I

NBS Measurement Services:

Fricke Dosimetry in High-Energy

NBS Special Publication 250-4

Christopher G. Soares Eric L. Bright Margarete Ehrlich

U.S. Department of Commerce
National Bureau of Standards

Center for Radiation Research
The Center f o r R a d i a t i o n Research i s a major component of t h e N a t i o n a l Measurement L a b o r a t o r y i n t h e N a t i o n a l Bureau o f Standards. The Center p r o v i d e s t h e N a t i o n w i t h standards and measurement s e r v i c e s f o r i o n i z i n g r a d i a t i o n and f o r u l t r a v i o l e t , v i s i b l e , and i n f r a r e d r a d i a t i o n ; c o o r d i n a t e s and f u r n i s h e s e s s e n t i a1 support t o t h e N a t i o n a l Measurenent Support Systen.for i o n i z i n g r a d i a t i o n ; conducts research i n r a d i a t i o n r e l a t e d f i e l d s t o develop improved r a d i a t i o n measurement methodology; and generates, corrpiles, and c r i t i c a l l y evaluates d a t a t o meet major n a t i o n a l needs. The Center c o n s l s t s o f f i v e D i v i s i o n s and one Group.

Atomic and Plasma Radiation Division
C a r r i e s o u t b a s i c t h e o r e t i c a l and experimental research i n t o t h e soectroscopic and r a d i a t i v e p r o p e r t i e s o f atoms and h i g h l y i o n i z e d sbecies; develops w e l l - d e f i n e d atomic r a d i a t i o n sources as r a d i o m e t r i c or wavelength standards; develops new measurement techniques and methods f o r s p e c t r a l a n a l y s i s and plasma p r o p e r t i e s ; and c o l l e c t s , compiles, and c r i t i c a l l y evaluates spectroscopic data. The D i v i s i o n c o n s i s t s o f t h e f o l l o w i n g Groups:
• Atomic Spectroscopy

Atomic R a d i a t i o n Data Plasma R a d i a t i o n

Radiation Physics Division
Provides t h e c e n t r a l n a t i o n a l b a s i s f o r t h e measurement o f f a r u l t r a v i o l e t , s o f t x-ray, and e l e c t r o n r a d i a t i o n ; develops and disseminates r a d i a t i o n standards, measurement services, and d a t a f o r f o r these r a d i a tions; conducts t h e o r e t i c a l and experimental research w i t h e l e c t r o n , laser, u l t r a v i o l e t , and s o f t x - r a y r a d i a t i o n f o r measurement appl i c a t i o n s ; determines f u n d m e n t a l mechanisms o f e l e c t r o n and photon i n t e r a c t i o n s w i t h matter; and develops advanced e l e c t r o n - and photon-based measurement techiques. The D i v i s i o n c o n s i s t s o f t h e f o t l o w i n g Groups:
a Far UV Physics a Electron Physics

Photon P h y s i c s

Radiometric Physics Division
Provides n a t i o n a l measurement standards and support s e r v i c e s f o r u l t r a v i o l e t , v i s i b l e , and i n f r a r e d r a d i a t i o n ; provides standards dissemination and measurement q u a l i t y assurance services; conducts research i n o p t i c a l r a d i a t i o n , pyrometry, photometry, and quantun radiometry; and develops s p e c t r o r a d i o m e t r i c and spectrophotometric standards and c a l i b r a t i o n procedures. The D i v i s i o n c o n s i s t s o f t h e f o l lowing Groups: S p e c t r a l Radiometry Spectrophotometry Radiometric Measurement Services

Radiation Source and Instrumentation Division
develops, operates, and improves major NBS r a d i a t i o n f a c i l i t i e s i n c l u d i n g t h e e l e c t r o n L i n a c and r a c e t r a c k m i c r o t r o n ; develops, designs, and b u i l d s e l e c t r o n i c and mechanical i n s t r u n e n t a t i o n f o r r a d i a t i o n prograns and f a c i l i t i e s ; provides n a t i o n a l l e a d e r s h i p i n t h e s t a n d a r d i z a t i o n o f n u c l e a r i n s t r u n e n t a t i o n ; and develops new competence i n r a d i a t i o n sources and i n s t r u n e n t a t i o n . The D i v i s i o n c o n s i s t s o f t h e f o l l o w i n g Groups:
a

A c c e l e r a t o r Research L i n a c Operations Electronic Instrunentation Mechanical I n s t r u n e n t a t i o n

Ionizing Radiation Division
Provides primary n a t i o n a l standards, measurement services, and b a s i c data f o r a p p l i c a t i o n s o f i o n i z i n g r a d i a t i o n ; develops new methods o f chemical and p h y s i c a l dosimetry; conducts t h e o r e t i c a l and experimental research on t h e tundamental p h y s i c a l and chemical i n t e r a c t Ions of i o n i z i n g r a d i a t i o n w i t h matter; p r o v i d e s essent ia1 standards and measurement support s e r v i c e s t o t h e N a t i o n a l Measurement Support System f o r I o n i z i n g Radiation; and develops and operates r a d i a t i o n sources needed t o p r o v i d e p r i m a r y r a d i a t i o n standards, f i e l d s , and w e l l - c h a r a c t e r i z e d beams o f r a d i a t i o n f o r research on r a d i a t i o n i n t e r a c t i o n s and f o r developnent o f measurement methods. The D i v i s i o n c o n s i s t s o f t h e f o l l o w i n g O f f i c e and Groups: O f f i c e o f R a d i a t i o n Measurement R a d i a t i o n Theory R a d i a t i o n Chemistry and Chemical ooslmetry Neutron Measurements and Research Neutron Dosimetry a Radioactivity X-Ray Physics a Dosimetry

Nuclear Physics Group
Engages i n f o r e f r o n t research i n n u c l e a r and elementary p a r t i c l e physics; performs h i g h l y accurate measurements and t h e o r e t i c a l analyses which probe t h e s t r u c t u r e o f nuclear matter; and improves t h e q u a n t i t a t i v e understanding of- p h y s i c a l processes t h a t u n d e r l i e measurement science.

NBS MEASUREMENT SERVICES: FRICKE DOSIMETRY IN HIGH-ENERGY ELECTRON BEAMS
Christopher G. Soares

Eric L. Bright Margarete Ehrlich

Center for Radiation Research National Measurement Laboratory National Bureau of Standards Gaithersburg, MD 20899

U.S. DEPARTMENT OF COMMERCE, Malcolm Baldrige, Secretary
NATIONAL BUREAU OF STANDARDS, Ernest Ambler, Director Issued July 1987

Library of Congress ~atalo$ Card Number: 87-619834 National Bureau of Standards Special Publication 250-4 Natl. Bur. Stand. (U.S.), Spec. Publ. 250-4, 54 pages (July 1987) CODEN: XNBSAV

Commercial products-materials and instruments-are identified in this document for the sole purpose of adequately describing experimental or test procedures. In no event does such identification imply recommendation or endorsement by the National Bureau of Standards of a particular product; nor does it imply that a named material or instrument is necessarilythe best available for the purpose it serves.

U.S. GOVERNMENT PRINTING OFFICE WASHINGTON: 1987
For sale by the Superintendent of Documents, U.S. Government Printing Office, Washington, DC 20402-9325

PREFACE The c a l i b r a t i o n and r e l a t e d measurement s e r v i c e s o f t h e N a t i o n a l Bureau o f Standards are i n t e n d e d t o a s s i s t t h e makers and users o f p r e c i s i o n measuring i n s t r u m e n t s i n a c h i e v i n g t h e h i g h e s t p o s s i b l e l e v e l s o f accuracy, q u a l i t y , and p r o d u c t i v i t y . NBS o f f e r s o v e r 300 d i f f e r e n t c a l i b r a t i o n , s p e c i a l t e s t , and measurement assurance s e r v i c e s . These s e r v i c e s a1 low customers t o d i r e c t l y 1 i n k t h e i r rneasurernent systems t o measurement systems and standards m a i n t a i n e d b y NBS. These s e r v i c e s are o f f e r e d t o t h e p u b l i c and p r i v a t e o r q a n i z a t i o n s a l i k e . They are described i n N8S Special Pub1 i c a t i o n (SP) 250, NBS Ca7 i b r a t i o n Services Users Guide. The Users Guide i s b e i n g supplemented b y a number o f s p e c i a l p u b l i c a t i o n s ( d e s i g n a t e d as t h e "SP 250 S e r i e s " ) t h a t p r o v i d e a d e t a i l e d d e s c r i ~ t i o no f t h e important f e a t u r e s o f s p e c i f i c NRS c a l i b r a t i o n s e r v i c e s . These documents p r o v i d e a d e s c r i p t i o n o f the: ( 1 ) s p e c i f i c a t i o n s f o r t h e s e r v i c e ; ( 2 ) design p h i losophy and t h e o r y ; (3) NBS measurement system; ( 4 ) NBS o p e r a t i o n a l procedures; ( 5 ) assessment of measurement u n c e r t a i n t y i n c l u d i n g random and s y s t e m a t i c e r r o r s and an e r r o r budget; and ( 6 ) i n t e r n a l q u a l i t y c o n t r o l procedures used b y NBS. These documents w i l l present more d e t a i l than can be g i v e n i n an NBS c a l i b r a t i o n r e p o r t , o r t h a n i s g e n e r a l l y allowed i n articles i n s c i e n t i f i c journals. I n t h e past NBS has p u b l i s h e d such inforrnat i o n i n a v a r i e t y o f ways. T h i s s e r i e s w i l l h e l p make t h i s t y p e o f i n f o r m a t i o n more r e a d i l y a v a i l a b l e t o t h e user. This document ( S f 250-4), NBS Measurement Services: F r i c k e Dosimetry i n High-Enerqy E l e c t r o n Beams, by C . G. Soares, E. L. B r i g h t , and M. E h r l i c h , i s t h e f o u r t h t o he p u b l i s h e d i n t h i s new s e r i e s o f s p e c i a l p u b l i c a t i o n s . I t d e s c r i b e s t h e p r e p a r a t i o n and c a l i b r a t i o n o f f e r r o u s - s u l f ate ( F r i c k e ) chemical dosimeters used f o r t h e measurement o f absorbed dose t o water i n e l e c t r o n beans i n t h e enerqy ranqe from 5 t o 50 MeV (see t e s t nurnbers 48010M and 4F1011M i n t h e SP 250 ifsers Guide) I n q u i r i e s concerninq t h e t e c h n i c a l c o n t e n t o f t h i s document o r t h e s p e c i f i c a t i o n s f o r these s e r v i c e s should be d i r e c t e d t o t h e authors u r une o r t h e t e c h n i c a l ~ o n t a c t sc i t e d i n SP 250.

.

The Center f o r R a d i a t i o n Research (CRR) i s i n t h e process qf p u b l i s h i ~ q 21 documents i n t h i s SP 250 s e r i e s , c o v e r i n g a l l o f t h e c a l i b r a t i o n s e r v i c e s o f f e r e d by CRR. A complete l i s t i n g of these documents can b e found i n s i d e t h e back cover.

NRS would welcome suqqestions on how p u b l i c a t i o n s s ~ as h these rqiqht be ~nademore :rseful . Suggest ions are a l s o welcolnr concerning t h e need f o r new c a l i b r a t i o n s e r v i c e s , s p e c i a l t e s t s , and measurenent assurance programs

.

George A. U r i ano Director !4easurernent Services

C h r i s E. K u y a t t D irector Center f o r Radi a t i o n %search

ABSTRACT The NBS F r i c k e - D o s i m e t r y S e r v i c e ( a d v e r t i s e d i n NBS Speci a1 Pub1 ic a t i on 250, 1986-1988 and e a r l i e r e d i t i o n s ) i s d e s c r i b e d i n d e t a i 1. A f t e r a b r i e f h i s t o r i c a l i n t r o d u c t i o n and d e s c r i p t i o n o f t h e s e r v i c e , t h e t h e o r e t i c a l b a s i s ( i n c l u d i n y what q u a n t i t i e s a r e measured, how, and why) and t h e p h i l o s o p h y o f i n t e r n a l qual it y checks are discussed i n some d e t a i l . T h i s i s f o l l o w e d by a d e s c r i p t i o n of t h e p h y s i c a l setup and o f t h e step-by-step o p e r a t i ny and r e p o r t i ny procedures. Throughout t h i s s e c t i o n , t h e r e i s r e f e r e n c e t o sample r e c o r d s o f p a s t performance, i n o r d e r t o f a c i l i t a t e c o n t i n u i t y o f o p e r a t i o n i n t h e case o f personnel changes. The docurqent concludes w i t h a d i s c u s s i o n o f t h e u n c e r t a i n t i e s in v o l verf i n tlii s qeasurernent qual it y assurance s e r v i c e , s a f e t y c o n s i d e r a t i o n s , dnd an appendix c o n t a i n i n g samples o f a1 1 form l e t t e r s and o f t h e f i n a l r e p o r t m a i l e d t o the participants. Key words: absorbed dose t o water; bi-annual s e r v i c e ; chemical d o s i m e t r y ; dose i n t e r p r e t a t i o n ; dosirneter p r e p a r a t i o n ; e l e c t r o n therapy; f e r r o u s - s u l f a t e ( F r i c k e ) s o l u t i o n ; i n t e r n a l qua7 it y check; measurement qual it y assurance; p l a s t i c phantoa; spectrophotometry

TABLE OF CUNTENTS
1

...................................................... ............................................... 2 . Theory and Design Philosophy ........................................ 2.1 Theory ...................................................... 2.2 Design ........................................................ 2.3 System O p e r a t i o n ............................................... 2.3.1 S t a t i s t i c a l d i s t r i b u t i o n o f absorbance j r 0 ~ t . h i n t h e IIBS unsealed system ........................................ 2.3.2 I n t e r n a l q u a l i t y check on performance o f i n d i v i d u a l dosimeters ...........................................
2.4

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Abstract D e s c r i p t i o n of S e r v i c e 1.1 H i s t o r y 1.2 The S e r v i c e

............................................................. .............................................. i v

1 1 1

3 3 4 5
5

2.3.3 I n t e r n a l q u a l i t y checks on s p e c t r o p h o t o ~ n e t r y Upgrading t h e S e r v i c e .T

............ ..... ...................................

6
6
7

3

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Oescri p t i o n o f System and Operating Procedure 3.1 The Physical Setup
3.2
P r e p a r a t i o n o f Dosimeters and

............... ................................ 3.3 ............................................ 3.4 ................. ....................... 3.5 4 . Safety C o n s i d e r a t i o n s ............................................... References .......................................................... 32 Appendix 1. Forrns Used i n W r i t t e n Exchanges vrith P a r t i c i p a n t s ...... 33 Appendix 2 . Sample of Report t o P a r t i c i p a n t s ....................... 4 1
P r e - i r r d d i a t i o n b v i ti1 cobal t - 6 0 gainma rays R e s u l t s o f p r e - i r r a d i a t i o n s and t h e i r appl i c a t i o n t o i n t e r n a l qua1 i t y c o n t r o l Spectrophotometry : E n s u r i ng Long- and Short-Term Consistency and R e p r o d u c i b i l i t y Dose I n t e r p r e t a t i o n and Report t o P a r t i c i p a n t s U n c e r t a i n t i e s i n t h e Dose I n t e r p r e t a t i o n

3.2.1 3.2.2 3.2.3 3.2.4

............................................. Check ....... P r e p a r i ny t h e s a l u t i ons ................................. F i l l i n g t h e spectrophotometer c e l l s .....................
on T h c i r Performance

.......................

