of the situation for evaluation against project requirements


Revision Date 042 801 Page 9 of 12


1412 If the radionuclide found in the decontamination blank is confirmed to be present in one or more of the associated samples the activities are compared

14121 If the radionuclide activity in the decontamination blank exceeded 10 of activity found in one or more samples the prescribed corrective action is to reprocess all affected samples

14122 If the activity in the decontamination blank was less than 10 of the activity found in one or more samples the sample can be reported by qualifying the affected analytes A nonconformance memo is written to notify project management of the situation for evaluation against project requirements

1413 A failed decontamination blank indicates the need for further cleaning of ball mill or pulvizer Subsequent decontamination blanks should be processed to verify cleanliness prior to the next use Continued failure may indicate the need to modify the decontamination process

15 CONTINGENCIES FOR HANDLING OUT-OF-CONTROL OR UNACCEPTABLE DATA

151 Decontamination blanks

If there is insufficient sample to perform reprocessing of samples due to a failed decontamination blank the analyst must notify the Project Manager for consultation with the client and a Nonconformance Memo is written Affected samples will be identified in the case narrative

16 METHOD PERFORMANCE

161 Training Qualification

1611 The groupteam leader has the responsibility to ensure that this procedure is performed by an analyst who has been properly trained in its use and has the required experience see SOP CORP-QA-0013

1612 The analyst has the responsibility that heshe has successfully completed the necessary demonstration of proficiency samples read the SOP and understand the basic operation and theory of the instrumentation

162 Records ManagementDocumentation

1621 All records generated by this analysis will be filed and kept in accordance with SOPs and policies for records management and maintenance

163 Associated SOPs


Revision Date 042801 0 of 12


1631 STL St Louis Laboratory STL-RC-0004 Preparation of Soil Sludge and Filter Paper Samples for Radiochemical Analysis

1632 STL St Louis Laboratory STL-QA-0006 Sample Receipt and Chain-of-Custody

1633 STL St Louis Laboratory CORP-QA-0010 Nonconformance and Corrective Action

164 Appendices

1641 Appendix 1 Procedure Flowchart

17 POLLUTION PREVENTION

171 This procedure will be carried out in a manner consistent with all applicable federal state and local regulations regarding pollution control and prevention Specific controls due to the accidental release of hazardous materials can be found in the STL Chemical Hygiene Plan and facility attachments

172 To minimize the amount of unnecessary waste inserted into the radioactive waste stream any waste that frisks lt100 cpm above background with a GM 44-9 betagamma probe may be put into sanitary trash Any waste that frisks gt100 cpm above background must go into the radioactive waste stream

18 WASTE MANAGEMENT

181 Waste generated in the procedure must be segregated and disposed according to the facility hazardous waste procedure The Environmental Health and Safety Coordinator should be contacted if additional information is required

19 REFERENCES

191 STL Quality Management Plan current revision

192 STL St Louis Laboratory Quality Manual current revision

193 Handbook for Analytical Quality Control in Radioanalytical Laboratories LG Kanipe EPA-6007-77-088 August 1977

194 Nuclear Regulatory Commission Title 10 Code of Federal Regulations Part 50 Numerical Guides for Design Objectives and Limiting Conditions for Operation to




Meet the Criteria As Low As Reasonably Achievable for Radioactive Material in LightshyWater-Cooled Nuclear Power Reactor Effluents Appendix I





APPENDIX 1

PROCEDURE

Dry the sample at 105C for 4-12 hours

oes need to be ground

Clean grinder if necessary

he sample s enough to fit into Pulverize sample

grinder

Grind sample to a 50-100 mesh

Sample ready for analysis J

Ball mill sample

SOP NoRevision No

Revision DatePage

Controlled Copy No fs

STL-RC-0020 2

103000 1 of 26

S E V E R N T R E N T

SERVICES

STL St Louis

OPERATION-SPECIFIC STANDARD OPERATING PROCEDURE15 Rider Trail North

Prepared by

Approved by

Approved by

Approved by

Approved by

TITLE Determination of

Gross AlphaBeta Activity (SUPERCEDS SL13002 REVISION 2)

Technical Specialist

Quality Assurajace Manager bull

Environmental Health and Safety Coordinator

Laboratory Director

Earth City MO 63045

Tel 3142988566

Fax 314 298 8757

wwwstlHnccom


This document has been prepared by Severn Trent Laboratories (STL) solely for STLs own use and the use of STLs customers in evaluating its qualifications and capabilities in connection with a particular project The user of this document agrees by its acceptance to return it to STL upon request and not to reproduce copy lend or otherwise disclose its contents directly or indirectly and not to use it for any other purpose other than that for which it was specifically provided The user also agrees that where consultants or other outside panics are involved in the evaluation process access to these documents shall not be given to said parties unless those parries specifically agree to these conditions

THIS DOCUMENT CONTAINS VALUABLE CONFIDENTIAL AND PROPRIETARY INFORMATION DISCLOSURE USE OR REPRODUCTION OF THESE MATERIALS WITHOUT THE WRITTEN AUTHORIZATION OF SEVERN TRENT LABORATORIES IS STRICTLY PROHIBITED -SHIS UNPUBLISHED WORK BY STL IS PROTECTED BY STATE AND FEDERAL LAW OF THE UNITED STATES IF PUBLICATION OF THIS WORK SHOULD OCCUR THE FOLLOWING NOTICE SHALL APPLY

^COPYRIGHT 2000 SEVERN TRENT LABORATORIES 7NC ALL RIGHTS RESERVED

STL SI LOUIS is a cart of Severn Trent Laooratones Inc




SUMMARY OF METHOD

11 This SOP is applicable for the preparation and analysis of samples for gross alpha andor beta radioactivity

12 This method is applicable to determination of gross alpha andor gross beta activity in air filters water soilsediment and vegetation samples

121 For total sample activity an aliquot of aqueous sample is evaporated to a small volume treated with nitric acid to convert any chlorides to nitrates and transferred quantitatively to a tarred counting planchet The sample residue is dried and then counted for alpha andor beta radioactivity using a Gas Flow Proportional Counter

122 For the activity of dissolved matter an aliquot of aqueous sample is filtered through a 045-mm membrane filter The filtrate is evaporated to a small volume treated with nitric acid to convert any chlorides to nitrates and transferred quantitatively to a tarred counting planchet The sample residue is dried and then counted for alpha andor beta radioactivity using a Gas Flow Proportional Counter

123 For the activity of suspended matter an aliquot of aqueous sample is filtered through a 045-mm membrane filter The filter is transferred to a counting planchet The sample residue is dried and then counted for alpha andor beta radioactivity using a Gas Flow Proportional Counter

124 Air filter samples are counted for gross alpha andor beta activity without further processing if the filter is less than 2 inches diameter If the filter is greater than 2-inch diameter the sample is digested per STL-RC-0004 Preparation of Soil Sludge and Filter Paper Samples for Radiochemical Analysis and then an aliquot prepared like a liquid

125 Solid samples are analyzed for gross alpha andor beta activity as a dry powder unless DOE Method RP710 is requested When the QAS shows that RP710 is required an acid leach is performed per STL-RC-0004 Preparation of Soil Sludge and Filter Paper Samples for Radiochemical Analysis The digestate is then treated like a liquid

126 Oil samples are ashed in a muffle furnace then dissolved in nitric acid The sample is then transferred to a tarred planchet dried and counted for alpha andor beta radioactivity using a Gas Flow Proportional Counter

127 Gross Alpha and Gross Beta activity does not identify the radionuclide that is present Instead the activity is referenced as equivalent to Am-241 for Gross Alpha and Sr-90Y-90 for Gross Beta





21 This procedure applies to the preparation and analysis of samples for gross alpha andor beta radioactivity

22 Responsibilities

221 Counting Lab Supervisor to confirm that this procedure is followed for the determination of gross alpha andor gross beta activity in air filters water soilsediment and vegetation samples

222 Radiochemistry Group Leader (or designee) to delegate the performance of this procedure to personnel who are experienced with this procedure and with the equipment associated with the implementation of this procedure

223 AnalystTechnician performing this procedure to follow the instructions and to report any abnormalities to Counting Lab Team Leader immediately To confirm that all equipment used is working properly prior to starting this procedure

23 This SOP is applicable to EPA 6004-80-032 Prescribed Procedures for Measurement of Radioactivity in Drinking Water Method 9000 APHA Standard Methods for Water and Wastewater Method 7110 SW846 Method 9310 and DOEEM-0089T DOE Methods for Evaluating Environmental and Waste Management Samples Method RP710

24 Quality control limits (accuracy and precision for spikes) are also maintained in QuantlMS and are also dynamic Therefore they are not specifically listed in this document but can be retrieved at any time using TraQAr tools

25 Method detection limits are maintained in the Information Management System (QuantlMS) Because of their dynamic nature they are not specifically listed in this document but can be retrieved at any time using TraQAr tools Reporting limits will be proportionately higher for sample extracts that require dilution and for soil samples that require concentration adjustments to account for percentage moisture


Revision Date 103000 Page of 26


26 The Reporting Limits (RL) under routine operating conditions are summarized in the following table

Matrix Sample Volume Count Time Gross Alpha Gross Beta (Note 1) (Min) Reporting Limit Reporting Limit

Air 1 filter 100 1 pCifilter 1 pCifilter Water 0200 L 100 5pCiL 3pCiL Drinking 0500 L 100 2pCiL 15pCiL Water Soil OlOOg 100 lOpCig lOpCig Sediment Vegetation

Note 1 Sample volume may need to be adjusted in order not to exceed 100 mg of dried residue on planchet Volume shown is typical maximum volume used provided Total Solids does not exceed 500 ppm for waters and 200 ppm for drinking waters

DEFINITIONS

31 See Quality Assurance Management Plan (QAMP) for glossary of common terms

32 Minimum Detectable Activity (MDA) - The smallest amount of activity that can be detected given the conditions of a specific sample It is reported at the 95 confidence interval meaning that there is a 5 chance that a false signal was reported as activity and a 5 chance that true activity went undetected The MDA that is reported is a combination of counting error as well as preparation errors

INTERFERENCES

41 Since in this method for gross alpha and gross beta measurement the radioactivity of the sample is not separated from the solids of the sample the solids concentration is a limiting factor in the sensitivity of the method for any given sample

42 For a 2-inch diameter counting planchet (20 cm2) an aliquot containing 100 mg of dissolved solids would be the maximum aliquot size for that sample which should be evaporated and counted for gross alpha or gross beta activity

43 Radionuclides that are volatile under the sample preparation conditions of this method can not be measured Other radioactivities may also be lost during the sample evaporation and drying (such as tritium and some chemical forms of radioiodine) Some radioactivities such as the cesium and technetium radioisotopes may be lost when samples are heated to dull red color Such losses are limitations of the test method




44 Moisture absorbed by the sample residue increases self absorption and if unconnected leads to low-biased results For hygroscopic sample matrices the nitrated water solids (sample evaporated with nitric acid present) will not remain at a constant weight after being dried and exposed to the atmosphere before and during counting Those types of water samples need to be heated to a dull red color for a few minutes to convert the salts to oxides

45 Inhomogeneity of the sample residue in the counting planchet interferes with the accuracy and precision of the method

SAFETY


52 The Chemical Hygiene Plan (CHP) gives details about the specific health and safety practices which are to be followed in the laboratory area Personnel must receive training in the CHP including the written Hazard Communication plan prior to working in the laboratory Consult the CHP the Health and Safety Policies and Procedures Manual and available Material Safety Data Sheets (MSDS) prior to using the chemicals in the method



541 Nitric acid is known to be an oxidizer and corrosive


56 The preparation of all standards and reagents and glassware cleaning procedures that involve solvents will be conducted in a fume hood with the sash closed as far as the operations will permit or by other means of mechanical ventilation








611 Analytical Balance (4 - or 5 - place)

612 Beakers borosilicate glass various sizes

613 Bottle wash

614 Counting planchets stainless steel 50 cm (20) cleaned per STL-RC-0002 Preparation of Stainless Steel Planchets for Radiochemistry Analyses

615 Desiccator with desiccant Dri-Rite or equivalent

616 Drying oven with thermostat set at 105deg C plusmn 2 degC

617 Filter paper ash less Whatman 41 or ash less paper pulp and 045-mm membrane 50 cm

618 Gas flow proportional counting system

619 Graduated cylinder - size appropriate to sample volume

6110 Propane torch

6111 Hot plate-stirrer or heat lamp

6112 Calibrated pipettes Eppendorf or equivalent

6113 Policeman rubber or plastic

6114 Porcelain crucibles with lids approximately 30-ml capacity

6115 Muffle furnace programmable preferred

7




6116 Tongs or forceps

REAGENTS AND STANDARDS

71 All reagent preparation is documented in the reagent logbook All reagents are labeled with their unique ID name (and concentration if applicable) of the reagent the date prepared and the expiration date

72 Deionized Water Type n as described in ASTM Part 311193-74 obtained from the Milli-Q unit

CAUTION Refer to Material Safety Data Sheets (MSDS) for specific safety information on chemicals and reagents prior to use or as needed

73 Reagents

731 ASTM Type E water

732 Nitric acid concentrated (16N HNO3) - WARNING Corrosive liquid and hazardous vapor oxidizer

733 Sodium Sulfate

74 Prepared Reagents

NOTE Reagents are prepared from reagent grade chemicals unless otherwise specified below and reagent water

NOTE Replace lab-prepared reagents annually unless otherwise specified below As a minimum label all reagents with chemical name concentration date prepared and preparers initials and expiration date

741 4N Nitric acid (4N HNO3) - Add 250 ml of 16N HNO3 to 750 ml of reagent water and mix well

742 Sodium Sulfate (100 mgml Na2SO4) Dissolve lOg of Na2SO4 in 80 ml of DI water Dilute to 100 ml and mix well

75 Standards

751 All standards preparation documentation and labeling must follow the requirements of STL-QA-0002

CAUTION Radioactive




7511 Americium-241 calibrated - NIST traceable diluted to approximately 20 dpmml

7512 Strontium-90 calibrated - NIST traceable in equilibrium with Yttrium 90 diluted to approximately 20 dpmml CAUTION Radioactive


81 Aqueous samples should be preserved at the time of collection by adding sufficient nitric acid to a pH lt 2

82 Preserve soil samples by maintaining at 4deg plusmn 2degC from the time of sample collection

83 Samples must be analyzed within 28 days of sample collection

84 If samples are collected without acidification they should be brought to the laboratory within 5 days nitric acid added to bring the pH to 2 or less the sample shaken and then held for a minimum of 16 hours in the original container before analysis or transfer of sample If dissolved or suspended material is to be analyzed separately do not acidify the sample before filtering the sample The filtering may be performed in the field by the customer or by the laboratory

85 Samples may be collected in either plastic or glass containers

86 The maximum holding time is 180 days from sample collection for all matrices

QUALITY CONTROL

91 QC requirements

911 Each analytical batch may contain up to 20 environmental samples a method blank a single Laboratory Control Sample (LCS an MSMSD pair or a sample duplicate In the event that there is not sufficient sample to analyze an MSMSD or duplicate pair a LCS duplicate (LCSD) is prepared and analyzed

912 Samples that have assigned QC limits different than the standard limits contained in QuantlMS QC code 01 (unless permitted by QA) must be batched separately but can share the same QC samples

913 Additional MSMSDs or sample duplicates do not count towards the 20 samples in an analytical batch

914 A method blank must be included with each batch of samples The matrix for aqueous analyses is organic-free water and salt for solids




915 The LCS is spiked with all of the standard target compounds and is used to monitor the accuracy of the analytical process independent of matrix effects The matrix for aqueous analyses is organic-free water and sodium sulfate for solids

916 All LCS and MSMSD and results - whether they pass criteria or not mdash are uploaded into the QuantlMS system for maintenance and periodic update of limits

917 Instrument conditions must be the same for all standards samples and QC samples

918 All data will be reviewed by the analyst (1st review level) and then by a peer or supervisor (2nd level review)

92 Analyze quality control samples concurrent with routine samples The frequency of quality control samples is based on a batch of 20 samples or less of a similar matrix processed at the same time The minimum QC samples will consist of one method blank one LCS and one duplicate per batch

93 Activity in the method blank must be less than the Reporting Limit (RL) Samples associated with a noncompliant method blank must be reprepared with an acceptable method blank An exception to this corrective action is made if the method blank activity is above the RL but less than 10X the sample activity A comment should be made on the Data Review Sheet if the blank has an activity above the MDA calculated for the blank

94 The acceptable criteria for the LCS is plusmn3a from the mean as determined by laboratory control charts Samples associated with a noncompliant LCS must be reprepared with a compliant Laboratory Control Sample

95 A duplicate sample is analyzed every 20 samples or less Calculate the Relative Percent Difference (RPD) for all duplicate analyses The acceptance limit for the RPD is 25 for water samples and 40 for soils if the concentration in the sample and duplicate are 3

5 times the CRDL If the concentrations are below the CRDL the duplicate concentration should be within the 3s error of the sample If the duplicate does not meet the acceptance criteria the data for the batch will be flagged

96 Matrix spike shall be included with each batch of samples Exceptions are allowed only for samples in which Project Management clearly indicates either during project planning with the client or in the data report that the QC is not acceptable for Utah compliance The criteria for the MS is plusmn3s from the mean as determined by historical data Data associated with recoveries outside the limit will be flagged




97 Additional quality control measures will be performed if they are requested by the client The requirements of a client Quality Assurance Project Plan (QAPP) will have precedence over the requirements of this SOP in cases where they differ

98 Documentation

981 Measure and record a method blank and laboratory control sample with every analytical batch

982 The LCS and the ICVS must be made from a different stock than that used for the working calibration standards

983 The acceptable limits for the quality control samplesstandards are as follows

9831 The correlation coefficient of calibration must be 3 0995

9832 The CCVSs and ICVSs must be plusmn 15 of the true value

9833 Laboratory Control Samples must be plusmn 20 of the true value or as determined by control charts if so specified

9834 Matrix spikes should be plusmn 25 of the true value or as determined by control charting

9835 Relative Percent Differences should be within 20 for aqueous samples and within 35 for solid samples or laboratory generated control charts may be used for control limits

9836 The Method Blank ICB and CCB concentrations must always be less than the method or contract required detection limit









911 QC Program


10 CALIBRATION AND STANDARDIZATION

101 The ratio of count rate to disintegration rate of the detectors shall be obtained through calibration of the detectors for both alpha and beta activity determinations using geometries and weight ranges similar to those encountered when performing the gross analyses Refer to SOP SL13019 (to be replaced by STL-RD-0001) Calibration of the Low Background Gas Flow Proportional Counting System






11 PROCEDURE

111 One time procedural variations are allowed only if deemed necessary in the professional judgment of supervision to accommodate variation in sample matrix radioactivity chemistry sample size or other parameters Any variation in procedure shall be completely documented using a Nonconformance Memo and approved by a Technical Specialist and QA Manager If contractually required the client shall be notified The Nonconformance Memo shall be filed in the project file

1111 Any unauthorized deviations from this procedure must also be documented as a nonconformance with a cause and a corrective action described

112 Water Sample Preparation




1121 If total sample activity of an aliquot of aqueous sample is to be determined proceed to section 113

1122 If the activity of dissolved matter in an aliquot of aqueous sample is to be determined filter the desired aliquot through a 045-mm membrane filter Proceed to section 113 using the filtrate

1123 If the activity of suspended matter of an aliquot of aqueous sample is to be determined filter the desired aliquot through a 045-mm membrane filter The filter is analyzed per section 116

113 Aqueous Sample - Total Solid Screen

NOTE If the sample was previously radiation screened as per SOP SL13015 (to be superseded by STL-RC-0010) Screening Samples for the Presence of Radioactive Materials the total solid content can be determined from this procedure and this section omitted

1131 Record all sample preparation data on a sample worksheet or on the Weight file (Appendix 1) for the batch

1132 Agitate the sample container thoroughly

NOTE If alpha and beta are to be determined simultaneously from a single aliquot the net residue weights for alpha apply

