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NRC INSPECTION MANUAL DI

MANUAL CHAPTER 1232

COLLECTION, PREPARATION, AND SHIPMENT OF INDEPENDENT MEASUREMENT

SAMPLES

1232-01 PURPOSE

To provide requirements and guidance to NRC inspectors and NRC

contractors for collecting, processing, packaging, and shipping

samples to the Radiological and Environmental Sciences Laboratory

(RESL) in Idaho Falls, Idaho.

1232-02 OBJECTIVES

To improve the quality of results, to decrease turnaround time, to

tighten management control, and to recover costs from licensees and

applicants.

1232-03 DEFINITIONS

Splitting. Dividing a sample into two or more parts.

Urgent Samples. Samples that require immediate attention. These

samples will be processed with priority over other samples.

Routine Samples. Samples collected as part of a scheduled

inspection in accordance with an inspection procedure.

Nonroutine Samples. Samples collected as part of a reactive

inspection.

Inplant Samples. Samples collected inplant including effluent,

process streams and reactor coolant samples.

Environmental Samples. Samples collected in the environment,

including outfall water samples, vegetation, soils and sediments,

and milk.

1232-04 RESPONSIBILITIES AND AUTHORITIES

04.01 Project Manager, IE Headquarters
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a. Approves the types of analyses, scheduling, and number of

non-routine samples to be analyzed by RESL.

b. Resolves problems regarding the above.
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04.02 Regional Representative

a. Coordinates the flow of samples from the region to RESL.

b. Reviews sample handling, packaging, and paperwork.

1232-05 BASIC REQUIREMENTS

The two main purposes for analyzing samples in or near licensee

facilities are (1) to determine the capability of the licensee to

make accurate radiometric measurements and (2) to make independent

radiological assessments of situations. In the latter case, the

obtained information is needed to provide or justify the basis for

action.

To obtain accurate measurements on samples and make valid comparisons, it is necessary to have representative samples, samples that

are as close as possible with the licensee's samples, and samples

that reach RESL in a chemical and physical state to enable the

analyst to make meaningful determinations. Provided below are

procedures and guidance to achieve this goal.

05.01 Procedures and Materials for Collecting and Processing

Samples. Section SP-1, "Collecting, Pretreating, Packing, and

Shipping Samples to the Radiological and Environmental Science

Laboratory," of RESL's Laboratory Manual entitled, RESL Analytical

Chemistry Branch Procedures Manual, IDO-12096, 1982, provides the

required methodology.

In special cases, individuals collecting samples for analysis by

RESL may deviate from the usual field treatment or request special

treatment in the laboratory. However, deviations in sample

treatment or special requests should be made clear by noting them

on the sample container and Form ID F-5484.1A. When possible,

special requests should be discussed with Dale Olson (FTS 583-2532),

the RESL contact, before collecting samples.

05.02 Procedure for Filling Out Analytical Record Sheets, Form

ID F-5484.1A. An analytical record sheet, Form ID F-5484.1A, must

be included in the packages for each sample. No work will be

performed without a properly filled out form. A copy of this form

is shown in Figure 1. Please note: We are required by law to

recover the analytical costs from the licensee. Therefore, the

docket number must be provided along with the name of the facility.

This should be written in the space listed, "Sample From."

Give all information requested in the form to the left of and

including the column headed "Anal. for," except for the first column

headed "No." as shown on Figure 1. Fill out those columns of the

form as completely as possible. Make sure the sample identification

on the form is the same as on the bottle. Include pertinent

information, such as sample collection times, sample volumes on air

particulate filters and charcoal cartridges, and any specific

information that will assist the analyst, such as the presence of

higher than usual concentrations of acids, laundry waste, floor

drain samples, etc. If all of the usual analyses are not desired,
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state specifically those that are desired or those that are to be

omitted. Include requests for special sample treatment or analyses

such as: do not acidify; filter and analyze filtrate only, etc.