TABLE OF CONTENTS, CONTINUED

LIST OF TABLES Table 1. Table 2. Sample, Absorbances o f C e l l s Before P r c - i r r a d i a t i on..

17 ......... Page

Sample o f Spectrophoto~netry Record o f A l l C e l l s A f t e r Prey o f Cobalt-60 Gamma Radiation, P r i o r t o i r r a d i a t i o n w i t h 50 G Shipment Sample o f D i s t r i b u t i o n o f P o s i t i o n - C o r r e c t e d Absorbances...... S t a t i s t i c s , from Sample R e s u l t s Shown i n Table 3

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20 21

Table. 3 Table 4. Table 5. Table 6. Table 7 . Table 8. Table 9.

22

Check on G-Value and Product E G f o r t h e P a r t i c u l a r Sample Batch of F r i c k e Solution......................................

23
25

...... Constancy and L i n e a r i t y o f Cary Spectrophotometer, Plodel 16, between A p r i l 1971 and A p r i l 1974.. ........................... Sample o f Spectrophotometry Record A f t e r Shi pment and Associated Absorbed-Dose I n t e r p r e t a t i o n . . ..................... U n c e r t a i n t i e s i n t h e Dose I n t e r p r e t a t i o n s ......................
Sample, Absorbances o f 1 gZ Potassium N i t r a t e Sol u t i o o . .

25

27
30

TABLE O F CONTENTS. CONTINUED LIST O F FIGURES Fiyure 1

. Fiyure 2.
Figure 3 Figure 4 Figure 5

........................................ Mapping t h e Cross S e c t i o n o f t h e Cobalt-60 Gamma-Ray Beam Used f o r P r e . i r r a d i a t i o n ...........................................
Dosimeter Assembly [3] Weighing t h e S u l f u r i c A c i d Weighing t h e S a l t s

2
10

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12 13
15 16
18

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.........................................

. F i g u r e 6.
Figure 7 Figure 8

Aerating t h e Solution

F i l l i n g t h e Spectrophotometer C e l l s w i t h F r i c k e S o l u t i o n P r e - I r r a d i a t i o n w i t h Cobalt-60 Gamma R a d i a t i o n Spectrophotometry

......

............................................. F i g u r e 9 . Sample P l o t . Automatic Scan o f F e r r i c - I o n Absorbance-vsWavelength .................................................... . Sample. A n a l y s i s o f S p u r i n ~ l sAbsorbance Growth A A . ~ . o f Shipping and Home C o n t r o l s ....................................
F i y ~ l r 10 ~

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24

24
28

1 .
1.1

DESCKIPTION OF SERVICE History

Since 1967, t h e N a t i o n a l Bureau o f Standards (NBS) has been p r o v i d i n g a measurement-assurance s e r v i c e f o r t e s t i n g t h e s t a t u s o f d o s i m e t r y f o r e l e c t r o n ( F o r d e t a i l s see Chapter beams i n t h e energy range from about 5 t o 50 MeV. V I , I o n i z i n g R a d i a t i o n I!easurernents, t e s t numbers 48010M and 4KOllM - f o r m e r l y 8.58 and 8.5C - o f NRS Speci a1 Pub1 i c a t i on 250, The NBS C a l i b r a t i o nServices Users Guide 1986-1988.) The s e r v i c e , which i s d i r e c t e d m a i n l y toward X5tion-txeFCpy--amlications i n t h e U n i t e d States, was e s t a b l i s h e d upon t h e r e q u e s t o f t h e American A s s o c i a t i o n o f P h y s i c i s t s i n Medicine (AAPM) a t t h e t i m e o f t h e e l e c t r o n - t h e r a p y c l i n i c a l t r i a l s , f o r which u n i for13 d o s i m e t r y among a l l t h e p a r t i c i p a n t s waq ~ q q ~ n t i a l .I n i t i a l l y , i t was thought t h a t t h e s e r v i c e would be d i s c o n t i n u e d as soon as NBS c o u l d o f f e r in-phantom c a l i b r a t i o n s f o r r a d i a t i o n - t h e r a p y i n s t r u n e n t s i n terrns o f absorbed dose t o water, o r when r e l i a b l e methods would be a v a i l a b l e f o r a r r i v i n y a t absorbed dose t o water frorn exposure r~ieasurernents i n a i r [1] l w i t h s u i t a b l y c a l i b r a t e d i n s t r u ments. NBS i s now i n a p o s i t i o n t o perforin these c a l i b r a t i o n s , and r e l i a b l e niethods f o r d e r i v i n y absorbed dose t o water from exposure have been developed [El. Nevertheless, t h e s e r v i c e i s b e i n y c o n t i n u e d b i r ~ ~ th ee r e is a c o n t i n u i n y demand f o r t h e "measurement-qua1 it y assurance" i t p r o v i d e s f o r t h e d a i l y o p e r a t i o n of r a d i a t i o n - t h e r a p y departrrlents. D u r i n g i t s f i r s t year, t h e s e r v i c e was s u b s i d i z e d by t h e Bureau of R a d i o l o g i c a l Y e a l t h and t h u s c o u l d be o f f e r e d q u a r t e r l y and a t a f r a c t i o n o f a c t u a l c o s t . Since t h e end o f t h e subsidy, i t has been o f f e r e d serni - a n n u a l l y , and t h e charges cover t h e a c t u a l cost. Duriny t h e past- e i g h t e e n years, a t o t a l o f r o u g h l y 75 yroups have p a r t i c i p a t e d , sorne a n n u a l l y , most o f them semi -annual ly. Most o f t h e s e y roups use e l e c t r o n bearns f o r therapy. Occasional l y we accept r e q u e s t s from groups d e s i r i n g checks on t h e i r c o b a l t - 6 0 gamma-ray dosimetry. Requests from groups d e s i r i n g checks on t h e i r high-energy bremsstrahlung d o s i m e t r y a r e accepted o n l y w i t h t h e understanding t h a t t h e NBS dose i n t e r p r e t a t i o n from h i yh-energy bremsstrahl ung i s a s s o c i a t e d w i t h 1 a r g e r u n c e r t a i n t i es. Over t h e years, d e s c r i p t i o n s of t h i s s e r v i c e and r e v i e w s o f r e s u l t s have been publ ished. R e p r i n t s o f these and o t h e r p e r t i n e n t publ i c a t i o n s a r e f i l e d w i t h t h i s document and a r e a v a i l a b l e t o t h e p u b l i c upon request. The f o l l o w i n g h i ghl ig h t s are p a r t i a1 l y e x t r a c t e d from t h e publ ic a t i o n s .

1.2

The S e r v i c e

F e r r o u s - s u l f a t e ( F r i c k e ) dosimeters, prepared a t NBS and checked by means o f 60Co gamma p r e - i r r a d i a t i o n , are shipped t o t h e p a r t i c i p a t i n g i n s t i t u t i o n s w i t h t h e request t o i r r a d i a t e thern i n a p o l y s t y r e n e phantom, u s i n y t h e dosimeter depth and t h e phantom and f i e l d s i z e s s p e c i f i e d by t h e AAPM [2]. F i g u r e 1 shows t h e dosimeter assembly, c o n s i s t i n g of t h e f e r r o u s - s u l f a t e ( F r i c k e ) s o l u t i o n i n a ground-yl ass stoppered, r a d i a t i o n - r e s i s t a n t , q u a r t z spectrophotometer c e l l w i t h q u a r t z windows. The c e l l i s c r a d l e d i n a p o l y s t y r e n e block machined t o f i t i n t o a recess of t h e p a r t i c i p a n t ' s p o l y s t y r e n e

lNumbers i n b r a c k e t s i n d i c a t e t h e l i t e r a t u r e r e f e r e n c e s a t t h e end o f t h i s paper.

phantom. The dosirneters a r e shipped p r e - p a i d by a com~nercial d e l iv e r y service. Since t h e y c o n t a i n a c o r r o s i v e l i q u i d i n unsealed c o n t a i n e r s t h e y cannot be sent by mai 1 , and, i f a i r t r a n s p o r t a t h i g h a1 t i tudes i s i n v o l v e d , t h e packages must be marked f o r t r a n s p o r t a t i o n o n l y i n t h z ~ r e s s u r i z e d compartinent o f tile plane. (See a1 sa S e c t i o n 4 . )

F i yure 1.

Dosimeter Asseably [ 3 1. The stoppered spectrophotomet?r c e l l s a r e c r d d l e d i n a 5.1 cm x 7.6 cm x 2.0 cm ( h i g h ) p o l y s t y r e n e b l o c k , w i t h a styrofoam p l u g ( n o t shown) wedged i n above t h e stopper. The 3-mm p o l y s t y r e n e l i d i s p r e s e n t l y screwed on w i t h two r a t h e r t h a n w i t h t h e s i x screws shown.

The p a r t i c i p a n t s i r r a d i a t e a l l b u t one of t h e f u r n i s h e d dosimeters t o between 50 and 80 Gy (5000 and 8000 r a d ) t o water, u s u a l l y a t e l e c t r o n energies between 5 and 50 MeV, employing t h e s p e c i f i e d i r r a d i a t i o n yeometry. A f t e r i r r a d i a t i o n , t h e p a r t i c i p a n t s r e t u r n t h e dosimeters t o NBS f o r spectrophotometri c e v a l u a t i o n o f t h e f e r r i c - i on c o n c e n t r a t i o n i n terms o f absorbed dose t o water, u s i n g a v a l u e f o r t h e r a d i a t i o n - c h e m i c a l y i e l d compati b l e vrith t h e most r e c e n t ICRU recommendations C41. Return shipment i s prepaid by p a r t i c i p a n t s , and t h e r e s t r i c t i o n s on d e l i v e r y s e r v i c e and mode o f t r a n s p o r t a t i o n are t h e same as f o r shipment from NBS. The p a r t i c i p a n t s a r e asked t o r e t u r n t h e dosimeters w i t h i n t h r e e ~ o r kng i days from t h e i r r e c e i p t , if a t a l l p o s s i b l e . Once t h e e v a l u a t i o n i s completed, NBS i n f o r m s each p a r t i c i p a n t by mail o f h i s own t e s t r e s u l t s and o f t h e r e s u l t s o f a l l o t h e r p a r t i c i p a n t s , b u t w i t h o u t d i v u l y i ng t h e i r i d e n t i t i e s . I n a d d i t i o n , r e g u l a r
p a r t i c i p a n t s a c t i v e l y engaged i n r a d i a t i o n t h e r a p y a r e a l e r t e d by t e l e p h o n e i f

t h e i r dose i n t e r p r e t a t i o n s are b a d l y o u t o f l i n e , say, by 20 p e r c e n t o r more. A l l p a r t i c i p a n t s a r e f r e e t o d i s c u s s t h e i r r e s u l t s and p o s s i b l e problems w i t h NBS, e i t h e r by m a i l o r by telephone.

Appendix 1 c o n t a i n s a l l forms used i n w r i t t e n exchanges w i t h p a r t i c i p a n t s . A sample o f a f i n a l r e p o r t i s shown i n Appendix 2.

2.
2.1

THEORY AND DESIGN PHILOSOPHY Theory

The f e r r o u s - s u l f a t e ( F r i cke) d o s i m e t r y system has been d l scussed e x t e n The chemical changes i t undergoes upon exposure s i v e l y i n t h e 1i t e r a t u r e . [ 5 ] t o i o n i z i n g r a d i a t i o n a r e w e l l understood and l e a d t o changes i n o p t i c a l p r o p e r t i e s t h a t are r e a d i l y and a c c u r a t e l y measurable by r e l a t i v e l y s i m p l e o p t i c a l means. Because i t s n e t o p t i c a l absorbance i s p r o p o r t i o n a l t o t h e absorbed dose t o t h e system o v e r a wide range o f i r r a d i a t i o n l e v e l s , and t h e system c o n s i s t s mainly of w a t c r , i t l e n d s i t s e l f well t o a d e t e r m i n a t i o n of absorbed dose t o water, which i s t h e q u a n t i t y o f i n t e r e s t i n r a d i a t i o n therapy.

NBS uses t h e f o l l o w i ny c o n v e n t i o n a l dosimeter in y r e d i e n t s 2 :
0.001 M Fe(NH,),(SO,) ,.6H,O, dissolved i n

0.8 N H2S04, w e l l aerated, and

The NaCl d e s e n s i t i z e s t h e system a g a i n s t o r g a n i c f i n p u r i t i e s b u t causes an i n c r e a s e i n t h e r a t e dependence o f i t s r a d i ation-chemical y i e l d , Therefore, p a r t i c i p a n t s u s i n g pulsed e l e c t r o n beams a r e asked t o i r r a d i a t e a t dose r a t e s n o t exceeding 10 G y per niicrosecond p u l s e o r a t o t a l o f 350 Gy f o r any t r a i n o f ~nicrosecondp u l s e s [5]. A s i m p l i f i e d r e a c t i o n mechanism ( i .e., one t h a t does not consider t h e modifications caused by NaC1) i s shown below; i t demons t r a t e s how a e r a t i o n ( i .e., t h e p r o d u c t i o n and maintenance o f a s u f f i c i e n t amount o f O2 a t a1 1 t i m e s ) e n t e r s i n t o t h e r e a c t i o n and determines t h e Fe+++ yield;
Feff

+

O H -+ Fettt

+ OH-

2Meaning o f t h e symbols "M" and "N":
The synibol A: The mole i s t h e molecular w e i g h t o f a s u b s t a n c e expressed es o f t h e s o l u t e i n grams. ~ h e x o l a rt iy o f a s o l u t e i s t h e number o f 1m1 contained i n 1000 cm3 of s o l u t i o n . Therefore, a one-molar ( 1 PI) s o l u t i o n o f s u l f u r i c d c i d c o n t a i n s 98.08 y of s u l f u r i c a c i d per 1000 cm3 o f s o l u t i o n .

The symbol N: The n o r m a l i t y of a s o l u t i o n i s i t s e q u i v a l e n t gramm o l e c u l a r weight c o n c e n t r a t i o n . The e q u i v a l e n t yrdm-mol e c u l a r weight of an a c i d i s i t s molecular w e i y h t expressed i n grams, d i v i d e d by t h e number of hydrogen atoms per molecule. Therefore, a normal ( 1 N) s o l u t i o n o f s u l f u r i c a c i d c o n t a i n s 49.04 g of s u l f u r i c a c i d p e r 1000 c1n3 o f s o l u t i o n .