1133 Pipette a 10 ml aliquot on to a tared planchet

1134 Evaporate to dryness using a hot plate or heat lamp on low to medium heat

1135 Allow to cool in desicator for a minimum of 30 minutes

1136 Reweigh the planchet to estimate solids content of the sample

1137 From the net residue weight and sample volume used determine the sample volume required to meet the target residue weight using the formula given in step 121 with a target weight of 90 mg (not to exceed 100 mg) alphabeta dried residue on the planchet If only Gross Beta is being performed the target weight may be increased to 140 mg Compare the calculated volume to meet the weight limitation with the volume required to ensure that the MDA is below the Reporting Limit (Tables 174) The volume for analysis is the smaller of the two volumes

114 Aqueous Sample Total Activity




1141 Initiate appropriate sample worksheet for the samples to be analyzed and complete as required or begin a Weight file for recording planchet weights (Appendix 1)

1142 Shake the sample container thoroughly Measure a volume of sample previously determined in section 113 into an appropriately sized beaker Record volume of sample used

1143 If it is determined in step 1136 that only a small volume of sample is required the additional volume may be added in small aliquots directly to the planchet used to determine the volume needed to achieve the target sample weight If this is done skip steps 1146 through 1148 below

1144 Prepare a method blank from an aliquot of reagent water equivalent to the sample volumes Prepare LCS with a similar aliquot of reagent water spiked with 1 ml of the standards described in 731 and 732 Note separate LCSs must be prepared for alpha and beta analysis due to the beta emitting decay products of Am-241

115 Add 5 ml of 16N nitric acid to blank and LCS

1151 Evaporate to near dryness using a medium to low temperature hot plate or heat lamp DO NOT ALLOW LIQUID TO SPLATTER Do not allow residue to bake on hot plate

1152 Quantitatively transfer the sample to a tared stainless steel planchet

1153 Use a policeman if needed to complete the transfer Wash down the beaker wall with small portions of dilute HNO3 and add to the planchet

1154 Evaporate to dryness on a warm hot plate so that the sample does not boil Do not allow residue to bake on hot plate Remove sample from hot plate

NOTE Do not allow liquid to splatter

1155 Dry planchets in an oven at 105 plusmn 2 degC for a minimum of 2 hours This step may be eliminated if planchet is flamed as described in Section 11412

1156 Cool planchets in a desiccator for a minimum of 30 minutes Weigh the cooled planchets and record final weight

NOTE If alpha and beta are to be determined simultaneously from a single aliquot the net residue weights for alpha apply 100 mg (20 planchet)




1157 If moisture is present in the sample residue due to hygroscopic salts heat the planchet using a propane torch to a dull red color for a few minutes to convert the salts to oxides

1158 Store dry sample in a desiccator until counted for gross alpha andor beta activity

1159 Submit the sample for counting

11510 Calculate the activity the total error and the MDA per section 120

116 Oil


1162 Fill a 30 ml porcelain crucible V full with confetti made from Whatman No 41 filter paper or ashless paper pulp

1163 Place crucible on analytical balance then tare the balance

1164 Weigh to the nearest 00001 g approximately 1 to 2 gm sample of the oil onto the shredded filter paper Record the sample weight Cover with a crucible lid

1165 Prepare a method blank from shredded filter paper in a crucible Prepare a LCS from shredded filter paper that has been spiked with 1 ml of the solutions described in 731 and 732 in a crucible Note separate LCSs must be prepared for alpha and beta analysis due to the beta emitting decay products of Am-241

1166 If the sample is a mixture of oil and wateror is a sample spiked with an aqueous solution evaporate the water on a hot plate or under a heat lamp before muffling Do not allow residue to bake on hot plate A programmable muffle program may also be used to dry the water before ramping the temperature


1167 Heat the sample in a muffle oven for one hour at 750deg C

1168 Remove the sample from the muffle oven and allow the sample to cool to room temperature

1169 Add approximately 2 ml of 4 N HNO3 to the residue in the crucible

11610 Quantitatively transfer the sample to a tared stainless steel planchet with 4 N HNO3




11611 Use a policeman if needed to complete the transfer Wash down the crucible walls with small portions of dilute HNO3 and add to planchet from step 1149

11612 Evaporate to dryness on a warm hot plate or heat lamp so that the sample does not boil DO NOT ALLOW LIQUID TO SPLATTER Do not allow residue to bake on hot plate

11613 Dry the planchet in an oven at 105 plusmn 2 degC for a minimum of two hours This step may be eliminated if planchet is flamed as described in Section 11414

11614 Weigh the cooled planchet and record final weight

CAUTION Ensure that the solids content do not exceed the maximum allowed weight for the determination and planchet used

11615 If a green residue from chlorides which may be present forms obtain technical assistance on how to proceed




117 Filter Samples


1172 If the filter is 2 diameter or less secure the air filter in a stainless steel planchet with double-sided cellophane tape such that no portion of filter extends above the lip of the planchet Then proceed to step 11513

11721 Prepare a method blank for filter samples pound 2 by securing a blank filter into a planchet Prepare a LCS by securing a blank filter which has been spiked with 1 ml of the solutions described in 731 and 732 in a planchet Note separate LCSs must be prepared for alpha and beta analysis due to the beta emitting decay products of Am-241 Dry the planchets which have been spiked with the aqueous solutions under a heat lamp or in an oven (105 plusmn 2 degC) before proceeding to 11513

1173 If the filter is greater than 2 inches diameter digest the sample per STL-RCshy0004 Prepare a method blank and LCS from blank filters spiked as above which are digested in the same manner




1174 Shake the digested sample thoroughly Measure a volume of sample into an appropriately sized beaker Record volume of sample used

1175 Add 5 ml of 16N nitric acid

1176 Evaporate to near dryness using a medium to low temperature hot plate or heat lamp DO NOT ALLOW LIQUID TO SPLATTER Do not allow residue to bake on hot plate Do not allow residue to bake on hot plate


1178 Use a rubber policeman if needed to complete the transfer Wash down the beaker wall with small portions of dilute HNO3 and add to the planchet

1179 Evaporate to dryness on a warm hot plate so that the sample does not boil DO NOT ALLOW LIQUID TO SPLATTER Do not allow residue to bake on hot plate Remove sample from hot plate Allow to cool




11712 If moisture is present in the sample residue heat the planchet to a dull red color for a few minutes to convert the salts to oxides




118 Solid andor Soil Samples


1182 If the sample has already been prepared per STL-RC-0003 Drying and Grinding of Soil and Solid Samples proceed to step 1187 If the sample is to be leached per DOE Method RP710 proceed to STL-RC-0004 Preparation of




Soil Sludge and Filter Paper Samples for Radiochemical Analysis The digestate is then treated like a liquid (section 113)

1183 Remove an aliquot (typically 1 - 5 gm) with a spatula and place into a clean labeled aluminum pan (Aluminum weighing pans work well)

1184 Place sample on a hot plate or in a drying oven at approximately 105deg C and evaporate any moisture

1185 When dry remove from hot plate or oven and allow the sample to cool

1186 Using a metal spatula reduce the solid sample to a fine particle size

NOTE Sample size is restricted to 100 mg for alphabeta analysis

1187 Self adhesive label dots of the chosen planchet size can be used advantageously to hold finely divided solid material uniformly for gross alpha andor beta analysis Tare the prepared planchet

1188 Distribute the sample ash evenly in a tared stainless steel planchet

1189 Weigh and record the gross sample weight

11810 Prepare a method blank from 1 ml of the Na2SO4 solution

118101 Pipette directly into a tared planchet Prepare LCS in the same manner spiking with 1 ml of the standards described in 731 and 732 Note separate LCSs must be prepared for alpha and beta analysis due to the alpha emitting decay products of Sr-90 Evaporate on a hot plate DO NOT ALLOW LIQUID TO SPLATTER Do not allow residue to bake on hot plate

OR

118102 Use table salt for the blank and a soil standard reference material ie NIST Traceable Rocky Flats Soil for the LCS Prepare in the same fashion as the samples




119 Reprocessing planchets which are over the weight limit

12




1191 Rinse residue from planchet with 4 N HNO3 into a beaker Use a policeman if needed to complete the transfer

1192 Redissolve the residue into 4 N HNO3 Dilute the sample to a known volume

1193 Remove an aliquot which will keep the residue weight under the limit and transfer to the tared planchet

1194 Evaporate to dryness on a warm hot plate so that the sample does not boil Remove sample from hot plate Allow to cool


DATA ANALYSIS AND CALCULATIONS

121 To calculate the aqueous sample volume required (ml) use the following equation

target net residue weight (mg) initial aliquot volume (ml) ml required =

initial aliquot net residue weight (ing)

122 To calculate the density (mgcm2) use the following equation

ret residue weight (rrg) mg orr =

2027orf (2planchet)

123 To calculate the Activity (pCiunit mass or volume) use the following equation

R - R

2 2 2 E TF V A

Where

As = Activity of the sample Rs = Count rate of the sample (in cpm) RB = Count rate of detector background (in cpm) E = Detector efficiency TF = Transmission factor VA = Sample aliquot volume or mass

124 To calculate the total 2s error use the following equation

U A P = 1 9 6 A I (R s t s ) + ( R B t s ) A C

| (R s t s ) - (R B t s ) | J




Where

As = Activity of the sample Rs = Count rate of the sample (in cpm) RB = Count rate of detector background (in cpm) ts = Count time for analysis

125 To calculate the Minimum Detectable Activity use the following equation

465 JRB t _ + 271 M D A = -mdash shy

22 2 E TF V A t s

Where

MDA = Minimum Detectable Activity of the sample RB = Count rate of detector background (in cpm) E = Detector efficiency ts = Count time for analysis TF = Transmission factor VA = Sample aliquot volume

126 To calculate the Relative Percent Difference use the following equation

RPD = 100 4shyT

Where

As = Sample activity = Sample activity of the duplicate

127 To calculate the LCS recovery use the following equation

R = poundsect_ 100 TVX VLCS

Where

ALCS = LCS Observed activity TVLCs = True Value of the LCS

128 To calculate the MS(MSD) recovery use the following equation

SOP No STL-RC-002Q Revision No



A mdash Ashy

Where

AMS(MSD) MS(MSD) observed activity TVMS(MSD) True Value of the MS(MSD) AS Sample activity


The following represent data assessment for samples and acceptance criteria for QC measures and corrective actions for any failure in QC measurements


1311 Method Blank

13111 No target analyte may be present in the method blank above the reporting limit

1312 Laboratory Control Sample (LCS)

13121 All control analytes must be within established control limits for accuracy (Recovery) and precision (RPD) Exceptions are allowed only with QA and project management approval

1313 Matrix SpikeMatrix Spike Duplicate (MSMSD)

131311 All analytes should be within established control limits for accuracy (Recovery) and precision (RPD) Deviations from this may be the results of matrix effects which are confirmed by passing LCSs

13132No specific corrective actions are required in the evaluation of the MSMSD results provided that the batch LCS is in control Analysts should use sound judgment in accepting MSMSD results that are not within control limits especially if the LCS results are borderline


141 Method Blank




1411 The samples in the batch associated to the defective method blank are evaluated

14111 If the analyte found in the method blank is confirmed to not be present in any of the associated samples at any level the contamination did not affect those samples This represents a non-impact situation and no specific corrective action is taken A nonconformance memo is written to notify project management of the situation for evaluation against project requirements

14112If the analyte found in the method blank is confirmed to be present in one or more of the associated samples the concentrations are compared

141121 If the analyte concentration in the method blank exceeded 10 of concentration found in one or more samples the prescribed corrective action is to re-analyze all affected samples

141122 If the concentration in the method blank was less than 10 of the concentration found in one or more samples the sample can be reported by qualifying the affected analytes A nonconformance memo is written to notify project management of the situation for evaluation against project requirements

142 Laboratory control sample

1421 If any control analyte is out of control for accuracy ( Recovery) the associated samples are evaluated

14211If the recovery is biased high and the associated samples have no positive results for that analyte a non-impact situation ensues A nonconformance memo is written to notify project management of the situation for evaluation against project requirements

14212If the recovery is biased low and the associated samples have positive results for that analyte a minimal impact situation ensues A nonconformance memo is written to notify project management of the situation for evaluation against project requirements

14213If the recovery is biased high and the associated samples have positive results for that analyte the prescribed corrective action is reanalysis of the affected sample(s)

14214If the recovery is biased low and the samples have no positive results for that analyte the prescribed corrective action is reanalysis of the affected sample(s)




1422 If any control analyte is out of control for precision (RPD) the associated samples are evaluated All decisions about corrective action(s) are made in consultation with the project manager

1422llf there are no positive results in one or more samples a non-impact situation ensues for those samples A nonconformance memo is written to notify project management of the situation for evaluation against project requirements

14222If there are positive results for one or more analytes the likelihood of poor reproducibility increases and corrective action must be evaluated A nonconformance memo is written to notify project management of the situation for a project decision on whether the affected sample(s) should be reanalyzed


151 Method blanks

1511 If there is insufficient sample to perform re-analysis the analyst must notify the project manager for consultation with the client In this situation all associated samples are flagged with a C qualifier and appropriate comments in the narrative

152 LCS

1521 If the batch is not re-extracted and reanalyzed the reasons for accepting the batch must be clearly presented in the project records and the report (can be accomplished with an NCM) Acceptable matrix spike recoveries are not sufficient justification to preclude re-extraction of the batch

1522 If re-extraction and reanalysis of the batch is not possible due to limited sample volume or other constraints the LCS is reported all associated samples are flagged and appropriate comments are made in a narrative to provide further documentation

153 Insufficient sample

1531 If there is insufficient sample to repeat the analysis the project manager is notified via NCM for consultation with the client






1611 The groupteam leader has the responsibility to ensure that this procedure is performed by an analyst who has been properly trained in its use and has the required experience




18 WASTE MANAGEMENT


19 CLARIFICATIONS MODIFICATIONS AND ADDITIONS TO REFERENCE METHOD

191 Corrective actions for quality control samplesstandards not meeting the criteria stated in Section 9 are as follows

1911 Correlation coefficient stop analysis and rerun the standard curve

1912 CCVS ICVS stop analysis and reanalyze all samples analyzed after the last acceptable calibration verification standard

1913 Laboratory Control Sample re-prep and reanalyze all samples associated with the unacceptable LCS

1914 Matrix Spike matrix spike recoveries outside the suggested limit will be assumed to be due to matrix effect and will be flagged

1915 Duplicate RPDs outside the suggested limit will be assumed to be due to matrix effect and will be flagged

1916 Method Blank ICB CCB re-prep and reanalyze all samples associated with the unacceptable method blank For an unacceptable ICB investigate instrument




contamination and reanalyze the samples For an unacceptable CCB investigate instrument contamination and reanalyze all samples analyzed after the last acceptable CCB


1921 Procedural variations are allowed only if deemed necessary in the professional judgement of supervision to accommodate variation in sample matrix radioactivity chemistry sample size or other parameters Any variation in procedure shall be completely documented using a Nonconformance Memo and approved by the Technical Director and QAQC coordinator If contractually required the client will be notified The Nonconformance Memo will be filed in the project file

1922 Any unauthorized deviations from this procedure must be documented as a nonconformance with a cause and corrective action described A Nonconformance Memo shall be used for this documentation The original Nonconformance Memo will be filed in the project file


1931 Record all analysis data on a sample data sheets or in computer weighing file Include all method blanks LCSs duplicates and MSMSDs

1932 All raw data data run logs copies of standard logs and quality control charts are released to the Document Control Coordinator after review and approval

194 MDA Table

1941 The following tables show the MDAs achievable with this procedure when varying amounts of sample and varying count times are used with this SOP

1942 Liquids

Highest Lowest Transmission Minimum Count Achievable Background Efficiency Factor Volume (L) Time MDA (pCiL)

(cpm) (minutes)

Gross Alpha 0100 27 29 0100 1000 279

Gross Alpha 0100 27 29 0200 100 494

Gross Alpha 0100 27 29 0200 200 333

Gross Alpha 0100 27 29 0200 1000 139

Gross Beta 1500 40 90 0100 1000 229

Gross Beta 1500 40 90 0200 100 373

20




Gross Beta 1500 40 90 0200 200 260

Gross Beta 1500 40 90 0200 1000 114

195 Solids

Highest Lowest Transmission Minimum Count Achievable Background Efficiency Factor Weight (g) Time MDA (pCig)

(cpm) (minutes)

Gross Alpha shy 0100 27 20 1000 100 143 Leached Gross Alpha 0100 27 20 0100 100 1431

Gross Alpha 0100 27 20 0100 200 966

Gross Alpha 0100 27 20 0100 1000 405

Gross Beta shy 1500 40 78 1000 100 086 Leached Gross Beta 1500 40 78 0100 100 861

Gross Beta 1500 40 78 0100 200 601

Gross Beta 1500 40 78 0100 1000 264

196 Associated SOPs

1961 SL13019 Calibration of the Low Background Gas Flow Proportional Counting System

1962 STL-RD-0403 Daily Calibration Verification and Maintenance of the Low Background Gas Flow Proportional Counting System

REFERENCES

201 Quality Assurance Program Requirements for Nuclear Facilities ANSIASME NQA-1 (latest edition)

202 EPA 6004-80-032 Prescribed Procedures for Measurement of Radioactivity in Drinking Water Method 9000 August 1980

203 APHAAWWAWEF Standard Methods for Water and Wastewaters 18th Edition Method 7110 1992

204 Test Methods for Evaluating Solid Waste PhysicalChemical Methods SW846 Method 9310 Rev 0 September 1986

205 DOEEM-0089T Rev 2 DOE Methods for Evaluating Environmental and Waste Management Samples Method RP710 October 1994




206 STL Quality Assurance Management Plan

207 STL St Louis Quality Assurance Management Plan Laboratory Specific Attachment


209 Quanterra St Louis Laboratory STL-QA-0002 Standards Preparation Procedure

2010 Quanterra St Louis Laboratory STL-QA-0004 Automatic Pipetter Calibration

2011 Quanterra St Louis Laboratory STL-QA-0006 Sample Receipt and Chain-of-Custody

2012 Quanterra St Louis Laboratory STL-QA-0013 Personnel Training and Evaluation

2013 Quanterra St Louis Laboratory STL-RC-0002 Preparation of Stainless Steel Planchets for Radiochemistry Analyses

2014 Quanterra St Louis Laboratory SL13021 Operation of Low Background Gas Flow Proportional Counting System

SOP No STL-RC-0040 Date Implemented 042401

Revision No 0 __ _ _ bdquo -r ^rDV Revision Date 041301 UNCONTROLLED COPY P a geiof i4

Controlled Copy No


Title Total Alpha Emitting Isotopes of Radium (SUPERSEDES SL13003)

Teclîcal Specialist

ltmdash Approved by ^rgt

Quality Assurance Manager

^ S - Approved by

Environment Health and Safety Coordinator

^ Approved by

Laboratory Director


This document has been prepared by and remains the sole property of Severn Trent Services Incorporated (STL) It is submitted to a client or government agency solely for its use in evaluating STLs qualifications in connection with the particular project certification or approval for which it was prepared and is to be held proprietary to STL

The user agrees by its acceptance or use of this document to return it upon STLs request and not to reproduce copy lend or otherwise disclose or dispose of the contents directly or indirectly and not to use it for any purpose other than that for which it was specifically furnished The user also agrees that where consultants or others outside of the users organization are involved in the evaluation process access to these documents shall not be given to those parties unless those parties also specifically agree to these conditions


Revision No 0 Revision Date 041301

Page 2 of 14


Title Total Alpha Emitting Isotopes of Radium

10 SCOPE AND APPLICATION

11 This procedure describes the determination of total Radium for all isotopes emitting alpha radiation

12 This procedure applies to the analysis of these isotopes in water and in other media where dissolution and carrier exchange are readily available in the laboratory