Specify a date for the gross beta measurement at least 2 weeks from

the date the sample was shipped. This will allow for delays enroute

and for reconstitution of the sample after it is received at RESL.

If a charcoal cartridge or particulate filter must be returned to

the licensee, so state on the analysis sheet. List the analyses to

be performed, leaving an appropriate number of lines as suggested

on the attached sample sheet to facilitate the recording of results.

Do not fill out the blanks for "Samples Received," "Analysis

Completed," "Analyzed By," and "Serial No." Do not fill out column

"Inst. used" or any columns to the right of "Inst. used."

Note, on the top left side of the sheet, the checkoff to indicate

whether the sample is routine, nonroutine, and/or urgent. For

budgetary and administrative purposes, it is important to distinguish the types of samples. Check "Urgent" box only if samples are

really top priority. Urgent samples will displace and delay routine

samples, disrupt regular schedules, and result in substantially

increased analytical costs.

In addition, indicate on the form whether the sample was collected

in the plant, "Inplant," or in the environment, "Environ." Space

has been provided to indicate under which inspection module these

samples were collected, "NRC Mod #." We need this information and

sometimes it is difficult for RESL to categorize the particular

sample.

05.03 Procedure for Accessing RESL's Query Computer Program. To determine the status and analytical results of submitted samples,

a query program has been developed to access RESL's computer system.

The project manager will provide each region with a user name and

password. Access to the computer will be limited to the time period

5:30 to 17:30 MST Monday through Friday. Any computer terminal and

modem capable of 1200 baud transmission rate can be used.

Listed below are detailed instructions for using RESL's query

program.

a. Turn the terminal "on" and allow it to warm up.

b. Dial the FTS access code and 583-2009. When the call is

answered and the carrier signal is heard, hang up the receiver

and turn the switch on the modem to data, or do whatever is

necessary to make your particular modem operable.

c. To log onto the computer, press the return on the terminal.

You will be asked for your "user name" (each region will be

given a name).

d. Give your user name and the computer will request your

password (each region will be given a password).

e. Respond with your password; if it is correct, you will be

welcomed onto the computer and it will conversationally tell

you what to do to obtain your data. If the password is
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incorrect, you will not be allowed access and you will have

to begin "log on" again by returning to step c.

The dialogue that takes place is as follows:

Hello.

Welcome to the RESL data base, courtesy of which here is your

fortune cookie for today. (The computer provides a "gem" for

your enrichment).

When the program is ready it will display an "*" as a prompt

character. If the serial number of the desired sample is

known it may be entered after the prompt, terminated by a

return. If the serial number is unknown and a listing of the

serial numbers, associated comment line and submission date

is desired, simply hit the return key. You may halt or

continue the listing at any time by using the "control S,"

"control Q," or the "No scroll" key on your terminal.

Note the serial number(s) of the sample(s) in question.

Once the entire serial number list is displayed, enter the

serial number of the desired sample. All of the available

results for the specified serial number will then be displayed. The program will then ask if another query is

desired. If "yes," it proceeds with the next query. If the

answer is "no" the program will terminate.

f. Turn the switch on the modem from "data" to "voice" or do

whatever is necessary to disengage your particular modem.

g. Turn "off" the terminal.

05.04 Procedures for Packaging and Shipping Samples

a. General Information. Applicable Department of Transportation

(DOT) regulations in 49 CFR 170-178 and U.S. Postal Service

(USPS) Regulations in Publication #6, "Radioactive Materials,"

September 1983, must be followed in the packaging and shipment

of samples. The samples must be considered to be "radioactive

material" for purposes of transportation if their specific

activity exceeds 0.002 μCi/gram, and the radioactivity is

essentially uniformly distributed [see 49 CFR 173.403(y)].

