^T'L INST OF STAND & TECH R.I.C.

I isurement Services:

11105

Ntsr

NIST Special Publication 250-45

Radiation Processing Dosimetry Calibration

Services: IVlanual of Calibration Procedures

Jimmy C. Humphreys

James M. Puhl

Stephen M. Seltzer

William L McLaughlin

Marc F. Desrosiers

Vitaly Y. Nagy

Debra L. Bensen

Marlon L. Walker

C

00

57

.250-^15

98

U.S. Department of Commerce

Technology Administration

National Institute of Standards and Technology
fhe National Institute of Standards and Technology was established in 1988 by Congress to "assist industry in the development of technology . . . needed to improve product quality, to modernize manufacturing processes, to ensure product reliability ... and to facilitate rapid commercialization ... of products based on new scientific discoveries." NIST, originally founded as the National Bureau of Standards in 1901, works to strengthen U.S. industry's

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'At Boulder, CO 80303. ^Some elements at Boulder, CO.
NIST Special Publication 250-45

NIST MEASUREMENT SERVICES:

Radiation Processing Dosimetry Calibration

Services: Manual of Calibration Procedures

Jimmy C. Humphreys, James M. Puhl, Stephen M. Seltzer,

William L. McLaughlin, Marc F. Desrosiers, Vitaly Y Nagy,

Debra L. Bensen, and Marlon L. Walker

Ionizing Radiation Division

Physics Laboratory

National Institute of Standards and Technology

Gaithersburg, MD 20899-0001

March 1998

U.S. Department of Commerce

William M. Daley, Secretary

Technology Administration

Gary R. Bachula, Acting Under Secretary for Technology

National Institute of Standards and Technology

Raymond G. Kammer, Director
National Institute of Standards and Technology Special Publication 250-45

Natl. Inst. Stand. Technol. Spec. Publ. 250-45, 47 pages (Mar. 1998)

CODEN: NSPUE2

U.S. GOVERNMENT PRINTING OFFICE

WASHINGTON: 1998

For sale by the Superintendent of Documents, U.S. Government Printing Office, Washington, DC 20402-9325
TABLE OF CONTENTS

Page

SCOPE 1 REFERENCED DOCUMENTS 1 TERMINOLOGY 1

SIGNIFICANCE AND USE 3

CALIBRATION PROCEDURES 4

MEASUREMENT UNCERTAINTY 24

KEYWORDS 28

REFERENCES 28

APPENDIXES 30

ii

1. Scope

1.1 This document contains detailed descriptions of the procedures used in the high-dose

radiation dosimetry calibration services at the National Institute of Standards and Technology

(NIST). These services are provided to the radiation processing industry by NIST staff or by

personnel employed by an industry trade organization, operating at NIST using NIST calibration

facilities, as part of a cooperative research and development agreement (CRADA). NIST staff

provide oversight and ensure the quality of the calibration services.

2. Referenced Documents

2.1 ASTMStandards:

E 1 70 Terminology Relating to Radiation Measurements and Dosimetry

E 1249 Practice for Minimizing Dosimetry Errors in Radiation Hardness Testing of Silicon

Electronic Devices using Co-60 Sources

E 1250 Method for Application of Ionization Chambers to Assess the Low Energy Gamma

Component of Cobalt-60 Irradiators Used in Radiation-Hardness Testing of Silicon Electronic

Devices

E 1261 Guide for Selection and Calibration of Dosimetry Systems for Radiation Processing

E 1275 Practice for Use of a Radiochromic Film Dosimetry System

E 1 607 Practice for Use of the Alanine-EPR Dosimetry System

E 1707 Guide for Estimating Uncertainties in Dosimetry for Radiation Processing

2.2 International Organizationfor Standards:

ISO/IEC Guide 25 (1990) General requirements for the competence of calibration and testing

laboratories

2.3 American National Standards Institute:

ANSI/NCSL Z540-1-1994 Calibration Laboratories and Measuring and Test Equipment - General Requirements

2.4 National Institute ofStandards and Technology:

NIST Special Publication 250-44 High-Dose Radiation Dosimetry Calibration Services and

Measurement Assurance Program

3. Terminology

3.1 Descriptions of Terms Specific to This Document:

1
3.1.1 calibration - the process whereby the response of a dosimeter or measuring instrument is characterized through comparison with an appropriate standard that is traceable to, and consistent

with, a national standard.

3.1.2 dosimetry system - a system used for determining absorbed dose, consisting of

dosimeters, measurement instruments and their associated reference standards, and procedures

for the system's use. NOTE 1 - The types of dosimeters include reference standard dosimeters, transfer

standard dosimeters, and routine dosimeters. See Guide E 1261 for guidance on the

selection and calibration of the various dosimetry systems.

3. 1 .3 measurement assurance program - a documented program for the measurement process

that quantifies on a continuing basis the overall uncertainty of the measurements. This program

requires traceability to and consistency with national or international standards, and shall ensure

that the overall uncertainty meets the requirements of the specific application.

3. 1 .4 measurement traceability - the ability to demonstrate and document periodically that the

measurement results from a particular measurement system are in agreement with comparable

measurement results obtained with a national standard (or some identifiable and accepted

standard) to a specified uncertainty.

3.1.5 primary standard dosimeter - dosimeter, of the highest metrological quality, established

and maintained as an absorbed dose standard by a national or international standards

organization.

3. 1 .6 quality assurance - all systematic actions necessary to provide adequate confidence that a

calibration or measurement is performed to a predefined level of quality.

3.1.7 quality control - the operational techniques and procedures that are employed routinely to achieve and sustain a predefined level of quality.

3.1.8 quality manual - document stating the quality policy, quality system, and quality practices

of an organization.

3. 1 .9 quality system - organizational structure, responsibilities, procedures, processes, and

resources for implementing quality management.

3.1.10 radiation processing - the intentional irradiation of products or materials to preserve,

modify, or improve their characteristics.

3.1.11 reference standard dosimeter - a dosimeter, of high metrological quality, used as a

standard to provide measurements traceable to, and consistent with, measurements made using

primary standard dosimeters.

2
3.1.12 routine dosimeter - dosimeter calibrated against a primary-, reference-, or transferstandard dosimeter and used for routine absorbed dose measurement.

3.1.13 transfer standard dosimeter - a dosimeter, often a reference standard dosimeter, suitable

for transport between different locations, used to compare absorbed dose measurements.

3.1.14 verification - confirmation by examination of objective evidence that specified

requirements have been met.

NOTE 2 - In the case of measuring equipment, the result of verification leads to a

decision either to restore to service or to perform adjustments, or to repair, or to downgrade, or to declare obsolete. In all cases it is required that a written trace of the

verification performed be kept on the instrument's individual record.

3.1.15 working standard - a standard, usually calibrated against a reference standard, used

routinely to calibrate or check measuring instruments or devices.

3.2 Also see Terminology E 170.

4. Significance and Use

4. 1 The radiation industry needs a source of reliable, prompt, dosimeter calibration services to support accurate measurements of absorbed dose during radiation processing. Those

measurements, made routinely in industrial facilities, should be consistent with and traceable to the physical measurement standards maintained by an appropriate national or international

standards laboratory.

4.2 To ensure the provision of adequate services, a calibration laboratory should be operating

with a full measurement assurance program (MAP). The fundamental requirements for such a program include: (1) compliance with operational requirements of this document; (2)

documented procedures and in-house quality assurance (QA) program specific to the calibration

services provided; and (3) periodic performance evaluations, such as review by NIST staff and

measurement intercomparisons between national laboratories (1,2)'.

4.3 In addition to standard calibration services such as irradiation of dosimeters and supplying

transfer dosimeters for customer in-house source calibration, the calibration laboratory MAP can

provide technical information, troubleshooting (at the customer's facility if necessary), and serve

as an independent group for resolution of disputes. The MAP can also conduct long term studies

of dosimetry system characteristics, such as environmental effects, and evaluate new, emerging

dosimetry systems to assist in technology transfer to industry.

4.4 NIST SP250-44 sets forth general criteria that shall be satisfied by the calibration

^The bold numbers in parenthesis indicate references at the end of the text.

3
Dimensions

in mm

Holes:

13 mm dia

51.50

laboratory. These general criteria are completely consistent with ISO/IEC Guide 25 and its U.S.

equivalent ANSI/NCSL Z540-1 . Laboratories that meet these general requirements comply, for

calibration activities, with Guide 25/Z540 and the relevant requirements of the ISO 9000 series of

standards, including those of the model described in ISO 9002 when they are acting as suppliers

producing calibration results. 4.5 In addition to the general requirements of ISO/IEC Guide 25/ANSI Z540, NIST SP250-44

contains specific criteria for particular types of ionizing radiation, that is, gamma rays, electron

beams and x-ray (bremsstrahlung) beams. It contains the theoretical basis for the traceability of

dosimetry measurements used in the

calibration services.

4.6 This document contains the

procedures used in the handling of

customer's calibration requests, for the

generation of calibration reports (with

examples), and in the determination of

the uncertainties for the various

calibration services.

5. Calibration Procedures

5 . 1 Calibration Methods

5.1.1 The Pool source and Gammacell

^°Co gamma-ray irradiators ^, described

in detail in NIST SP250-44, are used to

calibrate a variety of types of dosimeters

including liquid solutions sealed in glass

ampoules such as eerie cerous sulfate

and dichromate, thin radiochromic solid

films, and thick solid slabs such as Red

Perspex. Each type of dosimeter requires a unique holder and geometry during

irradiation. For the liquid-in-ampoule

type, a polystyrene holder was used as shown in Fig. 1 . This holder is referred to as the "five-hole

cup" since the five circumferential holes are normally used to hold the dosimeters being

calibrated and the center hole is used for quality control dosimetry. The hole size was chosen so

that a 2-mL ampoule would fit snugly. Red Perspex dosimeters are normally sealed in aluminum

pouches by the manufacturer and are not opened until after irradiation. The usual method for

handling these during calibration is to fold the pouch tightly around the slab of each dosimeter

' O

Support

Rod

Figure 1 - Five-Hole Cup

for Ampoule Irradiation

^The mention of commercial products throughout this document does not imply

recommendation or endorsement by the National Institute of Standards and Technology, nor does it imply that the products identified are necessarily the best available for the purpose.

