Six Sigma at Cytec - Innovation and Six Sigma
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1
Six Sigma at Cytec
Innovation and Six Sigma
2
MotivationSix Sigma Training: Total Trained vs. Spending - 2001-2005
720707622
9701000
0102030405060708090
100110120
2001 2002 2003 2004 2005
Nu
mb
er t
rain
ed
0
200
400
600
800
1000
1200
Budget (K$ USD)
Managers
Green Belts
Black Belts
Master BlackBelts
0102030405060708090
100110120
2001 2002 2003 2004 2005
0
200
400
600
800
1000
1200
0102030405060708090
100110120
2001 2002 2003 2004 2005
0
200
400
600
800
1000
1200
0102030405060708090
100110120
2001 2002 2003 2004 2005
0
200
400
600
800
1000
1200
0102030405060708090
100110120
2001 2002 2003 2004 2005
0
200
400
600
800
1000
1200
0102030405060708090
100110120
2001 2002 2003 2004 2005
0
200
400
600
800
1000
1200
3
Guiding Thoughts
1. To make more money, we should learn more about our products and processes.
2. To learn, we should employ the scientific method (a.k.a. induction/deduction).
3. To employ the scientific method, we should select a tool set and methodology based on critical thinking.
4
Guiding Thoughts
TOOLS LEARNING PROFIT
5
Guiding Thoughts
1. To make more money, we should learn more about our products and processes.
2. To learn, we should employ the scientific method (a.k.a. induction/deduction).
3. To employ the scientific method, we should select a tool set and methodology based on critical thinking.
6
Critical Factors
All factors:
Y1 = f(x1, x2, x3…xn)
Y2 = f(x4, x5, x6…xm)
...
Critical factors:
Y* = f(x1*, x3*, x7*)
Y = f(x)
7
Science and Technology
• To paraphrase David Lilley, CEO…
– We are Cytec – our name indicates our focus on technology.
– We develop technically advanced solutions that differentiate our products from our competitors’ products.
– We sell technology in addition to products.
• The generation of knowledge is an important part of Cytec’s culture and success.
8
Learning and Financial Gain
Project goals
Financial gain
9
Learning and Financial Gain
Project goals
Financial gain
Benefits offinancial gain
10
Learning and Financial Gain
Project goals
Financial gain
Benefits offinancial gain
11
Learning and Financial Gain
Project goals
Financial gain Knowledge gain
Benefits offinancial gain
12
Learning and Financial Gain
Project goals
Financial gain Knowledge gain
Benefits offinancial gain
Benefits ofknowledge gain
13
EISTC Level in CS2 recovered
0
5
10
15
20
25
30
35
1 20 39 58 77 96 115 134 153 172 191 210 229 248 267 286 305 324 343 362 381
Number of Batch
EIS
TC
leve
l % w
/w Implementation of recommendations
14
When is Six Sigma Necessary?
Mike Farrington – Whirlpool Corp.
15
When is Six Sigma Necessary?
Mike Farrington – Whirlpool Corp.
16
When is Six Sigma Necessary?
Mike Farrington – Whirlpool Corp.
17
When is Six Sigma Necessary?
Mike Farrington – Whirlpool Corp.
18
When is Six Sigma Necessary?
Mike Farrington – Whirlpool Corp.
19
The Challenge for Six Sigma
• Tie together all the pieces that support…
TOOLS LEARNING PROFIT
20
1. To make more money, we should learn more about our products and processes.
2. To learn, we should employ the scientific method (a.k.a. induction/deduction).
3. To employ the scientific method, we should select a tool set and methodology based on critical thinking.
Guiding Thoughts
21
The Scientific Method
Statistics for Experimenters, Box, Hunter, and Hunter, Wiley, 1978.
22
DMAIC
Define
Measure
Analyze
Improve
Control
23
Science and Critical Thinking
“Science is not any particular method or set of techniques. It is a way of reasoning.