Below this activity, the packages may be shipped as would any

other nonradioactive laboratory sample. Liquids below this

specific activity may be sent without absorbing material if

packaged in 1-quart "Cubitainers." As an added precaution

against leakage, the "Cubitainer" lid should be screwed on

tightly and black electrical tape should be used to secure the

cap and neck of the container. The "Cubitainer" should be

placed inside a heavy-gage plastic bag, excess air removed,

and the bag sealed. The bagged "Cubitainer" is placed in the

cardboard carton and mailed.

Nonliquid samples will be packaged, marked and labeled as

required in accordance with applicable requirements for
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mailable or non-mailable packages as described below.

Particulate filters will be placed inside glassine envelopes

and sent in regular mailing envelopes or packages as required

by the radioactivity present.

Gas samples are to be shipped in the same package as received,

using care to position the polyfoam at the ends of the inner

container to protect the fragile arms of the gas bulb. Should

the surface activity of the packaged gas sample exceed the

permissible limits, the inner container must be packaged

within a larger outer container so as to reduce the external

radiation.

b. Mailable Radioactive Sample Packages. If the sample specific

activity exceeds or is suspected to exceed the 0.002 μCi/gm

level, the next threshold to consider is whether the package

activity exceeds one-tenth of a "small" or "limited" quantity,

pursuant to 49 CFR 171.8 and 173.421, 173.421-1, and 173.421-2

or USPS Publication #6, paragraph IIA. For solids this

mailable limited quantity is 10-4 times its A2 value in 49 CFR

173.435 or 10-5 times its A2 value for liquids. As such, the

packages must be "strong, tight" with the radiation level on

the package not to exceed 0.5 mrem/h at any point. The USPS

requirements for "limited quantity" are essentially identical

to the DOT requirements of 49 CFR 173.421, 173.421-1, and

173.421-2 for a "limited quantity," except that the USPS

further requires that liquids must additionally be packaged

within a leak resistant and corrosion resistant secondary

inner container, surrounded by sufficient suitably positioned

absorbent material to absorb at least twice the volume of

liquid radioactive contents in the event of leakage from the

secondary inner container.

The external surface of the package may not have "significant"

removable radioactive surface contamination as prescribed by

49 CFR 173.443(a), and the inner packages must be marked

"RADIOACTIVE" or if there is no inner package, the outside of

the package itself must be so marked.

Mailable radioactive packages may also be carried by an

individual on a passenger-carrying aircraft, since the DOT

requirements for air carriage of radioactive packages do not

apply to "limited quantities" other than the requirements for

reporting of incidents [see 49 CFR 173.421-1(b)(2)] which are

applicable. It is important to remember that the certification/notice described by 49 CFR 173.421-1 (a) should be

prepared and accompany the package.

c. Non-mailable Packages. If the limits of USPS Publication #6,

paragraph IIA and Table 1 therein are exceeded, the package

is non-mailable, but it may be offered for transport to a

carrier or transported in private carriage, subject to the

applicable DOT regulations for a "limited quantity" (10-3

times A2 for solids and 10-4 times A2 for liquids) or as a Type

A package with contents not exceeding A1 or A2 (49 CFR

173.403(a) and (b), 173.412, and 173.415).
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Limited quantity, non-mailable packages are excepted from

specification packaging and labeling requirements. A marking

requirement identical to that for mailable packages does

apply, but the shipping documentation requirement is much less

than that for Type A, non-mailable packages, wherein specification 7A packaging, marking and labeling, and shipping paper

documentation is required. It is important to remember that

the DOT Specification 7A is a "performance" specification,

requiring that each shipper of such a specification maintain

on file a supporting documentation which attests to the

results of the demonstration testing of the packaging design

against the Type A performance tests [see 49 CFR 173.412,

173.415, 178.350, and 173.465]. Additionally, the package is

subject to the requirements for liquids as prescribed in

173.412(n), requiring absorbent materials or a

double-containment system.