F e r r i c - i o n y i e l d i s d e f i n e d as t h e number of Fe+++ i o n s formed i n t h e It m y be d e t e r F r i c k e s o l l r t i o n per u n i t o f absorbed dose t o t h e s o l u t i o n . mined s p e c t r o p h o t o m e t r i c a l l y w i t h h i g h accuracy by t h e change i n absorbance of t h e s o l u t i o n , which i s t h e l o g a r i t h m t o t h e base t e n o f t h e r a t i o of i n c i d e n t t o t r a n s m i t t e d r a d i a n t energy F l u x Absorbance i s p r o p o r t i o n a l t o t h e molar c o n c e n t r a t i o n o f t h e Fe+++ i o n s and t h e o p t i c a l p a t h l e n g t h , w i t h t h e p r o p o r t i o n a l it y c o n s t a n t r e f e r r e d t o as t h e mol a r 1 i near a b s o r p t i o n c o e f f i c i e n t , o r t h e rnolar e x t i n c t i o n c o e f f i c i e n t ( B e e r ' s law). The change i n o p t i c a l d e n s i t y measured w i t h a spectrophotometer w i t h good o p t i c a l p r o p e r t i e s i s equal t o t h e change i n absorbdnce. I n general , absorbance depends on t h e wavelength and t h e temperature a t which t h e measurements a r e made. A t a g i v e n temperature and wavelength, t h e average absorbed dose t o t h e F r i c k e s o l u t i o n , DF , t h e n i s o b t a i n e d frorn t h e change i n absorbance, AA, as:

-

where AA i s t h e change i n absorbance, p i s t h e d e n s i t y o f t h e F r i c k e s o l u t i o n , e i s t h e o p t i c a l p a t h l e n y t h , E i s t h e molar l i n e a r a b s o r p t i o n c o e f f i c i e n t , and G(Fe+++) i s t h e Fstt+ i o n y i e l d . The average absorbed dose t o water,

&,

i s o b t a i n e d as

[41

For measurements o f absorbances a t 2 5 O C , a t t h e 304-nm a b s o r p t i o n peak, a t an o p t i c a l p a t h l e n y t h o f 0.01 in, and assuming a F r i c k e - s o l u t i o n d e n s i t y of 1024 kg m-3 and a product o f E G(Fst++) = 352 x 10-6 m2 kg-1 Gy-1 [4], t h e expressions reduce t o

and

2.2

Design

A t t h e t i m e t h e s e r v i c e was f i r s t implemented as a stop-gap procedure, simplicity o f design and o p e r a t i o n was o f t h e essence. Making t h e expensive b u t re-usable stoppered q u a r t z spectrophotometer c e l l s an i n t e g r a l p a r t o f t h e F r i c k e d o s i ~ n e t e r s (see f i g . 1) reduces h a n d l i n g t i m e and p o s s i b l e sources of containi n a t i o n o f t h e Fricke s o l u t i o n .

An a1 t e r n a t i v e would be t o t r a n s f e r t h e s o l u t i o n f i r s t i n t o s p e c i a l l y c l eaned, d i sposabl e b o r o s i 1 i c a t e ampoul es ; f 1ame-seal t h e ampoul es w i t h o u t damage t : , t h e s o l u t i o n f r o m c o n t a c t w i t h gases escaping f r o m t h e heated g l a s s ; and keep t h e s o l u t i o n i n t h e sealed ampoules u n t i l ready f o r f i n a l readout. The s o l u t i o n would t h e n be t r a n s f e r r e d once rnore, t h i s t i m e i n t o a spectrophotometer c e l l t h a t would remain i n t h e spectrophotometer and would be f i l l e d , r i n s e d and r e - f i l l ed u n t i l t h e c o n t e n t s of a1 1 t h e ampoules was read out. Such a procedure seemed t o o e l a b o r a t e f o r a stop-gap s e r v i c e , b u t t h e adopted Because t h e system i n c o r p o r a t i n g unsealed dosirneters d l so has i t s draw-backs. F r i c k e s o l u t i o n i s c o r r o s i v e , t h e unsealed dosirneters have t o be shipped by c a r r i e r s o t h e r than t h e U.S. M a i l and f l o w n e i t h e r a t lo^ a l t i t u d e o r i n p r e s s u r i z e d compartments. F r i c k e s o l u t i o n i n unsealed c e l l s a1 so i s rnore prone t o succumb t o i n f l u e n c e s o f t h e e n v i ronment t h a n s o l u t i o n i n sealed ampoul es, causi ny a 1d r y e r dependence o f spurious absorbance y r o w t h 3 on d o s i ~ n e t e r h i s t o r y . The r e s u l t i n y a d d i t i o n a l u n c e r t a i n t y i n t h e dose i n t e r p r e t a t i o n would be unacceptable i n a NUS c a l i b r a t i o n s e r v i c e , b u t i s a c c e p t a b l e i n a s e r v i c e w i t h t h e p r i m a r y f u n c t i o n o f having t h e p a r t i c i p a n t s compare t h e i r a b i l i t y t o measure absorbed dose t o water w i t h t h a t o f t h e i r peers. The s e r v i c e was designed t o be r u n on a small s c a l e ( o f f e r e d t w i c e a year, n o t over f o r t y p a r t i c i p a n t s a t a t i m e ) , w i t h manual dosiineter p r e p a r a t i o n and a l ~ t o m a t i o no n l y i n t h e s p e c t r o p h o t o m e t r i c - r e a d o u t and d a t a hand1 i n g stages. A d i s c u s s i o n of a p o s s i b l e upgrading and expansion o f t h e s e r v i c e i s given i n s e c t i o n 2.4.
2.3

System Operati on Statistical distribution -of absorbance growth i n t h e - NBS unsealed system.

2.3.1

P r i o r t o t h e s t a r t of t h e s e r v i c e , an experiment was performed t o a s c e r t d i n t h e i n f l u e n c e of i r r a d i a t i o n l e v e l and s t o r a g e c o n d i t i o n s on absorbance growth d u r i n g a p e r i o d o f about f o u r weeks between p r e p a r a t i o n and f i n a l readout o f t h e F r i c k e s o l u t i o n k e p t i n t h e stoppered spectrophotometer c e l l s . The c e l l s were i r r a d i a t e d a t NBS t o d i f f e r e n t exposure l e v e l s , and one-ha1 f o f them were t h e n shipped c r o s s - c o u n t r y whi 1e t h e o t h e r ha1 f rernai ned a t N8S. There was no s i g n i f i c a n t dependence o f s p u r i o u s absorbance y r o d h on exposure l e v e l (and t h u s on absorbance l e v e l ) , and t h e r e was no s i g n i f i c a n t d i f f e r e n c e between t h e average absorbance growth o f shipped c e l l s and t h o s e rernai n i ng a t NBS, t h e average absorbdnce growth amounting t o between 0.003 and 0.004, which corresponds t o between U.8 and 1.1 G y t o t h e s o l u t i o n . Over t h e years, a record has Seen k e p t o f t h e standard d e v i a t i o n of t h e averaye absorbance growth on i d e n t i c a l l y p r e - i r r a d i a t e d F r i c k e - d o s i m e t r y c o n t r o l c e l l s, some of which were shipped and t h e r e s t rernai ned a t NBS. The d i s t r i b u t i o n o f t h e absorbance growths has a tendency t o be rnore s y m r w t r i c a l f o r t h e shipped b a t c h than f o r t h e b a t c h remaining a t NBS, which shows a " t a i l " on t h e s i d e o f l a r g e r absorbance growth.[3]

3 I n t h i s paper, t h e t e r m "spurious absorbance g r o w t h " i s used t o mean absorbance growth n o t caused by i o n i z i n g r a d i a t i o n but, e.g., by autooxidation.

2.3.2

I n t e r n a l q u a l i t y check on performance --o f individua ldosimeters. -

I n o r d e r t o check on t h e performance o f t h e F r i c k e dosimeters p r i o r t o t h e i r use, i t was decided t o p r e - i r r a d i a t e a l l t h e f r e s h l y - f i l l e d s p e c t r o photometric c e l l s , about 50 o r 60 a t a tirne, w i t h G°Co gammd r d d i a t i ~ n to a y t o water. T h i s procedure was adopted a f t e r i t l e v e l o f between 40 and 50 G had been e s t a b l i s h e d [3] t h a t t h e response o f t h e dosimeters t o 60C0 gamma I r r a d i a t i o n and readout r a d i a t i o n and t o h i yh-energy e l ectrorls vras a d d i t i v e . of each dosimeter b e f o r e a c t u a l use p e r m i t s ( a ) a s t a t i s t i c a l study o f t h e random v a r i a t i o n s frorn dosiineter t o dosimeter i n t h e response t o a g i v e n i r r a d i a t i o n l e v e l , as measured s p e c t r o p h o t o m e t r i c a l l y ; ( b ) t h e d e t e c t i o n and e l i m i n a t i o n frorn f u r t h e r use o f dosimeters w i t h responses f a r removed f r o m t h e mean f o r t h e p a r t i c u l a r batch; and ( c ) t h e e v a l u a t i o n o f t h e absorbed doses administered by t h e p a r t i c i p a n t s from h; yher (and t h e r e f o r e more p r e c i s e ) absorbance l e v e l s . I f a system employing sealed ampoules were adopted i n t h e f u t u r e , t h e advantages o f i n d i v i d u a l dosimeter readouts p r i o r t o shipment would be l o s t s i n c e t h e ampoules would have t o be re-opened and t h e s o l u t i o n P r e - i r r a d i a t i o n of a1 1 t r a n s f e r r e d t o s p e c t r o p h o t o ~ ~ ~ ec te erl l s f o r readout. dosimeters c o u l d c o n t i n u e i f r a i s i n g t h e absorbance l e v e l f o r t h e readout were s t i l l found t o be o f advantage, b u t a p o r t i o n o f each s o l u t i o n batch would have t o be s e t a s i d e f o r p r e - i r r a d i a t i o n as an i n t e r n a l q u a l i t y check. Since t h e dosimeters can be used f o r d e t e r m i n i n g doses up t o more t h a n 300 G y w h i l e p a r t i c i p a n t s a r e being asked t o d e l i v e r o n l y about 50 Gy, i t i s i n p r i n c i p l e p o s s i b l e t o use t h e same s e t o f dosimeters up t o s i x times, as l o n g as l i n e a r i t y b e t ~ e e no p t i c a l absorbance and absorbed dose has been e s t a b l i s h e d t o h o l d f o r t h e p a r t i c u l a r b a t c h over t h e range o f absorbances employed. I n p r a c t l c e , t h e dosimeters so f a r have never been used f o r lnore than one t e s t s e r i e s . But, s i n c e 1983, t h e number o f dosimeters requested f o r any one s e r i e s has exceeded t h e number o f dosimeters a v a i l a b l e . Therefore, two consecutive m a i l i n g s , about s i x t o e i g h t weeks a p a r t , Mere made p e r s e r i e s , u s i n g sorne o f t h e dosimeters f o r a second round o f i r r a d i a t i o n s , w i t h s a t i s f a c t o r y r e s u l t s . However, t h e r e a r e some i n d i c a t i o n s t h a t t h e r e p r o d u c i b i l i t y o f t h e dose i n t e r p r e t a t i o n decreases s l i g h t l y w i t h consecutive dosimeter use because o f an i n c r e a s e i n spurious absorbance growth and g r o w t h v a r i a b i 1 it y . For t h i s reason, t h e number o f avai 1 abl e spectrophotometer c e l l s and accessories was increased d u r i n g 1986.

-

2.3.3

I n t e r n a l qua1 it y checks on spectrophotometry [ 6 ]

Wave1 ength scale. Because o f spectrophotometer v a r i a b i l it y i t i s recommended t h a t t h e spectrophotorneter wavelength s c a l e be p e r i o d i c a l l y checked. It was decided t o perform t h i s check p r i o r t o each s e r i e s o f spectrophotometer readouts by d e t e r m i n i n g t h e wavelength s e t t i n g near 304 nm f o r which t h e f e r r i c - i o n absorbance shows a maximum, and t o make a l l readouts a t t h i s wave1 ength. Molar l i n e a r a b s o r p t i o n c o e f f i c i e n t f o r f e r r i c i o n s . It. i s f u r t h e r recommended t h a t t h e rnol a r l i n e a r a b s o r p t i o n c o e f f i c i e n t f o r f e r r i c i o n s f o r t h e p a r t i c u l a r spectrophotometer i n use- be determi ned. Thi s procedure has been f o l l o w e d throughout t h e years t h e F r i c k e - d o s i m e t r y s e r v i c e has been i n o p e r a t i o n , re-determinations having been performed whenever t h e r e was a change i n spectrophotorneter, spectrophotometer components o r spectrophotometer adjustment. The p r e p a r a t i o n o f t h e f e r r i c - i on s o l u t i o n i s d e s c r i b e d i n d e t a i 1 i n Appendix S2 t o t h e ASTM Standard [ 6 ] .