The standards are intellectual rather than procedural. The method of observation, formalization, and testing must vary with
the nature of the problem.”
Scientific Method and Social Problems, Edgar G. Miller, in Science 109, 290, 1949.
24
What are we trying to accomplish?
• We want to learn and innovate, so we can be more profitable.
• We want to take advantage of the power of Six Sigma:– Focus on variability reduction– Statistical experimentation– Consistent project management
• We want to foster creativity and innovation through critical thinking.
25
DMAIC
Define
Measure
Analyze
Improve
Control
26
Critical Factors
All factors:
Y1 = f(x1, x2, x3…xn)
Y2 = f(x4, x5, x6…xm)
...
Critical factors:
Y* = f(x1*, x3*, x7*)
Y = f(x) gainknowledge
27
1. To make more money, we should learn more about our products and processes.
2. To learn, we should employ the scientific method (a.k.a. induction/deduction).
3. To employ the scientific method, we should select a tool set and methodology based on critical thinking.
Guiding Thoughts
28
Alternatives to DMAIC
• The thought map…
(Six Sigma Associates)
LEGEND:
ProblemQuestions/issues
THEORIESPredictions
Data/informationCollection
Results
ActionsComments
Links
29
Thought Map Model
P rob lem
T H E O R Y
D ata C o llec tionS tra teg ies (P ro 's/C on 's)
P red ic tion s
R esu lts/C on clu sion s
S o lu tion s
T H E O R Y
D ata C o llec tionS tra teg ies (P ro 's/C on 's)
P red ic tion s
A n aly zeD ata
E xecu tion
(Q u estion s/O b servation s)
. . . .
MO
DIF
IED
TH
EO
RIE
S
30
Advantages ofThought Maps
• Drives learning, captures ideas (good and bad)
• Flexible, robust
• Captures the journey as well the results
– Example: What didn’t work?– Example: What else might we have done?– Example: What unexpected things happened?
31
Advantages ofThought Maps
• Transparent and accessible
• Excellent group tool, promotes discussion
• Not hard to learn
• Hard to do “wrong”
32
Disadvantages ofThought Maps
• Messy
• Potentially unfocused
• Difficult to standardize
• Difficult to file
• Difficult to evaluate
• Not sequential (in time) in the usual sense
• Not time based
33
Core Processes
Learn
Develop people
Develop the Organization
Short Courses
Green Belt training
Black Belt training
Master Black Belt training
Project Leadership training
Mentoring
$$
Manager training
Project Selection
Candidate Selection
Project Tracking
Project Closure
Certification
Rewards and recognition
Managing by data and metrics
34
Thought Map Example
35
WE CAN MAKE CRUDE XAND PURIFY BY
RECRYSTALLIZATIONAND STEAM
DISTILLATION
Path 1
This route has been fullydeveloped technically (lab
scale). However, capitalinvestiment required at site
makes price of productunacceptably high.
This path is not feasiblewith current customer and
specifications. Seemonthly reports of (people)
from (dates) for moreinformation.
How can the process for production of X from A be developed to meet customerspecifications for a 50% solution in water by (date)?
APHA color < 10pH 7.0-9.0
chloride content <1200 ppmcost < (price)
Others: metals, bromide, alkylhalide, etc. - refer to customer documentation.
Route currently under investigation for processdevelopment:
A + B + C --> X + Y
Other routes have been investigatedextensively (see monthly reports 1974-2002)
Can product from thecurrent lab process be
purified to meet thespecifications? IMPURITIES CONTAINING
Cl- (P, Q) WILL BEPRESENT IN ALL
SAMPLES of A
Path 2
CoV work showed that theamount of Cl- impuritiesdepends heavily on the
solvent used for storage.Variation in the range of10000-20000 ppm was
observed.
