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Chapter 10
Raw Data Definition and Documentation Edward J . Panek
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Agricultural Research Center, Chemicals Division, BASF Corporation, Research Triangle Park, NC 27709 The current EPA Regulations (40 CFR 160) require that " a l l raw data, documentation records, protocols, specimens, and final reports generated as a result of a study shall be retained". The types and amounts of raw data generated in agrochemicals research are illustrated using a small planned field residue program as an example. This example is also used to illustrate documentation of this data using hierarchical paper files and relational electronic data base f i l e s . The archival needs for storage of this data are also given. This paper is concerned with the definition and documentation of primary raw data, or in other words, raw data directly associated with a study. Items such as standard operating procedures, methods, personnel qualifications and training records can be considered secondary raw data. Thus, even though these items are also archived, they are not considered explicitly here. But since they are just other examples of paper and/or electronic records, the same archival methods can be used. Most definitions of raw data concentrate on paper and/or electronic records. A good, concise definition is found in the FIFRA Good Laboratory Practice document (1): " 'Raw data means any worksheets, records, memoranda, notes, or exact copies thereof, that are the result of original observations and activities of a study and are necessary for the reconstruction and evaluation of the report of that study. In the event transcripts of raw data have been prepared (e.g., tapes which have been transcribed verbatim, dated, and verified accurate by signature), the exact copy or exact transcript may be substituted for the original source as raw data. 'Raw data may include photographs, microfilm or microfiche copies, computer printouts, magnetic media, including dictated observations, and recorded data from automated instruments." Another major type of raw data is samples. These are mainly retained aliquots of test chemicals and the biological samples generated in field residue trials, metabolism studies, and environmental fate studies. The chemical samples are to be archived f
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0097-6156/88/0369-0061 $06.00/0 © 1988 American Chemical Society Garner and Barge; Good Laboratory Practices ACS Symposium Series; American Chemical Society: Washington, DC, 1988.
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f o r the l i f e of the r e g i s t r a t i o n or f o r as l o n g as the q u a l i t y o f the p r e p a r a t i o n a f f o r d s e v a l u a t i o n . The b i o l o g i c a l samples a r e n o r m a l l y r e t a i n e d o n l y u n t i l the a n a l y s i s r e s u l t s a r e v e r i f i e d ( a u d i t e d ) and/or u n t i l the known s t o r a g e s t a b i l i t y i s r e a c h e d . N e v e r t h e l e s s , the a r c h i v a l c h a l l e n g e r e p r e s e n t e d by the l a r g e volume o f these b i o l o g i c a l samples i s o n l y s l i g h t l y d i m i n i s h e d by t h e i r s h o r t e r s t o r a g e time. The types o f a r c h i v a l s t o r a g e f a c i l i t i e s needed a r e f u n c t i o n s of g e n e r a l a r c h i v a l needs and the types of items to be a r c h i v e d . G e n e r a l a r c h i v a l needs a r e c o n t r o l l e d a c c e s s , s a f e and a p p r o p r i a t e s t o r a g e , and r e t r i e v a b i l i t y . The t y p e s of items to be a r c h i v e d i n c l u d e paper, f i e l d samples, t e s t c h e m i c a l samples, and e l e c t r o n i c records. In g e n e r a l the f o l l o w i n g t y p e s of a r c h i v e f a c i l i t i e s a r e needed: sample f r e e z e r s and c o l d rooms, t e s t c h e m i c a l f r e e z e r s , f i l e c a b i n e t s and/or boxes f o r paper, and magnetic media f o r e l e c t r o n i c records storage. Raw
Data from a Planned
F i e l d R e s i d u e Program