ICKU r e c e n t l y recornmended t h e use of a f i x e d p r o d u c t o f t h e molar l i n e a r The v a l u e recommended a b s o r p t i o n c o e f f i c i e n t and t h e f e r r i c - i on y i e l d . [5] f o r t h e product agrees t o w i t h i n 1 p e r c e n t w i t h t h e v a l u e based on our measured molar 1 inear a b s o r p t i o n c o e f f i c i e n t and t h e f e r r i c - i o n y i e l d used by The r e c e n t ICRU recommendations have now been i n c o r us t h r o u g h 1985 [7]. porated i n our procedure and a r e r e f l e c t e d i n t h e c o n s t a n t s g i v e n i n eqs. ( 3 ) and (4) ( s e c t - i n n 2.1). However, we p l a n t o c o n t i n u e t h e p r a c t i c e of re-determi n i ny t h e molar 1 inear a b s o r p t i o n c o e f f i c i e n t experimental l y when t h e need a r i s e s . Constancy and L i n e a r i t y . As a check on t h e constancy and l i n e a r i t y o f t h e spectrophotometer over t h e one- t o two-month p e r i o d o f any g i v e n t e s t s e r i e s , i t was sugyested t h a t an independent check be kept on these parameters by rledns o f absurbdnce ~neasurernents on s e v e r a l d i ' l u t i o n s o f a "1 g%" s o l u t i o n o f p o t a s s i urn n i t r a t e ( i .e., an aqueous s o l u t i o n c o n t a i n i ng 1 g o f p o t a s s i urn n i t r a t e per 100 crn3), which has an a b s o r p t i o n peak a t a wavelenyth o f about 302 nm, i.~., c l o s e t o t h e f e r r i c - i o n a b s o r p t i o n peak used f o r F r i c k e dosilnetry.[8] Since then, Standard Reference M a t e r i a l SRM 2031, c o n s i s t i n g o f metal-on-quartz f i l t e r s f o r t h e v e r i f i c a t i o n o f s p e c t r o p h o t o m e t r i c absorbance s c a l e s i n t h e u l t r a v i 01 e t , has become avai 1a b l e. [9] Thi s m a t e r i a1 may rep1 ace the potassiu~n-nitratesolution i n the future. 2.4 Upgrading t h e S e r v i c e

I n p r e p a r a t i o n f o r a p o s s i b l e upgrading o f t h e F r i c k e - d o s i m e t r y measurement assurance s e r v i c e t o a c a l i b r a t i o n s e r v i c e , s w i t c h i n g t o a system
employing sealed dosimeters i s contemplated i f a d d i t i o n a l experiments p r o v e

t h a t such a system would l o a d t o a more u n i f o r m s p l ~ r i o u s absorbance growth and t h e r e f o r e t o a h i g h e r r e p r o d u c i b i l i t y i n dose i n t e r p r e t a t i o n f r o m absorbance d i f f e r e n c e s . For t h i s purpose, a semi-automatic ampoule-seal i n g 11nit was c o n s t r u c t e d . I t s design i s p a t t e r n e d a f t e r a u n i t i n use by t h e N a t i o n a l Physical Laboratory i n Teddington, England. A1 so, thought i s being g i v e n t o automati ng t h e r i n s i ny and f i11 i ng o p e r a t i o n s o f t h e spectrophotometer c e l l s o r g l a s s ampoules. F u r t h e r p r e p a r a t i o n s f o r u p y r a d i n y t h e s e r v i c e would e n t a i l s t u d i e s f o r o b t a i n i n y t h e c o r r e c t i o n s r e q u i r e d t o produce adequate agreement d i t h t h e r e s u l t s of c a l i b r a t i o n s i n terms o f absorbed dose t o water by o t h e r methods. Such c o r r e c t i o n s may be needed because o f t h e p h y s i c a l inhornogenei t i e s i n t r o d u c e d i n t h e dosimeter-phantom systern by t h e presence o f g l a s s and o f an a i r space. Upgrading t h e s e r v i c e rnay a l s o r e q u i r e d t l e a s t a temporary i n c r e a s e i n t h e s t a f f assigned t o t h e p r o j e c t d u r i n g t h e p r e p a r a t i o n p e r i o d , and probably some permanent s t a f f r e d s s i ynrnents o r a d d i t i o n a l cherni s t r y t r a l n l n y of t n e present s t a f f .

3. 3.1

DESCRIPTION O F SYSTEM AND OPEKATING PKOCEOUKE The Physical Setup. (Most o f t h e i t e m s enumerated a r e s h o w i n t h e f i g u r e s o f s e c t i o n s 3.2 and 3.3.)

A t t h e t i m e t h i s document i s b e i n g prepared, t h e setup c o n s i s t s o f :
s around 150 c y l i n d r i c a l 10-mm path1 e n y t h q u a r t z spectrophotometer c e l l s w i t h q u a r t z wi ndows and ground-y 1ass stoppers ; e L u c i t e racks, b u i l t t o o r d e r i n t h e NBS Shops, each h o l d i n g 10 s p e c t r o photometer c e l l s i n two rows o f f i v e , each row b e i n g i d e n t i f i e d by a l e t t e r and each c e l l l o c a t i o n by a number;
o t h e chemical s: c o n c e n t r a t e d (96%) s u l f u r i c acid, sodi urn c h l o r i d e , ferrous-ammonium s u l f a t e , and potassium n i t r a t e , a l l o f reagent yrade;
o two y l ass-stoppered 2000-cm3 g l a s s v o l u m e t r i c f l a s k s f o r p r e p a r i ng and s t o r i n y t h e rri cke s o l u t i o n ;

e one g l ass-stoppered 500-cm3 g l a s s v o l u m e t r i c f l ask f o r p r e p a r i ng and s t o r i ng t h e potassium n i t r a t e sol u t i o n ;
GI two 500-ca3 y l a s s wash b o t t l e s , each w i t h p l a s t i c t u b i n g and a r u b b e r b a l l o o n f o r pressure f i l l i n g t h e c e l l s w i t h e i t h e r s p e c i a l l y p u r i f i e d d i s t i l l e d water4 o r F r i c k e s o l u t i o n t h r o u g h a y l a s s tube drawn i n t o a narrow nozzl e;

o a s u c t i o n pump w i t h p l a s t i c t u b i n g connected t o a small g l a s s b o t t l e w i t h droppiny p i p e t t e f o r emptying t h e c e l l s ;

access t o a w a t e r - p u r i f y i n g s e t u p ;
s access t o two e l e c t r o n i c scales, one having a 0.1 kg c a p a c i t y and 1-my s c a l ? d i v i s i o n s , and t h e o t h e r having an 1-kg c a p a c i t y ;

-

a an a c r y l i c p l a t f o r m w i t h a s u r f a c e r u l e d i n 2.5-crn squares f o r s u p p o r t i n y t t l e spectrophotometer c e l l s h o r i z o n t a l l y i n a v e r t i c a l 60Co gamma-ray beam;
a

access t o an u l t r a s o n i c c l e a n e r eqllipped w i t h a s t a i n 1 e s s - s t e e l 1 i n e r ;

e access t o an up-to-date, computer-compatible spectrophotometer w i t h good o p t i c a l p r o p e r t i e s , equi pped w i t h t e m p e r a t u r e - c o n t r o l f o r t h e c e l l compartment ;

s

access t o a micro-computer,

f o r d a t a a c q u i s i t i o n and d a t a h a n d l i n g ; and

e v a r i o u s accessories, e.g., t h r e e d u s t - f r e e c a b i n e t s , a graduated g l a s s c y l i n d e r , beakers, a weigni ng dish, a s p a t u l a , tweezers wl t n f l e x i b l e t i p s , a funnel

.

4Unless o t h e r w i s e noted, t h e d i s t i l l e d water r e f e r r e d t o l a t e r always i s t h e speci d l 1y p u r i f i e d d i s t i l l e d water produced j n t h e w a t e r - p u r i f y i n y setup, t h a t was used t o prepare a1 1 t h e s o l u t i o n s .

I n i t i a l l y , a1 1 y l assware t o be used f o r t h e F r i c k e s o l u t i o n was cleaned w i t h h o t concentrated s u l f u r i c acid, t h e b o t t l e s were f i l l e d w i t h t h e a c i d and t h e n heated on a h o t - p l a t e u n t i l t h e a c i d almost S o i l e d ; t h e o t h e r items were immersed i n almost b o i l i n g s u l f u r i c a c i d and r i n s e d several t i m e s i n d i s t i l 1ed water b e f ~ r eand a f t e r t h e s u l f u r i c - a c i d c l e a n i n g procedure. The s p e c t r o photometer c e l l s and t h e i r stoppers were in i t i a1 l y r i nsed s e v e r a l t i m e s w i t h d i s t i l l e d water. A f t e r b e i n g placed i n t h e i r racks, t h e y were f i l l e d s e v e r a l times w i t h d i s t i l l e d water and emptied between f i l l i n g s a1 t e r n a t e l y by s u c t i o n and shaking. The c e l l s then were f i l l e d w i t h 0.8-normal s u l f u r i c a c i d and stoppered; racks and c e l l s were i~nrnersed up t o t h e c e l l necks i n a b a t h o f s i n y l y - d i s t i l l e d water f o r 1 5 minutes o f u l t r a s o n i c cleaning. Also, t h e cross s e c t i o n of t h e 60Co gamma-ray beam i n room B034 used f o r t h e p r e - i r r a d i a t i o n o f a l l F r i c k e dosimeters was i n i t i a l l y mapped a t t h e i r r a d i a t i o n d i s t a n c e o f 147.9 cm f r o 1 1 t h e source by means o f r e a d i nys o f a 1aboratory-standard i o n i z a t i o n chamber placed on t h e support p l a t f o r r n and rnoved across t h e hparn cross s e c t i o n i n 7.5-crn steps t o o b t a i n a g r i d o f absorbance-correction f a c t o r s f o r a l l F r i c k e - d o s i m e t e r l o c a t i o n s . The r e s u l t i n g a r r a y o f c o r r e c t i o n f a c t o r s i s s h o w i n f i g u r e 2 f o r t h e source and d i s t a n c e used through 1985. A t t h e t i m e o f + r e p a r a t i o n o f t h i s document, t h e source i s being replaced by a source o f h i g h e r a c t i v i t y i n room 8035, i n o r d e r t o reduce t h e i r r a d i a t i o n time.
The prucedures discussed above a r e n o t repeated p r i o r t o each subsequent use. The stoppered c e l l s ( s t i l l f i l l e d w i t h F r i c k e s o l u t i o n , and s i t t i n g i n t h e i r r a c k s ) , t h e wash b o t t l e s , t h e beaker f o r washiny t h e stoppers, and u t e n s i l s such as wei y h i n g d i s h , s p a t u l a , tweezers, s u c t i o n b o t t l e , a r e s t o r e d i n t h e d u s t - f r e e c a b i n e t s whose doors had been r e p l a c e d by cheese c l o t h t o prevent condensation o f water on t h e s t o r e d a r t i c l e s . P r i o r t o t h e preparat i o n o f a new s e t o f dosimeters, a l l glassware i s t h o r o u g h l y r i n s e d w i t h d i s t i l l e d water.

3.2

P r e p a r a t i o n o f Dosimeters and Check on t h e i r Performance

Preparing t h e F r i c k e s o l u t i o n , f i l l ing t h e spectrophotometer c e l l s and s t a r t i n g t h e performance check ( p r e - i r r d d i a t i o n of t h e f i r s t b a t c h o f between 50 and 60 c e l l s ) t a k e s a t l e a s t one day. P r i o r t o s t a r t i n g , a t l e a s t s i x oncgal 1on we1 1-cleaned brown g l ass b o t t l e s equi pped w i t h screw caps 1ined w i t h aluminum f o i l a r e f i l l e d w i t h t h e s p e c i a l d i s t i l l e d water from t h e waterp u r i f i c a t i o n system ~ n an i t a i ned by t h e Dosimetry Group o f t h e I o n i z i ny R a d i a t i o n D i v i s i o n . The system p r e s e n t l y c o n s i s t s o f one h i gh-capaci t y Raven s t i l l and t h e M i l l i - K O 60 system o f t h e M i l l i p o r e Corporation, equipped w i t h one organic a b s o r p t i o n stage, two d e i o n i z i n g stages and one f i l t r a t i o n stage. I n s t e a d o f g i v i n g a lenythy d e s c r i p t i o n o t t h e procedure, c o p i e s a r e shown i n t h e f o l l o w i n g o f t y p i c a l payes from d a t a books, g i v i n g t h e step-by-step r e c o r d o f t h e procedures f o r p r e p a r i n y t h e F r i c k e dosimeters and c a r r y i n y out t h e i n t e r n a l qua1 i t y checks on dosimeter performance.

2

4

6

8

1 0

12

1 4

1 6

18

C O L U M N NUMBER

Figure 2.

Mapping t h e Cross Section o f t h e Cobalt-60 Gamma-Ray Beam i n Room 8034, Used f o r P r e - I r r a d i a t i o n ; scale: 1 cm = 2.5 cm e n c i r c l e d numbers: o t h e r numbers : s o l i d - l i n e envelope: dashed l i n e : c o r r e c t i o n f a c t o r s from data p o i n t s in t e r p o l ated c o r r e c t i o n f a c t o r s

52 l o c a t i o n s w i t h c o r r . f a c t o r s

G

1.015

extending envelope t o i n c l u d e 10 f u r t h e r l o c a t i o n s , w i t h c o r r . f a c t o r s < 1.019

Preparing th e s o l u t i ons (a) Weighing t h e i n g r e d i e n t s (sample f r o m Data Book 837, pp. 160 and 163) S u l f u r i c Acid, Baker reagent grade, 96.3p er ce n t , f re sh - (see f i g . 3 ) graduate c y l i n d e r i n beaker, t a r e d on M e t t l e r balance model H 1200 46 crn3 o f H,S04 i n t o c y l i n d e r poured wefyht o f a c i d 84.45 g 6 delivered s 84.05 g i n t o 2000-crn3 f l a s k A graduate c y l i n d e r i n beaker, t a r e d a g a i n poured 46 cm3 of H , S O , i n t o cylinder
weight o f acid
5

-

-

delivered

- -- s

-83.90g

53.50

y , i n t o 2000-cm3 f l a s k B

6

Ferrous-arnmoni urn s u l f a t e , same b o t t l e as f o r l a s t t e s t ~ e r i e s ,weighed ~ . --on M e t t l e r balance, model H K ( s e e fig . 4) d i s h alone tne salt should be is d i s h alone the s a l t should be 4.13160 g 0.78430 g 4.915909 5 4.91585 g, i n t o 2000-cm3 f l a s k B 4.13162 g 0.78430 y 4.91592 9 4.91596 g i n t o 2000-cm3 f l a s k A

9

.

*

is

.

5

Sodium c h l o r i d e , same b o t t l e as f o r l a s t t e s t s e r i e s , 5 weighed on M e t t l e r --balance H 1 6 T G e f i g . 4) ---------d i s h alone a t h e salt should be d i s h alone the s a l t should be is d i s h alone 4.13162 - - - - - - . - ---0.11690 4.24852
a
a

s
g

m

a

4.13163 g 0.11690 g into2000-cm3flaskA
5

. . 44.24553-c .24894g, . . . . . 4.13156 y

5All

reayents are p e r i o d i c a l l y rep1 aced.

6Pi-ior t o adding t h e weighed i n g r e d i e n t s , a l l f l a s k s had been f i l l e d p d r t i a l l y

w i t h water. Note t h a t , throughout t h e t e x t , t h e t e r m "water" u n l e s s o t h e r w i s e s t a t e d i s used t o mean t h e s p e c i a l l y d i s t i l l e d water from t h e water p u r i f i c a t i o n system d e s c r i b e d ill s e c t i o n 3.2 (p. 14).

Figure 3.

deigiliny the S u l f u r i c Acid

Note rubber apron dnd f a c e s h i e l d .

F i g u r e 4.

Wei ghi ny t h e S a l t s .
The weighed p o r t i o n s a r e t r a n s f e r r e d q u a n t i t a t i v e l y f r o m t h e

weighing d i s h i n t o t h e v o l u m e t r i c f l a s k s through a c l e a r , d r y funnel, and washed down w i t h water from t h e wash b o t t l e .

Potassium n i t r a t e , same b o t t l e as f o r l a s t t e s t s e r i e s , weighed on M e t t l e r balance H 16
II

d i s h alone the s a l t should be is
0

a
8

a

a

s

4.13376 5.00000 ---9.13376 9.13366

g g g

a
9

g i n t o 500-crn3 f l a s k

d i s h alone

4.13350g

A l l f l a s k s f i led t o neck j u n c t i o n w i t h water a t about l l : 0 0 a.m. (b) F i n i s h i n g t h e stock s o l u t i o n s -

A f t e r having allowed enough t i m e f o r a l l s o l i d i n g r e d i e n t s t o d i s s o l v e c o m p l e t e l y and f o r t h e s o l u t i o n t o r e t u r n t o room temperature:
e A l l v o l u m e t r i c f l a s k s a r e f i l l e d w i t h water t o t h e i r marks and stoppered ;
o The F r i c k e - s o l u t i o n f l a s k s a r e shaken about 50 t i m e s , by t u r n i n g them upside down and back again w i t h a r o t a r y motion (see f i g . 5 ) ; d u r i n g t h i s procedure, stoppers a r e 1oosened p e r i o d i c a l l y t o p e r m i t a i r pressure t o equalize.