P, Q ARISE AS ACONSEQUENCE OF
EXTENDED STORAGE OFA IN SOLVENT. PURE A
SHOULD BE USEDRATHER THAN A THATHAS BEEN STORED INSOLVENT - THIS WILL
REDUCE THE MEAN ANDVARIATION IN IMPURITY
LEVELS.
Does the starting materialhave impurities?
MS IS “REPORTEDLY”VALID AND AGREES WITH
CUSTOMER MS, BUTSHOULD BE CHECKED.
Path 3
Initial MSE foundmeasurement error was
~500 ppm. This isunacceptable for this
application.
CoV study indicated asystematic effect related to
the stirring time, and thetime between sample
preparation and analysis.
Is the Cl- measurementsystem valid?
CoV study to determinethe levels of chloride indifferent lots of starting
material A
CoV study to determinethe variability in chloridelevels in different lots of
pure A.
Variability is less than thatof the MS (<12 ppm, 6
sigma)
Embed MSE in Cov study
ALL SAMPLES SHOULD BESTIRRED FOR AT LEAST
(TIME) AT (SETTING)BEFORE ANALYSIS.
Second MSE to evaluate theeffect of changes in
measurement procedure
Measurement error reducedto ~12 ppm (6 sigma) -
sufficient for thisapplication. N13.
Path 4
Can the standard variablesbe used to increase purity to
sufficient levels withoutfurther purification steps?
Path 5
Can Cl- be removedchemically by addition of
(reagent)?
Path 6
Can (person)’s method forchloride removal be
employed?
Consider optimizing:
mode of additionstoichiometry
stirringreaction temperaure
reaction timetype of solvent
amount of solventfiltration procedurerotavap procedure
others?
Could this route beimplemented at another
plant?
See path 4 detail
Current best conditionsproduce chloride levels of1100 ppm with variation of
~50 ppm (6 sigma) andsuccessfully meet color and
pH specifications.
STANDARD VARIABLESCAN BE OPTIMIZED TO
REDUCE CHLORIDECONTENT OF PRODUCTBEFORE PURIFICATION.
THIS METHOD HAS BEENDEMONSTRATED FOR Br-,AND MAY WORK FOR Cl-AS WELL. SHOULD NOTAFFECT pH OR COLOR.
Study factor effects usingsequential DOEs
Study this treament optionusing whole plot/split plot
DOE designs
This treatment had noeffect on chloride or pH
(DOE2), but removed colorto give final product thatbeat color specification.
Include this treatment instandard procedure from
now on.
Stir all samples for (time) at(setting) before analysis.
TREATMENT WITH(reagent) DOES NOTAFFECT CHLORIDE
CONTENT OR pH, BUTDOES REMOVE COLORED
IMPURITY.
THIS METHOD HAS BEENDEMONSTRATED FOR
RELATED CASES, BUT ISUNKNOWN WITH X AND A.
Study this treament optionusing whole plot/split plot DOE
designs
See path 6 detail
This treatment had no effect onchloride under a wide variety of
conditions.
STILL ROOM FORIMPROVEMENT IN THIS
AREA. (SEE PATH 4 DETAIL)
Best previous procedure typically saw <10000ppm chloride, but often as high as 50000 ppm
before purification. Had seen as low as 3000 ppmonce. APHA color ranged from 75-150 units. pH
was approximately 4.5.
36
How can the process for production of X from A be developed to meet customerspecifications for a 50% solution in water by (date)?
APHA color < 10pH 7.0-9.0
chloride content <1200 ppmcost < (price)
Others: metals, bromide, alkylhalide, etc. - refer to customer documentation.
37
How can the process for production of X from A be developed to meet customerspecifications for a 50% solution in water by (date)?
APHA color < 10pH 7.0-9.0
chloride content <1200 ppmcost < (price)
Others: metals, bromide, alkylhalide, etc. - refer to customer documentation.