4
Cavity for films

Figure 2 - Holder for Radiochromic Thin Film Irradiation

Dimensions in mm j i

• ^ i i and place it into the hole or the

five-hole cup normally occupied

by an ampoule. The

radiochromic thin film

dosimeters are normally

irradiated in polystyrene twopiece square slab holders as shown in Fig. 2. The slab

assembly, with several

radiochromic films sealed in the

interior cavity, is held vertically

during irradiation. The

dosimeters are held in the

various holders or cups described in order to provide reproducible geometries as well as provide

approximate electron equilibrium conditions. Electron equilibrium is created when an

appropriate thickness of buildup material surrounds the dosimeter so that the incident photon

fluence generates a constant secondary electron spectrum. The exact thickness of the buildup

material is not very critical. For example, for ^°Co gamma rays, a thickness of 3 mm to 5 mm of

polystyrene is adequate. The Pool source and Gammacells provide nearly isotropic incident

photon fluences. This makes the ratio measurements discussed in Section 7.8 of SP250-44

necessary since the buildup material thickness can not be constant in all directions with

practically achievable geometries. The dose rates for all sources and configurations are given in

Table 1 . The conversion of absorbed dose values in water to dose in silicon was done with the use of ratios of mass energy absorption coefficients.

5.1 .2 The liquid-in-ampoules type dosimeters are not sensitive to external environmental

effects and require no special preparation before irradiation. The Red Perspex type dosimeters are sealed in an aluminized pouch by the manufacturer to provide a constant relative humidity for the

dosimeters. These pouches must remain intact until after irradiation for the dosimeters to perform

properly. The FWT radiochromic thin film dosimeters are sensitive to humidity and must be

conditioned at a relative humidity of approximately 45% to 50% for at least 16 h then sealed in

aluminized trilaminate pouches before irradiation.

5.1.3 Nearly all dosimeters are sensitive to temperature during irradiation to some extent. It is important to know that temperature so as to be able to apply a correction factor if necessary.

Even more desirable is to be able control the temperature during irradiation. The temperature in

GC-232 Gammacell can reach 50 °C if not controlled. A Turbo-Jet gas cooling system is used to maintain the temperature of the dosimeters and holders at 23 °C during all irradiation.

5
Table 1 Dose Rates for ^"Co Sources for December 31, 1996

filename = B140 P5-90 c:\qpw\DR97c.WBl

Effective 3/1/97

Co-60 half-life value is adjusted from 1925.34 davs to 1925.12 davs

Domen Water Calorimeter Transfer Calibration

Source in B036 under 5 cm water at 100 cm source

for 14.5 cm by 14.5 cm field size

7—< 1/11 1 f\ r\ i~A A. For 1/1 1/90 Dose rate = 1.8144 Gy/min

Fnr 1 11^ 1 l^fi Flan<;prl time = 2546 days

i^o-ou Uaiiy uecay consiani inz / vyzo. iz ) — 3.60054e-04

L^ccdy Lurrcciiuii laciur 0.399837

LJiJoC lalC 0.72546 Gy/min

or 0.012091 Gy/s

Absorbed Dose Rate in Water

(jCziz Ratio Gy/s Gy/min kGy/h

3.5 mm Single-hole vial geometry 248.6 3.005 180.3 10.82

5.0 mm Polystyrene Film Block Geometry 0.9870 2.966 178.0 10.68

4.2 mm polystyrene 5-hole cup Perspex Geometry 0.9710 2.918 175.1 10.51 4.2 mm Dolvstvrene 5-hole cud Ampoule Geometry 0.9560 2.873 172.4 10.34 uLziz m btamiess steel uewar

3.5 mm Single-hole vial geometry 239.9 2.901 174.0 10.44

5.0 mm Polystyrene Film Block Geometry 0.9913 2.875 172.5 10.35

4.2 mm polystyrene 5-hole cup Perspex Geometry 0.9692 2.811 168.7 10.12

4.2 mm polystyrene 5-hole cup Ampoule Geometry 0.9599 2.784 167.1 10.02

3.5 mm Single-hole vial geometry 75.18 0.9090 54.54 3.272

5.0 mm Polystyrene Film Block Geometry 0.9889 0.8989 53.93 3.236

4.2 mm polystyrene 5-hole cup Perspex Geometry 0.9730 0.8844 53.07 3.184

4.2 mm oolvstyrene 5-hole cup Ampoule Geometry 0.9595 0.8722 52.33 3.140

FlOl Pool Source

3.5 mm Single-hole vial geometry 26.85 0.3246 19.48 1.169

5.0 mm Polystyrene Film Block Geometry 0.9941 0.3227 19.36 1.162

4.2 mm polystyrene 5-hole cup Perspex Geometry 0.9883 0.3208 19.25 1.155

4.2 mm polystyrene 5-hole cup Ampoule Geometry 0.9749 0.3164 18.99 1.139

for Gammacell and Pool, Combined Relative Expanded Uncertainty = 1.8%; dose rate (Silicon) = dose rate (Water) * 0.913

elapsed time = 366 days, decay correction factor = 0.876534

B036 Co-60 Vertical Beam Geometry Gy/s Gy/min Gy/h

B036 s.d.=30.0 cm, coll=20 x 20 6 mm ps plate 2.676e-02 1.605e+00 96.32

B036 s.d.=41.6 cm, coll=20 x 20 6 mm ps plate 1.944e-02 1.167e+00 70.00

B036 s.d.= 105 cm, coll=20 x 20 6 mm ps plate 6.227e-03 3.736e-01 22.42

B034 Co-60 Vertical Beam

B034 s.d.= 15.0 cm, coll.= 25 x 25 6 mm ps plate 5.306e-03 3.184e-01 19.10 B034 s.d.=100 cm, coll.= 25 x 25 6 mm ps plate 9.476e-04 5.685e-02 3.411 B034 s.d.= 130 cm, coll.= 25 x 25 6 mm ps plate 6.568e-04 3.941e-02 2.364

for vertical beams. Combined Relative Expanded Uncertainty = 2.2%; dose rate (Silicon) = dose rate (Water) * 0.896

6
5.2 Quality Control Procedures

5.2. 1 Calibrated NIST radiochiomic thin film dosimeters are used for quality control (QC)

during irradiation of customer-supplied radiochromic thin film dosimeters. The procedures are as follows:

5.2. 1 . 1 A new batch of radiochromic dosimeters is calibrated by irradiation to various absorbed

dose values over the dose range of interest. For example, for a range of 1 kGy to 50 kGy, 10 dose

points might be used, with 5 dosimeters irradiated at each dose value. Each dosimeter film is marked with a code to maintain its identity through all subsequent operations. All dosimeters are analyzed (read out) before irradiation as well as after irradiation. After the pre-irradiation

analysis, the dosimeters are stored under controlled humidity conditions of 45% to 50% R.H. for

at least 16 h to allow for equilibration of the water content of the films. Five films are stacked,

with a thin black polyethylene square on the top and bottom of the stack, and placed in the

polystyrene block assembly shown in Fig. 2. The black polyethylene squares are needed because

experimental evidence indicates an over response of the top and bottom films in the stack,

probably a result of fluorescence from the polystyrene during irradiation. The polystyrene block

assembly is then heat sealed in a trilaminate pouch (a polyethylene layer inside, then a thin

aluminum sheet, then a Mylar layer outside) in the controlled humidity environment. Each sealed

block assembly is irradiated to a specific dose value in one of the NIST ^°Co irradiators with the

block held in a reproducible position in the center of the source array geometry. After a storage

time of at least 1 6 h, the dosimeters are analyzed and the results provide a calibration of that

batch of radiochromic films (see 5.3 for details on the analysis and data reduction procedures).

The remainder of the unirradiated batch may be used for QC during irradiation of customersupplied dosimeters.

5.2.1.2 Unirradiated QC dosimeters are analyzed before irradiation and then stored, along with

the customer-supplied dosimeters, in the 45% to 50% R.H. environment for at least 16 h. A stack

of customer dosimeters ( a maximum of five) and three QC dosimeters are placed in the

polystyrene block assembly and sealed in the laminated pouch as described in 5.2.1.1.

5.2. 1 .3 The sealed block assembly is irradiated to the specified absorbed dose in one of the

NIST ^°Co irradiators and stored for at least 16 h (overnight) to allow for full development of the

film response. The pouch is opened, the films removed and the NIST QC films separated from

the customer's films. The QC films are then analyzed and the indicated dose values are compared

with the target dose. If the results are within the specified control limits (discussed in Section 7)

then the irradiation is considered satisfactory. If the results are outside the control limits then the

irradiation must be investigated and appropriate corrective action taken. All QC results are recorded as part of the calibration report and test folder.

5.2.2 Calibrated alanine pellets are used for QC for all irradiations that do not involve

radiochromic thin films. The procedures are as follows:

7
5.2.2.1 A batch of NIST-fabricated alanine dosimeter pellets is produced as described in detail

in section 7.8 of NIST SP 250-44. The dosimeters are sorted by height and those in the range of

2.5 mm to 2.7 mm are used for subsequent dosimetry measurements. The variation in mass of

these pellets is about 2.2 %. Bruker-fabricated pellets may also be employed; these have a mass

variation of about 1.7 %. The new alanine batch is calibrated in a manner similar to that used for

radiochromic films discussed in 5.2.1. The differences in the procedures are that the alanine

dosimeters do not require humidity equilibration (after the initial conditioning during fabrication) or sealing, and the alanine dosimeters are calibration over two dose ranges. The Low Dose range

extends from 10 Gy to 2 kGy; the High Dose range extends from 1 kOy to 100 kGy (or higher).

The alanine pellets are irradiated in the single-hole cup shown in Fig. 9 of NIST SP 250-44

during calibration. Five pellets are placed in the hole and irradiated for each dose value required.

Five dose points are used per decade of dose. The dosimeters are analyzed and the calibration

response functions are determined as described in 5.3.

