Article Title: Design of Experiment: Free Lead Conversion in Lead-acid

Batteries
And its effect on Performance

Authors: Mr. Brian Roush, University of Central Missouri

Dr. Jeffrey M. Ulmer, University of Central Missouri

Keywords: Design of Experiments, Process Improvement, Quality, Quality

Management
DOE: FREE LEAD CONVERSION 2

Table of Contents

Defining the Problem 3

Understanding Free Leads.......................................................................................................4

Current Free Lead Conversion...............................................................................................4

Components of the Experiment 6

Experimental Factors...............................................................................................................6

Overall Objective......................................................................................................................7

Baseline Data Collection and Compilation.............................................................................7

Collect sample for % Free Lead analysis and % Moisture Loss.............................................7

Design/Performance of the Experiment 8

Modified Curing Trial, Based on Sister Cure Profile Temperatures...................................8

Background Information........................................................................................................8

General Experimental Outline................................................................................................9

Controlled Paste Mix Peak Temperature Trial....................................................................10

Background Information......................................................................................................10

General Experimental Outline..............................................................................................11

Data Analysis 11

Modified Curing Trial, Based on Sister Cure Profile Temperatures.................................11

Controlled Paste Mix Peak Temperature Trial....................................................................12

Action 13

Conclusion 13

References 15

Appendix 16
DOE: FREE LEAD CONVERSION 3

Defining the Problem

Battery manufacturing facilities typically experience a drop in cold cranking amps (CCA)

during lab testing for quality assurance. The industry standard for testing CCA is 30 second test

with a drop in voltage to no less that 7.2 volts. In this scenario, the facility is finding some (but

not all) tested batteries failing this test. The CCA results in failed batteries are 6.8 volts after 30

seconds. When this condition came to light many factors were considered as root cause. The

initial suspected root cause was considered to be temperature related. It is a known factor that

increased temperatures affect battery performance. Teams of quality and engineering personnel

gathered to investigate ambient temperature, battery temperature during the formation process

and humidity during the assembly process. During this time, a conversation began regarding free

lead levels. A cursory investigation had been ongoing for approximately 15 months regarding

free lead levels before and after curing. This investigation was nothing more than a moderate

attempt to track free leads alone in an attempt to understand curing oven performance. No

documentation was made on product type or differentiation between shifts.

The process of producing sealed lead batteries requires a conversion of free leads in order

to ensure maximum energy transfer in the finished product. The industry standard for final free

lead conversion in positive plates is <3%, for negative plates that value is <5% free leads. If the

final conversion results are higher than these values, the batteries tend to lose performance.

Using a scenario that could be found in most any battery manufacturing facility, this paper will

attempt to understand free leads, determine the result on performance and recommend an action

plan. The scenario is based in real world situations.

DOE: FREE LEAD CONVERSION 4

Understanding Free Leads

In the plate manufacturing process there is a relatively high free lead content. This is

because the original lead oxide contains a high proportion of free lead. Free leads are essentially

non-oxidized lead particles with limited surface area. Limited surface area contributes to voltage

loss on discharge of the battery. It also leads to less than full formation and a reduction in the

initial capacity (Prout, 1993; Sharif, Kumar, Murthy, Vijayanand, Ambalavanan, 2011; and Rus,

Constantin, Taralunga and Rus, 2005). It is important to monitor and control the conversion of

free leads according to the purpose of the product being made. “From the steps involved in the

positive plate manufacturing process, curing is a key stage during in which the paste is converted into

a cohesive, porous mass, with a good adherence to the grid” (R us, Constantin, Taralunga and Rus,

2005. p. 1). The curing process converts free leads into either tri-basic (3BS) or tetra-basic (4BS) in

the positive plates. The process of obtaining 3BS or 4BS has to do with temperature and humidity

control as well as how long the paste sits before being applied to the grid in the plate making process

(Rus, et al; Sharif, et al; Webster, 1986). The chemical reactions that take place in order to convert

free leads in the curing process are beyond the scope of this paper. Most importantly, the

effectiveness of the curing process can be assessed by monitoring free leads and moisture loss after

the curing cycle has completed.