Route currently under investigation for processdevelopment:
A + B + C --> X + Y
Other routes have been investigatedextensively (see monthly reports 1974-2002)
Best previous procedure typically saw <10000ppm chloride, but often as high as 50000 ppm
before purification. Had seen as low as 3000 ppmonce. APHA color ranged from 75-150 units. pH
was approximately 4.5.
38
How can the process for production of X from A be developed to meet customerspecifications for a 50% solution in water by (date)?
APHA color < 10pH 7.0-9.0
chloride content <1200 ppmcost < (price)
Others: metals, bromide, alkylhalide, etc. - refer to customer documentation.
Route currently under investigation for processdevelopment:
A + B + C --> X + Y
Other routes have been investigatedextensively (see monthly reports 1974-2002)
Can product from thecurrent lab process be
purified to meet thespecifications?
Does the starting materialhave impurities?
Is the Cl- measurementsystem valid?
Can the standard variablesbe used to increase purity to
sufficient levels withoutfurther purification steps?
Can Cl- be removedchemically by addition of
(reagent)?
Can (person)’s method forchloride removal be
employed?
Best previous procedure typically saw <10000ppm chloride, but often as high as 50000 ppm
before purification. Had seen as low as 3000 ppmonce. APHA color ranged from 75-150 units. pH
was approximately 4.5.
39
How can the process for production of X from A be developed to meet customerspecifications for a 50% solution in water by (date)?
APHA color < 10pH 7.0-9.0
chloride content <1200 ppmcost < (price)
Others: metals, bromide, alkylhalide, etc. - refer to customer documentation.
Route currently under investigation for processdevelopment:
A + B + C --> X + Y
Other routes have been investigatedextensively (see monthly reports 1974-2002)
Can product from thecurrent lab process be
purified to meet thespecifications?
Does the starting materialhave impurities?
Is the Cl- measurementsystem valid?
Can the standard variablesbe used to increase purity to
sufficient levels withoutfurther purification steps?
Can Cl- be removedchemically by addition of
(reagent)?
Can (person)’s method forchloride removal be
employed?
Best previous procedure typically saw <10000ppm chloride, but often as high as 50000 ppm
before purification. Had seen as low as 3000 ppmonce. APHA color ranged from 75-150 units. pH
was approximately 4.5.
LEGEND:
ProblemQuestions/issues
THEORIESPredictions
Data/informationCollection
Results
ActionsComments
Links
40
WE CAN MAKE CRUDE XAND PURIFY BY
RECRYSTALLIZATIONAND STEAM
DISTILLATION
Path 1
How can the process for production of X from A be developed to meet customerspecifications for a 50% solution in water by (date)?
APHA color < 10pH 7.0-9.0
chloride content <1200 ppmcost < (price)
Others: metals, bromide, alkylhalide, etc. - refer to customer documentation.
Route currently under investigation for processdevelopment:
A + B + C --> X + Y
Other routes have been investigatedextensively (see monthly reports 1974-2002)
Can product from thecurrent lab process be
purified to meet thespecifications? IMPURITIES CONTAINING
Cl- (P, Q) WILL BEPRESENT IN ALL
SAMPLES of A
Path 2
Does the starting materialhave impurities?
MS IS “REPORTEDLY”VALID AND AGREES WITH
CUSTOMER MS, BUTSHOULD BE CHECKED.
Path 3
Is the Cl- measurementsystem valid?
Path 4
Can the standard variablesbe used to increase purity to
sufficient levels withoutfurther purification steps?
Path 5
Can Cl- be removedchemically by addition of
(reagent)?
Path 6
Can (person)’s method forchloride removal be
employed?
STANDARD VARIABLESCAN BE OPTIMIZED TO
REDUCE CHLORIDECONTENT OF PRODUCTBEFORE PURIFICATION.
THIS METHOD HAS BEENDEMONSTRATED FOR Br-,AND MAY WORK FOR Cl-AS WELL. SHOULD NOTAFFECT pH OR COLOR.