5.2.2.2 Unirradiated alanine dosimeters from the calibrated batch are used to monitor the dose

received by customer's dosimeters of various types such as Red Perspex, eerie cerous ampoules,

and dichromate ampoules. Three alanine pellets are placed in a polystyrene cylinder the same

size as the liquid dosimeter ampoule; the cylinder is placed in the center hole of the five-hole cup

shown in Fig. 1 and the customer's dosimeter ampoules are placed the outer five holes. The

assembly is irradiated to the required dose and the QC alanine dosimeters are analyzed according

to the procedures given in 5.3. The indicated dose values are compared with the target dose. If

the results are within the specified control limits (discussed in Section 7) then the irradiation is considered satisfactory. If the results are outside the control limits then the irradiation must be

investigated and appropriate corrective action taken. All QC results are recorded as part of the

calibration report and test folder.

5.3 Dosimeter Analysis Procedures

5.3.1 Radiochromic Film Analysis

5.3.1.1 Analysis (read out) of the radiochromic thin film dosimeters is done with a Gary model

3e spectrophotometer. Read out of each film is performed both before and after irradiation. The

read out procedures is as follows:

(a) Turn on power to control computer (Compac 386), go to Windows, run the Gary

software program (indicated by the Gary 13e icon) in a DOS window so that the DOS

Editor can be used in another window.

(b) Turn on power to Gary 3e spectrophotometer; let it warm up for at least one hour.

The Gary software starts diagnostic checks of the instrument by turning on the UV lamp

and scanning for the emission line 656.1 nm to calibrate the wavelength scale.

(c) The computer program boots up with operating parameters set up to read

8
FWT-60-00 radiochromic films. The parameters are shown in Table 2.

(d) Run a baseline to zero the instrument over the wavelength range 610 nm to 500 nm

with empty film holders in both reference (rear) and sample (front) light beams in the

sample compartment. The split holder shown in Fig. 3 is used to hold a FWT-60-00 film in

the sample light beam. A solid (non-split) version of the holder masks the reference beam

exactly the same as the split holder masks the sample beam.

Handle films with tweezers at the comers to avoid scratching near the center where the

light beam passes through. Number each

film in a corner with a small code number

using a fine permanent marker pen.

(f) Place the film in the split holder and

place the holder in the sample holder in the

spectrophotometer sample compartment.

Read the absorbance values at 605 nm and

510 nm.

(g) The absorbance data is acquired by means of a software program called WLPG.ADL.

This program is listed in Appendix 1 . To start this program, go to the Calculator page in the

Gary software. Start the WLPG program. This initiates Reports Display . As each film is read out in turn a data set is generated on the monitor screen as shown in the example in

Table 3.

(h) Upon exiting the WLPG.ADL program, it takes you to the DOS Editor. This pulls up

the current.rep file where the film absorbance data colected above is stored. Edit the data to delete the colunm text headers to leave numerical data only. Save as new file name, e.g., test folder number (hd9616), with an extension of .Al for pre-irradiation data, or an

extension of . A2 for post-irradiation data.

5.3.1 .2 The thickness of each FWT-60-00 film is measured in order to be able to normalize the

absorbance data to unit thickness. The thickness is measured as follows:

(a) Power to the Mitutoyo electronic thickness gauge (bottom unit) should be left on at

all times to minimize warmup drift. If started from power-off mode, allow at least one hour

warmup time. Turn on power to Mitutoyo Mulfiplexer (top unit) and set all switches to up

position. The gauge unit data is routed through the Multiplexer unit into the serial port on

the Compac 386 control computer as an ASCII string. The gauge unit display should read in

"mm" with a resolution of 0.1 \im (the resolution may be changed with a rotary switch on

the rear of the gauge unit).

(e)

Film Plane

Opening for Light Beam .Q,

Figure 3 - Radiochromic Film Holder

9
the rear of the gauge unit).

(b) The film thickness is measured with a cartridge head connected to the electronic

gauge unit; the head is mounted on a rigid gauge stand. The cartridge plunger tip is raised

and lowered onto the stand anvil by a hand-operated vacuum plunger attached to the

cartridge. To check the "zero" of the unit initially, lift the tip, place a piece of clean lens

paper under it, lowering the tip onto the anvil, then pulling the lens paper out. This removes

any dirt on the tip or anvil. Raise and lower the tip several times and reset the zero if

necessary with the control knobs on the front of the gauge unit. Repeat this procedure until a stable zero reading is obtained.

Table 2

Gary 3e Spectrophotometer Parameters

; Method Name Routine FWT-60-00

Photometric Mode Absorbance

Ordinate (Y) Min. / Max. 0.0000 / 4.0000

Abscissa (X) Min. / Max. 500.00/610.00

Spectral Bandwidth (nm) 4.0

Signal Averaging Time (s) 1.000

Data Interval (s) 1.000

Wavelength Scan Rate (nm/min) 60.000

Lamps On Visible

Baseline Correction On

Auto Scaling Yes

Auto Store Data No

Auto Store Report Yes

Table 3

Sample Data from Film Readout

Film ID

1

A @ 605 nm

2.8137

A ({^ 5 1 0 nm

0.4158

2 1.6882 0.2494

3 0.8441 0.1247

10
(c) Go into the Film Thickness program from the icon in the main Windows display.

This is a DOS Basic program called thread.bas : see the print out of the program in

Appendix 2. This program provides prompts on the monitor to step the operator through

the thickness measurement process to ensure reliable data. The process is as follows:

(1) A prompt asks for the starting film number;

(2) Take a "zero" reading with no film. If a stable zero is indicated, then a film

reading is requested;

(3) Raise the cartridge tip and place the first film on the anvil under the tip. The

program reads the thickness once a second. If the same reading is recorded on

consecutive reading, the program accepts the data, beeps to alert the operator, and

outputs the data to the printer. The program then advances the film number

counter and waits to read zero again. The program runs in background while the

absorbance measurements are being made with the spectrophotometer. Thus, the

thickness of a given film can be measured immediately after the absorbance is measured.

(4) When all films thicknesses are measured, the program prompts the operator to hit

the space bar and four options are given:

Save file and quit;

Reset film counter;

Continue;

Quit.

The usual choice is to save the file and quit. The file is saved temporarily In

"thread.t". The program asks for another file name (e.g., test.t). After saving the

file, the program checks to see if it is a duplicate. Then the program asks if the

operator wants to check the file; if "Yes," then it goes to the DOS Editor.

(5) After exiting the Film Thickness program, the computer returns to DOS Basic.

5.3. 1.3 The radiochromic film analysis data is reduced by importing the absorbance and

thicknesses data into a Quattro Pro spreadsheet. The response is calculated by the formula (A2-

Al)/T. A software program called TableCurve is used to calculate dose. Once the calibration

plot is fitted, the doses for can be determined by using the program option [Evaluate] , selecting

[ X = Root at Y ], and putting in the values of the response (Y). An example of that calibration

data and the fitted response curve is shown in Fig. 4. The fitted polynomial equation is y = a +

bx + cx^ + dx^ the fitted parameters are: a= 0.6290; b= 1.7013; c= -0.0100; d= 2.6729.

11
y=a+bx+cx^2+dx'^3

Eq#=2040 r2=0.99968938

80 -r

60 -

^40-

<^

20 -

0 -| i

1

1

1 i

1 i1

i 1 i 1

1

0 10 20 30 40 50 60 70 Dose, kGy

*. Y Actual —^ Y Predicted

5.3.2 Alanine Dosimeter Analysis

5.3.2.1 Analysis (read out) of the alanine dosimeter pellets is done with a Bruker model ESC 106

electron paramagnetic resonance (EPR) spectrometer. The spectrometer is used with a model

TM9222 microwave resonant cavity (Fig. 5). The procedure consists of three stages: preparation;

signal measurements; and data analysis.

5.3.2.2 Preparation

(a) Choose an optimal time for the measurements (3). This depends on the dose range:

1 0 Gy to 1 00 Gy 1 2 or more hours after irradiation

0. 1 kGy to 25 kGy 48 h to 100 h after irradiation

25 kGy to 1 00 kGy 48 h to 72 h after irradiation

Calibration and test pellets must be irradiated approximately simultaneously.

(b) After irradiation, each alanine pellet is marked on top with an identification number with a permanent ink pen. The mass of each pellet is measured before EPR analysis with a Denver

Instrument Company model 160 electronic balance to the nearest 0.1 mg. Program "a 160" on COMPAQ386/25e can be used for automatic input of the masses into the computer.

12
The process is as follows: Put in a plastic sample tray and tare the balance. Go into the A160

program from the icon in the main Windows display. This is a DOS Basic program called

al60.bas: see the print out of the program in Appendix 3

.

(1) A prompt asks for the starting pellet number; then it generates a file name to store the data and waits for the user to accept the name.

(2) The program looks for a "zero" reading. If a stable zero is indicated, then the

program begins reading the sample mass.

(3) The program makes continuous mass measurements and increments a seconds

counter. If the mass value drifts, the counter is reset to zero. If the value remains

unchanged for ten seconds, the value is accepted. The program beeps twice.

(4) The program then waits for a stable zero reading to indicate the sample is being

changed and the zero has not drifted. If the balance goes to zero and remains for

two seconds, the program will beep once to indicate it ready to read the next

sample. If the balance settles somewhere beyond zero, the user must press tare.

(5) When all pellets are measured, the program prompts the operator to hit any key.

Two choices are given: Q to quit or B to stay in basic. The usual choice is Q.

(c) Log in in the EPR Logbook. This records details of the user, time of use, sample, etc.

(d) Turn on cooling water to the spectrometer magnet using the blue flat control valve on the

pipeline behind the magnet. No other controls of the water system should be touched.

Adjust the water pressure to about 40 psi, if required.

(e) Turn on the magnet power. The switch is on the bottom front of the magnet. Turn on the

control console red power switch located on the top right of the electronics rack behind the

console glass door.