Current Free Lead Conversion

As mentioned above, the industry standard for final free lead conversion in positive plates

is <3%, for negative plates that value is <5% free leads. If the final conversion results are higher

than these values, the batteries tend to lose performance. The data collected during the 15 months

of simple tracking of free leads included a range of all 22 curing ovens. 75 tests were performed

with all ovens having some form of ‘out of control’ free lead results. (Out of control is relative in

this instance since there is no specification nor control limits governing oven performance.)
DOE: FREE LEAD CONVERSION 5

The summary results post-curing can be seen in Table 1 below. (Full tracking results can

be found in Appendix 1.)

Free Pb Finish + Free Pb Finish -

8 COUNT 31
10.67% PERCENTAGE 41.33%
1.42 MEDIAN 4.22
1.72 MEAN 4.75

Table 1

Positive plates tended to convert free leads better than negative plates with 10.67% of

tested plates being out of control (above 3%). The negative plates, however, failed miserably

with 41.33% being out of control (above 5%). This data would be consistent with the results

found in failed product (called ‘cells’ for the sake of this paper) in highly scrutinized areas. In

one area in particular, if an individual ‘cell’ fails at any point in the process control and quality

assurance checks every part of that ‘cell’s’ assembly is examined. If a thorough examination of

the ‘cell’ through a complete tear down does not reveal some physical defect in parts or

production then that underperforming ‘cell’ will have it’s build data examined, especially

regarding plates. Negative plates have been found to have a greater impact on cell performance

when there are failures in the formation process. Research of documentation reveals that a

change in plate lot is typical in failed ‘cell’. Tying a 41.33% failure rate on free lead conversion

in negative plates with an identification of a change in plate lot on failed ‘cells’ leads this

researcher to believe that free leads need to be examined as a potential root cause of CCA

failures on other product.

DOE: FREE LEAD CONVERSION 6

Data collected by manufacturing process engineering suggests that there may be factors other than

curing that are (negatively) impacting the conversion of free leads at process steps prior to curing. The

dots in the graphs below (Table 2) are the combination of free lead results from two plates taken from the

same rack. There is a large degree of variability in the data, both in the before curing % free lead and the

after curing % free lead.

Table 2

Components of the Experiment

Experimental Factors

The original design of this experiment was a simple single factor. One factor was going

to be manipulated in an attempt to determine its effect on free lead conversion. Oven doors

during loading was to be the factor. With the question being asked: What effect does open oven

doors during the loading process have on free lead conversion? However, as with any multi-

departmental issue, other ideas came to the forefront and this single factor experiment morphed

into a fractional factorial experiment. Oxide production, paste mixing, plate making and plate

curing all became part of this design. The result is a not-quite-completed experiment with mixed

results.
DOE: FREE LEAD CONVERSION 7

Overall Objective

Seeking to improve process consistency, reducing variability which is expected to lead to

product performance consistency, reducing variability

Use Starting Target Ranges for % Free Lead of:

 Oxide (ball mill): 20-35%

 Paste mixing: 10-15%

 Cured positive paste: <2%

 Cured negative paste: <5%

These targets are based on literature (Pavlov, n.d.; Prout, 1993; Rus, et al, 2005), as well

as previously accrued battery industry knowledge.

Baseline Data Collection and Compilation

Examine % Free Leads through the manufacturing process, and identify areas of the

process (process step – oxide, paste mix, pasting, curing) where the most variability is seen.

Collect sample for % Free Lead analysis and % Moisture Loss

Oxide

 Samples at the mill

 Samples at the mixer

Mixed Paste

 Capture all relevant process variables (mostly available in paste mix data base - %

moisture loss, peak temperature, end of acid mix temperature, etc.)

 Samples at the mixer (consistent, comparable data point available on all mixes)

 Samples after the mix is complete, over time

DOE: FREE LEAD CONVERSION 8

Pasted Plates Paste

 Capture all relevant process variables (downtime, equipment issues, etc.…)

 Capture all relevant input variables (mixed paste time, temperatures, trim water,

% moisture loss, etc.)

Cured Plates Paste

 Capture all relevant process variables (plate type negative or positive, plate size,

rack position, location on rack, in stack, time of paste mix – oven start, etc.)