121 The barium sulfate from the last part of the 228Ra procedure (STL-RC-0041) can be counted for total alpha radiation if a sequential procedure is desired Care should be taken to ensure even distribution of the precipitate on each planchet prior to counting The time of the last barium sulfate precipitation should be recorded and used in calculating the ingrowth factor

13 Responsibilities

131 Radiation Safety Officer (RSO) (or hisher designee) indicates to the analyst any necessary precaution that should be taken to protect hisher health and safety based on sample classification into hazardous and radioactive categories

132 Laboratory Manager (or hisher designee) delegate the performance of this procedure to personnel that are experienced with the procedure and with the equipment associated with implementation of the procedure

133 Radiochemistry Laboratory Manager (or designee) to delegate the performance of this procedure to personnel who are experienced with this procedure and with the equipment associated with the implementation of this procedure

134 Analyst Apply any precautions noted by the procedure to adhere to the instructions contained in the procedure and to perform this procedure independently only when formally qualified Follow the instructions and to report any abnormalities immediately to the supervisor for the Radiochemistry Preparation Lab Inspect worksheets for accuracy and completeness inspect sample for proper volume and size inspect equipment for proper operation and inspect balances to ensure that the calibration is not out of date



Page 3 of 14

20 SUMMARY OF METHOD

21 Barium and lead are used to coprecipitate radium as the sulfate Following chelation with EDTA (Ra-Ba) sulfate is precipitated purified and counted in a gas flow proportional counter measuring alpha radiation only Total radium is quantified by applying correction factors for ingrowth of 226Ra progeny gravimetric yield and counting efficiency

30 DEFINITIONS

31 See STL Quality Management Plan (QMP) for glossary of common terms

32 Minimum Detectable Activity (MDA) - The smallest amount of radioactivity that can be detected given the conditions of a specific sample It is reported at the 95 confidence interval meaning that there is a 5 chance that a false signal was reported as activity and 5 chance that true radioactivity went undetected

40 INTERFERENCES

41 This procedure screens for 226Ra by measuring the alpha emitting radium isotopes It follows that if there is no detectable radium alpha activity there would be no 226Ra above the specified detection limit

42 Waters that contain large amounts of barium will cause a bias to the gravimetric yield

50 SAFETY

51 Procedures shall be carried out in a manner that protects the health and safety of all STL Associates

52 Eye protection that satisfies ANSI Z871 (as per the Chemical Hygiene Plan) laboratory coat and appropriate gloves must be worn while samples standards solvents and reagents are being handled Disposable gloves that have been contaminated will be removed and discarded other gloves will be cleaned immediately VITON gloves may be worn when halogenated solvents are used for extractions or sample preparation Nitrile gloves may be used when other solvents are handled [Note VTTON is readily degraded by acetone all solvents will readily pass through disposable latex rubber gloves]



Page 4 of 14

53 The following materials are known to be hazardous

531 The following materials are known to be corrosive nitric acid acetic acid citric acid sulfuric acid and ammonium hydroxide

532 The following materials are known to be oxidizing agents nitric acid

54 Exposure to chemicals must be maintained as low as reasonably achievable therefore unless they are known to be non-hazardous all samples must be opened transferred and prepared in a fume hood or under other means of mechanical ventilation Solvent and

waste containers will be kept closed unless transfers are being made

55 The preparation of standards and reagents will be conducted in a fume hood with the sash closed as far as the operations will permit or by other means of mechanical ventilation

56 All work must be stopped in the event of a known or potential compromise to the health and safety of a STL Associate The situation must be reported immediately to a laboratory supervisor

60 EQUIPMENT AND SUPPLIES

61 Low background gas proportional counter Tennelec LB4000 or equivalent

62 Electric stirring hot plates

63 Centrifuge

64 IR drying lamp

65 Analytical balance

66 Stainless steel planchets

67 Glassware as appropriate

68 Suction filtering apparatus

SOP No STU-RC-0040 Date Implemented 042401


Page 5 of 14

70 REAGENTS AND STANDARDS

71 Distilled or deionized water ASTM Type H (1 991 ) from the Millipore unit

72 Acetic acid (1 74 N 998) concentrated glacial CH3COOH specific gravity 1 05

73 Ammonium hydroxide (15 N 566) concentrated NUtOH sp gr 090

74 Ammonium sulfate (200 mgL) - dissolve 200 grams (NFL^SC^ in 300 ml deionized water Bring to a volume of 1 000 ml

75 Barium carrier - dissolve 2846 g BaCl2-2H2O in 750 ml deionized water Add 5 ml 16N HNO3 Dilute to 1000 ml

751 Standardize the barium carrier solution using the following procedure

7511 Pipette 10 ml barium carrier solution (16 mgml Ba) into six separate labeled centrifuge tubes containing 15 ml DI HÔ

7512 Add 1 ml 18 N sulfuric acid with stirring and digest precipitate in a hot water bath for approximately 1 0 min

7513 Cool centrifuge and decant the supemate into appropriate waste container

7514 Wash precipitate with 15 ml DI water centrifuge and decant the supemate

7515 Transfer the precipitate to a tared stainless steel planchet with a minimum amount of DI water

7516 Dry on a heat source Store in desiccator until cool and weigh as barium sulfate

7517 Record the net weights of the precipitates and calculations in the Rad Standards Preparation Log Assign the solution a unique number

76 Citric acid (1M) - dissolve 192g of CeHsCVFbO in water and dilute to 100 ml

77 EDTA reagent basic (025M) - dissolve 20g NaOH in 750ml water heat and slowly add 93g [ethylenedinitrilo] tetraacetic disodium salt (CioHi4O8N2Na22H2O) while stirring Dilute to 1 liter



Page 6 of 14

78 Lead carrier (15 mgml) - dissolve 2397g Pb(NO3)2 in water add 05 ml 16N HN03 and dilute to 100 ml with water

79 Methyl orange indicator (01) - dissolve 01 g methyl orange indicator in 100 ml water

710 Nitric acid (16 N 704) concentrated HN03 sp gr

711 Sulfuric acid (18 N) - Cautiously mix 1 volume 36N H2S04 (concentrated) with 1 volume of water


CAUTION During preparation of reagents associates shall wear lab coat gloves safety glasses with side shields face shield (discretionary) and laboratory approved shoes as a minimum Reagents shall be prepared in a fume hood

80 SAMPLE COLLECTION PRESERVATION AND STORAGE

81 All samples may be collected in glass or plastic containers

82 Preserve all aqueous samples with nitric acid to a pH of less than 2

83 Samples must be analyzed within 180 days of the collection date

90 QUALITY CONTROL

91 Prepare and analyze quality control (QC) samples concurrent with routine samples The frequency of QC samples is determined for each particular project In the absence of specific instruction from Project Management the frequency of quality control samples is based on a batch of 20 samples or less of a similar matrix For up to 20 samples include one blank one spike and one duplicate sample

92 For aqueous samples deionized water (DI fÔ) is used as a blank Measure an aliquot DI H2O into the appropriate size beaker and adjust the pH to less than 2 using 16 N HN03

93 Prepare a spike sample (LCS) according to the expected level of radioactivity in the samples being prepared



Page 7 of 14

931 Approximately 10-30 dpm is adequate for an environmental water sample with no known history of radioactive contamination

932 The spike for a batch of samples suspected to contain radioactivity should contain the same quantity of radioactivity as the samples If unknown the spike should be approximately 2-5 times the target detection limit

94 For duplicates use two aliquots of equivalent volume when possible If there is insufficient sample volume to achieve this take the volume required for the original sample and less for the duplicate

95 Calculate the activity associated with the blank sample and report as the method detection limit It is common for DI water to exhibit count rates greater than Rt but the calculated activity must be less than the contract required detection limit

96 The recovery of the barium carrier solution should exceed 35 and be less than 110

97 Record data for all QC samples in the appropriate logbook

98 Reextract any sample where the barium recovery (R) is identified to be less than 35 or greater than 110 Reextract the entire batch if R for the blank or LCS exceed these limits If the samples exhibit the same characteristics after the second analysis notify the project manager Report the results of both analyses Identify the data in the case narrative of the client report and explain the matrix interference

99 Reextract the batch of sample when the associated LCS does not fall within plusmn 3 standard deviations from the lab generated control limits

910 Identify any batch where the activity in the blank exceeded the Contract Required Detection Limit (CRDL) A sample shall be reextracted if the calculated result was gt CRDL and lt lOx CRDL Process the samples including a blank and LCS with this batch

911 Evaluate the results of the duplicate analysis Identify any batch where the duplicate activity exceeded plusmn 3x the standard error of the original activity Identify the batch in the case narrative in client report Reextraction is required only if requested by the client



Page 8 of 14


101 The Gas Proportional Counting System must be characterized such that the response to (RashyBa)SCgt4 is firmly established and the appropriate correction factors have been established and documented See SOP STL-RD-0404

110 PROCEDURE



113 Initiate a sample worksheet for the samples to be analyzed and complete as required See Figure 1

114 Confirm that sample is acidic pH less than 2 using pH paper If not acidic add 2 ml 16N HNOa per liter of sample and mix thoroughly Notify laboratory supervisor and initiate a nonconformance

115 Ensure that sample container is capped tightly and shake it thoroughly Transfer to a beaker an aliquot of appropriate size Label beaker with sample ID number Record all data on sample worksheet

116 Add 1 M citric acid in the ratio of 5 ml per liter Add methyl orange indicator until the persistence of a red color Mix thoroughly

117 Add 10 ml standardized barium carrier and 2 ml of lead carrier heat and stir until incipient boiling

118 Add ammonium hydroxide dropwise until the solution changes from pink to yellow or the pHisgt65



Page 9 of 14

119 Add 18N sulfuric acid until the red color reappears or the pH is lt 2 then add 5 ml ammonium sulfate Stir the samples for a minimum of 15 minutes and turn off the heat of the stirrer Remove the stir bar

1110 Cover the beaker and allow the precipitate to settle for at least four to six hours Note the lead and barium sulfate should be clearly separate from the solution

1111 Remove the clear supemate using suction and discard into the appropriate waste container Quantitatively transfer the precipitate to a 50 ml centrifuge tube using a strong jet of deionized

1112 Centrifuge for 10 minutes at a speed sufficient to cause the precipitate to form a pellet Pour off liquid and save the BaS04 precipitate

1113 Carefully add 10 ml 16N HNOa Cap tube and vortex to ensure complete mixing Centrifuge for 10 minutes at a speed determined as in 5810 Pour off the liquid and save the BaSCgt4 precipitate

1 114 Repeat preceding step once using deionized water as a rinse Save the BaSCU precipitate and proceed to the next step

1115 Add 20 ml basic EDTA reagent heat in a hot water bath and stir until precipitate dissolves Add a few drops ION NaOH if precipitate does not readily dissolve

1116 Add 1 ml (NH^SC^ (200 mgml) and stir thoroughly Add 1 74N CH3COOH until barium sulfate precipitates then add 2 ml excess Note date and time of BaSCgt4 precipitation on the sample data sheet Digest in a hot water bath until precipitate settles Centrifuge and discard supemate

1117 Wash precipitate with 1 0 ml water Centrifuge and discard supemate

1118 Transfer precipitate to a tared stainless steel planchet with a minimum amount of water

1 1181 Dry on a hot plate on medium heat Cool in a dessicator and then weigh planchet

11182 Heat the planchet again using the infrared lamp Weigh the planchej a second time to confirm that the weight of the planchet has not changed (plusmn 0005 mg)



Page 10 of 14

11183 Repeat steps 11181 and 11182 until the weight of the planchet is constant 1119 Record the final weight of the planchet to determine the chemical recovery for the barium

carrier solution

1120 Submit planchet for counting at alpha voltage only


121 The following definitions are used for all of the equations described in this section

466 = statistically derived constant 222 = conversion factor dpmpCi 196271= constants RS = sample count rate in alpha cpm Rb = background count rate in alpha cpm ts = sample counting time in minutes tb = background counting time in minutes 1 = Lambda decay constant for 222Rn 00075 hr1

t = time between the barium sulfate precipitation and the midpoint of the counting in hours

Eff = detector efficiency for alpha only V = volume or mass in appropriate units R = chemical recovery () gravimetric yield of barium carrier solution

Calculated by dividing the net weight of the barium precipitate (step 1119) by the mass of barium added (step 117) Note that the maximum recovery used in the equation is 10

I = ingrowth factor to correct for the increase in alpha count rate from radium progeny

122 Calculate the Critical Count Rate (CCR) using the equation below

123 Calculate the 226 Ra ingrowth factor (I) as follows



Page 11 of 14

124 Calculate the sample MDA for samples when any one of the following conditions are met

0 Rs less than Rb 0 Rs less than the CCR as described in the preceding paragraph 0 The calculated activity less than the error value This will occur when Rs is greater

then Rb and it indicates interference such that an accurate determination is not possible under these conditions

1241 The MDA is defined as the smallest amount of activity we are able to detect given the conditions of a specific sample It is reported at 95 confidence interval meaning that there is a 5 chance that a false signal was reported as activity and a 5 chance that true activity went undetected

1242 The following formula is used to calculate MDA of total radium (pCi per unit mass or volume)

466jRbxt +271 MDA = -1mdash---shy

222 xEjfxVxRxlxt

125 For samples where the count rate is greater than the CCR the activity and error must be calculated using the equations given below

Activity (A) total radium (pCi per unit mass or volume)

A

Error (E) total radium (pCi per unit mass or volume)

1961 raquo E =

222

1251 Calculate and report results with associated error to two significant places DO NOT report an error with more significant digits than the associated activity

126 Calculate the Relative Percent Difference (RPD) for all duplicate analysis using the equation below



Page 12 of 14

= original-duplicate original +duplicate

1261 Report the RPD values in the appropriate logbook Consult the acceptance range and notify the laboratory supervisor of values that out of control

127 Calculate the percent recovery on spiked sample using the equation below

observed value Recovery = x 100

exp ected value

1271 Review the data and notify the laboratory supervisor of any values that exceed the control limits

128 If the client has requested 226-Ra results and 228-Ra analysis has been performed the 226-Ra results are calculated as follows

Ra226 (pCiunit volume) = TRA (pCiunit volume) - (Ra228 (pCiunit volume) x (


Training Qualification

The groupteam leader has the responsibility to ensure that this procedure is performed by an analyst who has been properly trained in its use and has the required experience


This procedure will be carried out in a manner consistent with all applicable federal state and local regulations regarding pollution control and prevention Specific controls due to the accidental release of hazardous materials can be found in the STL Chemical Hygiene Plan and facility attachments



Page 13 of 14

150 WASTE MANAGEMENT

Waste generated in the procedure must be segregated and disposed according to the facility hazardous waste procedure The Health and Safety Director should be contacted if additional information is required

160 REFERENCES

161 US Nuclear Regulatory Commission Regulatory Guide 415 Quality Assurance for Radiological Monitoring Programs (Normal Operations) - Effluent Streams and the Environment


163 Alpha Emitting Radium Isotopes in Drinking Water Method 9030 Prescribed Procedures for Measurement of Radioactivity in Drinking Water EPA 6004-30-032 Section 6 Environmental Protection Agency

164 STL Quality Management Plan latest revision

165 STL St Louis Laboratory Quality Assurance Manual Laboratory Specific Attachment

166 Associated SOPs

1661 STL St Louis Laboratory Standards Preparation STL-QA-0002 Standards Preparation Procedures

1662 STL St Louis Laboratory Automatic Pipetter Calibration STL-QA-0003 Instrument Calibration Procedures

1663 STL St Louis Laboratory Sample Receipt and Chain of Custody STL-QA-0006 Sample Receipt Procedures

1664 STL St Louis Laboratory Tersonnel Training and Evaluation STL-QA-0013 Quality Control Procedures

1665 STL St Louis Laboratory Nonconformance and Corrective Action STL-QA-0026 Miscellaneous Procedures



Page 14 of 14

1666 STL St Louis Laboratory Preparation of Soil Sludge and Filter Paper Samples for Radiochemical Analysis STL-RC-0004 Radiochemistry Procedures

1667 STL St Louis Laboratory Radium 228 in Water STL-RC-0041 Radiochemistry Procedures

1668 STL St Louis Laboratory Evaluation of the Sample Transmission Factor for the Gas Proportional Counting System STL-RD-0404 Radiochemistry Procedures

1669 STL St Louis Laboratory Operation of the Low Background Gas Flow Proportional Counter STL-RD-0402 Radiochemistry Procedures

16610 STL St Louis Laboratory Radium 226 and Radon 222 by Radon Emanation STL-RC-0042 Radiochemistry Procedures

170 MISCELLANEOUS


1711 All counting data and hard copies of summary sheets must be maintained in the radiochemistry operational files These must be kept in reasonable order such that timely retrieval is possible



Pa9e 1UNCONTROLLED COPY Controlled Copy No X^


TITLE Radium 228 in Water

(SUPERSEDES SL13010)

Prepared by

Reviewed by Technical Specialist


Approved by __ EnvironmentfHealth and Safety Coordinator







Page 2 of 18


Title Radium 228 in Water


11 This method covers the determination of Radium 228 (228Ra) by direct measurement of its syjo

beta emitting progeny Actinium ( Ac) It is applicable to liquid or other media where complete dissolution and carrier exchange are readily achievable in the laboratory For media where chemical dissolution is impractical non-destructive measurement of the three

bullyjo

principal photons of Ac by gamma spectrometry is better suited

12 The barium sulfate precipitate from this procedure contains all radium isotopes and therefore can be used for 226Ra also

13 Responsibilities

131 Radiochemistry Laboratory Manager or designee delegates the performance of this procedure to Associates who have been trained and qualified in its use The Laboratory Manager is responsible to ensure that this procedure is followed for all samples analyzed under its scope

132 Preparation Laboratory Supervisor ensures that this procedure is performed by an analyst who has been properly trained in its use and has the required experience

133 Analyst Applies any precautions noted by the procedure to adhere to the instructions contained in the procedure and to perform this procedure independently only when formally qualified Follows the instructions and reports any abnormalities immediately to the supervisor for the Radiochemistry Preparation Lab Inspects worksheets for accuracy and completeness inspects sample for proper volume and size inspects equipment for proper operation and inspects balances to ensure that the calibration is not out of date


21 Radium isotopes are collected by coprecipitation with barium and lead sulfate and purified by precipitation from EDTA solution After a suitable ingrowth period 228Ac is separated and carried on yttrium oxalate purified and counted for the presence of total beta radiation The precipitation and counting are performed in a manner consistent with the time requirements of the 613 hour half life of 228Ac By applying correction factors for ingrowth and decay and appropriately calibrating the beta counter 228Ra is quantified



Page 3 of 18

30 DEFINITIONS

31 See STL Quality Assurance Management Plan (QAMP) for glossary of common terms

40 INTERFERENCES

41 Strontium 90 (^Sr) or other beta emitting radionuclides that are carried by the yttrium oxalate precipitate (ie certain mixed fission or activation products) will yield a positive bias to the 228Ra values

42 Samples which contain excess barium could cause inaccurate chemical yield determinations

43 Excessive barium chemical yields may also be caused by improper handling The BaSCU can be redissolved and precipitated a second time to check this

50 SAFETY


52 Eye protection that satisfies ANSI Z871 (as per the Chemical Hygiene Plan) laboratory coat and appropriate gloves must be worn while samples standards solvents and reagents are being handled Disposable gloves that have been contaminated will be removed and discarded other gloves will be cleaned immediately VTTON gloves may be worn when halogenated solvents are used for extractions or sample preparation Nitrile gloves may be used when other solvents are handled [Note VTTON is readily degraded by acetone all solvents will readily pass through disposable latex rubber gloves]


531 The following materials are known to be corrosive acetic acid ammonium hydroxide nitric acid sodium hydroxide and sulfuric acid

532 The following material is a known oxidizing agent nitric acid

54 Samples shall be screened and classified before being handled by the Associate Controls shall be implemented to limit exposures to Category HI samples as defined by the Radiation Safety Officer