THIS METHOD HAS BEENDEMONSTRATED FOR
RELATED CASES, BUT ISUNKNOWN WITH X AND A.
Best previous procedure typically saw <10000ppm chloride, but often as high as 50000 ppm
before purification. Had seen as low as 3000 ppmonce. APHA color ranged from 75-150 units. pH
was approximately 4.5.
41
WE CAN MAKE CRUDE XAND PURIFY BY
RECRYSTALLIZATIONAND STEAM
DISTILLATION
Path 1
This route has been fullydeveloped technically (lab
scale). However, capitalinvestiment required at site
makes price of productunacceptably high.
This path is not feasiblewith current customer and
specifications. Seemonthly reports of (people)
from (dates) for moreinformation.
How can the process for production of X from A be developed to meet customerspecifications for a 50% solution in water by (date)?
APHA color < 10pH 7.0-9.0
chloride content <1200 ppmcost < (price)
Others: metals, bromide, alkylhalide, etc. - refer to customer documentation.
Route currently under investigation for processdevelopment:
A + B + C --> X + Y
Other routes have been investigatedextensively (see monthly reports 1974-2002)
Can product from thecurrent lab process be
purified to meet thespecifications? IMPURITIES CONTAINING
Cl- (P, Q) WILL BEPRESENT IN ALL
SAMPLES of A
Path 2
Does the starting materialhave impurities?
MS IS “REPORTEDLY”VALID AND AGREES WITH
CUSTOMER MS, BUTSHOULD BE CHECKED.
Path 3
Is the Cl- measurementsystem valid?
Path 4
Can the standard variablesbe used to increase purity to
sufficient levels withoutfurther purification steps?
Path 5
Can Cl- be removedchemically by addition of
(reagent)?
Path 6
Can (person)’s method forchloride removal be
employed?
Could this route beimplemented at another
plant?
STANDARD VARIABLESCAN BE OPTIMIZED TO
REDUCE CHLORIDECONTENT OF PRODUCTBEFORE PURIFICATION.
THIS METHOD HAS BEENDEMONSTRATED FOR Br-,AND MAY WORK FOR Cl-AS WELL. SHOULD NOTAFFECT pH OR COLOR.
THIS METHOD HAS BEENDEMONSTRATED FOR
RELATED CASES, BUT ISUNKNOWN WITH X AND A.
Best previous procedure typically saw <10000ppm chloride, but often as high as 50000 ppm
before purification. Had seen as low as 3000 ppmonce. APHA color ranged from 75-150 units. pH
was approximately 4.5.
42
WE CAN MAKE CRUDE XAND PURIFY BY
RECRYSTALLIZATIONAND STEAM
DISTILLATION
Path 1
This route has been fullydeveloped technically (lab
scale). However, capitalinvestiment required at site
makes price of productunacceptably high.
This path is not feasiblewith current customer and
specifications. Seemonthly reports of (people)
from (dates) for moreinformation.
How can the process for production of X from A be developed to meet customerspecifications for a 50% solution in water by (date)?
APHA color < 10pH 7.0-9.0
chloride content <1200 ppmcost < (price)
Others: metals, bromide, alkylhalide, etc. - refer to customer documentation.
Route currently under investigation for processdevelopment:
A + B + C --> X + Y
Other routes have been investigatedextensively (see monthly reports 1974-2002)
Can product from thecurrent lab process be
purified to meet thespecifications? IMPURITIES CONTAINING
Cl- (P, Q) WILL BEPRESENT IN ALL
SAMPLES of A
Path 2
Does the starting materialhave impurities?
MS IS “REPORTEDLY”VALID AND AGREES WITH
CUSTOMER MS, BUTSHOULD BE CHECKED.
Path 3
Is the Cl- measurementsystem valid?