3.2.2

F i l l i n g t h e spectrophotometer c e l l s (see f i g . 6 ) Sample o f C e l l - R i n s i n g and - F i l l i n g Record ( f r o m Data Book 837, p. 161)

( a ) R i n s i n g w i t h Water cells cells cells cells sucked shaken sucked shaken out out out out and and and and filled filled filled filled with with with with water, water, water, water, finished finished finished finished

-

10 min. r e s t 11:20 a.m.; 10 min. r e s t 1330 p.m.; 10 min. r e s t 1:46 p.m.; 10 min. r e s t .

11 a.m.;

71n 1986, t h e f u n c t i o n o f t h i s s o l u t i o n was t a k e n over by a standard r e f e r e n c e m a t e r i a l . (See s e c t i o n 3.3)
8A

c l o s e t o 1.00000 g% s o l u t i o n was r e q u i r e d a t t h e time, because t h e s o l u t i o n was used f o r a l o n g - t e r m constancy check of t h e spectrophotometer's absorbance scale. To prepare such a s o l u t i o n , b o t h t h e weighing d i s h and t h e s a l t have t o be i n temperature and r e l a t i v e - h u m i d i t y e q u i l i b r i u m w i t h t h e balance (and t h e room). Repeated weighings, about one m i n u t e a p a r t , have t o be made u n t i l weight constancy i s reached. T h i s procedure i s n o t r e q u i r e d when t h e potassium n i t r a t e s o l u t i o n i s used s i m p l y t o e s t a b l i s h t h e l o c a t i o n o f t h e absorbance peak and o f absorbance-scale l i n e a r i t y .

9 P r i o r t o adding t h e weighed i n g r e d i e n t s , t h e f l a s k was f i l l e d p a r t i a l l y w i t h water.

Figure 5.

Aerating the Solution. Aerating prior t o f i l l i n g of individual spectrophotorneter c e l l s ensures t h e same degree of i n i t i a1 aeration of t h e dosimeters, Normally, rubber aprons are worn during t h i s process.

Figure 6. Fill i ny the Spectrophotometer Cells with Fricke Solution. Singly d i s t i l led water bathes the racks and the outside of the c e l l s .

( b ) -Ferrous-Sul fa t e Rinses c e l l s sucked c e l l s sucked c e l l s sucked last (final) out and f i l l e d , o u t and f i l l e d , o u t and f i l l e d , f i l l , completed finished finished finished a t about 2:08 2:32 3:00 3:40 p.m.; 10 min. r e s t p.m. ; 10 min, r e s t p.m.; 10 min. r e s t p.m.

A l l c e l l s stoppered by about 4 p.m.; d i s t i l l e d water; l e t d r y o v e r n i y h t . l o

racks and c e l l s washed w i t h s i n y l y

P r e - i r r a d i a t i on w i t h cobal t - 6 0 gamma r a y s
rack.

p p

P r i o r t o p r e - i r r a d i a t i o n , spectrophotornetry i s done on t h e c e l l s of one (Sp~r.t.rnphotnmetry i s d i s r ~ . r s s e d i n ,nore d e t a i l i n s e c t i o n 3.3.) This f u r n i s h e s t h e average backyround absorbance r e q u i r e d f o r o b t a i n i n g t h e n e t absorbance of t h e p r e - i r r a d i a t e d c e l l s f o r a check on t h e G-value o f t h e p a r t i c u l a r b a t c h o f F r i cke s o l u t i o n . F i g u r e 7 shows t h e p r e - i r r a d i a t i o n setup i n room B 034, used t h r o u g h 1985; f i g u r e 2 (paye 10) t h e a s s o c i a t e d beam c r o s s s e c t i o n ; and t a b l e 1 a bdlflplt2 uT t h e dbsurbdnce r e c o r d i n one rack, o b t a i n e d p r l o r t o i r r a d i a t i o n . Table 1. Sample, Absorbances of C e l l s Before P r e - i r r a d i a t i o n , Required f o r Check on G-Val ue and E G. Product, from Data Book 837, page 99. a Cell Designation Absorbance (Average of 15 r e a d i n g s , and I Side a

stands-rd

devi a t i on) Side b

a ~ l lreadings done w i t h a s l i t w i d t h corresponding t o 2 nm i n wavelength, a t a
f 0.05"C. The d e s i g n a t i o n s , " s i d e a" and " s i d e b y " i d e n t i f y t h e c e l l windows f a c i n g t h e u l t r a v i o l e t source. W e r o u t i n e l y r e v e r s e t h e c e l l s f o r t h e second r e a d i ng s i n c e specks o f d i r t on t h e c e l l windows may i n f l u e n c e t h e r e a d i n g t o a d i f f e r e n t e x t e n t i n t h e two geometries.

w a v e l e n y t h s e t t i n g o f 301 nm and a teniperdture o f 25.00

l O I f d e s i r e d , i r r a d i a t i o n o f f i r s t b a t c h o f 50 t o 60 c e l l s may be s t a r t e d immediately a f t e r d r y i n g t h e c e l l s i n d i v i d u a l l y w i t h a l i n t - f r e e c l o t h .

F i yure 7.

Pre-i r r a d i a t i o n w i t h Cobalt-60 Gamma Radiation i n Room 0034. The surface of t h e support i s ruled, w i t h rows and columns rnarked as i n f i g u r e 2 (page 15). The fixed-distance support v i s i b l e a t shoulder h e i g h t i s not i n t h e beam.

Sample o f P r e - i r r a d i a t i o n Record ( f r o m Data Book 856, p. 39) Exposure r a t e on day o f l a s t c a l i b r a t i o n ( A p r i l 24, 1985): 46.98 R/h.

Exposure r a t e s i n a i r , a t p o i n t o f c e l l i r r a d i a t i o n s : -0.0003601 x 195 = 43.79 K/h. On Novernber 6, 1985, 1 = 46.98 e -0.0003601 x 199 = 43.73 R1h. On November 10, 1985, 1 = 46.98 e The number 0.0003601 i s t h e decay c o n s t a n t f o r t h e c o b a l t - 6 0 gamma r a y source, and 195 and 199, r e s p e c t i v e l y , i s t h e number o f days from t h e l a s t c a l i b r a t i o n t o r o u y h l y t h e rniddle o f t h e planned i r r a d i a t i o n s . Correspondi ng absorbed-dose r a t e s t o t h e F r i cke s o l u t i o n : On November 6, 1985, On November 10. 1985.

bF bF

= 43.79 = 43.73

x x

0.961 = 42.09

rad/b (0.4209 Gylh).

0.961 = 42.03 r a d / h (0.4203 Gy/h).

The f a c t o r , 0.961, was o b t a i n e d e m p i r i c a l l y as t h e r a t i o o f DF/X,ll averaged over s i x t e e n d e t e r m i n a t i o n s d u r i n g t h e p e r i o d o f 1967 t h r o u g h 1974. (Sce D a t a DF was computed from measured n e t absorbance, u s i n g t h e Book 767, page 34.) recommended G-value f o r c o b a l t - 6 0 garnma r a y s and t h e measured v a l u e of t h e molar 1i n e a r a b s o r p t i o n c o e f f i c i e n t (see t a b l e 5, page 23). For each of t h e two s e t s of i r r a d i a t i o n s , a r e c o r d i s k e p t o f t h e f o l l o w i n g data: Time s e t and t i m e d e l i v e r e d ; d a t e and t i m e when t i m e r was s t a r t e d and d a t e when t i m e r stopped; t i m e r r e a d i n g a t b e g i n n i n g and end o f i r r a d i a t i o n ; t o t a l l o s e d e l i v e r e d t o t h e F r i c k e s o l u t i o n , as computed from r a t e and time. 3.2.4 R e s u l t s o f p r e - i r r a d i a t i ons and t h e i r a p p l i c a t i o n t o i n t e r n a l qua1 it y control of shown this not

A sample o f t h e spectrophotornetry r e c o r d o f a l l c e l l s a f t e r p r e i r r d d i a t i o n and p r i o r t o shipment i s shown i n t a b l e 2. The d i s t r i b u t i o n correspondi ng t o t h e d a t a i n t a b l e 2 i s posi t i o n - c o r r e c t e d absorbances l2 i n t a b l e 3 and i t s s t a t i s t i c a l a n a l y s i s i s g i v e n i n t a b l e 4. Studies o f t y p e a r e used t o e l i m i n a t e c e l l s w i t h very h i g h and v e r y l o w absorbances, s i n c e i t cannot be r u l e d o u t t h a t t h e i r absorbance growth w i t h tirne does shuw c h d r a c t e r i s t i c s d i f f e r e n t f rum t h a t o f o t h e r c e l l s.

llNote t h a t , f o r c o b a l t - 6 0 gamma rays, DF = 1.004 Dw 1.004 x 0.869 X pen,w = 0.970 X i n a i r , where DF and Dw a r e t h e absorbed doses t o t h e F r i c k e s o l u t i o n and t o water, r e s p e c t i v e l y , and pen ,w i s t h e energy-absorption c o e f f i c i e n t o f water f o r c o b a l t - 6 0 garnma rays. Thus, t h e e f f e c t o f t h e q u a r t z window o f t h e c e l l amounts t o a decrease i n absorbed dose o f r o u y h l y one percent. 12For d e t a i l s on p o s i t i o n c o r r e c t i o n s , see s e c t i o n 3.1, f i g u r e 2.

Table 2.

Sample o f Spectroghotometry Record o f A l l C e l l s A f t e r Prey o f Cobalt-60 Gamma R a d i a t i o n , P r i o r t o i r r a d i a t i o n w i t h 50 G (Frorn Data Book 837, p. 104.) Readou Geomet ry Side a Correction Factor t o Absorb- Temp. ~bsorbance~ ante "C B e f o r e Shipment Side b Absorb- Temp. ance "C Average Absorbance, GeometrycorrectedC

Cell No.

Position d u r i ng Pre-Irrad. Row, Column

----

-----

0-1 -2 -3 -4 -5 P- 1 -2 -3 -4 -5

Q-1

-2 -3 -4 -5 R-1 -2 -3 -4 -5
S-1

-2

-3
-5

-4
etc.

10 11 10 10 10 10 10 10 9 9 9 9 9 9 8 8 8 8 8 8 8 7 7 7

, 12

, , ,
, ,

, ,
, , 3

,
, , , ,

,
,

,

,
, 9 ,

,

7 , e t c . etc.

14 5 7 9 11 13 15 4 6 8 10 12 14 3 5 7 9 11 13 15 4 6 8 10

1.017 1.014 1.007 1.003 1.000 1.004 1.010 1.018 1.010 1.004 1.000 1.002 1.006 1.012 1.014 1.007 1.004 1.003
etc.

0.2172 0.2149 0.2178 0.2231 0.2265 0.2231 0.2188 0.2189 0.2205 0.2188 0.2308 0.2213 0.2238 0.2253 0.2209 0.2188 0.2207 0.2208 0.2224 0.2217 0.2163 0.2159 0.2232 0.2188 0.2192
etc.

24.92 24.93 24.93 24.96 24.94 24.94 24.92 24.95 24.94 24.94 24.99 24.97 24.97 24.99 25.01 24.99 24.99 24.98 25.00 24.97 25.03 25.03 25.04 25.02 25.01
etc.

I

0.2173 0.2129 0.2166 0.2219 0.2226 0.2232 0.2178 0.2184 0.2140 0.2193 0.2306 0.2221 0.2239 0.2247 0.2220 0.2189 0.2243 0.2203 0.2231 0.2211 0.2179 0.2170 0.2227 0.2208 0.2192
etc.

24.92 24.90 24.94 24.93 24.93 24.90 24.93 24.94 24.95 24.93 24.97 24.97 24.98 24.98 24.96 24.97 24.97 24.98 25.00 25.00 25.02 25.00 25.04 25.03 25.04
etc.

0.2188 0.2169 0.2196 0.2238 0.2255 0.2238 0.2201 0.2224 0.2203 0.2206 0.2314 0.2217 0.2248 0.2273 0.2254 0.2210 0.2234 0.2206 0.2232 0.2227 0.2197 0.2195 0.2245 0.2207 0.2139
etc.

---a~ re l al d i n g s done w i t h a s l i t w i d t h c o r r e s p o n d i n g t o 2 mrn i n wavelength, wavelength s e t t i n g of 301 nrn. The d e s i y n a t i o n s , " s i d e a" and " s i d e b," i d e n t i f y t h e c e l l windows f a c i ny t h e u l t r a v i o l e t source.
at a

b ~ h i si s a c o r r e c t i o n t o t h e exQosure d u r i n g p r e - i r r d d i d t i o n , p r o p o r t i ondl t o absorbance.

which i s

he

s ~ n a l ltemperature f l u c t u a t i o n s recorded d i d n o t w a r r a n t a c o r r e c t i o n .

Tab1 e. 3

Sample of D i s t r i b u t i o n o f P o s i t i o n - C o r r e c t e d Absorbances (From t a b l e 2; see D a t a Book 837, p . 109.)

-- --- . -- - --

Ahsorbance Interval

L

Cell Desiyndtion
- - - - - - - - - -- -- - - -- -- - - - - - - - - - - . - . . . -- . . -. .-- - . .-- - - - - - - - - - - - - --- - - -- - . . .. . . .

. - -- -

Cel I s

ti- 1 5-4
C-3

6-4

F i r s t Readout S e s s i o n

Second Readout S e s s i o n

NOTE:

The c e l l s d e s i g n a t e d 4-4,

1-5,

X-4,

V-5,

and 4 - 1 were e l i m i n a t e d .

Table 4.