(f) On the prompt of the control computer, put in User Profile name. This entails specifying the

directory where acquired data is stored or creating such a directory if it does not exist. For

example, the directory could be called "ha/alanine." The User Profile should also include

the appropriate calibration file. If the operator does not specify a predefined user profile, the

spectrometer must be calibrated manually using Calibration (c) option in the main menu;

the name of the calibration file selected from the list must match the specification on the

front wall of the cavity.

(g) If a sample tube is not in the microwave cavity, place it there. Make sure the correct size

Tefion collets (see Fig. 5) are used to mount the chosen sample tube (normally, a collet of a smaller inner diameter is needed to support the tube from beneath). The tube must be held

13
firmly enough to preclude any swinging, yet

allow its rotation. It must be in the lowest

attainable position in the cavity with its horizontal surface in contact with the lower

collet.

Place one of the alanine pellets into the

sample tube in the cavity. Pellets are inserted

into and removed from the sample tube with

a vacuum pickup tool.

Press the F3 function key, then the right cursor arrow in the lower row of the cursor key panel to switch to the Tune mode. If

there is no dip observable in the display,

adjust the frequency to center the dip by

means of knob 1 on the knob control.

(j) Press the Page-Up key to initiate the auto-tune procedure. After the systems returns to the

"Operate" mode, decrease the microwave attenuation to 7 dB by pressing the right of the

two 'Home' keys (the attenuation value is displayed in the second line of the right half of

the upper window). Then, press the key to start the fme-tune procedure. Leave the

instrument working for at least 30 mins.

(k) Press F3 to activate the main menu and load an appropriate automation routine, such as "replmeas.cmd" by using "Acquisition (A)" / "Automation Editor (L)" option.

(1) Load an appropriate parameter or spectrum file by pressing F (File) and then J (Directory of

Parameter Files) or I (Directory of Spectrum Files). Directory hO:/alanine/templates

contains a number of files with predefined parameters for Bruker and NIST pellets

irradiated to various doses.

(m) Create an Excel spreadsheet for the measurement data by copying and adjusting the file "template.xls". Copy the measured masses of pellets into it either manually or by opening

the file created by program "al60" as a new Excel worksheet (comma delimited).

5.3.2.3 Signal Measurements

(a) Put a pellet into the sample tube in the cavity by means of the vacuum pickup tool.

Figure 5 - Bruker Microwave Cavity

14
(b) If the pellet has been irradiated to a new dose, adjust the receiver gain. On a page

containing the chosen set of parameters (transferred from a previous recording or read from

a template file), make a trial spectrum acquisition (Acquisition (A), Signal Channel (C))

and, if necessary, change the gain using menu option Parameters (P) / Signal Channel

Parameters (C). The optimal receiver gain provides a signal that does not exceed the

receiver gain gauge and, at the same time, provides 5-digit readings of the derivative

minimum and maximum values. In some low-dose measurements, the 5-digit result is not

practical. In that case just get as much signal as possible without exceeding the

receiver gain gauge.

(c) Select a page with appropriate parameters and start the automation routine using menu

option Acquisition (A) / Execute automation routine (E). It will automatically record the

spectra of both alanine and ruby, and then transfer the parameter of the alanine spectrum to the next available page.

(d) Rotate the sample tube by 90 degrees and start the routine again.

(e) Measure the signal intensities on the last four pages using menu option Data Handling (D) / Pick Picking (D) / Find Extremal Values (M). In each case, transfer the absolute values of

the readings "Min" and "Max" in the bottom of the screen to the spreadsheet.

(f) Repeat this section until all samples are measured.

53.2.4 Data Processing

(a) In the spreadsheet, calculate the alanine response (S) using the formula: S= averaged

alanine signal amplitude / averaged ruby signal amplitude / receiver gain / pellet mass. Where appropriate, make response adjustments to the difference between the temperatures

during irradiation of calibration and test pellets. The response increases with temperature at a rate of 0.15%/deg C.

(b) Dose interpretation of the response of each alanine dosimeter is by means of the calibration

response functions discussed in 5.2.2.1. The Low Dose range (10 Gy to 2 kGy) response

function is linear. The fitted Low Dose least squares curve for a typical alanine batch is shovm in Fig. 6. The fitted linear equation is y = a + bx; the fitted parameters in this case

are: a = 1.0448; and b = 0.17522. The High Dose range response function is nonlinear; a

fitted curve is shown in Fig. 7. The fitted equation is: S = a 1 -exp

where S = the normalized EPR signal ; D = absorbed dose, in kGy;

and typical fitted parameters are: a = 10.3943; b = 72. 2446; c = 0.243093.

15
400

100-

0 0.5 1 1.5 2 Dose (kGy)

Figure 6 - Alanine Batch 9b Low Dose Calibration Curve

10

0 50 100 150 Dose (kGy)

Figure 7 - Alanine Batch 9b High Dose Calibration Curve

A software program called TableCurve is used to fit the data sets for both the Low Dose

and High Dose ranges. Once the calibration plot is fitted, the doses for test pellets can be

determined by using the program option [Evaluate] , selecting [ X = Root at Y ], and

putting in the values of the normalized signals (Y).

If doses in a material other than water is desired, multiply the determined doses by /^e„ ratios (material/water) weighted over the calibration source energy spectrum.

16
5.4 Handling ofCalibration Requests

5.4.1 The process for calibration of customer-supplied dosimeters is shown schematically in

the flowcharts in Figs. 8a and 8b. These show the various administrative levels involved and the

documents and actions required to complete a calibration. The steps in the process (with step

numbers keyed to those in the flowchart) are as follows:

(1) The customer request a calibration or information;

(2) A fee schedule is supplied to the customer (an example is shown in Appendix 4);

Irradiate Page 1

Customer

CP/OMS

Division

Control Log

Documents

Dosimeters; Actions

Shipping &

Receiving

( Start ) ^hr^ 1 a 1 Customer P.O. Request Prepared

Fee Schedule

Supplied 0 P.O. Received

Test Folder Prepared

[fl-p.o. Logged

Folder to Division

Return to Customer

5r

Dosimeters

Inspected

Dosimeters

Received

Request New

Dosimeters

OK

Log

Updated

Q.C.;

Irradiation Data Collected

Irradiate Dosimeters

Dosimeters Unpacked

& ID Assigned

mData xAnalyzed/

OK

and

Not

Consistent

31

Resolve

Figure 8a - Procedures for Calibration Irradiations of Customer-Supplied Dosimeters

(3) The customer prepares a purchase order and returns it;

17
(4) Upon receipt of the hard copy of the purchase order, it is logged in the Control Log

(5) And a copy sent to the Calibration Program/Office of Measurement Services (CP/OMS)

for that office to generate a Test Folder (11);

(6) Customer's dosimeters are received in the Division; note that no calibration work is done past this step until a hard copy of the purchase order is in hand;

(7) The dosimeters are unpacked and appropriately tagged for identification throughout the

calibration process;

(8) The dosimeters are visually inspected for damage or flaws;

(9) If the dosimeters are flawed in any way that would prevent proper calibration they are returned to the customer with an explanation;

(10) The customer is requested to supply new dosimeters; if the customer complies, the

dosimeters are processed from step (6) on again;

(11) The Test Folder generated by the CP/OMS office is sent to the Division;

(12) The Test Folder is received by the Division;

(13) If the dosimeters are considered to be satisfactory in step (8), then they are irradiated to the requested doses;

(14) The Control Log is updated with the Test Folder information and the irradiation data

(i.e., irradiation source used, date and time of irradiation, dosimeter(s) ID, temperature during

irradiation, dose rate, etc.);

(15) The NIST quality control dosimeters irradiated along with the customer's dosimeters are analyzed and that data and the irradiation data are recorded;

(16) The QC and irradiation data are examined and analyzed;

(17) If the QC data is not consistent with the irradiation data (i.e., the indicated dose is different from the expected dose), then the problem must be resolved;

(18) If the QC data is satisfactory (i.e., within control dose limits) then it is recorded in the

Control Log;

(19) The data is used to prepare the Calibration Report;

18
(20) The customer's dosimeters are ready to be shipped baclc;

(21) The dosimeters are packed appropriately;

(22) The dosimeters are shipped back to the customer by the requested method; this

information is recorded in the Control Log;

(23) The dosimeters are received by the customer;

Irradiate Page 2

Customer

CP/OMS

Division

Dosimeters Returned

From

Control ^ Q.C.Data

Log Logged

Documents

Dosimeters; Actions

Shipping &

Receiving

Prepare Report

Dosimeters Ready to Ship

[ID-Dosimeters Packed

mCalibration Report to Customer

24 Calibration Technician Review

Dosimeters Shipped

Division Review &

Approval

Supervisor Review

Calculate Fee

Bill to Customer

Return

Test Folder

' Payment by Customer

Log& I Calibration

| Folder Closed

Complete

Test Folder

Documents

Filed

End

Figure 8b - Procedures for Calibration Irradiations of Customer-Supplied Dosimeters

(24) The completed Calibration Report is reviewed by the Calibration Technician (i.e., the

person that did the calibrations);

(25) The Group Leader reviews the Calibration Report and if approved;

19
(26) The Calibration Report is reviewed by the Division Chief and if approved;

(27) The Calibration Report is sent to the customer;

(28) The calibration fees are calculated by the Calibration Technician;

(29) The Test Folder is completed with the calibration fees;

(30) The Test Folder is returned to the CP/OMS office;

(31) The Control Log is updated with the QC data from step (16) and the date of completion

of the Test Folder;

(32) The CP/OMS office sends a bill to the customer;

(33) The customer makes payment to the CP/OMS office;

(34) All documents within the Division are filed; the calibration process is completed.