CoV study to determinethe levels of chloride indifferent lots of starting
material A
Embed MSE in Cov study
Path 4
Can the standard variablesbe used to increase purity to
sufficient levels withoutfurther purification steps?
Path 5
Can Cl- be removedchemically by addition of
(reagent)?
Path 6
Can (person)’s method forchloride removal be
employed?
Could this route beimplemented at another
plant?
STANDARD VARIABLESCAN BE OPTIMIZED TO
REDUCE CHLORIDECONTENT OF PRODUCTBEFORE PURIFICATION.
THIS METHOD HAS BEENDEMONSTRATED FOR Br-,AND MAY WORK FOR Cl-AS WELL. SHOULD NOTAFFECT pH OR COLOR.
THIS METHOD HAS BEENDEMONSTRATED FOR
RELATED CASES, BUT ISUNKNOWN WITH X AND A.
Best previous procedure typically saw <10000ppm chloride, but often as high as 50000 ppm
before purification. Had seen as low as 3000 ppmonce. APHA color ranged from 75-150 units. pH
was approximately 4.5.
43
WE CAN MAKE CRUDE XAND PURIFY BY
RECRYSTALLIZATIONAND STEAM
DISTILLATION
Path 1
This route has been fullydeveloped technically (lab
scale). However, capitalinvestiment required at site
makes price of productunacceptably high.
This path is not feasiblewith current customer and
specifications. Seemonthly reports of (people)
from (dates) for moreinformation.
How can the process for production of X from A be developed to meet customerspecifications for a 50% solution in water by (date)?
APHA color < 10pH 7.0-9.0
chloride content <1200 ppmcost < (price)
Others: metals, bromide, alkylhalide, etc. - refer to customer documentation.
Route currently under investigation for processdevelopment:
A + B + C --> X + Y
Other routes have been investigatedextensively (see monthly reports 1974-2002)
Can product from thecurrent lab process be
purified to meet thespecifications? IMPURITIES CONTAINING
Cl- (P, Q) WILL BEPRESENT IN ALL
SAMPLES of A
Path 2
CoV work showed that theamount of Cl- impuritiesdepends heavily on the
solvent used for storage.Variation in the range of10000-20000 ppm was
observed.
Does the starting materialhave impurities?
MS IS “REPORTEDLY”VALID AND AGREES WITH
CUSTOMER MS, BUTSHOULD BE CHECKED.
Path 3
Initial MSE foundmeasurement error was
~500 ppm. This isunacceptable for this
application.
Is the Cl- measurementsystem valid?
CoV study to determinethe levels of chloride indifferent lots of starting
material A
Embed MSE in Cov study
Path 4
Can the standard variablesbe used to increase purity to
sufficient levels withoutfurther purification steps?
Path 5
Can Cl- be removedchemically by addition of
(reagent)?
Path 6
Can (person)’s method forchloride removal be
employed?
Could this route beimplemented at another
plant?
STANDARD VARIABLESCAN BE OPTIMIZED TO
REDUCE CHLORIDECONTENT OF PRODUCTBEFORE PURIFICATION.
THIS METHOD HAS BEENDEMONSTRATED FOR Br-,AND MAY WORK FOR Cl-AS WELL. SHOULD NOTAFFECT pH OR COLOR.
THIS METHOD HAS BEENDEMONSTRATED FOR
RELATED CASES, BUT ISUNKNOWN WITH X AND A.
Best previous procedure typically saw <10000ppm chloride, but often as high as 50000 ppm
before purification. Had seen as low as 3000 ppmonce. APHA color ranged from 75-150 units. pH
was approximately 4.5.
44
WE CAN MAKE CRUDE XAND PURIFY BY
RECRYSTALLIZATIONAND STEAM
DISTILLATION
Path 1
This route has been fullydeveloped technically (lab
scale). However, capitalinvestiment required at site
makes price of productunacceptably high.
This path is not feasiblewith current customer and
specifications. Seemonthly reports of (people)
from (dates) for moreinformation.