Page 4 of 18


55 Exposure to chemicals must be maintained as low as reasonably achievable therefore unless they are known to be non-hazardous all samples must be opened transferred and prepared in a fume hood or under other means of mechanical ventilation Solvent and waste containers will be kept closed unless transfers are being made




61 Low background gas proportional counter


63 Centrifuge

64 IR Drying Lamp or equivalent







Page 5 of 18


71 Distilled or deionized water ASTMII (1991) from the Millipore unit

72 Acetic acid 174N glacial CH3COOH (concentrated) specific gravity 105 998

73 Ammonium hydroxide 15N NTLjOH (concentrated) sp gr 090 566

74 Ammonium oxalate 5 Dissolve 5g (NH4)2C20-H20 in water and dilute to 100ml

75 Ammonium sulfate 200mgml Dissolve 20g (NH4)2S04 in water and dilute to 100ml

76 Ammonium sulfide 2 Dilute 10ml (NH^S (20-24) to 90 ml water total volume 100ml

77 Barium carrier 16mgml standardized Dissolve 2846g BaCl2-2H2O in water add 05 ml 16N HNO3 and dilute to 100 ml with water


7711 Pipette 10 ml barium carrier solution (16 mgml Ba) into six separate labeled centrifuge rubes containing 15 ml DIH2O

7712 Add 1 ml 18 N sulfuric acid with stirring and digest precipitate in a hot water bath for approximately 10 min






78 Citric acid 1M Dissolve 192g C6H8O7-H2O in water and dilute to 100ml



Page 6 of 18

79 EDTA reagent basic (025M) shy dissolve 20g NaOH in 750ml water heat and slowly add 93g [ethylenedinitrilo] tetraacetic disodium salt (CioHi4O8N2Na2-2H2O) while stirring Dilute to 1 liter

710 Lead carrier 15mgml Dissolve 2397g Pb(NO3)2 in water add 05 ml 16N HN03 and dilute to 100ml with water

711 Lead carrier 15mgml Dilute 10ml lead carrier (15mgml) to 100ml with water

712 Methyl orange indicator 01 Dissolve 01g methyl orange indicator in 100ml water

713 Nitric acid 16N HNO3 (concentrated) specific gravity 142 704

714 Nitric acid 6N Mix 3 volumes 16N HNO3 (concentrated) with 5 volumes of water

715 Nitric acid IN Mix 1 volume 6N HN03 with 5 volumes of water

716 Sodium hydroxide 18N Dissolve 72g NaOH in water and dilute to 100ml

717 Sodium hydroxide 1 ON dissolve 40g NaOH in water and dilute to 100ml

718 Strontium carrier 10 mgml Dissolve 2416g Sr(NO3)2 in water and dilute to 1 liter

719 Sulfuric acid 18N Cautiously mix 1 volume 36NH2SO4 (cone) with 1 volume of water

720 Yttrium Carrier 18 mgml standardized Add 3828 grams of yttrium nitrate tetrahydrate (Y(NO3)3-4H2O) to a volumetric flask containing 20 ml of DI water Continue stirring with a magnetic stirring plate while adding 5 ml of 16N HNO3 After total dissolution dilute to 1 Liter with water

7201 Standardize the yttrium carrier using the following procedure

72011 Add 10 ml DI water to a 50 ml centrifuge tube

72012 Add 10 ml of Yttrium carrier (18 mgml) using a Class A pipet

72013 Add 70 ml of 18N NaOH Stir well and digest in a hot water bath until the yttrium hydroxide coagulates This should take at least 5 minutes



Page 7 of 18

72014 Centrifuge and decant the supemate into the appropriate waste container

72015 Dissolve the precipitate in 2ml 6N nitric acid Heat and stir in a hot water bath about 5 minutes Add 5 ml water and precipitate yttrium hydroxide with 3 ml ION sodium hydroxide Heat and stir in a hot water bath until precipitate coagulates Centrifuge and discard supernate

72016 Dissolve precipitate with 1 ml IN nitric acid and heat in a hot water bath a few minutes Dilute to 5ml with DI water and add 2ml 5 ammonium oxalate Heat to coagulate centrifuge and discard supernate

72017 Add 10ml water 6 drops IN nitric acid and 6 drops 5 ammonium oxalate Heat and stir in a hot water bath a few minutes Centrifuge and discard supernate

72018 To determine yttrium yield quantitatively transfer the precipitate to a tared stainless steel planchet using a minimum amount of water Dry with a heat source to constant weight and count in a gas flow proportional counter for total beta radiation Record tare and gross weights on sample worksheets

t


721 Yttrium carrier 9 mgml Dilute 50 ml yttrium carrier (18 mgml) to 100 ml with water

722 Strontium-yttrium mixed carrier 09 mgml Sr+2 09 mgml Y3 a Solution A Dilute 100 ml yttrium carrier (18 mgml) to 100 ml b Solution B Dissolve 04348 g Sr(NO3)2 in water and dilute to 100 ml

7221 The mixed carrier is made by adding equal volumes to a flask






Page 8 of 18

83 Samples should be stored for no more than 180 days

90 QUALITY CONTROL

91 Prepare and analyze quality control (QC) samples concurrent with routine samples The frequency of QC samples is determined for each particular project In the absence of specific instruction from Project Management the frequency of quality control samples is based on a batch of 20 samples or less of a similar matrix For up to 20 samples include 1 blank 1 spike and 1 duplicate sample

92 For aqueous samples deionized water (DI) is used as a blank since reagents are prepared using DI as opposed to tap water Measure an aliquot DI into the appropriate size beaker and adjust the pH to less than 2 using HNO3 See Table I for appropriate volumes

93 Prepare a LCS in the range of the expected sample activity See Table n for appropriate activity ranges

94 Use two aliquots of equivalent volume when possible If there is insufficient sample volume to achieve this take the volume required for the original sample and less for the duplicate


96 The recovery of the barium and yttrium carriers should exceed 35 and be less than 110


98 Reextract any sample where the barium or yttrium recovery is identified to be less than 35 or greater than 110 Reextract the entire batch if the recovery for the blank or LCS exceed these limits If the samples exhibit the same characteristics after the second analysis notify the project manager Report the results of both analyses Identify the data in the case narrative of the client report and explain the matrix interference

TABLE I

SAMPLE TYPE

Environmental Water Sample Ground Surface or Well Water

Finished drinking water or other sample where the volume exceeds 1000 ml



Page 9 of 18

BLANK VOLUME

1000 ml

Same volume as sample

TABLE H SAMPLE TYPE ACTIVITY LEVEL

FOR SPIKE Finished drinking 7-16dpmperspike water Environmental Water 7-30 dpm per spike sample from area with no known tiistory of contamination Environmental water within the range of samples from area expected sample with known history of activity contamination Radioactive samples within range of that are marked as expected sample such and require activity not to exceed small volumes (less 025 nCi per spike than 100 ml) due to oigh activity



Page 10 of 18





101 The gas flow proportional counter must be calibrated in order to measure the absolute efficiency of each detector (in cpmdpm) The transmission factor (TF) must also be measured over the density range of the procedure See SOP STL-RD-0404

110 PROCEDURE




114 Confirm that sample is acidic pH less than 2 using pH paper If not acidic add 2ml 16N HN03 per liter of sample and mix thoroughly Notify laboratory supervisor and initiate a Nonconformance

115 Ensure that sample container is capped tightly and shake it thoroughly Transfer an aliquot of the sample (typically 1 liter) to an appropriate size beaker Label beaker with sample ID number and volume Record all data on sample worksheet



Page 11 of 18

116 NOTE The sample volume may vary according to the contract required detection limits Review the Quality Assurance Summary for additional information

117 Add 1M citric acid in ratio of 5 ml per liter Add methyl orange indicator until the persistence of a red color Mix thoroughly

118 Add 10 ml lead carrier (15 mgml) 2ml strontium carrier (10 mgml) 10 ml barium (Standardized) carrier (16 mgml) and 1 ml yttrium carrier (18 mgml) stir well Heat to incipient boiling and maintain at this temperature for about 30 minutes

119 Add 15N ammonium hydroxide until a definite yellow color is obtained then add a few drops excess Precipitate lead and barium sulfates by adding 18N sulfuric acid until the red color reappears then add 025 ml excess Add 5 ml ammonium sulfate (200 mgml) for each liter of sample Stir frequently and keep at a temperature of approximately 90degC for 30 minutes

1110 Cool sample for at least 30 minutes Allow precipitate to settle to the bottom of the beaker for a least 6 hours Decant the supernatant and discard taking care to avoid disturbing the precipitate

1111 Quantitatively transfer precipitate to a 50 ml centrifuge tube taking care to rinse last particles out of beaker with a strong jet of deionized water Centrifuge and discard supernatant

1112 Wash the precipitate with 1 Oml 16N HNOs centrifuge and discard supemate

1113 Repeat Step 1111 onetime

1114 Wash the precipitate with 1 Oml DIHaO centrifuge and discard supemate

1115 Add 20 ml basic EDTA reagent heat in a hot water bath (approximately 80degC) and stir until precipitate dissolves

1116 Add 1 ml strontium-yttrium mixed carrier and stir thoroughly Add a few drops ION NaOH if any precipitate forms

1117 Add 2ml ammonium sulfate (200mgml) and stir thoroughly Add 174N acetic acid until barium sulfate precipitates then add 2 ml excess Digest in a hot water bath until precipitate settles Centrifuge and discard supernatant



Page 12 of 18

1118 Add 20 ml basic EDTA reagent heat in a hot water bath and stir until precipitate dissolves Repeat steps 1114 through 1116 Note the time of last barium sulfate precipitation This is the beginning of the 228Ac ingrowth time Record the date and time on the sample worksheet

1119 Dissolve the precipitate in 20 ml basic EDTA reagent as before then add 20 ml standardized yttrium carrier (9 mgml) and 1 ml lead carrier (15 mgml) If any precipitate forms dissolve it by adding a few drops of ION NaOH Cap the tube and allow it to age at least 36 hours

11191 NOTE While it is desirable for each sample to age 36 hours prior to continuing less time is acceptable The equations given in this procedure allow for the calculation of an ingrowth factor for any time between 4 and 44 hours

1120 Add 03 ml ammonium sulfide and stir well Add ION sodium hydroxide drop-wise with vigorous stirring until lead sulfide precipitates then 10 drops excess Stir intermittently for about 10 minutes Centrifuge and decant supernatant into a clean tube

1121 Add 1 ml lead carrier (15 mgml) 01 ml ammonium sulfide and a few drops ION sodium hydroxide Repeat precipitation of lead sulfide as before Centrifuge and filter supernatant through 045 mm syringe filter into a clean tube Wash filter with approximately 5ml water Discard residue

1122 Check availability of gas proportional counter

1123 Once yttrium hydroxide is precipitated the analysis must be carried to completion to avoid excessive decay of228Ac

1124 Ensure that the hot water bath is at the desired temperature 70-85degC

1125 Add 7 ml 18N sodium hydroxide stir well and digest in a hot water bath until yttrium hydroxide coagulates usually about 5 minutes Centrifuge and decant supernatant into a clean labeled 50 ml centrifuge tube Save for barium yield determination Step 1128

1126 Note time of yttrium hydroxide precipitation this is the end of the 228Ac ingrowth time and beginning of 228Ac decay time Record time on the sample data sheet (End of Ingrowth)



Page 13 of 18

1127 Dissolve the precipitate in 2ml 6N nitric acid Heat and stir in a hot water bath about 5 minutes Add 5ml water and precipitate yttrium hydroxide with 3 ml ION sodium hydroxide Heat and stir in a hot water bath until precipitate coagulates Centrifuge and discard supemate

1128 Dissolve precipitate with 1 ml IN nitric acid and heat in a hot water bath a few minutes Dilute to 5ml with DI water and add 2ml 5 ammonium oxalate Heat to coagulate centrifuge and discard supemate

1129 Add 10ml water 6 drops IN nitric acid and 6 drops 5 ammonium oxalate Heat and stir in a hot water bath a few minutes Centrifuge and discard supemate


1131 To the supernatant from Step 1123 add 4 ml 16N nitric acid and 2ml ammonium sulfate (200mgml) stirring well after each addition Add 174N acetic acid until barium sulfate precipitates then add 2ml excess Digest in a hot water bath until precipitate settles Centrifuge and discard supemate

1132 Add 20ml basic EDTA reagent heat in a hot water bath and stir until precipitate dissolves Add a few drops ION NaOH if precipitates does not readily dissolve

1133 Add 1 ml ammonium sulfate (200 mgml) and stir thoroughly Add 174N acetic acid until barium sulfate precipitates then add 2 ml excess

11331 NOTE If 226Ra is requested record date and time of BaS04 on 226Ra data sheet

1134 Digest in a hot water bath until precipitate settles Centrifuge and discard supemate

1135 Wash precipitate with 10ml water Centrifuge and discard supemate


1137 Dry on a hot plate on medium heat Cool planchets in a dessicator Weigh the planchet

1138 Heat the planchet again using the hot plate Weigh the planchet a second time to confirm that the weight of the planchet has not changed (plusmn 5)



Page 14 of 18

1139 Repeat steps 1131 and 1132 until the weight of the planchet is constant

1140 Record the final weight of the planchet to determine the chemical recovery for the barium carrier solution

1141 Submit the planchets to the counting room for total beta radiation


121 Calculate the results using the equations given below for Activity Error and Minimum Detectable Activity (MDA)

yyo

Ra Activity (pCiunit volume or mass) =

222xVxYxExei l-e^ 1-e

228Ra Error (pCiunit volume or mass) (95 confidence) =

t tb

222xVxYxExe-xfb 1-e1 1

Ra-228 MDA (pCiunit volume or mass)

where

Rs = sample count rate cpm tj = sample count time minutes Rb = background count rate cpm tb = background count time minutes E = counter efficiency for 228Ac cpmdpm Y = fractional chemical yield of yttrium carrier multiplied by fractional chemical

yield of barium carrier Ba chemical yield =



Page 15 of 18

net weight of BaSO4 (mg) weight of BaSO4 added (mg)

Y chemical yield =

net weight ofYoxalate (mg) weight ofYoxalate added (mg)

where

222 = conversion dprnpci 1 = decay constant for 228Ac 0001 884 minutes1

t j = the time interval (in minutes) between the first yttrium hydroxide precipitation in Step 1 1 20 and the start of the counting time

t2 = the time interval of counting in minutes ta = the ingrowth time of

77S Ac in minutes measured from the last barium sulfate

precipitation in Step 1 115 to the first yttrium hydroxide precipitation in Step 1120

V = aliquot size in appropriate units of volume or mass

122 Using data entered on sample worksheet perform calculations in the following order

Determine the critical count rate (CCR) using the following equation

CCR = b + Rb

123 Calculate the MDA for samples when any one of the following conditions are met

o Rs is less than Rb o Rs is less than the critical level the calculated activity is less than the error value

This will occur when Rs is greater than Rb and it indicates interference such that an accurate determination is not possible under these conditions




Page 16 of 18

RPD - x100 Original + Duplicate 2

Report the RPD values on the Sample Worksheet Section 9 specifies the acceptance criteria for duplicates


bdquo observed value n recovery =-x 100 expected value

Report the recovery values for both barium and yttrium on the Sample Worksheet Section 9 specifies the acceptance criteria for chemical recovery

126 Calculate the blank samples as MDA It is normal for DI blanks to have count rates greater than Rb but the calculated activity value must be less than the target detection limit









Page 17 of 18



160 REFERENCES

161 Radium 228 in Drinking Water Method 9040 Prescribed Procedures for Measurement of Radioactivity in Drinking Water Section 8 EPA 6004-30-032 (1980)

162 Percival D R and Martin D B Sequential Determination of Radium-226 Radium-228 Actinium-227 and Thorium Isotopes in Environmental and Process Waste Samples Analytical Chemistry 46-1742-2749 (1974)

163 US Nuclear Regulatory Commission Retaliatory Guide 415 Quality Assurance for Radiological Monitoring Programs (Normal Operations) - Effluent Streams and the Environment


165 STL Quality Assurance Manual current revision

166 Associated SOPs




1664 STL St Louis Laboratory Personnel Training and Evaluation STL-QA-0013 Quality Control Procedures




Page 18 of 18






170 MISCELLANEOUS


1711 All counting data and hard copies of summary sheets must be maintained in the project file These must be kept in reasonable order such that timely retrieval is possible

SOP NoRevision No

Revision Date-Page

Implementation Dateshy

STL-RC-0110 1

103000 1_ of 19

042401


SERVICES

STL St Louis

13715 Rider Trail North OPERATION-SPECIFIC STANDARD OPERATING PROCEDURE City MO 63045

Tel 3142988566

Fax 314 298 8757

www stl me com TITLE

Analysis of Total Uranium by Laser-induced Phosphorimetry


Prepared by

Approved by

Approved by

Approved by

Approved by

Technial Specialist

DualityAssurance Manager


Laboratory Director


This document has been prepared by Severn Trent Laboratories (STL) solely for STLs own use and the use of STLs customers in evaluating its qualifications and capabilities in connection with a particular project The user of this document agrees by its acceptance to return it to STL upon request and not to reproduce copy lend or otherwise disclose its contents directly or indirectly and not to use it for any other purpose other than that for which it was specifically provided The user also agrees that where consultants or other outside parties are involved m the evaluation process access to these documents shall not be given to said parties unless those parties specifically agree to these conditions

THIS DOCUMENT CONTAINS VALUABLE CONFIDENTIAL AND PROPRIETARY INFORMATION DISCLOSURE USE OR REPRODUCTION OF THESE MATERIAL^ WITHOUT THE WRITTEN AUTHORIZATION OF SEVERN TRENT LABORATORIES IS STRICTLY PROHIBITED ~THTS UNPUBLISHED WORK BY STL IS PROTECTED BY STATE AND FEDERAL LAW OF THE UNITED STATES IF PUBLICATION OF THIS WORK SHOULD OCCUR THE FOLLOWING NOTICE SHALL APPLY

SCOPVRIGHT 2000 SEVERN TRENT LABORATORIES INC LL RIGHTS RESERVED STL St LCUIS is a part or Severn Trent Laboratories Inc




SUMMARY OF METHOD

11 This SOP provides detailed instructions for the preparation of liquid samples for determination of total uranium in water by laser induced phosphorimetry

12 A water sample preserved with nitric acid to a pH of lt 2 is thoroughly shaken to suspend any particulates A 5 ml aliquot is wet ashed in a leached 20 ml scintillation vial to remove any organics present The wet ashed sample is diluted to 50 ml with 08N nitric acid

13 A 10 ml sample aliquot is put into a glass 50 ml cuvette and 15 ml of Uraplex is added to the sample and mixed The sample is then ready for analysis by the Kinetic Phosphorescence Analyzer (KPA)



22 This SOP provides instructions for the calibration of the Kinetic Phosphorescence Analyzer (KPA) and the analysis of liquid samples

23 This SOP is suitable for measurement of uranium concentrations above 10 ngml (Minimum Detectable Activity) Detection limits may be improved by using a quartz cuvette

24 Method detection limits are maintained in the Information Management System (STLIMS) Because of their dynamic nature they are not specifically listed in this document but can be retrieved at any time using TraQAr tools

25 Responsibilities


252 It is the responsibility of the Radiochemistry Group Leader or designate to review data prior to release from the lab

26 Quality control limits (accuracy and precision for spikes) are also maintained in STLIMS and are also dynamic Therefore they are not specifically listed in this document but can be retrieved at any time using TraQAr tools

DEFINITIONS


3




32 Minimum Detectable Activity (MDA) - The smallest amount of activity that can be detected given the conditions of a specific sample It is reported at the 95 confidence interval meaning that there is a 5 chance that a false signal was reported as activity and a 5 chance that true activity went undetected The MDA for this procedure (1 ngml) was determined by analyzing a series of standards near this activity