The t y p e s and amounts of raw d a t a g e n e r a t e d w i l l be i l l u s t r a t e d by f o l l o w i n g a p l a n n e d f i e l d c r o p r e s i d u e program from i t s d e f i n i t i o n ( p r o t o c o l ) s t a g e to the f i n a l r e p o r t . The a r c h i v a l / d o c u m e n t a t i o n needs w i l l then be s i m i l a r l y i l l u s t r a t e d . Protocol. The f i r s t s t e p i s t o d e f i n e the program ( i . e . , w r i t e the protocol). Key t e c h n i c a l elements to d e f i n e a r e : 1) the c r o p o r o t h e r use, 2) the use r a t e ( s ) , t i m i n g s of a p p l i c a t i o n s and a p p l i c a t i o n t e c h n i q u e s , 3) the t e s t c h e m i c a l and i t s f o r m u l a t i o n , 4) raw a g r i c u l t u r a l commodities to h a r v e s t and the s c h e d u l e , and 5) test locations. Each o f these elements g e n e r a t e s i n f o r m a t i o n , i . e . , raw d a t a . The c h o i c e s of g e n e r a l t e s t l o c a t i o n s and the h a r v e s t commodities f o r each c r o p a r e d e f i n e d by USDA and US EPA information (2-3). Test Chemical. Once the t e s t c h e m i c a l and i t s f o r m u l a t i o n have been d e f i n e d , the needed amount i s p r e p a r e d and packaged, the b a t c h i s a n a l y z e d , and p o r t i o n s a r e s h i p p e d to the t e s t l o c a t i o n s . Retained samples a r e c o r r e c t l y s t o r e d . I f the s t o r a g e s t a b i l i t y of t h i s f o r m u l a t i o n has not been d e t e r m i n e d , some o f the r e t a i n e d samples a r e used to d e t e r m i n e i t s s t o r a g e s t a b i l i t y under t y p i c a l s t o r a g e conditions. I n t h i s and subsequent d a t a g a t h e r i n g s t e p s the i n v e s t i g a t o r s c o l l e c t i n g the d a t a need t o be i d e n t i f i e d . F i e l d L o c a t i o n s . F o r each f i e l d t e s t l o c a t i o n a v a r i e t y o f i n f o r m a t i o n i s c o l l e c t e d and r e c o r d e d i n a d d i t i o n to the samples which a r e collected. Seven g e n e r a l c a t e g o r i e s of i n f o r m a t i o n can be d e f i n e d . Three s i m p l e ones a r e : 1) t e s t d e s i g n o r p l o t p l a n , 2) location and 3) f i e l d use h i s t o r y f o r s e v e r a l y e a r s . Field soil characteriz a t i o n 4) i n c l u d e s s c r e e n a n a l y s i s ( s o i l t y p e ) , pH measurement, and o r g a n i c m a t t e r c o n t e n t . Weather i n f o r m a t i o n 5) includes daily temperatures and r a i n f a l l and/or i r r i g a t i o n s d u r i n g the t e s t . A p p l i c a t i o n r e l a t e d d a t a 6) c o n s i s t s o f d a t e s , a p p l i c a t i o n modes, weather c o n d i t i o n s a t a p p l i c a t i o n , c a l c u l a t i o n s and c a l i b r a t i o n s . H a r v e s t i n f o r m a t i o n 7) i n c l u d e s c r o p name, p a r t , amount, d a t e , and collector.
Garner and Barge; Good Laboratory Practices ACS Symposium Series; American Chemical Society: Washington, DC, 1988.
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F i e l d Samples. Each f i e l d sample i s packed i n an a p p r o p r i a t e c o n t a i n e r and l a b e l e d . I n a d d i t i o n to the h a r v e s t i n f o r m a t i o n l i s t e d above, i n f o r m a t i o n on the h i s t o r y of the sample ( s t o r a g e c o n d i t i o n s and i n t e r v a l s ) n e a r the f i e l d l o c a t i o n and on shipment to the l a b o r a t o r y i s g e n e r a t e d . A n a l y s i s Information. As w i t h each f i e l d t e s t l o c a t i o n , f o r each sample or s e t of samples a v a r i e t y o f i n f o r m a t i o n i s a l s o g e n e r a t e d i n the l a b o r a t o r y . T h i s i n f o r m a t i o n can be grouped i n t o f o u r general categories. Sample h a n d l i n g r e c o r d s 1) include receipt c o n d i t i o n , p r o c e s s i n g and s u b - s a m p l i n g , s t o r a g e c o n d i t i o n s and sample a c c e s s i n f o r m a t i o n . A n a l y s i s p r o c e d u r e r e c o r d s 2) include the sample s i z e s , a l i q u o t i n g , d i l u t i o n s , e t c . f o r the method of a n a l y s i s u s e d . These methods u s u a l l y c o n t a i n e x t r a c t i o n , c l e a n - u p , and d e r i v a t i z a t i o n s t e p s . The a n a l y s i s method i s a p p l i e d to t r e a t e d samples, c o n t r o l samples and method r e c o v e r y samples ( s p i k e d c o n t r o l samples). These r e c o r d s may be i n the form o f bench s h e e t s or l a b o r a t o r y notebooks. Chromatographic i n f o r m a t i o n 3) includes the a c t u a l a n a l y s e s of the samples mentioned above, as w e l l as the i n f o r m a t i o n on i n j e c t i o n s t a n d a r d s ( s t a n d a r d i z a t i o n or c a l i b r a t i o n ) and the i n s t r u m e n t l o g books. C a l c u l a t i o n i n f o r m a t i o n 4) shows how the a n a l y s i s p r o c e d u r e and s t a n d a r d i z a t i o n d a t a a r e used w i t h the c h r o m a t o g r a p h i c d a t a to d e t e r m i n e t e s t c h e m i c a l (and d e g r a d a t i o n p r o d u c t ) c o n c e n t r a t i o n s i n the h a r v e s t e d commodities. F i n a l Report. information.