20
5.4.2 The process for the supply of NIST transfer dosimeters to a customer for irradiation in

the customer's in-house radiation facility is shown schematically in Fig. 9a and 9b. The steps in generating the paper work (i.e., P.O., Test Folder, Control Log updates, etc.) are essentially the

same as for the process when customer-supplied dosimeters are calibrated. The real difference is that NIST-supplied transfer standard dosimeters are sent to the customer. These dosimeters may

Transfer Page I

Customer

CP/OMS

Division

Control Log

Documents

Dosimeters; Actions

Shipping &

Receiving

( Start )

T]TCustomer J P-o. 1 Request \ Prepared

Fee Schedule

Supplied

P.O. Received

Test Folder Prepared

P.O. Logged

older to Division

S^TFansfer

Dosimeters Packed

Transfer

Dosimeters Shipped

Customer

Irradiation of Dosimeters

Log

Updated

17

OK

Data

Collected Data

Analyzed

Analyze

Dosimeters

Irradiated Dosimeters Returned

Not

Consistent

Resolve

Figure 9a - Procedures for NIST-Supplied Transfer Dosimeters for Customer Irradiation

be alanine pellets or radiochromic films, as requested by the customer. However, it is generally

recommended that alanine pellets be used because of the wider dose range, lack of known dose

rate effect, and better precision and stability of that dosimetry system. The steps in the process of

using transfer dosimeters will not be listed in the detail given in 5.4.1 for the irradiation of

customer dosimeters because of the redundancy in many steps. Only those areas where the

procedures are different will be discussed.

(1) to (5) Steps are the same as in 5.4.1;

21
Cavity for Pellets

Figure 1 0 - Polystyrene Alanine Capsule

for Co^° Gamma Irradiation

(6) Alanine pellets are supplied in an appropriate

package depending on whether

intended for Co^° gamma-ray

irradiation or electron-beam

irradiation. For Co^° gammas, the

capsule shown in Fig. 10 is supplied; for electron beams, the

flat holder shown in Fig. 1 1 is supplied. For radiochromic films,

the slab holder shown in Fig. 2 is supplied for either gamma or

electron beam irradiation.

(7) Packaged transfer dosimeters, including control dosimeters, are shipped to the

customer. Instructions are included on suggested dosimeter handling techniques and

information on irradiation conditions required for correct data interpretation (see an example in Appendix 5).

Cavities for Pellets

Figure 1 1 - Polystyrene Alanine Pellet

Holder for Electron Beam Irradiations

(8) to (9) Same as in 5.4.1;

( 1 0) Irradiation of dosimeters by customer

with in-house source;

(11) Irradiated dosimeters, along with

unirradiated controls, are returned to NIST;

(12) Dosimeters are analyzed;

(13) Control Log is updated from both test folder and data from irradiation of

dosimeters;

(14) Dosimeter readout data is collected;

(15) Data analysis is performed;

(16) If data is not consistent, i.e., indicated dose values from dosimeters are different from

expected doses reported from the customer, than the results must be resolved. This may

22
Transfer Page 2

Customer

CP/OMS

Division

From 1

7

Control r7^T_J~^Da'a

Log ^ T ^ Logged

Documents

Dosimeters; Actions

Shipping &

Receiving

Prepare Report

I 19^Calibration -H Technician Review

Division Review &

Approval

Calibration Report to Customer

Bill to Customer

Return

Test Folder

m] ^

1 23^^*^ , M ^

, TSupervlsor Calculate Complete Review Fee Test Folder

Payment by Customer

Log&

Calibration Folder Closed

Documents

Filed

End

Figure 9b - Procedures for NIST-Supplied Transfer Dosimeters for Customer Irradiation

require another set of dosimeters being irradiated by the customer;

(17) to (29) All subsequent steps are the same as in 5.4.1.

5 . 5 Calibration Reports

5.5.1 The requirements for content and format of calibration reports to be sent to customers

are covered in NIST SP250-44. Examples of both types, i.e., for NIST calibration irradiation of

customer-supplied dosimeters and NIST transfer dosimeters supplied for customer irradiation, are shown in Appendix 6.

23
6. Measurement Uncertainty

6.1 To be meaningful, a measurement shall be accompanied by an estimate of uncertainty.

Components of uncertainty shall be identified as belonging to one of two groups:

a) components based on the statistical analysis of a series of observations or

b) components based on other methods of analyses.

Additional information is given in ASTM Guide E 1 707 and references 4 and 5, where these

components are referred to as Type A and Type B, respectively. In reporting uncertainty, other

classifications such as precision and bias may be useful.

NOTE 3 - The identification of Type A and Type B uncertainties in this document uses the

methodology adopted in 1993 by the International Organization for Standardization (ISO)

for estimating uncertainty. This is different from the way that uncertainty has been

traditionally expressed in terms of "precision" and "bias," where precision is a measure of

the extent to which replicate measurements made under specific conditions are in

agreement, and bias is a systematic error. The purpose of using the method of expressing

uncertainties as Type A and Type B recommended in the ISO Guide to the Expression of

Uncertainty in Measurement (5) is to promote an understanding of how uncertainty

statements are arrived at and to provide a basis for the international comparison of

measurement results.

NOTE 4 - ASTM Guide E 1707 defines possible sources of error in dosimetry performed in

radiation processing facilities and offers procedures for estimating the resulting magnitude

of the uncertainties in the measurement results. Basic concepts of measurement, estimate of

the measured value of a quantity, "true" value, error and uncertainty are defined and

discussed. Components of uncertainty are discussed and methods are given for evaluating

and estimating their values. Their contributions to the standard uncertainty in the reported

values of absorbed dose are considered and methods are given for calculating the combined

standard uncertainty and an estimate of overall (expanded) uncertainty.

6.2 The components of uncertainty involved in a measurement shall be estimated or determined. The overall uncertainty in the measurement may be estimated from a combination of

these components, and the procedure for combining these components shall be specifically stated or referenced in all results.

6.3 The relative standard uncertainties associated with measurement of absorbed dose with

alanine dosimeters from any radiation source are shown in Table 4. The components are assumed

to be uncorrected and are combined in quadrature, i.e., by taking the square root of the sum of

the squares. The combined relative standard uncertainty is multiplied by a coverage factor of two

which corresponds approximately to a 95% confidence level.

24
Table 4

Uncertainties of Alanine Absorbed Dose Measurements

Source of Uncertainty Type A (%) TypeB(%)

Interspecimen scatter 0.71 —

Reproducibility and repeatability 0.08 —

System drift 0.20

Pellet mass determination 0.10

Combined separately 0.71 0.22

Combined relative standard uncertainty 0.75

Relative expanded uncertainty (combined x 2) 1.5

6.4 The uncertainties associated with measurement of absorbed dose with radiochromic film

dosimeters are shown in Table 5.

Table 5

Uncertainties of Radiochromic Film Absorbed Dose Measurements

Source of Uncertainty TypeA(%) Type B (%)

Interspecimen scatter 1.00

Repeatability and reproducibility 0.10

Spectrophotometer zero drift 0.20

Thickness measurement 0.40

Combined separately 1.00 0.45

Combined relative standard uncertainty 1.10

Relative expanded uncertainty (combined x 2) 2.2

6.5 The relative uncertainties in absorbed dose values for irradiations of any type of dosimeters

in the standard geometries in both Gammacells and the Pool Source is shown in Table 6.

25
Table 6

Uncertainties in Absorbed Dose (in water) Values

for Irradiations in the Gammacells or the Pool Source

Source of Uncertainty Type A (%) Type B (%)

Calorimeter measurement of Vertical Beam source 0.16 0.32

Scaling procedure -- 0.35

Source ratio measurement data 0.35

Source decay, half life — 0.01

Irradiation timing 0.17

Geometry correction factor 0.61

Irradiation temperature correction 0.02

Combined separately 0.74 0.47

Combined relative standard uncertainty 0.88

Relative expanded uncertainty (combined x 2) 1.8

To convert the dose values from dose in water to dose in silicon requires the use of ratios of mass

energy absorption coefficients and contributes an additional Type B component of 0.30% to those in Table 6. Thus the combined separately Type B value increases to 0.55%, the total

combined value increases to 0.93%, and the total combined x 2 increases to 1 .9%.

6.6 The relative uncertainties in the use of alanine transfer standard dosimeters in

measurements of absorbed dose is shown in Table 7.

26
Table 7

Uncertainties in Absorbed Dose (in water) Values for Alanine Transi"er Dosimeters

Source of Uncertainty Type A (%) Type B (%)

Alanine single-hole cup dose rate 0.36 0.47

Alanine dose measurement (from Table 4) 0.71 0.22

Irradiation temperature correction 0.10

Elapsed time between irradiation and analysis 0.25

Dose value derived from calibration curve 0.50

Combined separately 0.80 0.77

Combined relative standard uncertainty 1.1

Relative expanded uncertainty (combined x 2) 2.2

The Type A relative uncertainty shown for the single-hole cup dose rate alanine response is smaller than that shown in Table 6 because the dosimeters are calibrated in that fixed geometry

for GC-232 only.

6.7 The relative uncertainties associated with the use of radiochromic film transfer standard

dosimeters in shown in Table 8.

Table 8

Uncertainties in Absorbed Dose (in water) Values for

Radiochromic Film Transfer Dosimeters

Source of Uncertainty Type A (%) Type B (%)

Film block dose rate 0.40 0.47

Film dose measurement (from Table 5) 1.0 0.45

Energy spectra correction 0.50

Elapsed time between irradiation and analysis 0.50

Dose value derived from calibration curve 1.80

Combined separately 1.1 2.0

Combined relative standard uncertainty 2.3

Relative expanded uncertainty (combined x 2) 4.6

27
As was the case for the alanine transfer dosimeters, the Type A uncertainty for the film block

dose rate is smaller than that shown in Table 6 for the same reason: the calibration was

performed in a fixed geometry in the GC-232 source only.

6.8 The uncertainty values provided may change. It shall be the responsibility of the calibration

laboratory to notify each affected client of any such changes, and the corrected values of all affected quantities previously reported to that client.

7. Control Limits

7.1 The control limits referred to in Section 5 on quality control are derived from the

uncertainties associated with each type of dosimeter employed. For the alanine dosimeter system,

the combined relative standard uncertainty from Table 4 is 0.61%. For a safety factor of three, the

control limits would be 3 x 0.61 or ±1.83%. Similarly, for the radiochromic film dosimeter

system, the combined relative standard uncertainty from Table 5 is 1.1 0% and the control limits

would be 3 X 1.10 or ±3.30%.