INTERFERENCES

41 Method interferences may be caused by organics chlorides and reducing metals if samples were not properly wet ashed After the sample is wet ashed and diluted to 50 ml with 08N nitric acid caution should be taken not to pipette any solids from the bottom of vial when taking aliquot for analysis

42 Care should be taken not to touch cuvettes optical surfaces Finger oils will increase sample background

43 Quartz cuvettes if used must be scrupulously cleaned with lint-free wipes between analyses as the cell faces are optical elements and could result in high background To clean cuvettes use the following steps

431 Empty sample from cuvette

432 Rinse cell with 08M nitric acid Aspirate rinse acid Repeat

433 Rinse cell with deionized water Aspirate rinse water Repeat twice Methyl alcohol may be used as a supplemental cleaner for the cell if necessary When methyl alcohol is used to clean the cell thorough rinsing with reagent water is necessary to remove all traces of alcohol before the cell is used

434 Dry outside of cuvette with a clean lint free tissue

SAFETY






53 Consult the Health and Safety Policies and Procedures Manual for information on Personal Protective Equipment Eye protection that satisfies ANSI Z871 (as per the Chemical Hygiene Plan) laboratory coat and appropriate gloves must be worn while samples standards solvents and reagents are being handled Disposable gloves that have become contaminated will be removed and discarded other gloves will be cleaned immediately VTTON gloves may be worn when halogenated solvents are used for extractions or sample preparation Nitrile gloves may be used when other solvents are handled [Note VTTON is readily degraded by acetone all solvents will readily pass through disposable latex rubber gloves]


541 The following materials are known to be corrosive nitric acid sulfuric acid

542 Hydrogen peroxide and nitric acidare known to be oxidizers

543 Chemicals known to be flammable are methyl alcohol






611 Kinetic Phosphorescence Analyzer (Chemchek KPAWin Software V 127)

612 Volumetric Pipettes

613 Volumetric Flasks




614 Quartz cuvettes (50 ml) for low detection limits below 10 ngml

615 Glass cuvettes (50 ml)

616 Pipetter 0 -10 ml capability

617 Eppendorf pipetters 1000 jil 500 ul 100 (il 50 jil 50 ml

REAGENTS

71 Reagents


712 Deionized Water Type H as described in ASTM Part 311193-74 obtained from the Milli-Q unit

713 Uraplex proprietary complexing agent for uranium (Chemchek Instrument Inc) or equivalent Refrigerate Uraplex when not in use Dilute with reagent water and use diluted Uraplex within one month of dilution

714 Hydrogen Peroxide (H2O2) 30

715 Nitric acid concentrated (HNO3) 16M

716 Uranium Standards At least two separtate manufacturers or lots of standards are required One set of standards at a miniumum must be traceable to EPA or NIST standards or otherwise certified by the manufacturer The primary standards have an expiration date defined by the manufacturer Intermediate solutions prepared from the stock will be disposed of after 6 months or upon expiration of the primary whichever comes first Working standards prepared from the Intermediate will expire in 90 days from preparation or upon the expiration of the parent whichever comes first

717 Ottawa sand may be used for Method Blank and LCS for soil samples


721 Reagents are prepared from reagent grade chemicals unless otherwise specified

722 Deionized water is used throughout Deionized water is monitored for interfering impurities by analyzing blank reagent water




723 Replace lab prepared reagents annually unless otherwise specified below As a minimum label all reagents with chemical name concentration date prepared preparers initials and expiration date if less than one year from preparation

724 08N Nitric acid (HNO3) Add 5 ml of concentrated nitric acid to 50 ml of reagent water and dilute to 100 ml with reagent water Mix well

725 Uranium standards are prepared in acid leached volumetric flasks (use procedure in section 68) to prevent contamination from natural uranium in glass Standards are prepared for low range and high range calibration curves in 08M nitric acid

726 Low range standards are prepared with a concentration range of 10 ngmlshy100 ngml High range standards are prepared with a concentration range of 100 ngml - 2000 ngml

727 The 2000 ngml standard described in section 728 is also used as the LCS solution of which 10 ml is pipetted into 4 ml of deionized water

73 Standards


732 Reference Standard A solution of uranium in URAPLEX containing 10 mL of 100 ngmL of uranium in a filled cell The reference standard should give 20-70 counts per pulse Prepare Reference Standards daily

SAMPLE COLLECTION PRESERVATIVES AND STORAGE

81 Preserve water samples by adding 2 ml concentrated nitric acid per liter at the time of sample collection and refrigerate at 4deg plusmn 2degC



84 The maximum holding time for all samples is 6 months from date of collection

QUALITY CONTROL

91 QC requirements

911 A verification standard shall be run immediately following calibration and at least once per shift thereafter Acceptable limits for the verification standard are 90shy




110 of true value If the results for a verification standard are outside these limits the analysis must be stopped a new calibration must be performed and all samples run after the last valid verification standard must by reanalyzed

912 All standard analyses must comply with the criteria outlined in section 8 before analyses can be performed

913 Measure and record a method blank and two laboratory control sample with every analytical batch of 20 samples or less

914 The activity in the method blank must be less than the contractual Minimum Detectable Activity (MDA)

915 The acceptable limit for the recovery of the spike in the LCS is determined by laboratory generated control tables which will give upper and lower limits of acceptability

916 A duplicate sample is analyzed every 20 samples or less Calculate the Relative Percent Difference (RPD) for all duplicate analyses The acceptable limit for the RPD is 20

917 Matrix spikematrix spike duplicates will be analyzed on a project-specific basis The suggested limits for the MSMSD are those determined for the LCS by control tables

918 Samples associated with method blanks or laboratory control samples which fail the criteria of section 12 must be prepared and re-analyzed with an acceptable blank and LCS For projects requiring matrix spike and or matrix spike duplicate analysis data will be reported with appropriate flags when the results fall outside the suggested control limits No reanalysis will be performed for out-of-control matrix spike or matrix spike duplicates unless specifically requested by a project manager


9191 Samples that have assigned QC limits different than the standard limits contained in STLIMS QC code 01 (unless permitted by QA) must be batched separately but can share the same QC samples


9193 A method blank must be included with each batch of samples The matrix for aqueous analyses is organic-free water





9195 All LCS and MSMSD and results - whether they pass criteria or not mdash are uploaded into the STLEMS system for maintenance and periodic update of limits



92 Documentation









9236 The Method Blank ICB and CCV concentrations must always be less than the method or contract required detection limit



10








96 QC Program



101 Prepare a reference cell by adding 10 ml of 100-300 ngml natural uranium and 15 ml of Uraplex to the reference cuvette Cap mix well and wipe the outside of the reference cuvette with a lint-free tissue Place the reference cell in the reference cell holder on the KPA10

102 Prepare a background sample by combining 10 ml of 08N nitric acid and 15 ml of Uraplex in a cuvette Cap mix well and wipe the outside of the reference cuvette with a lint-free tissue Load cell for analytical measurement

103 Instrument Calibration

1031 Place BKGD curverte into holder on KPA machine 10311 Click + icon (Add new sample) 10312 Enter BKGD into sample ED 10313 Selct BKGDnd from sample type 10314 Highlight analysis number at left edge of screen 10315 Click analyze 10316 Click analyze from submenu 10317 Click yes in dialogue box 10318 Click ok in dialogue box

1032 KPA will automatically start and process BKGD in the high and low range 1033 When KPA is finished remove curvette empty and clean




1034 Make a 10 mgml calibration standard using 10 ml of 10 ngml calibration standard mixed with 15 ml wraplex in the curvette

1035 Place calibration standard in holder on KPA machine 10351 Click + icon 10352 Enter CAL1 into sample ID 10353 Selct CalStd from sample type 10354 Enter appropriate reagent number into Standard ED 10355 Enter 1 into Standard Concentration (ugL)

1036 Highlight Analysis No at left edge of screen 10361 Click analyze 10362 Click analyze from submenu 10363 Click yes in dialogue box 10364 Click ok in dialogue box

1037 KPA will automatically start 1038 If calibration is acceptable (see 104) repeat steps 1035 through 1037 using

50 ngml 100 ngml 500 ngml 1000 ngml 1500 ngml and 2000 ngml 1039 When all calibration standards are processed click book icon display

calibration 10310 The calibration grid is displayed

103101 All discrepancies must be less than+bull-100 If not re-run calibration

103102 Click plot 103103 Click print 103104 Click exit

10311 Calibration is finished 10312 A copy of the plot and grid must accompany every batch

104 Acceptable calibrations will have the following characteristics

1041 The lifetime for each measurement must be between 100 and 340 ms

1042 R2 for each measurement must be gt096 for 10 mgml and 099 for the others

1043 The correlation coefficient for the curves must be gt 099





11





PROCEDURE

111 AnalysisPreparation of Liquid Sample for Uranium Analysis

1111 Thoroughly shake the sample to suspend any particulates and pipet 50 ml into a liquid scintillation vial If preparing a spiked sample pipet 40 ml of deionized water (for a LCS) or 40 ml of sample (for a MS or MSD) into a scintillation vial and spike with the solution described in section 729

1112 Set on hot plate until dry

1113 Add 3 ml of 16N nitric acid and place on a hot plate at medium heat Add 05 ml of hydrogen peroxide (30) dropwise about 9 drops and wet ash to dryness Abserving reaction after each drop Allow samples to dry on hot plate

NOTE If sample residue does not appear white or translucent place the scintillation vial with sample residue in a muffle furnace and heat the sample forlhrat500plusmn25degC

1114 Dissolve residue in 50 ml of 08N nitric acid cap and mix

1115 Add 10 ml of sample to a sample cuvette and add 15 ml of Uraplex solution cap and mix Wipe the outside of the cuvette with a lint-free tissue Place the cuvette in the instrument for analysis

1116 In analyze mode select Fl and use the following instructions

11161 Enter Sample ID

11162 Enter Sample Description

11163 Select Concentration Range (HL)

11164Enter Final Volume after treating Aliquot

11165 Enter Sample Aliquot Volume

11166Check that sample cuvette is placed squarely into sample holder

11167Press enter to start analysis

NOTE Volume units must be the same




11168Print Report (F2)

11169Select Fl and repeat steps 1115 through 11167 to analyze additional samples

111610 Check sample printouts for lifetime and R2 criteria of acceptability (1051 and 1052) Samples that do not meet the criteria will be reanalyzed with the LCS to verify that it is out Samples will be reprepared and reanalyzed if the criteria is still not met Dilution of the sample may be required to achieve an acceptable analysis

111611 Record results on the sample data sheet (Figure 1)

111612 If the sample appearance or initial results indicate that a dilution is necessary a smaller amount of sample may be used and an appropriate amount of 08M nitric acid added to bring the volume to 10 ml


121 The KPA instrument calculates the uranium concentration giving the results in units of nanograms uranium per milliliter in the analyzed sample These results can also be reported in units of activity (picocuries per liter) assuming that U238 constitutes the majority of the mass in the sample The following formula is used for the conversion

Activity (ngml Uranium) (337 x W4 pCing) (1000 mlL) (pCiL)

The error associated with the concentration (122) must be multiplied by the same factor

122 Total Uranium Measurement Uncertainty (TUMU) in ngml at 95 confidence level

Where

E AC SUS

196

instrument calculated error (ngml) instrument calculated concentration (ngml) Assumed to be 005 is the sum of the relative fractional procedural and other laboratory uncertainties two sigma error constant

123 Spike Recovery (LCS)




Recovery = ng found bull 100 ng added

Where

ng found = ng of uranium determined from analysis ng added = ng of uranium added to LCS

124 Spike Recovery (MS or MSD)

Recovery = ng found - ng sample bull 100 ng added

Where

ng found = ng of uranium determined from analysis ng sample = ng of uranium in original sample ng added = ng of uranium added to MS or MSD

125 Relative Percent Difference (RPD)

RPD = 2 sample1 - sample2 Vi bull 100 (sample + sample 2)2

Where

sample 1 = ng of uranium in the MS or duplicate sample 1 sample 2 = ng of uranium in the MSD or duplicate sample 2

126 The Minimum Detectable Activity (MDA) is calculated by the KPA instrument when analyzing the blank sample prepared in the laboratory




1314 Method Blank



i









141 Method Blank


1414 llf the analyte found in the method blank is confirmed to not be present in any of the associated samples at any level the contamination did not affect those samples This represents a non-impact situation and no specific corrective action is taken A nonconformance memo is written to notify project management of the situation for evaluation against project requirements

1415 If the analyte found in the method blank is confirmed to be present in one or more of the associated samples the concentrations are compared

1415 llf the analyte concentration in the method blank exceeded 10 of concentration found in one or more samples the prescribed corrective action is to re-analyze all affected samples

14152If the concentration in the method blank was less than 10 of the concentration found in one or more samples the sample can be reported by qualifying the affected analytes A nonconformance memo is written to notify project management of the situation for evaluation against project requirements











14251 If there are no positive results in one or more samples a non-impact situation ensues for those samples A nonconformance memo is written to notify project management of the situation for evaluation against project requirements

143 If there are positive results for one or more analytes the likelihood of poor reproducibility increases and corrective action must be evaluated A nonconformance memo is written to notify project management of the situation for a project decision on whether the affected sample(s) should be reanalyzed


151 Method Blank


15141 If the analyte found in the method blank is confirmed to not be present in any of the associated samples at any level the contamination did not affect those samples This represents a non-impact situation and no specific corrective action is taken A nonconformance memo is written

SOP NoRevision No

Revision DatePage

Implementation Date

STL-RC-0110 1

103000 16 of 19 042401

to notify project management of the situation for evaluation against project requirements






16141 If the recovery is biased high and the associated samples have no positive results for that analyte a non-impact situation ensues A nonconformance memo is written to notify project management of the situation for evaluation against project requirements











171 Method blanks


172 LCS







1814 The groupteam leader has the responsibility to ensure that this procedure is performed by an analyst who has been properly trained in its use and has the required experience see SOP CORP-QA-0013 The groupteam leader must document the training and PELCS sample performance and submit the results to the QA Manager for inclusion in associated training files







183 Associated SOPs

1834 STL-QA-0002 Standards Preparation

1835 STL-QA-0006 Sample Receipt and Chain-of-Custody

1836 STL-QA-0026 Nonconformance and Corrective Action

1837 STL-QA-0013 Personnel Training and Evaluation

1838 STL-QA-0004 Automatic Piperter Calibration



20 WASTE MANAGEMENT


202 General descriptions of radioactive waste streams are aqueous radioactive acidic aqueous radioactive basic radioactive solventsorganics and dry active waste The used columns are considered dry active waste

21 REFERENCES



213 Quanterra St Louis Laboratory Quality Assurance Manual Laboratory Specific Attachment current revision




214 American Society for Testing and Materials Volume 1101 Method D5174 Standard Test Method for Trace Uranium in Water by Pulsed-Laser Phosphorimetry



221 A Correlation coefficient stop analysis and rerun the standard curve





2219 Method Blank ICB CCB re-prep and reanalyze all samples associated with the unacceptable method blank For an unacceptable ICB investigate instrument contamination and reanalyze the samples For an unacceptable CCB investigate instrument contamination and reanalyze all samples analyzed after the last acceptable CCB

222 Records Management

2224 All raw data data summary sheets copies of standard logs quality control charts and extraction sheets are turned over to the Document Control Coordinator after they have been reviewed and approved

SOP No STL-RD-0201 Re vision No



1 042401

of 16 T R E N T

UNCONTROLLED COshyControlled Copy No p

SERVICES

STL St Louis

13715 Rider Trail North OPERATION-SPECIFIC STANDARD OPERATING PROCEDURE Clty M0 63045

Tel 3142988566 TITLE Fax 314 298 8757

wwwstl-inccom Daily Operations of an Alpha Spectroscopy System

(Supersedes SL 13013)

Prepared by


Approved by

J Quality Assurance Manager

Approved by Environmental HeaKn and Safety Coordinator



This document has been prepared by Severn Trent Laboratories (STL) solely for STLs own use and the ust of STLs customers in evaluating its qualifications and capabilities in connection with a particular project The user of this document agrees by its acceptance to return it to STL upon request and not to reproduce copy lend or otherwise disclose its contents directly or indirectly and not to use it for any other purpose other than that for which it was specifically provided The user also agrees that where consultants or other outside panics are involved in the evaluation process access to these documents shall not be given to said panics unless those parties specifically agree to these conditions

THIS DOCUMENT CONTAINS VALUABLE CONFIDENTIAL AND PROPRIETARY INFORMATION DISCLOSURE USE OR REPRODUCTION OF THESE MATERIALS WITHOUT THE WRITTEN AUTHORIZATION OF SEVERN TRENT LABORATORIES is STRICTLY PROHIBITED -THS UNPUBLISHED WORK BY STL is PROTECTED BY STATE AND FEDERAL LAW OF THE UNITED STATES IF PUBLICATION OF THIS WORK SHOULD OCCUR THE FOLLOWING NOTICE SHALL APPLY

^COPYRIGHT 2000 SEVERN TRENT LABORATORIES INC ALL RIGHTS RESERVED

STL St Louis s a part or Severn Trent LaDoratories nc

SOP No STL-RD-0201 Revision No 2



SUMMARY OF METHOD

11 This SOP provides detailed instructions for energy calibration efficiency determination quality control checks background and sample counting of the alpha spectroscopy system


21 This procedure applies to all alpha spectroscopy detectors and the computer assisted alpha spectroscopy analysis system

22 Responsibilities

221 Counting Lab Supervisor to confirm that this procedure is followed whenever the energy calibration or efficiency determination of the germanium spectroscopy system is performed



DEFINITIONS


INTERFERENCES

41 Alpha spectrometry has many potential interferences These are usually in the form of radionuclides with unresolved alpha emissions Poorly resolved alpha peaks are often due to high alpha activity rates or attenuation of the alpha emissions




SAFETY

51 Normal office dependent safety precautions must be taken in performing this SOP If personnel are required to perform any portion of the procedure in laboratory areas appropriate personal protective equipment and precautions must be utilized


521 Eye protection that satisfies ANSI Z871 (as per the Chemical Hygiene Plan) laboratory coat and appropriate gloves must be worn while samples standards solvents and reagents are being handled Disposable gloves that have been contaminated will be removed and discarded other gloves will be cleaned immediately


5221 The electronic instrumentation present a high voltage hazard Up to plusmn50 volts are applied to each alpha detector The analyst must be aware of high voltage hazards before performing any work that would require manipulating the electronic components of the alpha detector system









611 Alpha specrroscopy system utilizing a computer based data acquisition system


71 Reagents

711 All reagent preparation is documented in the reagent logbook All reagents are labeled with their unique ED name (and concentration if applicable) of the reagent the date prepared and the expiration date


713 Commercially prepared alpha standards with all appropriate NIST Source Certificate information

72 Standards


722 Calibration Standards


81 None

9 QUALITY CONTROL

91 Calibration and Quality Control Counting Schedule

911 Initial and continuing calibrations are to performed according to the following schedule

9111 Energy calibrations shall be established for the alpha spectroscopy systems monthly or when the calibration quality control check indicates an unacceptable change in the energy calibration parameters

SOP No STL-RD-02Q1 Revision No 2



9112 Efficiency calibrations shall be established for the alpha spectroscopy systems monthly or when the calibration quality control check indicates an unacceptable change in the efficiency calibration parameters

9113 Background subtraction spectrum shall be established for the alpha spectroscopy systems monthly or when the background quality control check indicates an unacceptable change in the daily background parameters

912 Routine pulser quality control verifications are to performed according to the following schedule

9121 The pulser energy peak centroid peak resolution peak area quality control for a detector shall be checked each day that the alpha spectroscopy system is used

92 Acceptance Criteria

921 Routine calibration background and pulser quality control parameters using the Boundary out-of-range test will be found unacceptable if the value is outside reasonable parameter tolerance