How can the process for production of X from A be developed to meet customerspecifications for a 50% solution in water by (date)?
APHA color < 10pH 7.0-9.0
chloride content <1200 ppmcost < (price)
Others: metals, bromide, alkylhalide, etc. - refer to customer documentation.
Route currently under investigation for processdevelopment:
A + B + C --> X + Y
Other routes have been investigatedextensively (see monthly reports 1974-2002)
Can product from thecurrent lab process be
purified to meet thespecifications? IMPURITIES CONTAINING
Cl- (P, Q) WILL BEPRESENT IN ALL
SAMPLES of A
Path 2
CoV work showed that theamount of Cl- impuritiesdepends heavily on the
solvent used for storage.Variation in the range of10000-20000 ppm was
observed.
P, Q ARISE AS ACONSEQUENCE OF
EXTENDED STORAGE OFA IN SOLVENT. PURE A
SHOULD BE USEDRATHER THAN A THATHAS BEEN STORED INSOLVENT - THIS WILL
REDUCE THE MEAN ANDVARIATION IN IMPURITY
LEVELS.
Does the starting materialhave impurities?
MS IS “REPORTEDLY”VALID AND AGREES WITH
CUSTOMER MS, BUTSHOULD BE CHECKED.
Path 3
Initial MSE foundmeasurement error was
~500 ppm. This isunacceptable for this
application.
CoV study indicated asystematic effect related to
the stirring time, and thetime between sample
preparation and analysis.
Is the Cl- measurementsystem valid?
CoV study to determinethe levels of chloride indifferent lots of starting
material A
Embed MSE in Cov study
ALL SAMPLES SHOULD BESTIRRED FOR AT LEAST
(TIME) AT (SETTING)BEFORE ANALYSIS.
Path 4
Can the standard variablesbe used to increase purity to
sufficient levels withoutfurther purification steps?
Path 5
Can Cl- be removedchemically by addition of
(reagent)?
Path 6
Can (person)’s method forchloride removal be
employed?
Could this route beimplemented at another
plant?
STANDARD VARIABLESCAN BE OPTIMIZED TO
REDUCE CHLORIDECONTENT OF PRODUCTBEFORE PURIFICATION.
THIS METHOD HAS BEENDEMONSTRATED FOR Br-,AND MAY WORK FOR Cl-AS WELL. SHOULD NOTAFFECT pH OR COLOR.
THIS METHOD HAS BEENDEMONSTRATED FOR
RELATED CASES, BUT ISUNKNOWN WITH X AND A.
Best previous procedure typically saw <10000ppm chloride, but often as high as 50000 ppm
before purification. Had seen as low as 3000 ppmonce. APHA color ranged from 75-150 units. pH
was approximately 4.5.
45
WE CAN MAKE CRUDE XAND PURIFY BY
RECRYSTALLIZATIONAND STEAM
DISTILLATION
Path 1
This route has been fullydeveloped technically (lab
scale). However, capitalinvestiment required at site
makes price of productunacceptably high.
This path is not feasiblewith current customer and
specifications. Seemonthly reports of (people)
from (dates) for moreinformation.
How can the process for production of X from A be developed to meet customerspecifications for a 50% solution in water by (date)?
APHA color < 10pH 7.0-9.0
chloride content <1200 ppmcost < (price)
Others: metals, bromide, alkylhalide, etc. - refer to customer documentation.
Route currently under investigation for processdevelopment:
A + B + C --> X + Y
Other routes have been investigatedextensively (see monthly reports 1974-2002)
Can product from thecurrent lab process be
purified to meet thespecifications? IMPURITIES CONTAINING
Cl- (P, Q) WILL BEPRESENT IN ALL
SAMPLES of A
Path 2
CoV work showed that theamount of Cl- impuritiesdepends heavily on the
solvent used for storage.Variation in the range of10000-20000 ppm was
observed.