S t a t i s t i c s , from Sample R e s u l t s Shown i n Table 3. Rook 837, p. 108.) A1 1 120 Cel I s 0.2212 Fi r s t Half (60 Cel l s ) 0.2205

(See a l s o Data Second H a l f (50 Cel I s ) 0.2218

Quantity Averaye Absorbance Standard D e v i a t i o n absol u t e percent Maxi mum Keadi ng a l l cells after elimination of outliersa
M i fli m u m Readi ny

-- ----- --- ---- --- ------------- - -- -- --- -- --------- -------- --- -- - --- - -----

0.2314 0.2296

0.2275 0.2251

0.2314 0.2296

a l l cel l s b

a~ee Note on t a b l e 3

The r e s u l t s shown i n t a b l e s 1 and 3 a r e f u r t h e r used t o o b t a i n a check on Ihe d e t a i l s a r e shown t h e [;-value o f t h e p a r t l c u l a r batch o t k r l c k e s o l u t i o n . i n tab1 e 5. The f ir s t q u a n t i t y , t h e average posi ti on-corrected absorbance growth due t o p r e - i r r d d i a t i o n , i s c a l c u l a t e d as t h e average absorbance from t a b l e 4 minus t h e average absorbance o f t h e t e n uni r r a d i a t e d c e l l s from t a b l e 1. The t h i r d q u a n t i t y , t h e G-value, i s ,obtained w i t h t h e a i d of t h e f i r s t and second q u a n t i t i e s and t h e experimental l y determined molar 1 inear absorption c o e f f i c i e n t ( i n both S T and conventional u n i t s ) ; i t i s compared 7 ] . The l a s t q u a n t i t y i s t h e p r o d u c t of t h e w i t h t h e recommended G-value [ G-val ue obtained f o r t h e p a r t i c u l a r F r i cke sol u t i on and t h e 1inear in01 a r a b s o r p t i o n c o e f f i c i e n t (see s e c t i o n 2.3.3) measured f o r our spectrophotometer, again given i n both S I and conventional u n i t s ; i t i s compared w l t h t h e Both t h e G-value o b t a i n e d f o r o u r recommended value f o r t h i s product [4]. s o l u t i o n , our geometry, and t h e product E G a r e seen t o be, on t h e average, Therefore, t h e w i t h i n 0.3 percent o f t h e r e s p e c t i ve recommended v a l ues s w i t c h taken i n 1986 f r o m i n t e r p r e t i n y t h e absorbed dose a d m i n i s t e r e d by t h e p a r t i c i p a n t s by means o f t h e measured value o f E, t h e recommended G-value, and our e m p i r i c a l geometry c o r r e c t i o n ( s e e f o o t n o t e 11, page 19), t o i n t e r p r e t i n g t h e absorbed dose by means o f t h e now recommended product, E G, d i d n o t a f f e c t our r e s u l t s s i g n i f i c a n t l y .

.

3.3

Spectrophotometry : Reproduci b i 1 it y

.

Ensuring Long- and Short-Term Consistency and

Preceding absorbance measurements, t h e F r i cke-dosimeter c e l l s a r e cleaned w i t h d i s t i l l e d water, u s i n g l i n t - f r e e c l o t h s ( " O p t i c C l o t h " made by Texwipe). C u r r e n t l y , t h e i r absorbance i s measured w i t h a Cary, Model 219, spectrophotorneter, as shown i n f i g u r e 8. D u r i n g t h e measurernents ( " r e a d o u t s " ) , t h e temperature i n t h e c e l l compartment i s kept c l o s e t o 25OC by means of a

re1a t i v e l y l a r g e - v o l ume (0.02 m3) t h e r m o s t a t i c a l l y c o n t r o l l e d c i r c u l a t i n g water bath. I n o r d e r t o b r i n g t h e temperature o f t h e dosimeter c e l l s c l o s e t o compartment temperature p r i o r t o readout, t h e loaded dosimeter racks are ztnred f o r about 30 minutes i n t h e b a t h compartment, above t h e water l e v e l . One c e l l a t a t i m e i s t h e n placed manually i n t h e c e l l compartment f o r readout on both sides. The t i m i n g of t h e readout i s computer-controlled. After a f i fteen-second delay , t h e r e i s a t h i rty-second readout p e r i o d , i n which f i f t e e n absorbance r e a d i ngs are a1 t e r n a t e d w i t h f i f t e e n temperature r e a d i ngs. The readings a r e averaged a u t o m a t i c a l l y and s t o r e d f o r o f f - 1 ine a n a l y s i s . The c e l l i s t h e n manually t u r n e d f o r readout on t h e o t h e r side, and t h e procedure i s repeated, b u t w i t h o u t t h e i n i t i a l delay. Control 1ing t h e readout schedule i n t h i s way ensures c o n s i s t e n t absorbance readings even though complete temperature e q u i l ib r i um ,nay not have been reached.

I n o r d e r t o check spectrophotometer performance, each readout session i s preceded by a number o f spectrophotometer t e s t s . F i g u r e 9 and t a b l e s 6 and 7 g i v e sample records o f such t e s t s .
F i g u r e 9 shows t h e r e c o r d o f a d e t e r m i n a t i o n o f t h e wavelength corresponding t o t h e f e r r i c - i o n a b s o r p t i o n peak, a t which t h e absorbances were t o be read d u r i n g the p a r t i c u l a r session. S h i f t s of a few nanometers a r e n o t unusual. (Note t h a t t h e a b s o r p t i o n peak f o r f e r r i c i o n s g i v e n i n t h e l i t e r a t u r e i s 304 nm.) Table 5. Check on G-Value and Product E G f o r t h e P a r t i c u l a r Sample Batch o f F r i c k e S o l u t i o n (from sample data shown i n t a b l e 4 and f i g u r e 10, and from eq. ( 3 ) o f s e c t i o n 2.1).
wantities A l l 120 C e l l s F i r s t Series o t bU C e l l s Second Series o f 60 c e l l s

Average posi tion-corrected absorbance growth "Ai rr Absorbed dose t o F r i c k e s o l u t i o n (OF) G-value z 0.0977 d. & ! i n u n i t s o f mol J 1
/E

0.2212-0.0413~0.1799

0.2205-0.0413=0.1792

0.2218-0.0413=0.1805

50 Gh! DF 1.615 x 10-6 mol J-1 1.608 or 15.551100 eV Value recornended by ICRU: 1.61
x x

50 G y 10-6 mol J-1 1.620 or 15.49/100 eV
x

50 G y 10-6 mol J-1 or 15.601100 eV evb

(using measured value o f E)

10-6 mo1 J-1 o r 15.5/100

[7]

Product

E G r 0.0977 dirr/DF i n u n i t s o f mz kg-1 6 y - I

351.5xlO-~rn2kg-lGy-~ 350.2~10-6m2kg-1Gy-1 352.7~10-6m2kg-1Gy-1 352 x
10-6

Value recommended by ICRU:

mz ~ g - 1 ~y-1 C41

a~rm ASTM Standard

E

1026-84 161.

b~or both high-energy electrons and cobalt-60 gamna rays.

F i gure 8.

Spectrophotometry Attendant i s i n s e r t i n g spectrophotorneter c e l l i n t o temperaturec o n t r o l 1ed readout cornpartrnent o f spect rophotometer. The c i r c u l at i n g water bath i s a t r i g h t , t h e computer d i s p l a y i n t h e center.

Wave Length, n m
F i g u r e 9. Sample P l o t , Automatic Scan o f F e r r i c - I o n Absorbance-vs-Wave1 ength S e t t i n g , Requi red t o Establ ish Wave1ength S e t t i n g f o r Absorption Peak. Spectrophotornetry was done a t a s e t t i n g o f 301 nm. (From Scan speed corresponded t o 0.1 nrn/s, Data Book 837, page 108.) s l i t width t o 0.2 nrn.

'able 6.

Sample, Absorbances o f 1 g% Potassium N i t r a t e S o l u t i o n , Obtained as a Check on t h e R e p r o d u c i b i l i t y o f Absorbance Readings Throughout t h e Data Roughly S i x Weeks Required t o Complete One ~ e s t . (From ~ Book 837, page 163.) Readout Session Absorbance f o r Cel

-

f ir s t session, s t a r t

-

s i d e b Absorbance .7 380

f i r s t session, end Before Shipment -.----second session, s t a r t

session s t a r t A f t e r Shipment
session end

a~ readings ll done w i t h a s l i t w i d t h corresponding t o 2 nm i n wavelength, a t a wavelength s e t t i n g o f 301 nm. 'The designations, "side a " and "side b," i d e n t i f y t h e c e l l windows f a c i n g t h e u l t r a v i o l e t source.

Table 7.

Constancy and L i n e a r i t y o f Cary Spectrophotometer, Model 16, between A p r i l 1971 and A p r i l 1974. The study was c a r r i e d o u t by measuring absorbance a t two l e v e l s o f c o n c e n t r a t i o n o f potassium n i t r a t e a t t h e a b s o r p t i o n peak. Date Peak Location n m 302.5 302.5 302 .O 302.5 3.0 2 .5 302.5 302.0 Net absorbance 1 gX KNO, 0.7071a 0.7082~ 0.7067~ 0. 7060a 0 .708ga 0.7073~ 0.7069~ Twice n e t absorbance 0.5 g% KNO, 0.7073~ 0.7164 0.7067 0.7014 0.7094 0.7058 0.7024~

A p r i l 1971

November 1971 A p r i l 1972 November 1972 A p r i l 1973 November 1973 A p r i l 1974

a~rom f i t t e d graphs

Table 6 g i v e s a sample r e c o r d o f t h e absorbances obtained on two c e l l s f i l l e d w i t h 1 g% p o t a s s i u m - n i t r a t e s o l u t i o n measured b e f o r e and a f t e r t h e two readout sessions p r i o r t o shipment o f t h e F r i c k e dosimeters and before and a f t e r t h e readout session some s i x weeks l a t e r , a f t e r dosimeter r e t u r n . The averages o f t h e absorbances a r e seen t o have remained e s s e n t i a l l y constant, i n d i c a t i n g spectrophotometer r e p r o d u c i b i l i t y . Known d i l u t i o n s p r o v i d e a check on absorbance-scale 1in e a r i t y . Table 7 shows t h e net (background-corrected) absorbance values f o r a 1 g% s o l u t i o n and t w i c e t h e corresponding values f o r a 0.5 g% s o l u t i o n , f o r an e a r l i e r spectrophotometer model, followed over a p e r i o d o f t h r e e years. Such a long-term absorbance-constancy check i s f a c i 1it a t e l l i f e x a c t l y t h e same c o n c e n t r a t i o n o f potassium n i t r a t e i s used each time. Since t h e spectrophotometer i n use s i n c e 1980 (Cary, Model 213) i s even more re1 i able than t h e Cary, Model 16, p o t a s s i urn-ni t r a t e readi ngs 1 a t e r were taken o n l y f o r t h e 1 g% s o l u t i o n (see t a b l e 6). S t a r t i n g i n 1986, system l i n e a r i t y and constancy t e s t s s i m i l a r t o t h o s e performed w i t h potassium n i t r a t e up t o then, w i l l be performed w i t h metal-onq u a r t z f i l t e r s , SKM 2031 [ 9 ] . Use o f these f i l t e r s w i l l save time. But w h i l e they have been a v a i l a b l e s i n c e 1980, they s t i l l r e q u i r e f u r t h e r p e r i o d i c checks o f long-term absorbance constancy. These checks a r e c a r r i e d o u t by t h e NBS Center f o r Analytic Chemistry. 3.4 Dose I n t e r p r e t a t i o n and Report t o P a r t i c i p a n t s

The average absorbance growth f o r t h e F r i c k e s o l u t i o n contained i n t h e spectrophotometer c e l l s measured b e f o r e and a f t e r shipment o f t h e c e l l s i s used t o compute t h e absorbed dose t o water, Dw ( i n grays), administered by t h e p a r t i c i p a n t s . Using eq ( 4 ) ( s e c t i o n 2.1), one obtains:

where dAirr i s t h e d i f f e r e n c e between t h e absorbance b e f o r e and a f t e r shipment o f t h e c e l l s i r r a d i a t e d by t h e p a r t i c i pants13 and dAKP i s t h e average d i f f e r e n c e between t h e absorbance b e f o r e and a f t e r s w e n t o f t h e shipped and .. unshipped ( "shi ppi ng " and "home") c o n t r o l c e l l s. sampi e val ues o f for not bAS ) fur c u n l r u l c e l l s and o f i n d i v i d u a l values o f (&Ai 10 shows f u r t f i e r i r r a 8 i a t e d c e l l s a r e shown i n column 6 o f t a b l e 8.14 ~ l g u r e t h e d i s t r i b u t i o n o f t h e i n d i v i d u a l values o f dsp from t a b l e 8, and gives t h e

-

IsHere, t h e absorbances before shipment are n o t geometry-corrected (as a r e those i n t a b l e 2) s i n c e t h e absorbances o f t h e q u a r t z windows o f t h e spectrophotometer c e l l s and o f t h e F r i c k e s o l u t i o n due t o p r e - i r r a d i a t i o n drop out when t h e d i f f e r e n c e s are formed. 14The sample record shown i n t a b l e 8 pre-dates t h e s w i t c h t o S I u n i t s f o r absorbed dose. It a l s o pre-dates I C R U Report 35, recommending t h e use of a f i x e d value f o r t h e product o f E G i n t h e computation o f absorbed dose from o p t i c a l absorbance. The absorbed-dose val ues shown were computed w i t h a G-value of 15.5/100 eV (non-SI) and a measured value f o r E of 217.7 m* mol-1. The complete r e p o r t included i n t h e appendix i n c o r p o r a t e s t h e same data.

Tab1 e 8. Sampl e o f Spectrophotometry Record A f t e r Shi pment and Associated (From Data Book 837, p. 104 and 105.) Absorbed-Dose ~ n t e r ~ r e t a t i o n . ~

D i f f e r e n c e , Absorbed Dose Abs. 0 . Readout Af. e r Shipment D i f f e r - Partict o Water, r a d Side b Side a Cell ( A A ~ - ) ipant ence AbsorbTemp. No. Absorb- Temp. NBS No. P a r t i c i p . ance OC OC X ance Or asP

-

0.2214 0.4132
A -

25.14 25.10 25.08
24.95

+ 0.0043
t0.1963

-5483

-

-5440

--

--

17

-0.75

-

0.2209
U.4i)bl

+ 0.0044
-+ 0.2005
tU.1808 + 0.1774

-SUSU

-SOUU

0.4039

24.85 24.88 24.94 25.12 25.16 25.15 25.12 25.13 25.16 25.16 25.18 25.16 25.16 25.19 25.18

4956 5600 5903 5906 5995

5000 6000 6000 6000 6000

-0.4278 0.4331 0.4338 0.4322 0.2197 0.2325 0.2262 0.2277 0.4052 0.4117 0.4015 0.4115 0.4088 0.2266 0.2224 0.2208 0.4378 0.4505

-0.99 + 0.89

18

+ 0.2113 + 0.2114
+ 0.2146

+ 7.14 + 1.64 + 1.59
+ 0.08
19

+ +

0.0005 0.0020 + 0.0042

---

--+0.0038 + 0.1767' + 0.1857 + 0.1785 + 0.1829 t0.1845 t0.0034

---

----

---

--

--

4935 5188 4985 5110 5154

--

4826 4990 4840 5045 5067

-

-

----

2.21 3.82 2.91 1.27 -1.69

20

- --- -25.18 + 0.0015

25.23 25.19 25.24 25.22 25.21

+ 0.0032
+ 0.2167
+0.2238 + 0.2216 +0.2255

--

--

6054 6251 6189 6298

5830 6020 6030 6120

- 3.70
-3.70 2.57 -2.83

-

21

. . -

----

\

a~ readings ll done w i t h a s l i t w i d t h corresponding t o 2 nm i n wavelength, a t a wavelength s e t t i n g o f 301 nm. The d e s i g n a t i o n s , " s i d e a" and " s i d e b," i d e n t i f y t h e c e l l windows f a c i n g t h e u l t r a v i o l e t source. Note t h a t t h i s t a b l e was prepared pr'ior t o t h e s w i t c h t o S I u n i t s and t h e use o f t h e p r o d u c t E G f o r colnputSng absorbed dose.