9211 The routine quality control check should be rerun to determine the statistical significance of the errant parameter

9212 If the errant parameter is found acceptable for the rerun the investigation will be noted in the instrument calibration and maintenance log

9213 Check the expiration date of the radioactive standard to confirm the material is current

9214 Check source positioning and all instrument settings

9215 Check all cables for any apparent damage and to confirm that all cables are routed to proper connectors and are in good working order

9216 If the errant parameter continues to fail for the rerun than go to section 93 of this procedure

93 If the instrument fails to meet the acceptance criteria outlined in section 92 and the corrective actions above do not resolve the problem the instrument must be declared Out of Service The detectorinstrument must be red-tagged IAW SOP CORP-QA-0010 Note this action in the instrument calibration and maintenance log and notify the Radiochemistry Laboratory Manager or designee of the status

10

SOP No STL-RP-0201 Revision No 2



931 The instrument may be returned to service once the malfunction has been corrected and the above acceptance criteria have been met Note this action in the instrument calibration and maintenance log


101 Alpha Detector System Energy and Efficiency Calibration

1011 Select Counting from the main menu

1012 Select Primary Calibration Check from the next menu

1013 Identify the alpha detector bank(s) to be calibrated

1014 Place the calibration standard(s) in the selected alpha detector chambers) establish vacuum turn on bias and start acquisition for the pre-set time (typically 6 hrs)

1015 Following acquisition of the spectrum select Create NAMESDAT from the Main Menu

10151 Enter the Banks to be processed

10152 Enter Prime for the Type of Configurations to be processed

10153 Press the PF1 key to continue

1016 Select Process configurations in NAMESDAT from the Main Menu

10161 The user will be prompted to interactively process the calibration spectrum The user may choose Yes or No

10162 The calibration spectrum will be processed by the software A QA report listing acceptable or not acceptable parameters will be printed automatically

1017 Note this action in the instrument calibration and maintenance log

102 Detector Background Counting


1022 Select Backgrounds from the next menu

11




1023 Identify the alpha detector bank(s) for background to be counted

1024 Remove any sample or calibration standard in the selected alpha detector chamber(s) place a claen stainless steel disc in the chamber establish vacuum turn on bias and start acquisition for the pre-set time (typically 1000 minutes)



10252 Enter Back for the Type of Configurations to be processed



10261 The background spectrum will be processed by the software AQA report listing acceptable or not acceptable parameters will be printed automatically


PROCEDURE

111 One time procedural variations are allowed only if deemed necessary in the professional judgment of supervision or the Quality Control Manager to accommodate variation in sample matrix radioactivity chemistry sample size or other parameters Any unauthorized deviations from this procedure must be documented as a nonconformance with a cause and a corrective action described If contractually required the client shall be notified The Nonconformance Memo shall be filed in the project file

112 Pulser Quality Control


1122 Select Pulser Check from the next menu


1124 Establish vacuum turn on pulser and start acquisition for the pre-set time (typically 2 minutes)






11252 Enter D for the Type of Configurations to be processed



11261 The pulser calibration spectrum will be processed by the software A QA report listing acceptable or not acceptable parameters will be printed automatically


113 Sample Counting


1132 Select Samples from the next menu

1133 Identify the alpha detector banks to be calibrated

11331 Enter the Batch to be counted

11332 Enter the Actinide to be counted


1134 Place the sample(s) in the selected alpha detector chamber(s) establish vacuum turn on bias and start acquisition for the pre-set time (typically 200 or 1000 minutes)

1135 The user will be prompted to enter information for the batch of samples as well as for the individual samples in the selected alpha detector chambers

1136 Note this action in the instrument run log

1137 Samples with a count rate of greater than 1 cps should be removed from the alpha counting system to prevent contamination of detector(s)

11371 Alpha detectors exposed to samples with count rates greater than 1 cps should be tagged out-of-survice until a background count can be performed per Section 102 of this SOP

12





11381 Enter SA for the Type of Configurations to be processed

11382 Enter the Batch to be processed

11383 Enter the Actinide to be processed






121 Data analysis is performed by AMS (Alpha Management System) a Canberra Industries product See Reference Section for the Canberra manuals that validate and verify the equations used The following data must be entered into this program or the default value verified

1211 Sample Identification Number

1212 Sample Date

1213 Sample aliquot used

1214 Tracer Identification Number

1215 Tracer volume used

1216 Spike value added (for LCS)

1217 MDA constant (466)

1218 Curries constant (271)

1219 Isotope of interest (library and regions)




12110 Matrix (water soil liquid solid)

122 Alpha Activity Concentration for each region of interest (ROI) in pCiunit volume

(CS-CB)A rT = imdash2 ^-L

222EAbYDVst s )

Where

ACTS = Activity of the sample Cs = Sample Counts CB = Background counts E = Detector efficiency Ab = Abundance of the alpha emission Y = Yield D = Decay tj = Count time for analysis VA = Sample aliquot volume

123 Alpha Uncertainty of Concentration (at 2s confidence level)

The 2-sigma (s) Total Propagated Uncertainty (TPU) term for each region of interest (pCiunit volume) is calculated by the computer software The software calculates the stochastic counting uncertainty and software reviews the nuclide library for the error in the nuclide half-life and abundance The software also reviews the standard certificate file to review the calibration standard uncertainty A 5 factor is added in quadrature (the square root of the sum of the squares) due to the error in the sample volume the chemical yield and geometry reproducibility

TPUs-(196) |ACTslVuc+U2E+U^b+U^ 2+U^+Uv

Where

Uc = Stochastic counting uncertainty

UE = Uncertainty in efficiency

UAb = Uncertainty in abundance

^11 2 = Uncertainty in half-life

UY = Uncertainty in yield

Uy = Uncertainty in volume -7

= Uncertainty in prep

13




124 Following is the alpha spectroscopy Minimum Detectable Concentration (MDC)

MDC = mdash V R B s + 271 222 E Ab Y D VA ts

Where

MDC = Minimum Detectable ActivityConcentration of the sample RB = Count rate of detector background (in cpm) E = Detector efficiency Ab = Abundance of the alpha emission Y = Yield D = Decay tj = Count time for analysis VA = Sample aliquot volume

125 Tracer Yield Recovery

Y _ (CT-CB) 14 3)c A K -f

Where

Y = Chemical Yield CT = Tracer Counts CB = Tracer ROI background counts AT = Tracer dpm ts = Count time for analysis E = Detector efficiency

DATA ASSESSMENT AND ACCEPTANCE CRITERIA

131 The following represent data assessment for samples and acceptance criteria for QC measures


1321 Method Blank


14








13232 No specific corrective actions are required in the evaluation of the MSMSD results provided that the batch LCS is in control Analysts should use sound judgment in accepting MSMSD results that are not within control limits especially if the LCS results are borderline

CORRECTIVE ACTIONS FOR OUT OF CONTROL DATA

141 Method Blank












14212 If the recovery is biased low and the associated samples have positive results for that analyte a minimal impact situation ensues A nonconformance memo is written to notify project management of the situation for evaluation against project requirements

14213 If the recovery is biased high and the associated samples have positive results for that analyte the prescribed corrective action is reanalysis of the affected sample(s)

14214 If the recovery is biased low and the samples have no positive results for that analyte the prescribed corrective action is reanalysis of the affected sample(s)




CONTINGENCIES FOR HANDLING OUT-OF-CONTROL OR UNACCEPTABLE DATA

151 Method blanks


15

16




152 LCS





METHOD PERFORMANCE






163 Associated SOPs

1631 STL St Louis Laboratory Maintenance of a Alpha Spectroscopy System STLshyRD-0203 Radiochemistry Procedures

164 Appendices

1641 Appendix 1 None






18 WASTE MANAGEMENT


19 REFERENCES

191 VMS Alpha Management Software (AMS) Users Manual 48-0721 Canberra Industries Inc (latest version)

192 VMS Spectroscopy Applications Package Users Manual 07-0196 Canberra Industries Inc (latest version)

193 Canberra Industries Nuclide Identification Algorithms and Software Verification and Validation Manual 07-0464

194 Canberra Industries Spectroscopy Applications Algorithms and Software Verification and Validation Manual 07-0368

195 US Nuclear Regulatory Commission Quality Assurance for Radiological Monitoring Programs (Normal Operations) - Effluent Streams and the Environment Regulatory Guide 415



















S E V E R N Revision Date 103000 Page 1 of 14 T R E N T

Implementation Date 042401 SERVICES UNCONTROLLED CO)

Controlled Copy No gt-^^ STL St Louis 13715 Rider Trail North

OPERATION-SPECIFIC STANDARD OPERATING PROCEDUBreg City MO 63045

Tel 314 298 8566 Fax 314 298 8757 www stl me com

TITLE Calibration and Maintenance

of a Alpha Spectroscopy System (Supersedes SL 0203)

Prepared by

Approved by

Approved by

Approved by

Approved by

TechnicalSpecialist

Duality Assurance Manager

^-bull^2t-^c ^yt Environmental Health and Safety Coordinator

Laboratory Director

Propnetary Information Statement

This document has been prepared by Severn Trent Laboratories (STL) solely for STLs own use and the use of STLs customers in evaluating its qualifications and capabilities m connection with a particular project The user of this document agrees by its acceptance to return it to STL upon request and not to reproduce CODV lend or otherwise disclose us contents directly or indirectly and not to use it for any other purpose other than that for which it was specifically provided The user also agrees that where consultants or other outside parties are involved in the evaluation process access to these documents shall not be given o said panics unless those parties specifically agree to these conditions

THIS DOCUMENT CONTAINS VALUABLE CONFIDENTIAL AND PROPRIETARY INFORMATION DISCLOSURE USE OR REPRODUCTION OF THESE MATERIALS WITHOUT THE WRITTEN AUTHORIZATION OF SEVERN TRENT LABORATORIES IS STRICTLY PROHIBITED THIS UNPUBLISHED WORK 3Y STL IS PROTECTED BY STATE AND FEDERAL LAW OF THE UNITED STATES IF PUBLICATION OF THIS WORK SHOULD OCCUR THE FOLLOWING VOTICE SHALL APPLY

gCOPVRIGHT 2000 SEVERN TRENT L ABORATORIES INC ALL RIGHTS RESERVED STL St Louis is G Dart or Severn Tren[ Laocratones Inc




SUMMARY OF METHOD

11 This SOP provides detailed instructions for the setup and maintenance of an alpha spectroscopy system


21 This SOP assures that the alpha spectroscopy system is functioning within acceptable limits These instructions are applicable to all alpha spectroscopy systems

22 Responsibilities

221 Counting Lab Supervisor to confirm that this procedure is followed whenever the energy calibration or efficiency determination of the alpha spectroscopy system is performed



3 DEFINITIONS


32 Out of Service - a detector or piece of equipment is not to be used for sample analysis until problems have been corrected Marked with a red tag to indicate its status

4 INTERFERENCES

41 None

SOP No STL-RD-02Q3 Re vision No 2



SAFETY










bull Revision Date 103000 Page 4 of 14




611 Alpha spectroscopy system utilizing a computer based data acquisition system


71 Mixed-alpha source with emissions in the spectral range of 3000 keV to 7500 keV shall be used to check this instrument


81 None

9 QUALITY CONTROL









10


















1014 Place the calibration standard(s) in the selected alpha detector chamber(s) establish vacuum turn on bias and start acquisition for the pre-set time (typically 6




hrs)













1024 Remove any sample or calibration standard in the selected alpha detector chambers) place a claen stainless steel disc in the chamber establish vacuum turn on bias and start acquisition for the pre-set time (typically 1000 minutes)






11




10261 The background spectrum will be processed by the software A QA report listing acceptable or not acceptable parameters will be printed automatically


PROCEDURE


112 Initial Setup

1121 Establish the normal instrument settings for all controls Suggested settings are tabulated in Attachment 1

11211 Detector specific high voltage settings and required polarity are listed on the detector manufactures certificate

1122 Pulser quality controls shall be checked before each use of the instrument

113 Energy CalibrationLinearity Check

1131 After counting the mixed-alpha source specified for this purpose verify that the peak search report identifies peaks for Am-241 Pu-241 U-238 and U-234

1132 Peak energies for Am-241 Pu-241 U-23 8 and U-234 must be within plusmn 100 keV of the following energies

U-238 41844 keV U-234 47615 keV Pu-239 51477keV Am-241 54791 keV

1133 Peak centroid channels for Am-241 Pu-241 U-238 and U-234 should be within plusmn 50 channels of the following suggested channels assuming 3500 keV offset 7000 keV maximum energy and 34 keVchannel slope (Other calibration parameter combinations are acceptable)

U-238 200 channel U-234 370 channel




Pu-239 484 channel Am-241 582 channel

1134 Record the calibration in the Alpha Calibration amp Maintenance Log Book

1135 If the peak search energies are outside the range specified in 1132 or if the program identifies out of specification data repeat section 112 Continued failure may require the assisstance of a certified repair technician

114 Weekly Maintenance

11411 None


121 None




1321 Method Blank






13232 No specific corrective actions are required in the evaluation of the MSMSD results provided that the batch LCS is in control Analysts

14




should use sound judgment in accepting MSMSD results that are not within control limits especially if the LCS results are borderline


141 Method Blank










15








14222 If there are positive results for one or more analytes the likelihood of poor reproducibiliry increases and corrective action must be evaluated A nonconformance memo is written to notify project management of the situation for a project decision on whether the affected sample(s) should be reanalyzed


151 Method blanks


152 LCS




16





METHOD PERFORMANCE






1622 Raw data associated with the current calibration check shall be maintained in the Radiochemistry Counting Lab for easy retrieval

1623 At the completion of a successful calibration check the raw data may be discarded

1624 When applicable copies of the raw data shall be maintained in the associated project file

1625 All manufacturer-supplied documentation including Standard Certificates shall be retained as quality documents in the Quality and Operations Files

1626 All laboratory documentation generated in sections 11 and 12 shall be retained as quality documents in the count room until

163 Associated SOPs

1631 STL St Louis Laboratory Daily Operations of an Alpha Spectroscopy System STL-RD-0201 Radiochemistry Procedures

164 Appendices

1641 Appendix 1 Typical Instrument Settings






18 WASTE MANAGEMENT


19 REFERENCES










20




CLARIFICATIONS MODIFICATIONS AND ADDITIONS TO REFERENCE METHOD










SOP NoRevision No

Revision DatePage

Implementation Date

STL-RD-0203 2

103000 14 of 14 042401

APPENDIX 1

Typical Instrument Settings

Alpha Detector +40 Volts

Energy Range (MeV) = 4-7 Pulser (MeV) = 5




1 of 43001

12 T R E N T

-ED COPY SERVICES

STL St Louts


TITLE Drying and Grinding

of Soil and Solid Samples (STL-RC-0003 Rev 2)

Prepared by



Approved by fajbufav~- EnvironmentapoundHealth and Safety Coordinator



This document has been prepared by Severn Trent Laboratories (STL) solely for STLs own use and the use of STLs customers in evaluating its qualifications and capabilities in connection with a particular project The user of this document agrees by its acceptance to return it to STL upon request and not to reproduce copy lend or otherwise disclose its contents directly or indirectly and not to use it for any other purpose other than that for which it was specifically provided The user also agrees that where consultants or other outside parties are involved in the evaluation process access to these documents shall not be given to said parties unless those parties specifically agree to these conditions

THIS DOCUMENT CONTAINS VALUABLE CONFIDENTIAL AND PROPRIETARY INFORMATION DISCLOSURE USE OR REPRODUCTION OF THESE MATERIALS WITHOUT THE WRITTEN AUTHORIZATION OF SEVERN TRENT LABORATORIES IS STRICTLY PROHIBITED THIS UNPUBLISHED WORK BY STL IS PROTECTED BY STATE AND FEDERAL LAW OF THE UNITED STATES IF PUBLICATION OF THIS WORK SHOULD OCCUR THE FOLLOWING NOTICE SHALL APPLY

bullpoundCOPYRIGHT 2000 SEVERN TRENT LABORATORIES INC ALL RIGHTS RESERVED STL St Louis is a part of Severn Trent Laboratories Inc


Revision Date 042801 of 12


SUMMARY OF METHOD





23 Responsibilities




DEFINITIONS


INTERFERENCES


SAFETY





















611 Drying Oven

612 Pulverizer

613 Ball mill

614 Paint cans



REAGENTS

71 Reagents

711 Quartz sand

72 Standards




QUALITY CONTROL

91 QC requirements




10








95 QC Program



101 None

1 1 PROCEDURE
























































121 None


























163 Associated SOPs







164 Appendices





18 WASTE MANAGEMENT


19 REFERENCES













APPENDIX 1

PROCEDURE





grinder



Ball mill sample

SOP NoRevision No

Revision DatePage


STL-RC-0020 2

103000 1 of 26


SERVICES

STL St Louis


Prepared by

Approved by

Approved by

Approved by

Approved by






Laboratory Director

Earth City MO 63045

Tel 3142988566

Fax 314 298 8757

wwwstlHnccom









SUMMARY OF METHOD















22 Responsibilities














DEFINITIONS



INTERFERENCES









SAFETY

















613 Bottle wash







6110 Propane torch






7









73 Reagents



733 Sodium Sulfate






75 Standards


CAUTION Radioactive













QUALITY CONTROL

91 QC requirements






















98 Documentation


















911 QC Program









11 PROCEDURE












































116 Oil
























117 Filter Samples






































OR






12















2027orf (2planchet)


R - R

2 2 2 E TF V A

Where




| (R s t s ) - (R B t s ) | J




Where




22 2 E TF V A t s

Where



RPD = 100 4shyT

Where




Where






A mdash Ashy

Where





1311 Method Blank








141 Method Blank






















151 Method blanks


152 LCS














18 WASTE MANAGEMENT




















194 MDA Table


1942 Liquids


(cpm) (minutes)

Gross Alpha 0100 27 29 0100 1000 279

Gross Alpha 0100 27 29 0200 100 494

Gross Alpha 0100 27 29 0200 200 333

Gross Alpha 0100 27 29 0200 1000 139

Gross Beta 1500 40 90 0100 1000 229

Gross Beta 1500 40 90 0200 100 373

20




Gross Beta 1500 40 90 0200 200 260

Gross Beta 1500 40 90 0200 1000 114

195 Solids


(cpm) (minutes)


Gross Alpha 0100 27 20 0100 200 966

Gross Alpha 0100 27 20 0100 1000 405


Gross Beta 1500 40 78 0100 200 601

Gross Beta 1500 40 78 0100 1000 264

196 Associated SOPs



REFERENCES




















Controlled Copy No






^ S - Approved by


^ Approved by

Laboratory Director






Page 2 of 14







13 Responsibilities







Page 3 of 14



30 DEFINITIONS



40 INTERFERENCES



50 SAFETY





Page 4 of 14











63 Centrifuge

64 IR drying lamp







Page 5 of 14



















Page 6 of 14











90 QUALITY CONTROL






Page 7 of 14













Page 8 of 14



110 PROCEDURE











Page 9 of 14















Page 10 of 14


carrier solution













Page 11 of 14







222 xEjfxVxRxlxt



A


1961 raquo E =

222





Page 12 of 14





exp ected value











Page 13 of 14



160 REFERENCES






166 Associated SOPs








Page 14 of 14






170 MISCELLANEOUS









Prepared by










Page 2 of 18






bullyjo



13 Responsibilities








Page 3 of 18

30 DEFINITIONS


40 INTERFERENCES




50 SAFETY









Page 4 of 18








63 Centrifuge








Page 5 of 18




















Page 6 of 18



















Page 7 of 18






t










Page 8 of 18


90 QUALITY CONTROL









TABLE I

SAMPLE TYPE





Page 9 of 18

BLANK VOLUME

1000 ml






Page 10 of 18






110 PROCEDURE








Page 11 of 18















Page 12 of 18













Page 13 of 18
















Page 14 of 18






yyo




t tb



where





Page 15 of 18


Y chemical yield =


where









CCR = b + Rb







Page 16 of 18















Page 17 of 18



160 REFERENCES






166 Associated SOPs








Page 18 of 18






170 MISCELLANEOUS



SOP NoRevision No

Revision Date-Page


STL-RC-0110 1

103000 1_ of 19

042401


SERVICES

STL St Louis


Tel 3142988566

Fax 314 298 8757




Prepared by

Approved by

Approved by

Approved by

Approved by

Technial Specialist



Laboratory Director








SUMMARY OF METHOD









25 Responsibilities




DEFINITIONS


3





INTERFERENCES








SAFETY


























REAGENTS

71 Reagents



















73 Standards








QUALITY CONTROL

91 QC requirements
























92 Documentation












10








96 QC Program




























11





PROCEDURE






























Where

E AC SUS

196







Where




Where




Where






1314 Method Blank



i









141 Method Blank



















151 Method Blank



SOP NoRevision No

Revision DatePage

Implementation Date

STL-RC-0110 1

103000 16 of 19 042401


















171 Method blanks


172 LCS














183 Associated SOPs








20 WASTE MANAGEMENT



21 REFERENCES





















1 042401

of 16 T R E N T


SERVICES

STL St Louis


Tel 3142988566 TITLE Fax 314 298 8757



Prepared by


Approved by












SUMMARY OF METHOD




22 Responsibilities




DEFINITIONS


INTERFERENCES





SAFETY
















71 Reagents




72 Standards




81 None

9 QUALITY CONTROL




















10






















11













PROCEDURE

















113 Sample Counting












12















1212 Sample Date














222EAbYDVst s )