The
f i n a l r e p o r t summarizes a l l o f the
above
Amounts of Raw D a t a . The t y p e s of paper and/or e l e c t r o n i c r e c o r d s g e n e r a t e d i n t h i s example a r e shown i n T a b l e I . Table Category Test Chemical F i e l d Location-Each F i e l d Samples-Each A n a l y s i s - E a c h Sample
I.
Types o f Records Generated Number 3 7 2 6
These c o n s i s t o f f i e l d d a t a s h e e t s , sample s t o r a g e r e c o r d s , bench s h e e t s or l a b o r a t o r y n o t e b o o k s , chromatograms, and s h i p p i n g p a p e r s . Some of the l a b o r a t o r y r e c o r d s , i n p a r t i c u l a r , can be e l e c t r o n i c r a t h e r than p a p e r . The amounts of each type o f r e c o r d g e n e r a t e d i n a p l a n n e d f i e l d r e s i d u e program depend on the number of t e s t l o c a t i o n s and the number o f raw a g r i c u l t u r a l commodities h a r v e s t e d . I n a s m a l l (10 l o c a t i o n s ) s i m p l e (2 commodities h a r v e s t e d ) program, 40 samples (20 t r e a t e d , 20 c o n t r o l s ) a r e h a r v e s t e d and a p p r o x i m a t e l y 170 d i r e c t r e c o r d s a r e g e n e r a t e d . Most of these r e c o r d s c o n s i s t of m u l t i p l e pages so t h a t a p p r o x i m a t e l y 400 pages (or e q u i v a l e n t ) o f r e c o r d s are c r e a t e d f o r t h i s program. The f o l l o w i n g e q u a t i o n dramatizes t h i s p o i n t .
Garner and Barge; Good Laboratory Practices ACS Symposium Series; American Chemical Society: Washington, DC, 1988.
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GOOD LABORATORY PRACTICES Weight Records Weight Sample
_
( I t i s a c t u a l l y more t r u e i f number i s s u b s t i t u t e d f o r weight above e q u a t i o n . ) Documentation/Archival
i n the
Needs
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The p r e v i o u s s e c t i o n s i n d i c a t e d the t y p e s o f items and t h e i r amounts g e n e r a t e d i n each o f the major s t e p s i n a p l a n n e d f i e l d r e s i d u e program. I n t h i s s e c t i o n a r c h i v a l needs r e l a t e d t o t h e s e items a r e given. These a r e grouped by a r c h i v a l r e q u i r e m e n t . A r c h i v e Management. An i n d i v i d u a l must be r e s p o n s i b l e f o r the archives. T h i s p e r s o n c o n t r o l s a c c e s s t o the a r c h i v e s , checks items i n and out o f the a r c h i v e s , and m a i n t a i n s t h e s e use ( a c c e s s ) records. Controlled Access. A c c e s s t o the p h y s i c a l a r c h i v e s ( e . g . , f i l e c a b i n e t s and f r e e z e r s ) i s c o n t r o l l e d by l o c k s and the a r c h i v e management. A c c e s s t o e l e c t r o n i c f i l e s i s c o n t r o l l e d by s e c r e t u s e r i d e n t i f i c a t i o n (ID) numbers. W e l l d e s i g n e d e l e c t r o n i c d a t a s t o r a g e s o f t w a r e r e c o r d s o r s t o r e s the ID number o f any u s e r t h a t e n t e r s o r changes d a t a and when t h a t e n t r y o r change o c c u r r e d . Storage C o n d i t i o n s . Storage c o n d i t i o n s a r e d e s i g n e d t o m i n i m i z e d e t e r i o r a t i o n o f the a r c h i v e c o n t e n t s . S i n c e the c o n t e n t s d i f f e r g r e a t l y , so must the optimum s t o r a g e c o n d i t i o n s . C h e m i c a l samples are t y p i c a l l y a r c h i v e d i n f r e e z e r s . B i o l o g i c a l samples are s t o r e d i n c o l d rooms or f r e e z e r s . Paper o r m i c r o f i l m r e c o r d s a r e s t o r