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INTER OFFICE MEMO TENNECO CHEMICALS, INC
To M. rreifeld Subject Lead Assay
At riemington at Burlington
date April 3, 1973
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As we concluded at an All-Disc task force meeting on 11/17/72, the atomic absorption assay method for lead is inadequate due to erratic results. Since that time, we have been successful in developing a gravimetric assay technique that is accurate and reproducible for lead analyses of dibasic lead stearate, tribasic lead sulfate and compound dry blends containing these stabilizers.
The method is based on the digestion of a sample in 1:1 HNOgil^SO^, foll
owed by oxidation with
driving off the HNOg and precipitating the
lead as the sulfate. The lead sulfate is filtered through a fared gooch
crucible and dried to constant weight from which the lead content is calcu-
lated (factor is 0.683). This method will be adopted as a standard proced
ure.
.
In the attached Table I (Lead Analyses), assay results are shown for dibasic lead stearate, tribasic lead sulfate and compound dry blend. It will be noted that all dibasic lead stearate samples are in-specification but that the Eagle-Picher tribasic lead sulfate samples are somewhat low. In a round robin interchange, Eagle-Picher confirmed the low lead assays and has stated that appropriate corrective action will be taken. The compound dry blend results indicate a fairly wide spread in results (0,61% - 0.82%) versus a theoretical result of 0.74%. A laboratory-prepared dry blend assayed at 0.73%. The dry blend assay results are limited and more data is required to assess actual plant control.
The lead assay method is currently being established in Burlington. Each raw material lot will be assayed for conformance to specification. Additional dry blend analyses will be performed on each 3805D lot produced, the target being six analyses per lot.
Attachment. HBC/jst
H.B. Carr
COLORITE 014841
tabu: I LEAD ANALYSES
Dibasic Lead Stearate
NL Industries DS 207 Specification for Pb: 50.4% - 52.2%
Compound lot Number Lot 7-112849
Sample Mix 1
tt Mix 23 IT Mix 49 TT Mix 59
Tt
Lot 7-013000 Lot 7-023102
Mix 137 _
Result
50.8% Rerun (51.1%)
52.2%
51.3%
51.3% Rerun (51.2%)
52.1%
51.8%
51.4%
DBLS Lot Numbe: NL Lot 2850
TT TT TT
TT Tt tt
TT Tt TT
T! TT TT
NL Lot 2875 NL Lot 2879
Tribasic Lead Sulfate
Eagle-Picher Epistatic 100 Specification for Pb: 83.5% - 84.5%
Compound Lot Number Lot 7-112849
Sample Mix 1
tt Mix 23
T! Mix 49 TT Mix 60
NL Industries Tribase Specification for Pb: 82.2% - 83.3%
(Tenneco) Result
(Eagle-Picher) Result
81.3% (EP Lot 27A-505)
81.9%
81.2% Rerun (81.5%)
(EP Lot 27A-505)
82.0%
81.0% (EP Lot 27A-505)
82,7% (NL Lot 172255A)
81. 8% _
COLORTTE 014842
TABLE I
LEAD ANALYSES
, (continued)
\
Dry Blend Pb content based on formulation: 0.74% (0.8% DBLS; 0.4% TBLS)
Compound Lot Number -1X2849
Sample Mix 7
it Mix 8 Tf Mix 9 ii Mix 10 ii Mix 17
ii Mix 64
Lab-Prepared Dry Blend TBLS 82,7% DBLS 51.3%
Result 0.82% Rerun (0.85%)
0.70%
0.75%
0.85%
0.61% Rerun (0.64%)
0.73%
0.73%
COLORITE 014843