Where





Where








13






Where



Y _ (CT-CB) 14 3)c A K -f

Where





1321 Method Blank


14










141 Method Blank



















151 Method blanks


15

16




152 LCS





METHOD PERFORMANCE






163 Associated SOPs


164 Appendices







18 WASTE MANAGEMENT


19 REFERENCES































Prepared by

Approved by

Approved by

Approved by

Approved by

TechnicalSpecialist



Laboratory Director








SUMMARY OF METHOD




22 Responsibilities




3 DEFINITIONS



4 INTERFERENCES

41 None




SAFETY


















81 None

9 QUALITY CONTROL









10






















hrs)



















11






PROCEDURE


112 Initial Setup

















11411 None


121 None




1321 Method Blank







14






141 Method Blank










15










151 Method blanks


152 LCS




16





METHOD PERFORMANCE











163 Associated SOPs


164 Appendices







18 WASTE MANAGEMENT


19 REFERENCES










20














SOP NoRevision No

Revision DatePage

Implementation Date

STL-RD-0203 2

103000 14 of 14 042401

APPENDIX 1







SUMMARY OF METHOD





23 Responsibilities




DEFINITIONS


INTERFERENCES


SAFETY





















611 Drying Oven

612 Pulverizer

613 Ball mill

614 Paint cans



REAGENTS

71 Reagents

711 Quartz sand

72 Standards




QUALITY CONTROL

91 QC requirements




10








95 QC Program



101 None

1 1 PROCEDURE
























































121 None


























163 Associated SOPs







164 Appendices





18 WASTE MANAGEMENT


19 REFERENCES













APPENDIX 1

PROCEDURE





grinder



Ball mill sample

SOP NoRevision No

Revision DatePage


STL-RC-0020 2

103000 1 of 26


SERVICES

STL St Louis


Prepared by

Approved by

Approved by

Approved by

Approved by






Laboratory Director

Earth City MO 63045

Tel 3142988566

Fax 314 298 8757

wwwstlHnccom









SUMMARY OF METHOD















22 Responsibilities














DEFINITIONS



INTERFERENCES









SAFETY

















613 Bottle wash







6110 Propane torch






7









73 Reagents



733 Sodium Sulfate






75 Standards


CAUTION Radioactive













QUALITY CONTROL

91 QC requirements






















98 Documentation


















911 QC Program









11 PROCEDURE












































116 Oil
























117 Filter Samples






































OR






12















2027orf (2planchet)


R - R

2 2 2 E TF V A

Where




| (R s t s ) - (R B t s ) | J




Where




22 2 E TF V A t s

Where



RPD = 100 4shyT

Where




Where






A mdash Ashy

Where





1311 Method Blank








141 Method Blank






















151 Method blanks


152 LCS














18 WASTE MANAGEMENT




















194 MDA Table


1942 Liquids


(cpm) (minutes)

Gross Alpha 0100 27 29 0100 1000 279

Gross Alpha 0100 27 29 0200 100 494

Gross Alpha 0100 27 29 0200 200 333

Gross Alpha 0100 27 29 0200 1000 139

Gross Beta 1500 40 90 0100 1000 229

Gross Beta 1500 40 90 0200 100 373

20




Gross Beta 1500 40 90 0200 200 260

Gross Beta 1500 40 90 0200 1000 114

195 Solids


(cpm) (minutes)


Gross Alpha 0100 27 20 0100 200 966

Gross Alpha 0100 27 20 0100 1000 405


Gross Beta 1500 40 78 0100 200 601

Gross Beta 1500 40 78 0100 1000 264

196 Associated SOPs



REFERENCES




















Controlled Copy No






^ S - Approved by


^ Approved by

Laboratory Director






Page 2 of 14







13 Responsibilities







Page 3 of 14



30 DEFINITIONS



40 INTERFERENCES



50 SAFETY





Page 4 of 14











63 Centrifuge

64 IR drying lamp







Page 5 of 14



















Page 6 of 14











90 QUALITY CONTROL






Page 7 of 14













Page 8 of 14



110 PROCEDURE











Page 9 of 14















Page 10 of 14


carrier solution













Page 11 of 14







222 xEjfxVxRxlxt



A


1961 raquo E =

222





Page 12 of 14





exp ected value











Page 13 of 14



160 REFERENCES






166 Associated SOPs








Page 14 of 14






170 MISCELLANEOUS









Prepared by










Page 2 of 18






bullyjo



13 Responsibilities








Page 3 of 18

30 DEFINITIONS


40 INTERFERENCES




50 SAFETY









Page 4 of 18








63 Centrifuge








Page 5 of 18




















Page 6 of 18



















Page 7 of 18






t










Page 8 of 18


90 QUALITY CONTROL









TABLE I

SAMPLE TYPE





Page 9 of 18

BLANK VOLUME

1000 ml






Page 10 of 18






110 PROCEDURE








Page 11 of 18















Page 12 of 18













Page 13 of 18
















Page 14 of 18






yyo




t tb



where





Page 15 of 18


Y chemical yield =


where









CCR = b + Rb







Page 16 of 18















Page 17 of 18



160 REFERENCES






166 Associated SOPs








Page 18 of 18






170 MISCELLANEOUS



SOP NoRevision No

Revision Date-Page


STL-RC-0110 1

103000 1_ of 19

042401


SERVICES

STL St Louis


Tel 3142988566

Fax 314 298 8757




Prepared by

Approved by

Approved by

Approved by

Approved by

Technial Specialist



Laboratory Director








SUMMARY OF METHOD









25 Responsibilities




DEFINITIONS


3





INTERFERENCES








SAFETY


























REAGENTS

71 Reagents



















73 Standards








QUALITY CONTROL

91 QC requirements
























92 Documentation












10








96 QC Program




























11





PROCEDURE






























Where

E AC SUS

196







Where




Where




Where






1314 Method Blank



i









141 Method Blank



















151 Method Blank



SOP NoRevision No

Revision DatePage

Implementation Date

STL-RC-0110 1

103000 16 of 19 042401


















171 Method blanks


172 LCS














183 Associated SOPs








20 WASTE MANAGEMENT



21 REFERENCES





















1 042401

of 16 T R E N T


SERVICES

STL St Louis


Tel 3142988566 TITLE Fax 314 298 8757



Prepared by


Approved by












SUMMARY OF METHOD




22 Responsibilities




DEFINITIONS


INTERFERENCES





SAFETY
















71 Reagents




72 Standards




81 None

9 QUALITY CONTROL




















10






















11













PROCEDURE

















113 Sample Counting












12















1212 Sample Date














222EAbYDVst s )

Where





Where








13






Where



Y _ (CT-CB) 14 3)c A K -f

Where





1321 Method Blank


14










141 Method Blank



















151 Method blanks


15

16




152 LCS





METHOD PERFORMANCE






163 Associated SOPs


164 Appendices







18 WASTE MANAGEMENT


19 REFERENCES































Prepared by

Approved by

Approved by

Approved by

Approved by

TechnicalSpecialist



Laboratory Director








SUMMARY OF METHOD




22 Responsibilities




3 DEFINITIONS



4 INTERFERENCES

41 None




SAFETY


















81 None

9 QUALITY CONTROL









10






















hrs)



















11






PROCEDURE


112 Initial Setup

















11411 None


121 None




1321 Method Blank







14






141 Method Blank










15










151 Method blanks


152 LCS




16





METHOD PERFORMANCE











163 Associated SOPs


164 Appendices







18 WASTE MANAGEMENT


19 REFERENCES










20














SOP NoRevision No

Revision DatePage

Implementation Date

STL-RD-0203 2

103000 14 of 14 042401

APPENDIX 1






















611 Drying Oven

612 Pulverizer

613 Ball mill

614 Paint cans



REAGENTS

71 Reagents

711 Quartz sand

72 Standards




QUALITY CONTROL

91 QC requirements




10








95 QC Program



101 None

1 1 PROCEDURE
























































121 None


























163 Associated SOPs







164 Appendices





18 WASTE MANAGEMENT


19 REFERENCES













APPENDIX 1

PROCEDURE





grinder



Ball mill sample

SOP NoRevision No

Revision DatePage


STL-RC-0020 2

103000 1 of 26


SERVICES

STL St Louis


Prepared by

Approved by

Approved by

Approved by

Approved by






Laboratory Director

Earth City MO 63045

Tel 3142988566

Fax 314 298 8757

wwwstlHnccom









SUMMARY OF METHOD















22 Responsibilities














DEFINITIONS



INTERFERENCES









SAFETY

















613 Bottle wash







6110 Propane torch






7









73 Reagents



733 Sodium Sulfate






75 Standards


CAUTION Radioactive













QUALITY CONTROL

91 QC requirements






















98 Documentation


















911 QC Program









11 PROCEDURE












































116 Oil
























117 Filter Samples






































OR






12















2027orf (2planchet)


R - R

2 2 2 E TF V A

Where




| (R s t s ) - (R B t s ) | J




Where




22 2 E TF V A t s

Where



RPD = 100 4shyT

Where




Where






A mdash Ashy

Where





1311 Method Blank








141 Method Blank






















151 Method blanks


152 LCS














18 WASTE MANAGEMENT




















194 MDA Table


1942 Liquids


(cpm) (minutes)

Gross Alpha 0100 27 29 0100 1000 279

Gross Alpha 0100 27 29 0200 100 494

Gross Alpha 0100 27 29 0200 200 333

Gross Alpha 0100 27 29 0200 1000 139

Gross Beta 1500 40 90 0100 1000 229

Gross Beta 1500 40 90 0200 100 373

20




Gross Beta 1500 40 90 0200 200 260

Gross Beta 1500 40 90 0200 1000 114

195 Solids


(cpm) (minutes)


Gross Alpha 0100 27 20 0100 200 966

Gross Alpha 0100 27 20 0100 1000 405


Gross Beta 1500 40 78 0100 200 601

Gross Beta 1500 40 78 0100 1000 264

196 Associated SOPs



REFERENCES




















Controlled Copy No






^ S - Approved by


^ Approved by

Laboratory Director






Page 2 of 14







13 Responsibilities







Page 3 of 14



30 DEFINITIONS



40 INTERFERENCES



50 SAFETY





Page 4 of 14











63 Centrifuge

64 IR drying lamp







Page 5 of 14



















Page 6 of 14











90 QUALITY CONTROL






Page 7 of 14













Page 8 of 14



110 PROCEDURE











Page 9 of 14















Page 10 of 14


carrier solution













Page 11 of 14







222 xEjfxVxRxlxt



A


1961 raquo E =

222





Page 12 of 14





exp ected value











Page 13 of 14



160 REFERENCES






166 Associated SOPs








Page 14 of 14






170 MISCELLANEOUS









Prepared by










Page 2 of 18






bullyjo



13 Responsibilities








Page 3 of 18

30 DEFINITIONS


40 INTERFERENCES




50 SAFETY









Page 4 of 18








63 Centrifuge








Page 5 of 18




















Page 6 of 18



















Page 7 of 18






t










Page 8 of 18


90 QUALITY CONTROL









TABLE I

SAMPLE TYPE





Page 9 of 18

BLANK VOLUME

1000 ml






Page 10 of 18






110 PROCEDURE








Page 11 of 18















Page 12 of 18













Page 13 of 18
















Page 14 of 18






yyo




t tb



where





Page 15 of 18


Y chemical yield =


where









CCR = b + Rb







Page 16 of 18















Page 17 of 18



160 REFERENCES






166 Associated SOPs








Page 18 of 18






170 MISCELLANEOUS



SOP NoRevision No

Revision Date-Page


STL-RC-0110 1

103000 1_ of 19

042401


SERVICES

STL St Louis


Tel 3142988566

Fax 314 298 8757




Prepared by

Approved by

Approved by

Approved by

Approved by

Technial Specialist



Laboratory Director








SUMMARY OF METHOD









25 Responsibilities




DEFINITIONS


3





INTERFERENCES








SAFETY


























REAGENTS

71 Reagents



















73 Standards








QUALITY CONTROL

91 QC requirements
























92 Documentation












10








96 QC Program




























11





PROCEDURE






























Where

E AC SUS

196







Where




Where




Where






1314 Method Blank



i









141 Method Blank



















151 Method Blank



SOP NoRevision No

Revision DatePage

Implementation Date

STL-RC-0110 1

103000 16 of 19 042401


















171 Method blanks


172 LCS














183 Associated SOPs








20 WASTE MANAGEMENT



21 REFERENCES





















1 042401

of 16 T R E N T


SERVICES

STL St Louis


Tel 3142988566 TITLE Fax 314 298 8757



Prepared by


Approved by












SUMMARY OF METHOD




22 Responsibilities




DEFINITIONS


INTERFERENCES





SAFETY
















71 Reagents




72 Standards




81 None

9 QUALITY CONTROL




















10






















11













PROCEDURE

















113 Sample Counting












12















1212 Sample Date














222EAbYDVst s )

Where





Where








13






Where



Y _ (CT-CB) 14 3)c A K -f

Where





1321 Method Blank


14










141 Method Blank



















151 Method blanks


15

16




152 LCS





METHOD PERFORMANCE






163 Associated SOPs


164 Appendices







18 WASTE MANAGEMENT


19 REFERENCES































Prepared by

Approved by

Approved by

Approved by

Approved by

TechnicalSpecialist



Laboratory Director








SUMMARY OF METHOD




22 Responsibilities




3 DEFINITIONS



4 INTERFERENCES

41 None




SAFETY


















81 None

9 QUALITY CONTROL









10






















hrs)



















11






PROCEDURE


112 Initial Setup

















11411 None


121 None




1321 Method Blank







14






141 Method Blank










15










151 Method blanks


152 LCS




16





METHOD PERFORMANCE











163 Associated SOPs


164 Appendices







18 WASTE MANAGEMENT


19 REFERENCES










20














SOP NoRevision No

Revision DatePage

Implementation Date

STL-RD-0203 2

103000 14 of 14 042401

APPENDIX 1




10








95 QC Program



101 None

1 1 PROCEDURE
























































121 None


























163 Associated SOPs







164 Appendices





18 WASTE MANAGEMENT


19 REFERENCES













APPENDIX 1

PROCEDURE





grinder



Ball mill sample

SOP NoRevision No

Revision DatePage


STL-RC-0020 2

103000 1 of 26


SERVICES

STL St Louis


Prepared by

Approved by

Approved by

Approved by

Approved by






Laboratory Director

Earth City MO 63045

Tel 3142988566

Fax 314 298 8757

wwwstlHnccom









SUMMARY OF METHOD















22 Responsibilities














DEFINITIONS



INTERFERENCES









SAFETY

















613 Bottle wash







6110 Propane torch






7









73 Reagents



733 Sodium Sulfate






75 Standards


CAUTION Radioactive













QUALITY CONTROL

91 QC requirements






















98 Documentation


















911 QC Program









11 PROCEDURE












































116 Oil
























117 Filter Samples






































OR






12















2027orf (2planchet)


R - R

2 2 2 E TF V A

Where




| (R s t s ) - (R B t s ) | J




Where




22 2 E TF V A t s

Where



RPD = 100 4shyT

Where




Where






A mdash Ashy

Where





1311 Method Blank








141 Method Blank






















151 Method blanks


152 LCS














18 WASTE MANAGEMENT




















194 MDA Table


1942 Liquids


(cpm) (minutes)

Gross Alpha 0100 27 29 0100 1000 279

Gross Alpha 0100 27 29 0200 100 494

Gross Alpha 0100 27 29 0200 200 333

Gross Alpha 0100 27 29 0200 1000 139

Gross Beta 1500 40 90 0100 1000 229

Gross Beta 1500 40 90 0200 100 373

20




Gross Beta 1500 40 90 0200 200 260

Gross Beta 1500 40 90 0200 1000 114

195 Solids


(cpm) (minutes)


Gross Alpha 0100 27 20 0100 200 966

Gross Alpha 0100 27 20 0100 1000 405


Gross Beta 1500 40 78 0100 200 601

Gross Beta 1500 40 78 0100 1000 264

196 Associated SOPs



REFERENCES




















Controlled Copy No






^ S - Approved by


^ Approved by

Laboratory Director






Page 2 of 14







13 Responsibilities







Page 3 of 14



30 DEFINITIONS



40 INTERFERENCES



50 SAFETY





Page 4 of 14











63 Centrifuge

64 IR drying lamp







Page 5 of 14



















Page 6 of 14











90 QUALITY CONTROL






Page 7 of 14













Page 8 of 14



110 PROCEDURE











Page 9 of 14















Page 10 of 14


carrier solution













Page 11 of 14







222 xEjfxVxRxlxt



A


1961 raquo E =

222





Page 12 of 14





exp ected value











Page 13 of 14



160 REFERENCES






166 Associated SOPs








Page 14 of 14






170 MISCELLANEOUS









Prepared by










Page 2 of 18






bullyjo



13 Responsibilities








Page 3 of 18

30 DEFINITIONS


40 INTERFERENCES




50 SAFETY









Page 4 of 18








63 Centrifuge








Page 5 of 18




















Page 6 of 18



















Page 7 of 18






t










Page 8 of 18


90 QUALITY CONTROL









TABLE I

SAMPLE TYPE





Page 9 of 18

BLANK VOLUME

1000 ml






Page 10 of 18






110 PROCEDURE








Page 11 of 18















Page 12 of 18













Page 13 of 18
















Page 14 of 18






yyo




t tb



where





Page 15 of 18


Y chemical yield =


where









CCR = b + Rb







Page 16 of 18















Page 17 of 18



160 REFERENCES






166 Associated SOPs








Page 18 of 18






170 MISCELLANEOUS



SOP NoRevision No

Revision Date-Page


STL-RC-0110 1

103000 1_ of 19

042401


SERVICES

STL St Louis


Tel 3142988566

Fax 314 298 8757




Prepared by

Approved by

Approved by

Approved by

Approved by

Technial Specialist



Laboratory Director








SUMMARY OF METHOD









25 Responsibilities




DEFINITIONS


3





INTERFERENCES








SAFETY


























REAGENTS

71 Reagents



















73 Standards








QUALITY CONTROL

91 QC requirements
























92 Documentation












10








96 QC Program




























11





PROCEDURE






























Where

E AC SUS

196







Where




Where




Where






1314 Method Blank



i









141 Method Blank



















151 Method Blank



SOP NoRevision No

Revision DatePage

Implementation Date

STL-RC-0110 1

103000 16 of 19 042401


















171 Method blanks


172 LCS














183 Associated SOPs








20 WASTE MANAGEMENT



21 REFERENCES





















1 042401

of 16 T R E N T


SERVICES

STL St Louis


Tel 3142988566 TITLE Fax 314 298 8757



Prepared by


Approved by












SUMMARY OF METHOD




22 Responsibilities




DEFINITIONS


INTERFERENCES





SAFETY
















71 Reagents




72 Standards




81 None

9 QUALITY CONTROL




















10






















11













PROCEDURE

















113 Sample Counting












12















1212 Sample Date














222EAbYDVst s )

