(19)
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superceded by the second one, identi-
fied "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.
Accordingly, we have
used the specifications from the sheet
marked
"tentative specifications"
for the following chart, which com-
pares the specifications
with the actual results of analysis.
DKP LOTS
Specifications 1R
2R 3R 4R 5R 6R 7R
-
-
-
-
-
-
-
Note... This entire
table was expunged from the delivered
document, by parties
unknown.
-
-
-
-
-
-
-
(20)
Specifications 1R
2R 3R 4R 5R 6R 7R
-
-
-
-
-
-
-
Note... This entire
table was expunged from the delivered
document, by parties
unknown.
-
-
-
-
-
-
-
The only discrepancy
apparent in the above chart is in the
criteria
for identity. The
specification lists reference standard
1R #2358,
while the analytical
record for lots 1R through 5R refer to
Reference #3701.
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
(21)
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 re-
ferenced lab notebook
(AR-93) again showed no evidence of a
heavy metals test.
The above discrepancies
were the only ones noted with respect
to
lots 1R through 7R
of DKP. All other criteria for identity
and
purity of DKP as
shown in the reports of analysis, conforms
to
Searle specification
sheet marked "tentative specifications
for
SC-19192". It
should be noted however that none of the
seven
lots of DKP met the
specifications on the sheet dated 12/4/69,
with respect to melting
range.
STABILITY AND HOMOGENEITY
OF DIET MIXTURES
A stability study
was initiated in January 1972, 2 months
after
the rat study (E-77/78)
had begun. The objective of the study