 Capture a variety of plates sizes – High free leads resulting from plates drying to

fast. Smaller plates could be expected to dry faster larger plates

Design/Performance of the Experiment

Modified Curing Trial, Based on Sister Cure Profile Temperatures

Background Information

Discussions had with other industry technical personnel from our sister plant indicated

that recent work was done with regards to curing / drying cycle profiles. The two key takeaways

were: During the curing portion of the profile the sister plant has an oven temperature set point

of 55°C (131°F), while this facility’s oven temperature set point is 60°C (140°F). This may be

important in two regards. First the lower temperature may prevent the plates from drying too

fast and not allowing the conversion of free lead to occur. Second, tetrabasic lead sulfate can

form in the cured (standard, Large+ batch) positive paste at and above 60°C, and this has been

observed with cured positive paste periodically.

During the drying portion of the profile the sister plants have an oven temperature set

point of 95°C (203°F), while this facility’s oven temperature set point is 99°C (210°F).
DOE: FREE LEAD CONVERSION 9

Additional information provided by showed profiles spending most of the curing portion at a set

point of 45°C (113°F) or 50°C (122°F).

General Experimental Outline

Conduct a small scale trial in a laboratory oven using the Sister Curing Profile provided

by our sister plant (not controlling oven humidity). Use positive and negative plates in this oven

trial. Record all relevant process inputs - including (but not limited to) – oxide at mixer % free

lead, paste mix peak temperature, paste mix trim water, paste mix use timing, mixed paste % free

lead, wet paste % free lead, stack heights, etc.

Sister Curing and Drying Program

Step 1 Step to 50OC.
Step 2 Hold at 50OC for 28 hours.
Step 3 Ramp at 20OC per hour to 95OC.
Step 4 Hold at 95OC for 16 hours.
Step 5 Step to 20OC.
Step 6 Hold at 20OC.
All steady state temperatures shall be within ± 5OC of the nominal value shown
above.
Typical duration to 50OC – 48.5 hours.

 Collect cured paste % free lead data from cured dried plate samples.

 Build test batteries from the plates cured via this cure / dry program

 Perform electrical testing to determine impact(s) battery performance

Potential Additional or Follow on Trials:

 Larger scale trial with Sister Curing and Drying Program with production oven

 Small scale trial (lab oven) using a different Sister Plant based cure profile trials –

using other Sister Curing and Drying Programs (Standard - Extended, Aviation

and Military)
DOE: FREE LEAD CONVERSION 10

 Small scale trial (lab oven) using Sister based temperature set points, but times

closer to those currently used for this facility curing and drying profile

 Larger scale trial using Sister based temperature set points, but time closer to

those currently used for this facility curing and drying profile (this would capture

more plate types and sizes that a small scale trial)

 Consider different controlled (‘high’) humidity curing options – either by not

venting ovens (production ovens vent out humidity), or by injecting humidity (1

lab oven capable, 1 production oven capable)

Controlled Paste Mix Peak Temperature Trial

Background Information

A review of paste mix peak temperatures collected from the paste mix database showed a

wide range of peak temperatures and end of acid mix temperatures. See the data summary in

Table 3 below.

Table 3
DOE: FREE LEAD CONVERSION 11

Note: the Lg. Batch+, Lg. Batch-, and X Batch- paste mix recipes are programmed such

that the temperature peak temperature recorded on the HMI (human machine interface) screen

is actually the temperature at the end of the acid addition step, not the highest temperature

during the paste mix cycle.

General Experimental Outline

 For 3 Lg. Batch+ Recipes, set mixer cooling start temperature to 55°C, 47°C,

39°C, (47°C is the current set point)

o measure free leads at paste mix, over time during pasting, after curing

o Potential follow on work, after initial free lead data is collected  build

test batteries using plates made from these paste mix batches, combining

with controlled Lg. Batch- paste mix batches

 For 3 Lg. Batch- Recipes, set mixer cooling start temperature to 52°C, 43°C,

35°C, (43°C is the current set point)

o Measure free leads at paste mix, over time during pasting, after curing

o Potential follow on work, after initial free lead data is collected  build

test batteries using plates made from these paste mix batches, combining

with controlled Lg. Batch+ paste mix batches

Data Analysis

Data collected and analyzed from Appendix 2.