Where





Where








13






Where



Y _ (CT-CB) 14 3)c A K -f

Where





1321 Method Blank


14










141 Method Blank



















151 Method blanks


15

16




152 LCS





METHOD PERFORMANCE






163 Associated SOPs


164 Appendices







18 WASTE MANAGEMENT


19 REFERENCES































Prepared by

Approved by

Approved by

Approved by

Approved by

TechnicalSpecialist



Laboratory Director








SUMMARY OF METHOD




22 Responsibilities




3 DEFINITIONS



4 INTERFERENCES

41 None




SAFETY


















81 None

9 QUALITY CONTROL









10






















hrs)



















11






PROCEDURE


112 Initial Setup

















11411 None


121 None




1321 Method Blank







14






141 Method Blank










15










151 Method blanks


152 LCS




16





METHOD PERFORMANCE











163 Associated SOPs


164 Appendices







18 WASTE MANAGEMENT


19 REFERENCES










20














SOP NoRevision No

Revision DatePage

Implementation Date

STL-RD-0203 2

103000 14 of 14 042401

APPENDIX 1





















































121 None


























163 Associated SOPs







164 Appendices





18 WASTE MANAGEMENT


19 REFERENCES













APPENDIX 1

PROCEDURE





grinder



Ball mill sample

SOP NoRevision No

Revision DatePage


STL-RC-0020 2

103000 1 of 26


SERVICES

STL St Louis


Prepared by

Approved by

Approved by

Approved by

Approved by






Laboratory Director

Earth City MO 63045

Tel 3142988566

Fax 314 298 8757

wwwstlHnccom









SUMMARY OF METHOD















22 Responsibilities














DEFINITIONS



INTERFERENCES









SAFETY

















613 Bottle wash







6110 Propane torch






7









73 Reagents



733 Sodium Sulfate






75 Standards


CAUTION Radioactive













QUALITY CONTROL

91 QC requirements






















98 Documentation


















911 QC Program









11 PROCEDURE












































116 Oil
























117 Filter Samples






































OR






12















2027orf (2planchet)


R - R

2 2 2 E TF V A

Where




| (R s t s ) - (R B t s ) | J




Where




22 2 E TF V A t s

Where



RPD = 100 4shyT

Where




Where






A mdash Ashy

Where





1311 Method Blank








141 Method Blank






















151 Method blanks


152 LCS














18 WASTE MANAGEMENT




















194 MDA Table


1942 Liquids


(cpm) (minutes)

Gross Alpha 0100 27 29 0100 1000 279

Gross Alpha 0100 27 29 0200 100 494

Gross Alpha 0100 27 29 0200 200 333

Gross Alpha 0100 27 29 0200 1000 139

Gross Beta 1500 40 90 0100 1000 229

Gross Beta 1500 40 90 0200 100 373

20




Gross Beta 1500 40 90 0200 200 260

Gross Beta 1500 40 90 0200 1000 114

195 Solids


(cpm) (minutes)


Gross Alpha 0100 27 20 0100 200 966

Gross Alpha 0100 27 20 0100 1000 405


Gross Beta 1500 40 78 0100 200 601

Gross Beta 1500 40 78 0100 1000 264

196 Associated SOPs



REFERENCES




















Controlled Copy No






^ S - Approved by


^ Approved by

Laboratory Director






Page 2 of 14







13 Responsibilities







Page 3 of 14



30 DEFINITIONS



40 INTERFERENCES



50 SAFETY





Page 4 of 14











63 Centrifuge

64 IR drying lamp







Page 5 of 14



















Page 6 of 14











90 QUALITY CONTROL






Page 7 of 14













Page 8 of 14



110 PROCEDURE











Page 9 of 14















Page 10 of 14


carrier solution













Page 11 of 14







222 xEjfxVxRxlxt



A


1961 raquo E =

222





Page 12 of 14





exp ected value











Page 13 of 14



160 REFERENCES






166 Associated SOPs








Page 14 of 14






170 MISCELLANEOUS









Prepared by










Page 2 of 18






bullyjo



13 Responsibilities








Page 3 of 18

30 DEFINITIONS


40 INTERFERENCES




50 SAFETY









Page 4 of 18








63 Centrifuge








Page 5 of 18




















Page 6 of 18



















Page 7 of 18






t










Page 8 of 18


90 QUALITY CONTROL









TABLE I

SAMPLE TYPE





Page 9 of 18

BLANK VOLUME

1000 ml






Page 10 of 18






110 PROCEDURE








Page 11 of 18















Page 12 of 18













Page 13 of 18
















Page 14 of 18






yyo




t tb



where





Page 15 of 18


Y chemical yield =


where









CCR = b + Rb







Page 16 of 18















Page 17 of 18



160 REFERENCES






166 Associated SOPs








Page 18 of 18






170 MISCELLANEOUS



SOP NoRevision No

Revision Date-Page


STL-RC-0110 1

103000 1_ of 19

042401


SERVICES

STL St Louis


Tel 3142988566

Fax 314 298 8757




Prepared by

Approved by

Approved by

Approved by

Approved by

Technial Specialist



Laboratory Director








SUMMARY OF METHOD









25 Responsibilities




DEFINITIONS


3





INTERFERENCES








SAFETY


























REAGENTS

71 Reagents



















73 Standards








QUALITY CONTROL

91 QC requirements
























92 Documentation












10








96 QC Program




























11





PROCEDURE






























Where

E AC SUS

196







Where




Where




Where






1314 Method Blank



i









141 Method Blank



















151 Method Blank



SOP NoRevision No

Revision DatePage

Implementation Date

STL-RC-0110 1

103000 16 of 19 042401


















171 Method blanks


172 LCS














183 Associated SOPs








20 WASTE MANAGEMENT



21 REFERENCES





















1 042401

of 16 T R E N T


SERVICES

STL St Louis


Tel 3142988566 TITLE Fax 314 298 8757



Prepared by


Approved by












SUMMARY OF METHOD




22 Responsibilities




DEFINITIONS


INTERFERENCES





SAFETY
















71 Reagents




72 Standards




81 None

9 QUALITY CONTROL




















10






















11













PROCEDURE

















113 Sample Counting












12















1212 Sample Date














222EAbYDVst s )

Where





Where








13






Where



Y _ (CT-CB) 14 3)c A K -f

Where





1321 Method Blank


14










141 Method Blank



















151 Method blanks


15

16




152 LCS





METHOD PERFORMANCE






163 Associated SOPs


164 Appendices







18 WASTE MANAGEMENT


19 REFERENCES































Prepared by

Approved by

Approved by

Approved by

Approved by

TechnicalSpecialist



Laboratory Director








SUMMARY OF METHOD




22 Responsibilities




3 DEFINITIONS



4 INTERFERENCES

41 None




SAFETY


















81 None

9 QUALITY CONTROL









10






















hrs)



















11






PROCEDURE


112 Initial Setup

















11411 None


121 None




1321 Method Blank







14






141 Method Blank










15










151 Method blanks


152 LCS




16





METHOD PERFORMANCE











163 Associated SOPs


164 Appendices







18 WASTE MANAGEMENT


19 REFERENCES










20














SOP NoRevision No

Revision DatePage

Implementation Date

STL-RD-0203 2

103000 14 of 14 042401

APPENDIX 1













121 None











Revision Date 042 801 of 12















163 Associated SOPs







164 Appendices





18 WASTE MANAGEMENT


19 REFERENCES













APPENDIX 1

PROCEDURE





grinder



Ball mill sample

SOP NoRevision No

Revision DatePage


STL-RC-0020 2

103000 1 of 26


SERVICES

STL St Louis


Prepared by

Approved by

Approved by

Approved by

Approved by






Laboratory Director

Earth City MO 63045

Tel 3142988566

Fax 314 298 8757

wwwstlHnccom









SUMMARY OF METHOD















22 Responsibilities














DEFINITIONS



INTERFERENCES









SAFETY

















613 Bottle wash







6110 Propane torch






7









73 Reagents



733 Sodium Sulfate






75 Standards


CAUTION Radioactive













QUALITY CONTROL

91 QC requirements






















98 Documentation


















911 QC Program









11 PROCEDURE












































116 Oil
























117 Filter Samples






































OR






12















2027orf (2planchet)


R - R

2 2 2 E TF V A

Where




| (R s t s ) - (R B t s ) | J




Where




22 2 E TF V A t s

Where



RPD = 100 4shyT

Where




Where






A mdash Ashy

Where





1311 Method Blank








141 Method Blank






















151 Method blanks


152 LCS














18 WASTE MANAGEMENT




















194 MDA Table


1942 Liquids


(cpm) (minutes)

Gross Alpha 0100 27 29 0100 1000 279

Gross Alpha 0100 27 29 0200 100 494

Gross Alpha 0100 27 29 0200 200 333

Gross Alpha 0100 27 29 0200 1000 139

Gross Beta 1500 40 90 0100 1000 229

Gross Beta 1500 40 90 0200 100 373

20




Gross Beta 1500 40 90 0200 200 260

Gross Beta 1500 40 90 0200 1000 114

195 Solids


(cpm) (minutes)


Gross Alpha 0100 27 20 0100 200 966

Gross Alpha 0100 27 20 0100 1000 405


Gross Beta 1500 40 78 0100 200 601

Gross Beta 1500 40 78 0100 1000 264

196 Associated SOPs



REFERENCES




















Controlled Copy No






^ S - Approved by


^ Approved by

Laboratory Director






Page 2 of 14







13 Responsibilities







Page 3 of 14



30 DEFINITIONS



40 INTERFERENCES



50 SAFETY





Page 4 of 14











63 Centrifuge

64 IR drying lamp







Page 5 of 14



















Page 6 of 14











90 QUALITY CONTROL






Page 7 of 14













Page 8 of 14



110 PROCEDURE











Page 9 of 14















Page 10 of 14


carrier solution













Page 11 of 14







222 xEjfxVxRxlxt



A


1961 raquo E =

222





Page 12 of 14





exp ected value











Page 13 of 14



160 REFERENCES






166 Associated SOPs








Page 14 of 14






170 MISCELLANEOUS









Prepared by










Page 2 of 18






bullyjo



13 Responsibilities








Page 3 of 18

30 DEFINITIONS


40 INTERFERENCES




50 SAFETY









Page 4 of 18








63 Centrifuge








Page 5 of 18




















Page 6 of 18



















Page 7 of 18






t










Page 8 of 18


90 QUALITY CONTROL









TABLE I

SAMPLE TYPE





Page 9 of 18

BLANK VOLUME

1000 ml






Page 10 of 18






110 PROCEDURE








Page 11 of 18















Page 12 of 18













Page 13 of 18
















Page 14 of 18






yyo




t tb



where





Page 15 of 18


Y chemical yield =


where









CCR = b + Rb







Page 16 of 18















Page 17 of 18



160 REFERENCES






166 Associated SOPs








Page 18 of 18






170 MISCELLANEOUS



SOP NoRevision No

Revision Date-Page


STL-RC-0110 1

103000 1_ of 19

042401


SERVICES

STL St Louis


Tel 3142988566

Fax 314 298 8757




Prepared by

Approved by

Approved by

Approved by

Approved by

Technial Specialist



Laboratory Director








SUMMARY OF METHOD









25 Responsibilities




DEFINITIONS


3





INTERFERENCES








SAFETY


























REAGENTS

71 Reagents



















73 Standards








QUALITY CONTROL

91 QC requirements
























92 Documentation












10








96 QC Program




























11





PROCEDURE






























Where

E AC SUS

196







Where




Where




Where






1314 Method Blank



i









141 Method Blank



















151 Method Blank



SOP NoRevision No

Revision DatePage

Implementation Date

STL-RC-0110 1

103000 16 of 19 042401


















171 Method blanks


172 LCS














183 Associated SOPs








20 WASTE MANAGEMENT



21 REFERENCES





















1 042401

of 16 T R E N T


SERVICES

STL St Louis


Tel 3142988566 TITLE Fax 314 298 8757



Prepared by


Approved by












SUMMARY OF METHOD




22 Responsibilities




DEFINITIONS


INTERFERENCES





SAFETY
















71 Reagents




72 Standards




81 None

9 QUALITY CONTROL




















10






















11













PROCEDURE

















113 Sample Counting












12















1212 Sample Date














222EAbYDVst s )

Where





Where








13






Where



Y _ (CT-CB) 14 3)c A K -f

Where





1321 Method Blank


14










141 Method Blank



















151 Method blanks


15

16




152 LCS





METHOD PERFORMANCE






163 Associated SOPs


164 Appendices







18 WASTE MANAGEMENT


19 REFERENCES































Prepared by

Approved by

Approved by

Approved by

Approved by

TechnicalSpecialist



Laboratory Director








SUMMARY OF METHOD




22 Responsibilities




3 DEFINITIONS



4 INTERFERENCES

41 None




SAFETY


















81 None

9 QUALITY CONTROL









10






















hrs)



















11






PROCEDURE


112 Initial Setup

















11411 None


121 None




1321 Method Blank







14






141 Method Blank










15










151 Method blanks


152 LCS




16





METHOD PERFORMANCE











163 Associated SOPs


164 Appendices







18 WASTE MANAGEMENT


19 REFERENCES










20














SOP NoRevision No

Revision DatePage

Implementation Date

STL-RD-0203 2

103000 14 of 14 042401

APPENDIX 1




















163 Associated SOPs







164 Appendices





18 WASTE MANAGEMENT


19 REFERENCES













APPENDIX 1

PROCEDURE





grinder



Ball mill sample

SOP NoRevision No

Revision DatePage


STL-RC-0020 2

103000 1 of 26


SERVICES

STL St Louis


Prepared by

Approved by

Approved by

Approved by

Approved by






Laboratory Director

Earth City MO 63045

Tel 3142988566

Fax 314 298 8757

wwwstlHnccom









SUMMARY OF METHOD















22 Responsibilities














DEFINITIONS



INTERFERENCES









SAFETY

















613 Bottle wash







6110 Propane torch






7









73 Reagents



733 Sodium Sulfate






75 Standards


CAUTION Radioactive













QUALITY CONTROL

91 QC requirements






















98 Documentation


















911 QC Program









11 PROCEDURE












































116 Oil
























117 Filter Samples






































OR






12















2027orf (2planchet)


R - R

2 2 2 E TF V A

Where




| (R s t s ) - (R B t s ) | J




Where




22 2 E TF V A t s

Where



RPD = 100 4shyT

Where




Where






A mdash Ashy

Where





1311 Method Blank








141 Method Blank






















151 Method blanks


152 LCS














18 WASTE MANAGEMENT




















194 MDA Table


1942 Liquids


(cpm) (minutes)

Gross Alpha 0100 27 29 0100 1000 279

Gross Alpha 0100 27 29 0200 100 494

Gross Alpha 0100 27 29 0200 200 333

Gross Alpha 0100 27 29 0200 1000 139

Gross Beta 1500 40 90 0100 1000 229

Gross Beta 1500 40 90 0200 100 373

20




Gross Beta 1500 40 90 0200 200 260

Gross Beta 1500 40 90 0200 1000 114

195 Solids


(cpm) (minutes)


Gross Alpha 0100 27 20 0100 200 966

Gross Alpha 0100 27 20 0100 1000 405


Gross Beta 1500 40 78 0100 200 601

Gross Beta 1500 40 78 0100 1000 264

196 Associated SOPs



REFERENCES




















Controlled Copy No






^ S - Approved by


^ Approved by

Laboratory Director






Page 2 of 14







13 Responsibilities







Page 3 of 14



30 DEFINITIONS



40 INTERFERENCES



50 SAFETY





Page 4 of 14











63 Centrifuge

64 IR drying lamp







Page 5 of 14



















Page 6 of 14











90 QUALITY CONTROL






Page 7 of 14













Page 8 of 14



110 PROCEDURE











Page 9 of 14















Page 10 of 14


carrier solution













Page 11 of 14







222 xEjfxVxRxlxt



A


1961 raquo E =

222





Page 12 of 14





exp ected value











Page 13 of 14



160 REFERENCES






166 Associated SOPs








Page 14 of 14






170 MISCELLANEOUS









Prepared by










Page 2 of 18






bullyjo



13 Responsibilities








Page 3 of 18

30 DEFINITIONS


40 INTERFERENCES




50 SAFETY









Page 4 of 18








63 Centrifuge








Page 5 of 18




















Page 6 of 18



















Page 7 of 18






t










Page 8 of 18


90 QUALITY CONTROL









TABLE I

SAMPLE TYPE





Page 9 of 18

BLANK VOLUME

1000 ml






Page 10 of 18






110 PROCEDURE








Page 11 of 18















Page 12 of 18













Page 13 of 18
















Page 14 of 18






yyo




t tb



where





Page 15 of 18


Y chemical yield =


where









CCR = b + Rb







Page 16 of 18















Page 17 of 18



160 REFERENCES






166 Associated SOPs








Page 18 of 18






170 MISCELLANEOUS



SOP NoRevision No

Revision Date-Page


STL-RC-0110 1

103000 1_ of 19

042401


SERVICES

STL St Louis


Tel 3142988566

Fax 314 298 8757




Prepared by

Approved by

Approved by

Approved by

Approved by

Technial Specialist



Laboratory Director








SUMMARY OF METHOD









25 Responsibilities




DEFINITIONS


3





INTERFERENCES








SAFETY


























REAGENTS

71 Reagents



















73 Standards








QUALITY CONTROL

91 QC requirements
























92 Documentation












10








96 QC Program




























11





PROCEDURE






























Where

E AC SUS

196







Where




Where




Where






1314 Method Blank



i









141 Method Blank



















151 Method Blank



SOP NoRevision No

Revision DatePage

Implementation Date

STL-RC-0110 1

103000 16 of 19 042401


















171 Method blanks


172 LCS














183 Associated SOPs








20 WASTE MANAGEMENT



21 REFERENCES





















1 042401

of 16 T R E N T


SERVICES

STL St Louis


Tel 3142988566 TITLE Fax 314 298 8757



Prepared by


Approved by












SUMMARY OF METHOD




22 Responsibilities




DEFINITIONS


INTERFERENCES





SAFETY
















71 Reagents




72 Standards




81 None

9 QUALITY CONTROL




















10






















11













PROCEDURE

















113 Sample Counting












12















1212 Sample Date














222EAbYDVst s )

Where





Where








13






Where



Y _ (CT-CB) 14 3)c A K -f

Where





1321 Method Blank


14










141 Method Blank



















151 Method blanks


15

16




152 LCS





METHOD PERFORMANCE






163 Associated SOPs


164 Appendices







18 WASTE MANAGEMENT


19 REFERENCES































Prepared by

Approved by

Approved by

Approved by

Approved by

TechnicalSpecialist



Laboratory Director








SUMMARY OF METHOD




22 Responsibilities




3 DEFINITIONS



4 INTERFERENCES

41 None




SAFETY


















81 None

9 QUALITY CONTROL









10






















hrs)



















11






PROCEDURE


112 Initial Setup

















11411 None


121 None




1321 Method Blank







14






141 Method Blank










15










151 Method blanks


152 LCS




16





METHOD PERFORMANCE











163 Associated SOPs


164 Appendices







18 WASTE MANAGEMENT


19 REFERENCES










20














SOP NoRevision No

Revision DatePage

Implementation Date

STL-RD-0203 2

103000 14 of 14 042401

APPENDIX 1




draft quality assurance project plan (qapp) supplements erm

Documents