7.2 Designate the target absorbed dose (discussed in Section 5), calculated from the irradiator

dose rate and irradiation time, as Dj. Then the dose indicated by the alanine quality control

dosimeters should be within the control limits: Dj ±1.83%. Similarly, the dose indicated by the

radiochromic film quality control dosimeters should be within Dj ±3.30%. If the doses indicated

by the quality control dosimeters are within the indicated limits than the quality control process is said to be in a state of control. If the indicated doses are outside the control limits, then the

quality control process is "out of control" and the process must be investigated and appropriate

remedial action taken.

8. Keywords - Absorbed dose; calibration laboratory; dosimeter; dosimetry system; electron

beam; gamma ray; ionizing radiation; radiation processing; reference standard dosimeter.

9. References

1. Inn, K.G.W., Coursey, B.M., Eisenhower, E.H., Walker, M.D., Humphreys, J.C., Heaton,

H.T., Duvall, K.C., "The role of the Office of Radiation Measurement in quality assurance," The

Science ofthe Total Environment, 130/131, Elsevier Science Publishers B.V., Amsterdam, 1993,

pp. 497-507.

2. McLaughlin, W.L., "Reference dosimetry and measurement quality assurance," Rad. Phys.

Chem. 40, 1989, pp. 945-951.

3. Nagy,V.Yu., Desrosiers,M.F., "Complex Time Dependence of the EPR Signal of Irradiated

L-a-Alanine," Appl. Radiat. Isot. 47(8), 1996, pp. 789-793.

28
4. Taylor, B.N. and Kuyatt, C.E., "Guidelines for Evaluating and Expressing the Uncertainty of

NIST Measurement Results," NIST Technical Note 1297, Natl. Inst. Stand.Tech., Gaithersburg,

MD, 1994.

5. "Guide to the Expression of Uncertainty in Measurement," International Organization for

Standardization, 1993, ISBN 92-67-10188-91

^Available from ISO Central Secretariat, Case Postale 56, CH-121 1 Geneva 20,

Switzerland.

29
Appendix 1

WLPG.ADL program:

{This program can be actived from either the User_resuh line or the }

{Calculator page. It will measure the nominated number of samples at 5 10 }

{and 605 nm. These wavelengths can be easily changed. The user will then }

dim A510[1000] A605[1000]

define readit

print("please wait, measuring sample",n, "...") A510[N] = read(510)

A605[N] = read(605)

TABLEDATA(n,A605[N],A510[N])

n=n+l

enddef

define finchek

print ("Are you ready to end session and exit?")

q$=input

if (q$="y") or (q$="Y") then finis=l

enddef

define recount

print("What is the new film number? ")

n^^input

enddef

define wlpg

STARTPRINT

SET(AUT0P,1)

print("Enter user name ")

name$=input

lprint("Operator: ",name$)

print("Enter your comment ")

comment$=input

lprint(" Comment: ",comment$)

IprintC'Date: ",recall_str(recall(5,35),0))

{ Author: Jim Puhl

{ Revised 4/10/97

}

}

30
print("What is the starting film number? ")

bnum=input

n=bnum

page=4

goto_page

TABLEFMT("DDZ","Z.DDDD","Z.DDDD")

TABLEHDRC FILM ID "," 605 nm 510 nm ") finis=0

do while fmis=0

statusstr("l=read 2=adjust counter 3=exit")

print ("ready for sample",n,", please choose 1-3 from the choices at the top:")

q=input

case q

1 :readit

2:recount

3:finchek

end

end

SET(AUTOP,0)

prog$="c:\command.com /c edit c:\varian\caryl3e\current.rep"

spawn_prog

enddef

31
Appendix 2

thread.bas (DOS Basic) program:

10 COLOR 15,1:CLS:DIM DA(IOOO)

20 PRINT" THREAD.BAS - DOWNLOAD THICKNESS DATA FROM MULTIPLEXER

5/1 3/96 jmp"

30XON$-CHR$(17) 'CTRL-Q

40XOFF$=CHR$(19) 'CTRL-S

50 INPUT "ENTER STARTING FILM NUMBER: ",SNUM:LOCATE 3,1 :PRINT " "; 60 F$="THREAD.T":OPEN "0",2,F$:PRINT "DATA WILL BE WRITTEN TEMPORARILY

TO ";F$

70 LOCATE 4,1 :J=0:L=4:C=1 :INPUT"Press ENTER to start the transmission. ",A$

80 LOCATE 23,1 :PRINT"Press <SPACEWAR> to stop the transmission " 90 OPEN "COM1 : 1 200,N,8, 1 " AS # 1

:

1 00 SNUM$=STR$(SNUM):SNUM$=SPACE$(4-LEN(SNUM$))+SNUM$

1 10 LOCATE L,C:PRINT"WAITING FOR ZERO READING...

120 C0$="1":PRINT#1,C0$:INPUT#1,DA$:I=I+1

130 DA$=MID$(DA$,4,9):DA=VAL(DA$):CLOSE 1 140 IF DA> .001 THEN GOTO 90 ELSE SOUND 2000,1 :SOUND 1000,1

150DA(1)=1:DA(2)-2:I=2

160 WHILE DA(I)oDA(I-l):OPEN "COM1:1200,N,8,1" AS #1

170 LOCATE L,C:PRINT SPC(27):LOCATE L,C:PRINT"READING ";SNUM$;"..."

180 T1=TIMER :T2=T1+1 :WHILE T2>=TIMER:PRINT "";:WEND:' wait one second

190 A$=INKEY$:IF A$o"" THEN CLOSE LGOTO 300

200 C0$=" 1 ":PRINT#1 ,C0$:INPUT#1 ,DA$:I=I+1

210DA$=MID$(DA$,4,9):DA(I)=VAL(DA$):TH$=RIGHT$(DA$,6)

220 LOCATE L,C:PRINT SNUM$;" ";TH$:CLOSE 1 :WEND

230 IF DA(I)< .01 THEN GOTO 150

240 IF L=19 THEN C=25 :L=4

250 IF L=37 THEN C=50 : L=4

260 0$=SNUM$+" = "+TH$+" mm " 270 SOUND 800,1 :LOCATE L,C:PRINT 0$:PRINT #2,SNUM$,TH$

280 LPRINT 0$:L=L+1 :SNUM=SNUM+1 :GOTO 90

290'

300 'SPACEWAR ROUTINE

310 LOCATE 23,1:PRINT SPACE$(75):LOCATE 22, LPRINT "1)";

320 INPUT " save file and quit 2) reset counter 3) continue 4) quit ";Q

330 LOCATE 22,1:PRINT SPACE$(75)

340 IF Q=3 THEN LOCATE 22, 1 :PRINT SPACE$(75):GOTO 80

350 IF Q=2 THEN LOCATE 22,1:INPUT "enter new counter number:";SNUM:GOTO 80

360 IF Q=l THEN CLOSE:GOTO 380

32
370 IF Qo 4 THEN GOTO 300 ELSE STOP

380 ON ERROR GOTO 410:INPUT "Filename";N$ : NAME N$ AS N$

390'

400 ' ERROR TRAP

410 IF ERR=58 THEN EX$="y":RESUME 430

420 IF ERR=53 THEN EX$-"N":RESUME 430

430 ON ERROR GOTO 0:IF EX$ o"y" THEN T$="0":GOTO 460

440 INPUT "FILE ALREADY EXISTS - A to append ,0 to overwrite or R to rename"

450 ON ERROR GOTO 0

460 IF T$="R" OR T$="r" THEN GOTO 380

470 IF T$="0" OR T$="o" THEN SHELL "DEL "+N$:SHELL "REN "+F$+" "+N$

480 IF T$="A" OR T$="a" THEN SHELL "COPY "+N$+" + "+F$

490 INPUT "WOULD YOU LIKE TO CHECK IT? (Y ORN)";Z$:

500 IF Z$="y" OR Z$="Y" THEN GOTO 510 ELSE GOTO 520

510 SHELL "edit "+N$:

520 STOP

33
Appendix 3

al60.bas (DOS Basic) program:

10 GOSUB 560:COLOR 15,l:CLS:ON ERROR GOTO 210

20 'COLOR 15,1:CLS:G0SUB 510:

30 PRINT "file A160READ.BAS last update 3/3/97"

40 INPUT "ENTER STARTING PELLET NUMBER: ";SPN

50 PRINT:PRINT " DATA WILL BE STORED TO FILE: ";F$

60 PRINT"Press ENTER to start the transmission or Q to quit."

70 A$=INKEY$:IF A$="" THEN GOTO 70

80 IF A$="Q" OR A$="q" THEN STOP

90 OPEN "COMl :4800,N,8,2,RS,CD,DS,CS" AS #1

100 PN=SPN:WAYT=10:OPEN "0",2,F$:CL0SE 2

1 1 0 PRINT"Press any key to stop the transmission " 120 LOCATE 24,l:GOSUB 290:T0=TIMER

130 I$=ES[KEY$:IF I$<>"" THEN CLOSE LGOTO 520

140 IF TIMER-TO > WAYT THEN GOSUB 230

150 LINE INPUT#1,A$:

1 60 NUM=VAL(MID$(A$,3,LEN(A$)))