I
L

Shipped Controls

(

22)

aJ
4

E

z
-.002

=

X
X X
0

X X X X X X X X X X X X X X X X X
-002 .004 -006 .008

Cut -off for Average

,0310-

X
.010

\I
,012 .014 .016 .018

X
.020

Spurious Absorbance Growth

Home Controls

(22)

L-

n

OJ

X

X

X

Cut-off for Average

E

z
X
-.002

2

X X X X X X X X X X X X
,002

X
DO6

X X X X X
j008 .010

,260 +

v
.012

X X
-014 .016 ,018 .020

0

.004

Spuricus Absorbance G r o w t h

O b t a i n i n g t h e Average Spurious Growth : Average, aASp

----22 home c o n t r o l s

22 s h i p p i ny c o n t r o l s

I1

-

--------

0.0038 0.0043 0.0040
1 . 1

+
+

U.0026

(stand. dev.) (stand. dev.) (stand. dev.)

t 0.0027

a1 1 44 c o n t r o l s
corresponding t o

0.0038

2 1.1

Gy

F i g u r e 10.

Sa~nple, A n a l y s i s o f Spurious Absorbance Growth MSp, of Shipp'lng and Home C o n t r o l s . (From Data Book 837, p. 107.) For t h e assessment o f t h e u n c e r t a i n t y i n t h e c o r - r e c t i on f o r s p u r i o u s absorbance growth ( t a b l e 9, p. 42), absorbance growth was averaged o v e r t e n t e s t series

.

averages o f t h e p l o t t e d data. The average o f t h e growth o f b o t h s h i p p i n g and home c o n t r o l s combined was used t o compute t h e absorbed-dose values shown i n col~rmn 7 o f t a b l e 8, which - a f t e r roundiny t o t h r e e s i g n i f i c a n t f i yures - i s i n c o r p o r a t e d l n t o t h e r e p o r t sent t o t h e p a r t i c i p a n t s . The r e p o r t a l s o conta'ns p l o t s o f t h e d i s t r i b u t i o n s o f t h e d i f f e r e n c e s between assigned doses and doses r e p o r t e d by t h e p a r t i c i p a n t s . A sample o f a complete r e p o r t t o t h e p a r t i c i p a n t s i s i n c l u d e d i n t h e appendix. 3.5 U n c e r t a i n t i e s i n * t h e Dose I n t e r p r e t a t i o n

I n a measurernent-assurance program o f t h e n d t u r e o f t h e e l e c t r o n dosimetry uni f o r ~ nt i y s e r v i c e , t h e u n c e r t a i n t i e s i n t h e i n d i v i d u a l dose i n t e r p r e t a t i o n s a r e of major i n t e r e s t . Two independent methods were used t o a r r i v e a t values f o r t h e o v e r a l l u n c e r t a i n t y . One i n v o l v e d a s e t o f measure~nentsof t h e d i f f e r e n c e s between dose i n t e r p r e t a t i o n s and a c t u a l l y d e l i v e r e d doses, and the o t h e r i n v o l v e d estimates o f t h e u n c e r t d j n t i e s a s s o c i a t e d w i t h t h e i r l d i v i d u d l s t e p s l e a d i n g t o a dose i n t e r p r e t a t i o n . T h e results a r e s h o w n i n t a b l e 9. To a r r i v e a t t h e t o t a l u n c e r t a i n t y e x p e r i m e n t a l l y ( f i r s t method), F r i c k e dosirneters were exposed a t t v ~ ol e v e l s o f c o b a l t - 6 0 gainma r a d i a t i o n and shipped t o a number o f p a r t i c i p a n t s who kept t h e packages f o r several days and t h e n r e t u r n e d thern t o iVBS f o r e v a l u a t i o n i n t h e usual manner.[4] The standard d e v i a t i o n o f t h e d i f f e r e n c e between t h e dose cornputed from exposure and t h a t deterini ned froin spectrophotometry o f the i n d i v i d u a l F r i c k e dosirneters was about 1.5 percent, corresponding t o an o v e r a l l u n c e r t a i n t y o f t h r e e tirlles t h i s (The " o v e r d l l " u n ~ e r . t d i n L y i~ con~ t d n d a r dd e v i d l i o n , o r z 4.5 percent. sidered t o have approximately t h e c h a r a c t e r o f a 99% c o n f i d e n c e 1 i m i t . ) I n t h e second method, t h e o v e r a l l u n c e r t a i n t y i n t h e dose i n t e r p r e t a t i o n was estimated f rorn t h e component u n c e r t a i n t i es i nvol ved in t h e in d i v i d u a l proI n t a b l e 9, t h e component u n c e r t a i n t i e s n o t based on repeated cedural steps. medsurements a r e e s t i m a t e d a t a l e v e l o f approximately one standard d e v i a t i o n , so t h a t they can be t r e a t e d l i k e standard d e v i a t i o n s . They a r e added i n quadrature t o o b t a i n a "combined" u n c e r t a i n t y , ~ h i c h i s m u l t i p l i e d by t h r e e t o o b t a i n t h e o v e r a l l u n c e r t a i n t y . The r e s u l t s o f t h e t ~ methods o a r e seen t o be comparable. The assessment o f t h e u n c e r t a i n t i e s i n t h e dose i n t e r p r e t a t i o n excludes t h e u n c e r t a i n t i e s i n t r o d u c e d by t h e s p e c t r d l p e r t u r b a t i o n s a r i s i n g from t h e use o f q u a r t z c e l l s and a p o l y s t y r e n e phantom r a t h e r than a homogeneous water medium. T h i s e x c l u s i o n i s j u s t i f i e d i n a rneasirrernent qua1 it y assurance s e r v i c e . I f t h e s e r v i c e were ever upgraded i n t o a c a l i b r a t i o n s e r v i c e , c o n s i d e r a t i o n would have t o be given t o whether o r n o t a c o r r e c t i o n f o r t h e e f f e c t o f t h e s p e c t r a l p e r t u r b a t i o n s was r e q u i red, and t h e a s s o c i a t e d u n c e r t a i n t i e s would have t o be assessed. It i s expected t h a t these u n c e r t a i n t i e s would be small compared t o t h e u n c e r t a i n t y i n t h e s p u r i o u s absorbance growth between readouts, which probably c o u l d be decreased m a t e r i a l l y by t h e use o f a sealed system. (See s e c t i o n 2.4.) 4. SAFETY CONSIDERATIONS

t h e F r i c k e d o s i m e t ~ r sa r e those u s ~ r a l l ytaken

The precautions taken d u r i n g t h e p r e p a r a t i o n , hand1 i n g , and s h i p p i n g o f in a c h e m i s t r y l a b o r a t o r y t h a t handles c o r r o s i v e l i q u i d s such as s u l f u r i c a c i d : Old c l o t h e s and rubber

Table 9.

U n c e r t a i n t i e s i n t h e Dose I n t e r p r e t a t i o n s

Estimated Procedure

1
a

Uncertai ntya, percent

F ir -s t Method
U n c e r t a i n t y i n dose in t e r - p r e t a t i o n d e r i v e d f ro~n repented

measurements i n a speci a1 l y d e s i yned experiment

1

1.5

Overall uncertai ntye Second Method U n c e r t a i n t y estimated f o r each i n d i v i d u a l s t e p i n v o l v e d i n t h e dose i n t e r p r e t a t i o n s : C a l i b r a t i o n o f spectrophotometer Measurement o f absorbance
b

4.5

b

C o r r e c t i o n f o r s p u r i o u s absorbance growth between f i r s t and second readoutC Choice o f r e f e r e n c e value,
E

G = 352

x

10-6 m 2 kg-'

Gy-1

b

Combi ned u n c e r t a i n t y ( d

Overall uncertai n t y( e l

a ~ the t one standard d e v i a t i on 1eve1

.

b ~ a s e don t a b l e 5.4,

ICRU Report 35 [4].

' ~ a s e d on t h e measurement of t h e p e r c e n t spontaneous growth f o r a l l c o n t r o l dosimeters i n t e n t e s t s e r i e s , a t an average electron-dose l e v e l corresponding t o an absorbance growth o f 0.20 ( i .e., about 56 Gy). d ~ n dvii d u a l u n c e r t a i n t i e s added i n quadrature. e ~ h r e etimes t h e u n c e r t a i n t y f o r Method 1 o r t h r e e times t h e "combined" u n c e r t a i n t y f o r Method 2.

aprons are worn by t h e s t a f f ; t h e concentrated s u l f u r i c a c i d i s t r a n s p o r t e d and s t o r e d i n a rubber " c a r r y i n g s l i n g , " and face s h i e l d s are worn by t h e s t a f f d u r i n g p o u r i n g and weighing o f t h e acid; a c i d - p r o o f composites, glass o r s t a i n l e s s s t e e l , a r e used as supports o f a l l c o n t a i n e r s o f t h e F r i c k e s o l u t i o n ; a1 1 l i q u i d waste i s poured i n t o s t a i n l e s s - s t e e l s i n k s equipped w i t h glass-1 ined waste pipes; t h e p o l y s t y r e n e blocks c o n t a i n i n g t h e stoppered Fricke-dosineteter c e l l s are sealed i n p l a s t i c bags and packed p r o f e s s i o n d l l y i n card-board boxes f o r t r a n s m i t t a l t o t h e p a r t i c i p a n t s by p r i v a t e c a r r i e r r a t h e r than t h e U.S. Mail; t h e box l a b e l s are marked w i t h a note c a u t i o n i n g t h e shipper t o s t o r e t h e boxes i n t h e pressurized compartment o f h i g h - f l y i n g a i r c r a f t . A1 so, t h e persons hand1 i n g t h e potassium n i t r a t e are cautioned t o handle i t w i t h care because o f i t s p o t e n t i a l l y e x p l o s i v e nature.

[I] For d e f i n i t i o n s of t h e r a d i a t i o n - d o s i m e t r y q u a n t i t i e s and u n i t s ( b o t h S I and s p e c i a l ) used i n t h i s document, see R a d i a t i o n Q u a n t i t i e s and U n i t s ; ICRU Report 19, I n t e r n a t i o n a l Commi s s i o n o f R a d i a t i o n U n i t s and Measurements, Bethesda, MD, 1971. [2] A P r o t o c o l f o r t h e D e t e r m i n a t i o n o f Absorbed Dose from High-Energy Photon and E l e c t r o n Beams, Task Group 21, R a d i a t i o n Therapy Committee, AAPM; Med. Phys. l O ( 6 ) : 741-771, 1983.
[3] E h r l i c h , M . and Lamperti, P. J. Uni forrni t y o f H i gh-Energy Electron-Beam C a l i b r a t i ons, Phys. Hed. Rio1 14(2), 305-314, 1969.

.

[4] R a d i a t i o n Dosimetry: E l e c t r o n Beams w i t h Energies Between 1 and 50 MeV; ICRU Report 35, I n t e r n a t i o n a l Commission o f R a d i a t i o n U n i t s and Measurements, Bethesda, MD, 1984. [5] See, e.g., s e c t i o n 5.3.2 o f ICRU Report 35 ( p r e c e d i n g r e f e r e n c e ) .

[6] Standard Method f o r Using t h e F r i c k e Dosimeter t o Measure Absorbed Dose i n Water, ASTM D e s i g n a t i o n E 1026-84, 1985 Book o f ASTM Standards, S e c t i o n 12, American S o c i e t y f o r T e s t i n g and M a t e r i a l s , P h i l adel p h i a, Pennsyl vani a, 1985. [7] R a d i a t i o n Dosimetry: X Rays and Gamna Rays w i t h tlaximurn Photon E n e r g i e s Between 0.6 and 50 MeV; ICRU Report 14, I n t e r n a t i o n a l Commi s s i o n on R a d i a t i o n U n i t s and Fleasurements, Rethesda, !ID, 1969. [8] Mavrodineanu, Q., communi c a t i o n . NBS Center f o r A n a l y t i c a l Chemistry, p r i v a t e

[9] Flavrodi neanu, R. and Bal dwi n, J . R., Standard Reference M a t e r i a1 s : Metal -On Q u a r t z F i 1 t e r s as a Standard Reference i.lateria1 f o r Spect rophotomet r y - SRM 2031 ; NBS Speci a1 Publ ic a t ion 260-68; U. S. Government P r i n t i n y O f f i c e , Washi nyton, D.C., 1980. A d d i t i o n a l References t o t h e NBS - F r i c k e Dosimetry S e r v i c e E h r l i c h , M. anrl Lamperti, P. I . , Electron-Therapy Dosimetry, pp. 365-370, NBS Special Publ i c a t i o n 456, Proceedi nys o f a Symposium on t h e Measurernents f o r t h e Safe Use o f R a d i a t i o n , h e l d a t NBS i n March, 1976; S. P. F i v o z i n s k y , e d i t o r ; U.S. Uepart~nent o f Commerce, N a t i o n a l Bureau of Standards, 1976. Soares, C. G. and E h r l i c h , M., NBS T r a c e a b i l i t y Program f o r R a d i a t i o n Therapy, pp. 89-97, Proceedi ngs o f a Meeting on Traceabi 1 it y f o r I o n i z i ny R a d i a t i o n Medsurernents, h e l d a t NBS i n !Say, 1980; H. T. Heaton 11, e d i t o r ; I1.S. Department o f Commerce, N a t i o n a l Bureau o f Standards, 1982.

*

Referenced 1 it e r a t u r e i s avai 1 a b l e on request from t h e Dosimetry Group, I o n i z a t i o n R a d i a t i o n D i v i s i o n , Center f o r R a d i a t i o n Research.

Appendix 1

Forrns Used i n W r i t t e n Exchanges w i t h P a r t i c i p a n t s

NATIONAL BUREAU OF STANDARDS UNIFORMITY CHECK, DOSIMETRY OF HIGH-ENERGY ELECTRON-BEAMS To All Participants: If you plan to participate in the service, you will need a polystyrene phantom. Directions for its construction are given in the "Protocol for the Dosimetry of High Energy Electrons", SCRAD, Physics in Medicine and Biology, Vol. 11, No. 4, p. 505,
October 1 9 6 6 , with the exception that the recess required for

the dosimeter units supplied by NBS is of different dimensions from the one described in the Protocol. The enclosed figure, from NBS SP 250-4 (1986), is a picture of the unit that will be sent to you for exposure. It consists of a stoppered spectrophotometer cell filled with ferrous-sulfate solution, held firmly in place in a polystyrene parallelepiped of outer
dirnerlsions

The dosimeter unit should fit snugly into the phantom recess. (It is suggested that the airspace on all sides be kept to a width of less than 0.5 mm.) The electron beam should be perpendicular to the 7.62 cm x 5.08 cm planes of the dosimeter unit. The center of the spectrophotometer cell should be in the center of the 10 cm x 10 cm field. The dosimeter may be irradiated at any phantom depth where the dose rate across the
thickness of the dosimeter i,s known. Because the dosimeter

averages absorbed dose over a depth of 1 cm, you should take this into account in your dose computation, especially below 10 MeV, since absorbed dose changes significantly over this depth, even near the depth-dose peak.