Modified Curing Trial, Based on Sister Cure Profile Temperatures

There is a large percentage of cured negative plate free leads that are coming out greater

than 5% (Table 4).  Work needs to be done to show that cured negative plate free leads >5% are

bad for battery performance.  This can be done by having test batteries built with negative plates
DOE: FREE LEAD CONVERSION 12

>5% free lead – by taking known plate locations on the racks with higher free leads and a high

free lead measurement to confirm, and comparing to known low free lead negative plate

locations confirmed by actual measurement. There is enough evidence here to show that

something needs to change, so start putting together a project plan outline for a modified cure

profile as previously discussed.

Table 4

Controlled Paste Mix Peak Temperature Trial

Data analysis is still ongoing due to the scope of the experiment. To date the following

data can be analysis in a preliminary assessment. The data for these CDF plots come from data

typed in by the operators to the paste mix database between July 2014 and August 2015, and are

what the tool screen reports as the peak temperature. The data was lightly screened to remove

unreasonable numbers. Except for the CATV positive recipe, this value represents the reading at

the end of acid addition. Higher temperatures may be seen before or after that point on the

standard large batch positive or either of the negative recipes but will not be represented in this

data.
DOE: FREE LEAD CONVERSION 13

CATV negative from mixer 4: The red line is empirical data and the blue line is

hypothetical normal.

Standard large batch negative from mixer 4: The red line is empirical data and the blue

line is hypothetical normal.

Action

No action is in play until the end of the experiment.

Conclusion

The testing and data collection has yielded valuable information regarding current

processes. It has also brought to light some procedural issues where operators may not be

following the Operating Procedures. More data is being collected before testing can begin in
DOE: FREE LEAD CONVERSION 14

earnest. The preliminary results indicate that curing conditions result in inconsistent free lead

conversion. It is yet undetermined as to whether this is an equipment problem or a process

problem. Questions remain unanswered: could a change in the curing profile produce better

results? Could a simple change in process (i.e.: closing the oven door during the loading process)

produce better results?

A solution can potentially be found to increase the conversion of free leads and tighten up

each process. This exercise was eye-opening with regard to how quickly the scope of an

experiment can swell out of control. It would have been better to conduct a simple single factor

test to prove out the value of lower free leads. This step was bypassed as technical issues became

known; involving research and industry standards. It is well understood that companies need to

optimize some processes with a simple experiment before running tests on three separate

departments concurrently. The potential fallacy is that the experiment will change too many

factors at once with no clear way to evaluate the results.

DOE: FREE LEAD CONVERSION 15

References

Pavlov, D. (n.d.). Curing of Battery Plates. Lead-Acid Batteries: Science and Technology, 363-

404.

Prout, L. (1993) Aspects of lead/acid battery technology: plate curing. Journal of Power

Sources, 41. 185-193.

Rus, E.M., Constantin, D.M., Taralunga, G., Rus, Al. (2005) The Influence of Curing Process on

the Lead-Acid Battery Performance. Retrieved on 15 September 2015 from

https://www.researchgate.net/publication/237703585_THE_INFLUENCE_OF_CURING_P

ROCESS_ON_THE_LEAD-ACID_BATTERY_PERFORMANCE

Sharif, M.M., Kumar, P.S., Murthy, K.S.N., Vijayanand, S., Ambalavanan, S. (2011) Influence

of Process Parameters on Paste Morphology in Lead-Aid Battery Cured Plates.

International Journal of Electrochemical Science. 91-102. Retrieved on 14 September 2015

from

http://www.researchgate.net/publication/268384336_Influence_of_Process_Parameters_on_

Paste_Morphology_in_Lead-Acid_Battery_Cured_Plates

Summers, D. (2010). Quality (5th ed.). Upper Saddle River, New Jersey: Prentice Hall.
DOE: FREE LEAD CONVERSION 16