1 70 IF NUMoONUM THEN LOCATE 24, 1 :PRINT

PN,NUM,0;:ONUM=NUM:T0=TIMER:GOTO 200

180 LOCATE 24,1:PRINT PN,NUM,CINT(TIMER-TO);

190 OPEN "a",3,"al60all.dat":PRINT#3,PN,NUM,CINT(TIMER-T0),TIME$:CLOSE 3

200 GOTO 130

210 PRINT ERR:RESUME NEXT

220 GOTO 130

230 PN$=STR$(PN):PL=LEN(PN$)4 :NUM$=STR$(NUM):NUML=LEN(NUM$)-1

240 OL$=RIGHT$(PN$,PL)+CHR$(44)+RIGHT$(NUM$,NUML)

250 OPEN "A",2,F$:PRINT #2,OL$:CLOSE 2

260 OPEN "o",2,"A161.0UT":PRINT #2,0L$:CL0SE 2

270 BEEP:'FOR 1=100 TO 3200 STEP 100:SOUND I,.5:NEXT I 280 PN=PN+1 :PRINT:PRINT "PRESS ANY KEY TO STOP":T0=TIMER

290 PRINT "WAITING FOR ZERO"

300 LINE INPUT#1,A$:

310 I$=INKEY$:IF I$<>"" THEN CLOSE LGOTO 510

320 NUM=VAL(MID$(A$,3,LEN(A$)))

330 TO^TIMER

340 I$=INKEY$:IF I$o"" THEN GOTO 510

350 IF TIMER-TO > 2 THEN GOTO 420

360 LINE INPUT#1,A$:

370 NUM=VAL(MID$(A$,3,LEN(A$)))

34
380 IF NUMoO THEN LOCATE 24,1 :PRINT,NUM,0;:T0=TIMER:GOTO 340

390 LOCATE 24,1:PRINT ,NUM,CINT(TIMER-TO);

400 OPEN "a",3,"al 60all.dat" :PRINT#3,"zero",NUM,CINT(TIMER-T0),TIME$:CLOSE 3

410 GOTO 340

420 IF NUM o 0 THEN GOTO 300

430 PRINT:'FOR 1=2500 TO 100 STEP -100:SOUND I,.5:NEXT I 440 BEEP:BT=TIMER:WHILE TIMER<BT+.5:PRINT"";:WEND:BEEP

450 PRINT "WAITESIG FOR PELLET# ";PN

460 LINE INPUT#1,A$:

470 I$=INKEY$:IF I$<>"" THEN GOTO 510

480 NUM=VAL(MID$(A$,3,LEN(A$)))

490 IF NUM <.03 THEN GOTO 460

500 RETURN

510 PRINT:PRINT "PRESS Q TO QUIT OR B TO STAY IN BASIC"

520 A$=INKEY$:IF A$="" THEN GOTO 520

530 IF A$="Q" OR A$="q" THEN SYSTEM

540 IF A$<>"B" AND A$o"b" THEN GOTO 520

550 STOP

560'

570 ' filename subroutine

580

DTE$=DATE$:M$=LEFT$(DTE$,2):D$=MID$(DTE$,4,2):Y$=RIGHT$(DTE$,2):ANUM=0

590 DTE$=Y$+M$+D$

600 F$=DTE$+CHR$(65+ANUM)+".DAT"

610 ON ERROR GOTO 640: NAME F$ AS F$

620'

630 • ERROR TRAP

640 IF ERR=58 THEN EX$="y":RESUME 660

650 IF ERR=53 THEN EX$="N":RESUME 660

660 ON ERROR GOTO 0

670 IF EX$ o"y" THEN GOTO 710

680 ANUM=ANUM+1 :IF ANUM <=25 THEN GOTO 600

690 IF LEN(DTE$)=6 THEN DTE$=DTE$+"A" :ANUM=0:GOTO 600

700 DTE$=LEFT$(DTE$,6)+CHR$(ASC(RIGHT$(DTE$,1))+1):ANUM=0:GOTO 600

710 RETURN

720 RETURN

35
Appendix 4

Fee schedule supplied to the customer:

February 21, 1997

From: James Puhl

NIST High-Dose Calibration Service

Building 245, Room C229

Gaithersburg, MD 20899

Dear Calibration Customer: New fees for high-dose calibration services are in effect.

Schedule No. Calibration of Dosimeters Cost

49010C Irradiated with ^Co Gamma Rays $589

Calibration irradiations are available for customer-supplied dosimeters (such as solid radiochromic or liquid

chemical types) or test samples that are sent to NIST, where they are packaged appropriately to provide electron equilibrium conditions. They are irradiated in the NIST standard cobalt-60 calibration facility to specfic,

agreed-upon absorbed dose values in the nominal "high-dose" range of 10-10^ Gy. The dosimeters are then sent back to the customer for analysis and evaluation. Dosimeters should not exceed dimensions of 1 cm x 2 cm x 5 cm. A typical uncertainty value for irradiations of radiochromic film with the standard Gammacell 220-232 is +

1.8 at an approximate level of confidence of 95%.

Schedule No.

49020C

Set of Three Transfer Reference Standard Dosimeters

Alanine Pellets or Radiochromic Film

Cost

$1916

49030C Each Additional Dosimeter $391

NIST will provide transfer standards in the form of calibrated alanine or radiochromic film dosimeters packaged

in polystyrene. The sealed, packaged dosimeters are sent to the customer for irradiation to nominal agreed-upon

absorbed dose levels in a prescribed geometrical arrangement. The unopened, packaged dosimeters are then

returned to NIST to be read, evaluated and the results reported, thus providing calibration of the customer's

irradiator. The absorbed dose range that is suitable for use with the transfer dosimeters is 1 to 50 kOy in water. The absorbed dose rate should be greater than 30 Gy/min. A typical uncertainty value for alanine transfer standard calibrations is + 2.2% at an approximate level of confidence of 95%. A typical uncertainty value for radiochromic film transfer standard calibrations is + 4.6% at an approximate level of confidence of 95%.

Schedule No. Additional Services Cost

49040S Spectrophotometric reading of dosimeters, optical density at one

to five wavelengths (each dosimeter).

$141

49041S Spectrophotometric reading of dosimeters, ultraviolet and visible

spectrum scan (each dosimeter).

$367

49050S Special measurement services. At cost

Please send requests and/or dosimeters to me at the above address. Be sure to specify the

name and phone number of a technical contact. Domestic orders require a purchase order and

foreign orders require pre-payment. If you have any questions, please contact me. PHONE: 301-975-5581 FAX: 301-869-7682 E-MAIL: jpuhl@nist.gov

36
Appendix 5

Instructions to customer for handling of radiochromic film transfer dosimeters:

Guidelines for the use of NIST Transfer Dosimeters

1 . Please do not open the packages at any time; they provide a controlled environment for the

dosuneters.

2. Please provide average temperature for each dosimeter during the irradiation period.

3. Other irradiation data to include with the returning dosimeters

• Irradiation geometry (i.e., orientation, position, surrounding materials)

• Type of source (i.e., if gamma-ray source, identify the specific isotope)

• How you wish for us to identify your source in the Report of Calibration

• Date and time of irradiation

• Length of the irradiation period

• Nominal dose and dose rate

• Any other pertinent information

4. The nominal absorbed doses received should be within the range of 1 kGy to 30 kGy for

alanine and 5 kGy to 30 kGy for film.

5. Please irradiate and return the dosimeters to us within 60 days to minimize the uncertainty

in the final results. Please use the following address for return shipment:

NIST

ATTN: JAMES PUHL

BLDG. 245, ROOM C229

GAITHERSBURG, MD 20899

37
Appendix 6

Examples of calibration reports:

1 1 ^^^^^f^ United States Department of Commerce

I [^1^ I National Institute of Standards and Technology

I Gaithersburg, MD 20899 USA

REPORT OF CALIBRATION

OF: FWT-eO Batch 6F5 Radiochromic Film Dosimeters

FOR: Ed's Sterilizers

10 Gamma Avenue

MegaRad.TX 99817

ATTN: Cobalt Jones

REF: P0# 232

DESCRIPTION: Batch 6F5 film dosimeters were supplied by Ed's Sterilizers in pre-sealed foil pouches. The dosimeters were irradiated under

controlled conditions using gamma radiation from a calibrated

^°Co irradiator, the NIST Gammacell 220-232. During

irradiation the pouches were held between two polystyrene

blocks with a wall thickness of 5 mm. The dates of irradiation,

values of dose rate, absorbed dose, and mean irradiation

temperature were as follows:

For December 31,1 996, film block, in Gammacell 220-232, /) = 1 0.68 kGy/h

Dosimeter

Identification Date of Irradiation (kGy/h)

Irradiation

Temp. °C

Absorbed

Dose

kGy(H,0)

Pouch 1 Nov 21, 1997 9.210 24.0 10.00

Pouch 2 Nov 20, 1997 9.211 24.0 20.00

Pouch 3 Nov 20, 1997 9.211 24.0 30.00

Pouch 4 Nov 21, 1997 9.210 24.0 40.00

Pouch 5 Nov 21, 1997 9.210 24.0 50.00

REFERENCE TEST 846/25601 8-97 Sep. 25, 1 997

NIST DB 932/018 HD9799

38
The last page of this Report describes uncertainties and related factors in high-dose

calibrations, such as the one covered by this Report of Calibration. If there are further

questions, they should be directed to the first individual named below.

Measurements were made by

J. M. Puhl, Calibrations Technician

(301)975-5581

Approved by

Stephen M. Seltzer, Leader

Radiation Interactions and Dosimetry Group

For the Director

National Institute of Standards and Technology

by

Bert M. Coursey, Chief

Ionizing Radiation Division

Physics Laboratory

REFERENCE TEST 846/25601 8-97

NIST DB 932/018

Page 2 of 3 Pages

39

Sep. 25, 1997

HD9799
UNCERTAINTIES AND RELATED FACTORS IN HIGH-DOSE CALIBRATIONS

High-Dose Calibrations in Standard Geometries

using the NIST Cobalt-60 Irradiators

(Relative expanded uncertainty: ± 1.8% at a 95% confidence level)

The high-dose calibrations at NIST involve the administration of ^°Co gamma radiation

under environmentally controlled conditions. The dose values are based on standard

water calorimeter measurements and EPR/Alanine dosimetry, which are corrected by

certain modifying factors (such as the estimated photon spectrum, radiation energy

absorption and attenuation factors, and source decay factors).

The uncertainty cited above is pertinent to absorbed dose in water in calibrated

geometries. A detailed list of the various sources of uncertainty and estimates of the

magnitude of those uncertainties that make up the overall uncertainty given above may

be obtained by requesting such information from NIST. The uncertainties are divided

into two types: A and B. Type A uncertainties are those evaluated by statistical

methods, often associated with random effects. Type B uncertainties are those

evaluated by other means, often associated with systematic effects.

Type A Uncertainties

The combined relative standard uncertainty evaluated by statistical methods is ± 0.7%

at an approximate level of confidence of 68%.

Type B Uncertainties

The combined relative standard uncertainty based on scientific judgement is estimated

to be ± 0.5% at an approximate level of confidence of 68%.