Note: Section 02, IE Procedure No. 86740 may be used as a

general guideline for DOT requirements, applicable to package

marking, labeling, preparation of shipping papers, etc.

d. Air Transport of Non-mailable Packages (Labeled Packages). Non-mailable, labeled, radioactive packages may not be carried

by an individual passenger on a passenger-carrying aircraft.

They may however, be offered to the carrier as air freight,

following the established provisions for packaging, marking,

labeling, and shipping paper description. Additionally, if

the package is to be offered for carriage on a

passenger-carrying aircraft, the shipper must certify on the

shipping papers that the radioactive material is for use in

research [see 49 CFR 175.700(c)] and indicate this accordingly

on the shipping papers [see 49 CFR 172.204 (c)(4)].

Independent measurement samples are considered to be for use

in research [see memorandum for John Buchanan from Alfred W.

Grella, dated September 4, 1986].

e. Mailability of Samples Based on Nonradiological Hazardous

Materials Considerations. In addition to considering the

mailability of a sample package based on its radioactive

nature, its mailability on the basis of any secondary

hazardous material characteristics also must be considered.

The general rules for such mailability are contained in USPS

Publication #52, "Acceptance of Hazardous, Restricted or

Perishable Matter," May 15, 1981.

Generally, the USPS rules allow as a mailable hazardous

materials package only those materials that meet the "limited

quantity" criteria of 49 CFR for the specific hazard class.

In the case of analytical samples, the most likely secondary

hazard which might exist would be its corrosivity due to

acidic solution. Therefore, a determination should be made

of whether the sample is a "corrosive material" even if it is

not a "radioactive material."

Pursuant to 49 CFR, a "corrosive material" is a liquid or

solid that causes visible destruction or irreversible

alterations in skin tissue at the site of contact or, in the
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case of leakage from its packaging, a liquid that has a severe

corrosion rate on steel. The quantitative test criteria for

determination of the above are prescribed in Section 49 CFR

173.240. Informal information has been obtained from DOT to

the effect that laboratory testing of nitric and hydrochloric

acids in aqueous solution has indicated that greater than 1%

by volume of either material would qualify as a "corrosive

material" pursuant to the test criteria. A corrosive liquid,

however, is excepted from 49 CFR packaging, marking, and

labeling requirements and is generally mailable subject to the

following:

1. Volume is limited to 16 ounces (approximately 500 ml) in

inside closed bottles. (If an air shipment, only one

bottle per package.)

2. Bottles must be cushioned by uncombustible, absorbent

material, and securely packed in tightly closed metal

containers, in an outside metal, wooden, or fiberboard

outer container.

3. Bottles and inside containers must have screw caps with

a minimum 11⁄2 turns, or soldering clips, or other means to

effect secure closure. Friction tape closure is not

acceptable.

In general, when a limited quantity radioactive material also

meets the definition of another hazard class, the requirements

for the other hazard class will prevail. The pertinent

requirements are found in 49 CFR 173.421-2.

For shipments that are made to a foreign country, the

inspector should check with the USPS Headquarters, Office of

Mail Classification, Washington, D.C. (telephone: (202)

245-5756) prior to shipment since the destination country

either may have a prohibition on air shipment by mail of such

materials or may have a different limit on allowable contents

or package surface radiation.

f. Shipping Samples

1. Mailing Address:

Department of Energy

Radiological and Environmental Sciences Laboratory

Analytical Chemistry Branch

CF 601

Scoville, Idaho 83415

Attention: Dale Olson

2. For "Urgent" samples, requiring quick turnaround time,

send samples via Federal Express or Emory Air Freight

(under 70 lb. Federal Express is preferred). Telephone

Dale Olson and inform him of the contents and when the

samples were sent.
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For your information: There is a local Idaho airline,

C&C Airfreight, which flies to Idaho Falls from Salt Lake

City each day at 8:00 a.m. Packages addressed to the

Scoville address will be delivered to Dale Olson out at

the site.

END

Enclosure:

Figure 1
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