Appendix

Appendix 1

Dates oven Oven Shif Load Load Free Pb Free Pb Free Pb Free Pb
run # t Start Finish Start + Finish + Start - Finish -
14020- 14020-
1/20/14 10 day 0731 1058 2.93 2.09 3.64 1.66
14022- 14022-
1/22/14 17 day 0627 0929 13.07 0.71 21.05 2.42
14027- 14027-
1/27/14 1 day 0534 1010 13.38 1.21 20.3 3.37
14041- 14041-
2/1/14 4 day 0738 1351 11.91 0.86 13.69 1.88
14036- 14036-
2/5/14 9 day 1108 1424 15.54 2.34 19.95 5.18
14038- 14038-
2/7/14 19 day 0617 1004 15.05 5.52 18.34 7
14043- 14043-
2/12/14 3 day 0627 0918 15.15 1.82 21.14 1.55
14045- 14045-
2/14/14 21 day 0819 1155 13.5 0.057 17.88 12.2
14048- 14048-
2/17/14 2 day 0606 1008 3.9 3.57 20.66 0.41
14050- 14050-
2/19/14 8 day 0608 1035 16.89 0.97 17.91 2.93
14052- 14052-
2/22/14 20 day 0600 1138 0.91 1.6 11.75 2.8
14055- 14055-
2/24/14 19 day 0412 1009 18.59 2.74 18.45 6.41
14057- 14057-
2/26/14 7 day 0614 0855 2.66 0.24 20.36 3.83
14059- 14059-
2/28/14 11 day 0732 1112 11.19 2.79 18.73 1.78
14062- 14062-
3/3/14 14 day 0554 0901 15.27 1.59 27.14 5.49
14064- 14064-
3/5/14 22 day 0806 1107 15.76 1.2 19.72 1.54
14066- 14066-
3/7/14 16 day 0240 0818 17.3 2.46 20.62 2.21
14069- 14069-
3/10/14 18 day 0616 1143 16.6 1.5 23.24 8.99
14071- 14071-
3/12/14 15 day 0604 1011 13.58 3.03 17.58 7.24
14073- 14073-
3/14/14 2 day 0816 1116 22.61 1.11 15.16 2.37
14076- 14076-
3/17/14 13 day 1056 1345 4.57 1.14 9.76 3.75
14080- 14080-
3/21/14 1 day 0328 0926 15.89 1.23 15.28 2.67
14084- 14084-
3/25/14 7 day 0928 1200 11.21 1.2 17.11 5.08
3/31/14 5 day 14090- 14090- 15.86 2.7 16.7 2.66
DOE: FREE LEAD CONVERSION 17

0906 1139
14092- 14092-
4/2/14 11 day 0112 1151 19.34 0.36 N/A  
4/3/14 12 day     13.23 2.42 15.89 4.37
14097- 14097-
4/7/14 17 day 0826 1108 12.36 1.01 16.96 5.67
14104- 140104-
4/14/14 8 day 0917 1429 15.07   17.94  
14112- 14112-
4/25/14 12 day 0601 1222 12.71 0.059 N/A  
14302- 14302-
9/1/14 16 day 1052 1338 N/A 2.71 N/A 3.98
14247- 14247-
9/2/14 5 day 0735 0913 14.24 2.17 13.51 7.17
14073- 14073-
9/4/14 2 day 0816 1116 13.21 0.56 17.78 5.9
14258- 14258-
9/17/14 13 day 1058 1329 14.41 16.9
14262- 14262-
9/19/14 1 day 0539 0804 13.1 3.61 17.99 4.63
14266- 14266-
9/25/14 7 day 1150 1415 13.3 1.38 17.69 4.99
14097- 14097-
9/25/14 17 day 0826 1108 N/A   N/A  
14269- 14269-
9/28/14 4 day 1001 1348 14.48 1.87 16.2 3.48
14251- 14251-
9/28/14 5 day 0633 1134 8.61 0.42 21.99 5.45
14084- 14084-
10/31/14 7 day 0928 1141 15.36 0.073 18.32 5.56
14310- 14310-
11/6/14 1 day 0630 1403 13.18 1.33 19.47 7.42
14317- 14317-
11/13/14 7 day 0903 1328 11.86 2.12 17.54 5.32
14322- 14322-
11/18/14 9 day 1023 1332 14.9 1.55 17.5 2.9
14335- 14335-
12/1/14 15 day 0932 1232 15.44 3.82 14.5 5.45
14337- 14337-
12/3/14 18 day 1014 1429 14.8 1.43 21.78 3.57
1/7/15 7 day     15.76 0.96 22.89 6.76
15027- 15027-
1/27/15 6 day 0829 1112 17.46 5.6 16.84 6.38
15030- 15030-
1/30/15 7 day 0930 1417 14.97 3.28 21.53 4.02
15044- 15044-
2/10/15 3 day 0619 1214 13.14 2.57 17.86 6.11
15041- 15041-
2/10/15 10 day 0539 1401 2.92 0.95 15.51 2.44
15047- 15047-
2/18/15 4 day 0756 1202 14.39 2.99 20.25 8.95
15051- 15051-
2/20/15 5 day 1029 1407 11.82 1.15 21.97 6.73
2/20/15 18 day 15049- 15049- 13.59 1.33 21.07 10.75
DOE: FREE LEAD CONVERSION 18