ANNOUNCEMENT TO ALL PAST PARTICIPANTS

UNITED STATES DEPARTMENT OF COMMERCE Netionel Bureau of Btenderda

Announcement of the Next Uni~ormityStudy of Dosimetrv of Hish-Enerav Electron Beams We plan to ship the next batch of ferrous-sulfate dosimeters between <dates>. Please let us know imediately whether or not you wish to participate, and if so, send us your purchase order before <date> and tell us how many dosimeters you require. Currently the fees are <cost> for the basic set of three dosimeters (two for irradiation and one uni~rad~ated control), and <cost> for each additional dosimeter. When you receive the dosimeters, please expose them according to tne airections tnat were glven to you previously. Administer between 50 and 80 Gy to water using a 10 cm x 10 cm field size. Return the dosimeters to us as soon as possible, preferably within three working days. Please do not tamper with the dosimeter unlts. After exposure, place them in the zip-lock bag and seal the bag for safety reasons. Use the same packing material, or material similar tc that used by us. Send the package by the same carrier as received, and mark the box, "Please ship in pressurized compartment or at low altitude". Please send return shipment prepaid to: Dr. Christopher Soares C-210 Rad Phys Building National Bureau of Standards Route 270 & Quince Orchard Rd. Gaithersburg, MD 20899 Sincerely.

Christopher Soares Dosimetry Group Note: It would be appreciated ~t you returned the dosimeters within three worklng days from the day of receipt. We are reserving the right. to refuse participation in the current study if the dosimet.ers are not returned within ten workina days after recelpt .

ANNOUNCEMENT TO GROUPS THAT INDICATED THEIR INTENTION TO PARTICIPATE, BUT DID NOT SUBMIT A PURCHASE ORDER

UNITED STATES DEPARTMENT OF COMMERCE National Buraau of Standards
Galtharsburg Mar {land

20e99

Announcement of the Next Uniformity Study of Dosimetry of High-Energy Electron Beams We plan to ship the next batch of ferrous-sulfate dosimeters between <dates>. since you nave already indicated your intention to participate, all that is required now is your purchase order. Currently the fees are <cost> for the basic set of three dosimeters (two for irradiation and one unirradiated control), and <cost> for each additional dosimeter. When you receive the dosimeters, please expose them according to the directions that were given to you previously. Administer between 50 and 80 Gy to water using a 10 cm x 10 cm field size. Return the dosimeters to us as soon as possible, preferably within three working days. Please do not tamper with the dosimeter units. After exposure, place them in the zip-lock bag and seal the bag for safety reasons. Use the same packing material, or material similar to that used by us. Send the package by the same carrier as received, and mark the box, "Please ship in pressurized compartment or at low altitude". Please send return shipment prepaid to: Dr. Christopher Soares C-210 Rad Phys Building National Bureau of Standards Route 270 & Quince Orchard Rd. Gaithersburg, MD 20899 Sincerely,

Christopher Soares Dosimetry Group

Notei It would be appreciated if you returned the dosimeters within three working days from the,day of receipt. We are reserving the right to refuse partlclpation In the current study if the dosimeters are not returned within ten working days sfter receipt.

ANNOUNCEMENT - TO GROUPS THAT INDICATED THEIR INTENTION TO PARTICIPATE, --------------AND SUBMITTED A PURCHASE ORDER --------------

8 . " "'4,.
UNITED STATES DEPCLRTMENTOF COMMERCE Nmtlonml Bureau of Stsndmrdm

Announcement of the Next Uniformity Study of Dosimetry of High-Enerw Electron Beams we plan to ship the next batch of ferrous-sulfate dos~meters between <dates>. When you receive the dosimeters, please expose them according to the directions that were given to you previously. Administer between 50 and 80 Gy to water using a 10 cm x 10 cm field size. Return the dosimeters,to us as soon as possible, preferably within three working days. Please do not tamper with the dosimeter units. After exposure, place them in the zip-lock bag and seal the bag for safety reasons. use the same packing material, or material similar to that used by us. Send the package by the same carrier as received, and mark the box, "Please ship in pressurized compartment or at low altitude". Please send return shipment prepaid to: Dr. Christopher Soares C-210 Rad Phys Building National Bureau of Standards Route 270 & Quince Orchard Rd. Gaithersburg, MD 20899 Sincerely,

Christopher Soares Dosimetry Group
Nnte:

Tt would be appreciated if you returned the dosimeters

within three working days from the day of receipt. We are reserving the right to refuse participation in the current study if the dosimeters are not returned within ten working days after receipt.

P l e a s e c o m p l e t e t h i s f o r m and s h i p i t bac'k w i t h t h e e x p o s e d d u s i metier s Dosimeter Number Dose* (Gy) E l e c t r o n Energy
( MeV

After
reseal

i r r a d i a t i o n , p l a c e t h e dosimeters i n t h e zip-lock
the bag
for

bag and

or m a t e r i a l
"F=GILE. CfiBIN."

s a f e t y r e a s o n s . U s e the s a m e p a c k i n g m a t e r i a l s i m i l a r t o t h a t used by u s . R e t u r n package b y t h e

same t y p e o f c a r r i e r a5 y o u r e c e i v e d i t 9 hark:ed: I F SENT BY AIR AT HIGH ALTITUDES,

KEEP I N PRESSURIZED

If a t a l l p o s s i b l e .

after
-Fur-

receipt.

r e t u r n t h e p a c k a y e w i t h i n t h r e e working d a y s P l e a s e s e n d r e t ~ ~ l -s n h ~ p m e n tp r e p a ~ d .
car

averaged over

e n c r q l e s 2 11:) M e V , p l e a s e 1 1 1 d i c a t e whether t h e ' d e p t h o f the d c ~ s i r n e t e r .

r 1 ~ 1 t . YUU

U .S. DEPARTMENT OF COMMERCE
N A T I O N A L B U R E A U OF S T A N D A R D S G A I T H E R S B U R G . M A R Y L A N D 20899

REPORT OF TEST

'-he elx-locje:j tables axid f i c j u r e r , c c n t a i r ~t h e I . . E ~ L \ ~ ~f ~ S the cur-1-er?t s t \ . ! d y f o r a l 1 p a r - t i c i p a n t j . A g r o u p : ~ ! . ~ m b c r -w a s a s r , i c _ l n ~ d t o path p a r t i c i l ~ a : . v t .T h e c 1 o s i r n e t ; e r . ; a r - e I i s t e d b y gr-or.~parid n o t n e c e s c A r i l y i r ; a l p h a b e t i c a l o r - d e : - . T h i s p r - o c e d u r a . t - ~ h lc i nut g i v i n g away a p a ! - t i c i p a i - ~ t ' s i d e n t i t y t o t h e r e s t o f i;ht-. p a r - t i . - i p a n t s . e r l a t j l e s pact1 p a l - t i c : i p a l i t t o ci3er.k. h i s s t a r l d i r t q anltir-lc~ h i s p r e r s w i t h r - r g a i IS t o a c c u r a c \ , t a s wei.1 a s c o ~ i s i s t e r ? c y of pel- f o r m a i - i c e , . T h e 1-ed ai- r o w i 17 t t ~ et a b l e ~ o i l - I t st o t t ~ ec,;i.-c.cl;.\ n u m b e r o f ?;he p ~ ~ i . t i c l p a l - i ti:\ t w h r 3 ~ 1t ! ? e ~ ~ r n r n u 1.0r.1 i ~ i L ~ C - ~ z~ i dtc i l - ~ ! ; ~ ~ d . The i i q r ~ r e sg i v r ~.3 statj.st:i-a1 S L I Y \ / E : Y 3f' t h e :-csinl t.2. C i ~ l - . eva!l-l..3--tic1-1 p r o i ~ d u ! - e c l i 7 1 . l est;:mat,er! e r r o ! ;?re t h o s e d i z c : u s . i e t j i n ,, .~l-~c:~ F r icl,c.-D~s~mi:.t!.y $;er'~,ice o f t h r . ! \ l a t i o n d l B t ~ r - e o l iaf ' , - ! s i i < j a r 1 3 5 " . M . E:t?1-1 i ~ t . 1 .N l 3 5 F , ; > ~ ~ i if3u!)1 il l c : & k i ~ 1 ~ . 25('.)-.&. : {A)-! F C pi-c.!rjl~< f, \-:f 2 C; TJ ,.. , 1 . ...' q,:. k: I? . .d -. ." C;.rf'" '. IJ?,!::~ hi; t h c? ] c ? t. t- o r i s a n d :!,:tbi:i 1 t - r;Ti clawma rays. A p p l i c d t i ~ r - i n.f t h p 3 1 - c d u c t 0 - F t h e i a r m e r l y u:..ed <~;il!.:t.r-f u r F 2 n d r.jn!.iZd c AII,:.~; KP'-.a*-c ..., - , - .=r g i s i ~ r !a ! ? = o r b e d - d n . . c . : ../+li!fs t.c) Iar-cqes- Lty c? T2+.c*,c)1-c f I . ( 1 ( 3 5 .

,-.

,

' :

"

Group No.

Dcsi meter Designation

NPS

fibsorbed Dose

Participant
{Gy)

( G y to w a t e r )

Dose Difference (Pct. of NES Dose)
'

Irradiated with:

Appendix 2.

Sample o f Report t o P a r t i c i p a n t s

U.S. DEPARTMENT OF COMMERCE
N A T I O N A L B U R E A U OF S T A N D A R D S GAITHERSBURG. MARYLAND 20899

R E P O R T OF TEST
June 26, 1986 To: All Participants in the Spring 1986 Uniformity Study of Dosimetry in Hiqh-Energy Electron Beams The enclosed tables and figures contain the results of the
current study for all participants. A group number was assigned
I

to each participant. The dosimeters are listed by group and not necessarily in alphabetical order. This procedure, while not giving away a participant's identity to the rest of the participants, enables each participant to check his standing among his peers with regard to accuracy as well as consistency of performance. The red arrow in the table points to the group number of the participant to whom the communication is addressed. The figures give a statistical survey of the results. Our evaluation procedure and estimated error are those discussed in "The Fricke-Dosimetry Service of the National Bureau of Standards1', M. Ehrlich, NBS Spec'al Publication 250-4 (1986). An EG product m2 kgmt oy-l was used for both electrons and of 352 x cobalt-60 gamma rays. Application of the product of the formerly used values for E and G would cause NBS-assigned absorbed-dose values to be larger by a factor of 1.005. Yours sincerely, ,
Y

Christopher G. Soares, Physicist
Ionizing Radiation Division

Center for Radiation Research Enclosures P.S. This is to remind you that our dosimeters average absorbed dose over a depth of 1 cm. At electron energies less than 10 MeV you should take this into account in your dose computation, since absorbed dose changes significantly over this depth, even near the depth-dose peak.

Report o f Test, Continued

Gr-ouo
No.

I ! o s i meter Desi U I - ) a t 1 on

Absur-l~ed Dn!z.e Pc~!seD i f f e t - . e n c : e NBS F'articiaant (F'ct. of iGv i n walzer) ((3~) NBS Dose!

It-racliated

with: 8 M e 0 el 13 Me\! el 10 MeV el
30 MeV '7.5 MeV b MeV 12 MeV 22 MeV

2 , . 2 62 (1)
LC;'

.

c d c?.

1

el el
el

e l el

6 MeV el
17

MeV

~l

l 15 MeV e
6 MeV el

9 MeV el
13 MeV el l 17 MeV e

20 MeV el
10 ML' >:rv

6 MeV el 9 MeV e l 12 MeV e l 15 MeV e l 19 MeV el Cobal t 6 0
7 MeV el
18 MeV e l 12 MeV el

l 9 MeV e
l 12 MeV e l b MeV e 1 5 MeV e l

Cobal t -60 Cuba1 t-60
8 MeV el

l 1 0 MeV e

Report of Test, Continued
G~OLIP

No.

UC~ meterS~ Desi q n a k i c)n

Absorbed Dose D o s e U i f f er7enc:e NBS Par-ticipant (Pet. c 2 f ( G v i n water) (Gv) NHS Uosej

Irr-adiated

with:
10 M E ? ~ el 10 M e V el
'7 M e V el 1 8 : ) M e V el 12 M e V el 9 Me0 e l 12 M e V el i U M e V el

--

12

L- 1 L-2
L-4

59.4 60.9
56. 5
I ='7

(50. ( : ) [ : I
60 00

.

4-1. 1 -1.3 -11.5

13

L-5 M- 1 M-3 M-4
M-5

.J,,

.5

5 0 0(1)
50. 00

.

50. 6
60. 5 58.9

50 ( 3 3
63.68 57. 9 0 6i.9&

.

-6.5

-1 0
+5.3

.

-0.5
- 6 . C)

61.0
C

N-2 N-3 N-4 N-5

3 50. €3 51.1 50.8
dl.

5(:)(:)(:I
c

. 50 .(1)(1) 65.57 49.64
59.85
(53. (:)C)

50. (30
dU. 00

-2.4 -1.4 -2. 0 -1.5 -4.5 -7.1 +I. 6 +1.4 +44. Y -2.0 I 2. +2 (1)

7 MeV 10 M e V 15 M e V 20 M e V 10 9 12 15

el

el
el el

0- 1 0-3 0-4 0-5 P-2

66.5 56.3 62.6 64 7 '34.3

63.47 52.26

.

63-52

MV > : r v M e V el M e V el M e V el b Me0 el

P -4
p-5 0- 1 0-5 8-4 0-5 R-T _.
R-4

61.1 63.9 61.8 51.2 49.1 51.4
60.2 48.4 e au. 3

63. 00
) : 0 50 ( 50. 00 50. 00

.

7 M e V el 10 M e V el 12 M e V el

.

-2.3 +1.9 -2.6
+0. 9 +3. 5
0.3

15 M e V el 20 MV >:rv 6 MV c r v 10 MV > : r v 12 M e V el 6 M e V el 17 M e V el 9 M e V el 12 M e V el 14 M e V el 12 M e V el 7 M e V el 10 M e V el 14 M e V el

H-2

60. 70

50.00
50. 00
fi

s-3
S-4

56.8
49- 6

.JU -

5 (3 .OC)

.(:)C)

-11.9
+1.O

V-4 0-5

4'3.9 C 1 6 .1

cL I

t-) -

5 0 (1)

. .

( : ) ( : )

+O. 3 -10. Y

9 MeV e l 20 M e V el

Report o f T e s t , Conti n ~ ~ e r i

Report o f Test, Continued

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