e d i n c o o l a r e a s where the chances f o r f i r e and l i g h t caused damage a r e minimized. E l e c t r o n i c media a r e s t o r e d under the above c o n d i t i o n s i n the absense of s t r o n g e l e c t r i c a l o r magnetic f i e l d s . Magnetic tapes need t o be backed-up (remade) p e r i o d i c a l l y . R e t r i e v a l Methods. The magnitude of r e c o r d s c r e a t e d i n our s m a l l example program c l e a r l y e s t a b l i s h e s t h a t the h e a r t o f any documentat i o n o r a r c h i v a l system i s the s y s t e m a t i c r e t r i e v a l of s p e c i f i c items. T h i s i s one of the s t r e n g t h s of e l e c t r o n i c d a t a systems. Thus the key i n f o r m a t i o n on our paper r e c o r d s i s a l s o c o n t a i n e d i n electronic f i l e s . These c r o s s - r e f e r e n c e d numbers a r e the key t o the e l e c t r o n i c r e l a t i o n a l data bases. Key f i e l d d a t a and sample s t o r a g e d a t a a r e e n t e r e d i n t o l o c a t i o n and sample number f i l e s i n QUIZ Software ( 4 ) . Laboratory a n a l y s i s i n f o r m a t i o n i s contained i n f i l e s generated u s i n g P e r k i n - E l m e r L a b o r a t o r y I n f o r m a t i o n Management System (LIMS) and Chromatographic L a b o r a t o r y A n a l y s i s System (CLAS) s o f t w a r e . Both of these systems have magnetic tape back-ups f o r the h a r d d i s k s . The h i e r a r c h i c a l paper d a t a f i l e i s o r g a n i z e d i n the same way the p l a n n e d f i e l d r e s i d u e t r i a l example was d e v e l o p e d . The p r o t o c o l and f i n a l r e p o r t a r e f o l l o w e d by t e s t c h e m i c a l i n f o r m a t i o n , t e s t l o c a t i o n i n f o r m a t i o n , a p p l i c a t i o n and h a r v e s t i n f o r m a t i o n , s h i p p i n g and s t o r a g e d a t a , and a n a l y s i s d a t a . The a n a l y s i s d a t a i s grouped by bench s h e e t to a s s i s t manual s e a r c h e s .
Garner and Barge; Good Laboratory Practices ACS Symposium Series; American Chemical Society: Washington, DC, 1988.
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Conclusions The types and amounts o f raw d a t a g e n e r a t e d i n a g r o c h e m i c a l s r e s e a r c h were i l l u s t r a t e d by u s i n g a s m a l l planned f i e l d r e s i d u e t r i a l as an example. The l a r g e amount o f raw d a t a g e n e r a t e d i n t h i s s m a l l example i n d i c a t e s how t h r o u g h l y b o t h the study and the a r c h i v a l s t o r a g e must be p l a n n e d . The d i v e r s i t y o f m a t e r i a l s t o be a r c h i v e d a l s o c o n t r i b u t e s t o the c o m p l e x i t y o f the a r c h i v a l needs. Acknowledgments
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To BASF C o r p o r a t i o n Chemicals D i v i s i o n f o r p e r m i s s i o n t o p u b l i s h t h i s paper and s u p p o r t d u r i n g i t s w r i t i n g a t the N o r t h C a r o l i n a beaches.
Literature Cited 1.
Code of Federal Regulations (40 CFR), Part 160, Good Laboratory Practice Standards. 2. Agricultural Statistics, U.S. Department of Agriculture, U.S. Government Print Office: Washington, DC, annual publication. 3. Schmitt, R.D. Pesticide Assessment Guidelines Subdivision O: Residue Chemistry, U.S. Environmental Protection Agency: Washington, DC, 1982. 4. A product of Quasar Systems Ltd., Ottawa, Ontario. RECEIVED February 2, 1988
Garner and Barge; Good Laboratory Practices ACS Symposium Series; American Chemical Society: Washington, DC, 1988.