1137 1418
15054- 15054-
2/23/15 16 day 0842 1550 10.48 1.03 15.48 3.45
15056- 15056-
2/27/15 20 day 1035 1430 10.05 1.45 12.08 9.22
15061- 15061-
3/2/15 2 day 0909 1424 4.15 1.4 22.55 3.17
15063- 15063-
3/4/15 8 day 1105 1422 15.38 2.56 8.2 2.18
15065- 15065-
3/6/15 9 day 0854 1418 13.8 1.07 15.35 3.24
15103- 15103-
4/15/15 2 day 1324 1550 10.26 3.33 24.25 5.58
14315- 14315-
11/11/14 6 days 0738 1141 11.86 0.7 18.52 2.05
15152- 15152-
6/2/15 3 days 0856 1215 15.4 1.44 18.28 3.21
15156- 15156-
6/5/15 20 days 1207 1603 15.27 2.89 18.65 6.71
15163- 15163-
6/12/15 10 days 0821 1113 11.75 2.38 18.48 4.09
15154- 15154-
6/15/15 9 days 0804 1140 16.35 1.13 16.24 3.03
15169- 15169-
6/19/15 4 days 1032 1408 14.06 0.75 15.28 3.53
15173- 15173-
6/22/15 5 days 1012 1321 13.07 1.15 22.65 7.71
15177- 15177-
6/26/15 18 days 0758 1206 16.25 1.79 18.19 3.06
15188- 15188-
7/8/15 14 days 0925 1422 14.69 1.44 19.57 3.24
swin 14086- 14086-
3/27/14 8 g 1208 1631 14.15 1.51 17 4.1
swin 14099- 14099-
4/9/14 6 g 1107 1456 14.77 1 20.83 4.33
swin
2/10/15 7 g     11.58 1.37 18.38 5.5
swin 15105- 15105-
4/15/15 1 g 1346 1742 16.85 1.41 17.91 6.06
swin 15107- 15107-
4/20/15 7 g 1200 1539 12.1 1.06 15.05 6
swin 15110- 15110-
4/20/15 8 g 1213 1737 16.2 2.15 18.56 5.96
swin 15112- 15112-
4/22/15 19 g 1415 1743 13.8 0.64 20.11 7.24
swin 15117- 15117-
4/28/15 16 g 1423 1915 13.51 1.006 16.27 3.12
DOE: FREE LEAD CONVERSION 19

