We obtained copies of three different specification sheets for DKP.  (See Exhibits 16-18.)  We could not determine with certainty which of the three specifications sheets was in effect at the time that the 7 lots of DKP used in this study were assayed, because only one of the three specification sheets was dated.  This resulted in ambiguities for two of the parameters measured: melting point and identity (IR Spectrum).  Specification memorandum dated Dec. 4, 1969 listed a melting range of 252-256 degrees C. Another specification sheet (not dated) entitled "Tentative Specification For SC-19192", listed a melting range of 241-246 degrees C.  A third specification sheet entitled "Specification for SC-19192,  Specification No. C 40606C" (not dated) listed a melting range "at about 243 degrees C.".

For identity (IR Spectrum) the first sheet (dated 12/4/69) specified that "The reference standard shall be considered to be TJT-12-32 until something better comes along".  The second and third sheets specify that the DKP "Conforms to IR #2358".

No data was made available as to dates, method of preparation and authentication of DKP references standards used.

Searle attorney Roger Thies was contacted about this point Aug. 1, 1977 and said he would attempt to obtain information regarding this point but later registered doubt as to whether anything would be found.

We asked Searle personnel to tell us which of the specification sheets was valid for the DKP used in study E-77/78.  We were told that the third sheet, identified with "No. C4060C", could not have been used since the number corresponded to a date in June, 1974.

It is not clear as to the exact date that the first sheet (dated 12/4/69) was superceded by the second one, identified "tentative specifications for SC-19192" because the second sheet was not dated or numbered.  However, Searle attorney Roger Thies told us that their "best guess" was that the sheet marked "tentative specifications for SC-19192" was the one used.

Examination of the laboratory notebooks referenced on the analytical records revealed other possible discrepancies.  For example, the analytical record A-9129 for DKP Lot 5R showed an assay (titration) of 100.0 percent.  The analytical record referenced two different lab notebooks assigned to two different analysts. Examination of lab notebook AR-68 assigned to Sandra Ann Carey revealed that she had analyzed 3 samples of lot 5R on 11/9/72. Results of the analysis showed that sample one had an assay (by titration) of 89.70 percent, sample two, 87.93 percent and sample three was discarded.

Apparently not satisfied with her results she repeated the assay on the same day (11/9/72) and obtain 93.23 percent (the average of 3 samples), still well below the specification of 99.0 percent.  The other lab notebook referenced was AR-57, assigned to E. Aranda.  This notebook showed that analyst Aranda performed an assay (titration) of lot 5R on 12/1/72 the results of which were 114.83 percent for 3 samples.  Apparently not satisfied with the results, he repeated the assay on 12/6/72 and obtained 100.4, 99.9 and 99.8 percent for an average of 100.0 percent.  This result (100.0 percent) was the only one reported on the analytical record A-9129.

The analytical record (A-7291) for DKP lot R shows a result of "less than 20 PPM" for the heavy metals test.  Two laboratory notebooks are referenced:  VSH-I, pages 260-263, and AR-23, page 269.  Examination of both of these books revealed no mention of a heavy metals test.

The analytical record (A-9805) for DKP lot 6R (JDR-5-30A) also showed a result of "less than 20 PPM" for heavy metals test. Examination of the referenced laboratory notebook (AR-77, page 83-86) revealed no evidence of a test for heavy metals.

The analytical record (A-9829) for DKP lot 7R (JDR-5-30B) again showed "less than 20 PPM" heavy metals.  Examination of the referenced lab notebook (AR-93) again showed no evidence of a heavy metals test.