Expanded Uncertainty

The type A and type B uncertainties have been combined in quadrature (the square

root of the sum of the squares) and multiplied by a coverage factor of 2 to yield a

relative expanded uncertainty of ± 1 .8% at an approximate level of confidence of 95%.

REFERENCE TEST 846/256018-97 Sep. 25, 1997

NIST DB 932/018 HD9799

Page 3 of 3 Pages

40
1 1 tf^^^^^ United States Department of Commerce

I I National Institute of Standards and Technology

I Gaithersburg, MD 20899 USA

REPORT OF CALIBRATION

OF: Ed's Sterilizers

'°Co Calibrator, s/n 10

by use of NIST

Transfer Dosimeters

FOR: Ed's Sterilizers

10 Gamma Avenue

Mega Rad, TX 99817

ATTN: Cobalt Jones

REF: P0# 232

Description: Transfer dosimetry packets, consisting of five calibrated FWT60-00 radiochromic dosimeters (NIST Batch #7f6a), held

between 5.0 mm thick blocks of polystyrene and sealed inside a thin polymer-aluminum laminate pouch (R.H. = 45% at time

of sealing), were sent to Ed's Sterilizers for irradiation in their

^°Co calibrator. Upon their return to NIST, the dosimeters were

analyzed on 11/23/97, using a Cary 3 spectrophotometer( S/N

1101115, 4.0 nm S.B.W.). Absorbed dose interpretations were

made from a calibration of this batch of radiochromic

dosimeters performed in March 1997. The results are summarized in the following table.

Dosimeter ID

NIST Interpolated

Dose, kGy(H^O)

875-879 10.99

880-884 11.01

885-889 11.09

REFERENCE TEST 846/25601 8-97 Sep. 25, 1 997

NIST DB 932/018 HD9799

Page 1 of 3 Pages

41
The last page of this Report describes uncertainties and related factors in high-dose

calibrations, such as the one covered by this Report of Calibration. If there are further

questions, they should be directed to the first individual named below.

Measurements were made by

J. M. Puhl, Calibrations Technician

(301)975-5581

Approved by

Stephen M. Seltzer, Leader

Radiation Interactions and Dosimetry Group

For the Director

National Institute of Standards and Technology

by

Bert M. Coursey, Chief

Ionizing Radiation Division

Physics Laboratory

REFERENCE TEST 846/25601 8-97

NISTDB 932/018

Page 2 of 3 Pages

42

Sep. 25, 1997

HD9799
UNCERTAINTIES AND RELATED FACTORS IN HIGH-DOSE CALIBRATIONS

Absorbed Dose Evaluations Based on Use of

Mailed Film Transfer Standard Dosimeters

(Relative expanded uncertainty: ± 4.6% at a 95% confidence level)

The use of NIST transfer standard dosimeters to calibrate the dose rate of the

customer's in-house radiation source is subject to the limitations and precautions

described in the letter accompanying the dosimeters. The customer must follow the

prescribed procedures carefully in order to ensure that the results obtained from the

transfer dosimeters are valid.

In the case of absorbed dose in water evaluation based on NIST radiochromic film

dosimeters (nominal dose range 5 x IOM0 5 x 10'* Gy) that are traceable to ^°Co

gamma-ray calibrations at NIST, the uncertainty value cited above (± 4.6%) may be

assumed as long as suitable care is exercised.

A detailed list of the various sources of uncertainty and estimates of the magnitude of

those uncertainties that make up the overall uncertainty given above may be obtained

by requesting such information from NIST. The uncertainties are divided into two types:

A and B. Type A uncertainties are those evaluated by statistical methods, often

associated with random effects. Type B uncertainties are those evaluated by other

means, often associated with systematic effects.

Type A Uncertainties

The combined relative standard uncertainty evaluated by statistical methods is ± 1.1%

at an approximate level of confidence of 68%.

Type B Uncertainties

The combined relative standard uncertainty based on scientific judgement is estimated

to be ± 2.0% at an approximate level of confidence of 68%.

Expanded Uncertaintv

The type A and type B uncertainties have been combined in quadrature (the square

root of the sum of the squares) and multiplied by a coverage factor of 2 to yield a

relative expanded uncertainty of ± 4.6% at an approximate level of confidence of 95%.

REFERENCE TEST 846/25601 8-97 Sep. 25, 1 997

NIST DB 932/018 HD9799

Page 3 of 3 Pages

43
UNCERTAINTIES AND RELATED FACTORS IN HIGH-DOSE CALIBRATIONS

Absorbed Dose Evaluations Based on Use of

Mailed Alanine Transfer Standard Dosimeters

(Relative expanded uncertainty: ± 2.2% at a 95% confidence level)

The use of NIST transfer standard dosimeters to calibrate the dose rate of the

customer's in-house radiation source is subject to the limitations and precautions

described in the letter accompanying the dosimeters. The customer must follow the

prescribed procedures carefully in order to ensure that the results obtained from the

transfer dosimeters are valid.

In the case of absorbed dose in v\/ater evaluation based on NIST alanine pellet

dosimeters (nominal dose range 1 x 10^ to 5 x 10^ Gy) that are traceable to ^°Co

gamma-ray calibrations at NIST, the uncertainty value cited above (± 1.8%) may be

assumed as long as suitable care is exercised.

A detailed list of the various sources of uncertainty and estimates of the magnitude of

those uncertainties that make up the overall uncertainty given above may be obtained

by requesting such information from NIST. The uncertainties are divided into two types:

A and B. Type A uncertainties are those evaluated by statistical methods, often

associated with random effects. Type B uncertainties are those evaluated by other

means, often associated with systematic effects.

Type A Uncertainties

The combined relative standard uncertainty evaluated by statistical methods is ± 0.7%

at an approximate level of confidence of 68%.

Type B Uncertainties

The combined relative standard uncertainty based on scientific judgement is estimated

to be ± 0.6% at an approximate level of confidence of 68%.

Expanded Uncertainty

The type A and type B uncertainties have been combined in quadrature (the square

root of the sum of the squares) and multiplied by a coverage factor of 2 to yield a

relative expanded uncertainty of ± 1 .8% at an approximate level of confidence of 95%.

REFERENCE TEST 846/25601 8-97 Sep. 25, 1 997

NIST DB 932/018 HD9799

Page 3 of 3 Pages

44
THE SP 250 SERIES ON NIST MEASUREMENT SERVICES*

SP 250-1 Spectral Radiance Calibrations PB871 79883

SP 250-2 Far Ultraviolet Detector Standards PB87227609

SP 250-3 Radiometric Standards in the Vacuum

Ultraviolet PB87227625

SP 250-4 Fricke Dosimetry in High-Energy Electron Beams

PB881 10374 SP 250-5 Alpha-Particle Calibrations PB881 68620

SP 250-6 Regular Spectral Transmittance PB881 08550

SP 250-7 Radiance Temperature Calibrations PB881 23674

SP 250-8 Spectral Reflectance PB88 109905 SP 250-9 Calibration of Beta-Particle-Emitting

Ophthalmic Applicators

PB88 108535 SP 250-10 Radioactivity Calibrations with the "4-n-" Gamma Ionization Chamber and Other

Radioactivity Calibration Capabilities

PB881 23708

SP 250-1 1 Dosimetry for High Dose Applications

PB88201587

SP 250-12 Neutron Personnel Dosimetry

PB87227617

SP 250-13 Activation Foil Irradiation with Californium

Fission Sources PB88217443

SP 250-14 Activation Foil Irradiation by Reactor Cavity

Fission Sources PB88217435

SP 250-15 Photometric Calibrations PB881 53747

SP 250-16 Calibration of X-Ray and Gamma-Ray

Measuring Instruments PB88211826

SP 250-17 The NBS Photodetector Spectral Response

Calibration Transfer Program

PB88201595

SP 250-18 Neutron Source Strength Calibrations PB88211818

SP 250-19 Calibration of Gamma-Ray-Emitting

Brachytherapy Sources PB891 93858

SP 250-20 Spectral Irradiance Calibrations PB881 23781 SP 250-21 Calibration of Beta-Particle Radiation Instrumentation PB88201579

SP 250-22 Platinum Resistance Thermometer

Calibrations PB88 138367 SP 250-23 Liquid-in-Glass Thermometer

Calibration Service PB891 28888

SP 250-24 Standard Cell Calibrations PB881 23690

SP 250-25 Calibration Service for Inductive Voltage Dividers SP 250-26 NBS Phase Angle Calibration Services PB88225636

SP 250-27 AC-DC Difference Calibrations PB892222616

SP 250-28 Solid-State DC Voltage Standard Calibrations PB88 168703 SP 250-29 Traceable Frequency Calibrations PB881 68364

SP 250-30 GOES Satellite Time Code Dissemination:

Description and Operation

PB881 68760

SP 250-31 Mass Calibrations PB891 53894

SP 250-32 A Calibration Service for 30 MHz

Attenuation and Phase Shift PB88238324

SP 250-33 A Calibration Service for Voltage Transformers and High-Voltage Capacitors

PB882252903

SP 250-34 High Vacuum Standard and Its Use

PB891 93841 SP 250-35 The Calibration of Thermocouples

and Thermocouple Materials PB89209340

SP 250-36 A Calibration Service for Current Transformers SP 250-38 NIST Leak Calibration Service SP 250-40 Absorbed-Dose Calibration of Ionization Chambers in a ^°Co Gamma-Ray Beam

SN003-003-03034-1 $2.00

* Entries Entries containing a stock number (SN003-003-) and price can be purchased from the Superintendent of Documents, U.S. Government Printing Office, Washington, DC 20402. GPO will accept checks, money orders, VISA, and MasterCard. For more infomation,

or to place an order, call (202) 783-3238. Be sure to cite the stock number on all orders.

Entries containing PB numbers can be purchased from the National Technical Information Service, Springfield, VA 22161. NTIS will accept American Express in addition to the payment methods listed for GPO. For more information call (703) 487-4650; to place an order

call (800) 336-4700. Be sure to cite the PB number on all orders.

Entries without stock or PB numbers are in preparation.
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