APPENDIX 2

Manufacturing Free
Pb Study
Process Development Free Pb
Sampling

Free
Start Pb %
Time of Moist Wei Wei Fre
collecti Collected ure ght ght e
Sample # Date on from Form Notes Loss (g) (g) Pb
10/6/ Mixer 3 10.0 2.36 23.
1 15 10:30 oxide cone Oxide     520 59 5%
10/6/ Mixer 4 10.0 2.53 25.
2 15 10:30 oxide cone Oxide     772 53 2%
10/6/ Hopper-new 10.1 1.41 14.
3 15 10:30 med + (+) Paste     138 64 0%
10/6/ Hopper-new 10.8 1.59 14.
4 15 11:25 med - (-) Paste     818 67 7%
10/6/ 10.4 1.73 16.
5 15 11:25 Mixer 3 (+) Paste     683 82 6%
10/6/ 10.2 2.45 24.
6 15 11:25 Mixer 4 (-) Paste     315 44 0%
10/6/ Mixer 3 10.4 2.65 25.
7 15 11:35 oxide cone Oxide     807 60 3%
10/6/ Mixer 4 10.1 2.51 24.
8 15 11:35 oxide cone Oxide     958 54 7%
10/6/ NXS 137 (+) Rack TS: 15279-1157, oven 19 end at 10.2 1.41 13.
9 15 11:45 Rack 259 fresh plate 10/8 00:11   488 65 8%
10/6/ G31 (-) fresh Rack TS: 15279-1211, oven 19 end at 10.3 2.28 22.
10 15 11:45 Rack 223 plate 10/8 00:11   137 24 1%
10/6/ 10.0 1.27 12.
11 15 12:30 Mixer 3 (+) Paste     027 10 7%
10/6/ 10.5 1.18 11.
12 15 12:30 Mixer 4 (-) Paste     805 14 2%
10/8/ Rack 200, 10.2 0.11 1.1
13 15 8:30 Oven 19 Cured (+) Plate Center/center of plate   034 68 %
10/8/ Rack 259, 10.1 0.10 1.0
14 15 8:30 Oven 19 Cured (+) Plate Center/center of plate   584 04 %
10/8/ Rack 223, 10.1 0.54 5.3
15 15 8:30 Oven 19 Cured (-) Plate Center/center of plate   453 24 %
10/8/ Rack 223, 10.2 0.26 2.6
16 15 8:30 Oven 19 Cured (-) Plate Center/center of plate   181 57 %
10/8/ Rack 205, 10.7 0.40 3.8
17 15 8:30 Oven 19 Cured (-) Plate Center/center of plate   230 56 %
10/8/ Rack 205, 10.2 0.31 3.1
18 15 8:30 Oven 19 Cured (-) Plate Center/center of plate   462 79 %
10/13 10.2 1.51 14.
19 /15 9:00 Mixer 3 (+) Paste   12.67 040 16 8%
10/13 Hopper-new 10.3 1.28 12.
20 /15 9:10 med + (+) Paste     836 84 4%
10/13 G31 (+) Fresh 10.1 1.17 11.
21 /15 9:10 Rack 150 Plate   10.09 275 76 6%
10/13 Hopper-new 10.3 1.25 12.
22 /15 9:15 med - (-) Paste     086 16 1%
10/13 Hopper-new 10.0 1.15 11.
23 /15 9:25 med - (-) Paste     205 91 6%
10/13 G31 (-) Fresh 10.3 1.15 11.
24 /15 9:30 Rack 344 Plate     303 11 1%
10/13 G31 (-) Fresh 11.0 1.67 15.
25 /15 11:30 Rack 344 Plate Rack sitting in open oven 9.1 574 68 2%
26 10/13 12:45 Rack 344 G31 (-) Fresh Rack sitting in open oven   10.7 1.65 15.
DOE: FREE LEAD CONVERSION 20

/15 Plate 540 27 4%

10/13 G31 (-) Fresh 10.2 1.63 15.
27 /15 14:32 Rack 344 Plate Rack sitting in open oven 9.22 715 57 9%
10/15 Hopper-new (+) CATV 10.6 1.60 15.
28 /15 9:10 med + Paste   11.53 099 47 1%
10/15 10.2 3.02 29.
29 /15 9:10 Mixer 3 Oxide     202 08 6%
10/15 Hopper-new (+) CATV 10.6 1.60 15.
30 /15 10:52 med + Paste   11.94 005 06 1%
10/15 Hopper-new (+) CATV 10.4 1.66 15.
31 /15 12:35 med + Paste   11.52 190 08 9%
10/15 10.4 2.73 26.
32 /15 12:35 Mixer 3 Oxide     545 13 1%
10/15 10.1 2.65 26.
33 /15 12:35 Mixer 4 Oxide     521 37 1%
10/21 Cured (+) G31 Collected from bottom of plate stack, 10.0 0.48 4.8
34 /15   Rack 150 Plate center/center of plate   819 01 %
10/21 Cured (+) G31 Collected from middle of plate stack, 10.6 0.35 3.3
35 /15   Rack 150 Plate center/center of plate   779 18 %
10/21 Cured (+) G31 Collected from near top of plate stack, 10.3 0.18 1.7
36 /15   Rack 150 Plate center/center of plate   640 11 %
10/21 Cured (-) G31 10.7 0.50 4.7
37 /15   Rack 344 Plate Center/center of plate   728 34 %
10/21 Cured (+) 10.0 0.06 0.7
38 /15   Rack 244 CATV Plate Center/center of plate   579 67 %
10/29 10.7 2.87 26.
39 /15 9:00 Mixer 3 Oxide     138 24 8%
10/29 Hopper-new (+) CATV 10.8 1.59 14.
40 /15 9:30 med + Paste     142 65 8%
10/29 Hopper-new (+) CATV 10.6 1.66 15.
41 /15 10:30 med + Paste     580 07 6%
10/29 Hopper-new (-) CATV 10.4 1.28 12.
42 /15 10:30 med - Paste     362 74 3%
10/29 10.4 2.94 28.
43 /15 10:25 Mixer 3 Oxide     823 11 1%
10/29 10.6 2.85 26.
44 /15 11:15 Mixer 4 Oxide     921 45 7%
10/29 10.6 2.88 27.
45 /15 12:00 Mixer 3 Oxide     232 97 2%
10/29 10.2 2.78 27.
46 /15 12:00 Mixer 4 Oxide     016 81 3%
10/29 Hopper-new (+) CATV 10.7 1.42 13.
47 /15 11:55 med + Paste     571 29 2%
10/29 Hopper-new (-) CATV 10.0 1.73 17.
48 /15 12:00 med - Paste     815 74 2%
10/29 (+) CATV 10.7 1.48 13.
49 /15 12:00 Mixer 3 Paste     640 30 8%
10/29 Hopper-new (+) CATV 10.3 1.51 14.
50 /15 2:30 med + Paste     800 60 6%
10/29 Hopper-new (-) CATV 10.4 1.76 16.
51 /15 2:30 med - Paste     067 34 9%
11/4/ Rack 339 Cured (-) ~2" from top of stack, center/center of 10.0 1.11 11.
52 15   Mid CATV Plate plate   041 46 1%
11/4/ Rack 339 Cured (-) 10.2 0.39 3.8
53 15   Mid CATV Plate Top of stack, center/center of plate   831 47 %
11/4/ Rack 339 Cured (-) 10.3 0.90 8.7
54 15   Mid CATV Plate Bottom of stack, center/center of plate   997 58 %
11/4/ Rack 339 Cured (-) ~2" from top of stack, center/tab side 10.6 0.35 3.3
55 15   Mid CATV Plate of plate   309 12 %
11/4/ Rack 316 Cured (-) ~2" from top of stack, center/center of 10.1 0.94 9.4
56 15   Mid CATV Plate plate   190 64 %
11/4/ Rack 23 Cured (+) ~2" from top of stack, center/center of 10.2 0.09 0.9
57 15   Top CATV Plate plate   499 10 %
11/4/ Cured (+) ~2" from top of stack, center/center of 10.1 0.08 0.9
58 15   Rack 285 CATV Plate plate   241 81 %
11/4/ Cured (+) 10.2 0.11 1.1
59 15   Rack 285 CATV Plate Top of stack, center/center of plate   355 12 %
60 11/4/   Rack 285 Cured (+) Bottom of stack, center/center of plate   10.7 0.68 6.3
DOE: FREE LEAD CONVERSION 21

15 CATV Plate 768 04 %

11/4/ Cured (+) ~2" from top of stack, center/tab side 10.3 0.11 1.1
61 15   Rack 285 CATV Plate of plate   625 23 %
11/4/ Rack 23 Cured (+) ~2" from top of stack, center/center of 10.3 0.10 1.0
62 15   Mid CATV Plate plate   341 25 %
11/4/ Rack 175 Cured (+) ~2" from top of stack, center/center of 10.5 0.07 0.7
63 15   Top CATV Plate plate   094 59 %
11/4/ Rack 339 Cured (-) 10.2 0.39 3.8
64 15   Mid CATV Plate Top of stack, center/center of plate   831 47 %
11/4/ Rack 339 Cured (-) 10.3 0.90 8.7
65 15   Mid CATV Plate Bottom of stack, center/center of plate   997 58 %
11/4/ Rack 339 Cured (-) ~2" from top of stack, center/tab side 10.6 0.35 3.3
66 15   Mid CATV Plate of plate   309 12 %