P, Q ARISE AS ACONSEQUENCE OF
EXTENDED STORAGE OFA IN SOLVENT. PURE A
SHOULD BE USEDRATHER THAN A THATHAS BEEN STORED INSOLVENT - THIS WILL
REDUCE THE MEAN ANDVARIATION IN IMPURITY
LEVELS.
Does the starting materialhave impurities?
MS IS “REPORTEDLY”VALID AND AGREES WITH
CUSTOMER MS, BUTSHOULD BE CHECKED.
Path 3
Initial MSE foundmeasurement error was
~500 ppm. This isunacceptable for this
application.
CoV study indicated asystematic effect related to
the stirring time, and thetime between sample
preparation and analysis.
Is the Cl- measurementsystem valid?
CoV study to determinethe levels of chloride indifferent lots of starting
material A
CoV study to determinethe variability in chloridelevels in different lots of
pure A.
Embed MSE in Cov study
ALL SAMPLES SHOULD BESTIRRED FOR AT LEAST
(TIME) AT (SETTING)BEFORE ANALYSIS.
Second MSE to evaluate theeffect of changes in
measurement procedure
Path 4
Can the standard variablesbe used to increase purity to
sufficient levels withoutfurther purification steps?
Path 5
Can Cl- be removedchemically by addition of
(reagent)?
Path 6
Can (person)’s method forchloride removal be
employed?
Could this route beimplemented at another
plant?
STANDARD VARIABLESCAN BE OPTIMIZED TO
REDUCE CHLORIDECONTENT OF PRODUCTBEFORE PURIFICATION.
THIS METHOD HAS BEENDEMONSTRATED FOR Br-,AND MAY WORK FOR Cl-AS WELL. SHOULD NOTAFFECT pH OR COLOR.
THIS METHOD HAS BEENDEMONSTRATED FOR
RELATED CASES, BUT ISUNKNOWN WITH X AND A.
Best previous procedure typically saw <10000ppm chloride, but often as high as 50000 ppm
before purification. Had seen as low as 3000 ppmonce. APHA color ranged from 75-150 units. pH
was approximately 4.5.
46
WE CAN MAKE CRUDE XAND PURIFY BY
RECRYSTALLIZATIONAND STEAM
DISTILLATION
Path 1
This route has been fullydeveloped technically (lab
scale). However, capitalinvestiment required at site
makes price of productunacceptably high.
This path is not feasiblewith current customer and
specifications. Seemonthly reports of (people)
from (dates) for moreinformation.
How can the process for production of X from A be developed to meet customerspecifications for a 50% solution in water by (date)?
APHA color < 10pH 7.0-9.0
chloride content <1200 ppmcost < (price)
Others: metals, bromide, alkylhalide, etc. - refer to customer documentation.
Route currently under investigation for processdevelopment:
A + B + C --> X + Y
Other routes have been investigatedextensively (see monthly reports 1974-2002)
Can product from thecurrent lab process be
purified to meet thespecifications? IMPURITIES CONTAINING
Cl- (P, Q) WILL BEPRESENT IN ALL
SAMPLES of A
Path 2
CoV work showed that theamount of Cl- impuritiesdepends heavily on the
solvent used for storage.Variation in the range of10000-20000 ppm was
observed.
P, Q ARISE AS ACONSEQUENCE OF
EXTENDED STORAGE OFA IN SOLVENT. PURE A
SHOULD BE USEDRATHER THAN A THATHAS BEEN STORED INSOLVENT - THIS WILL
REDUCE THE MEAN ANDVARIATION IN IMPURITY
LEVELS.
Does the starting materialhave impurities?
MS IS “REPORTEDLY”VALID AND AGREES WITH
CUSTOMER MS, BUTSHOULD BE CHECKED.
Path 3
Initial MSE foundmeasurement error was
~500 ppm. This isunacceptable for this
application.
CoV study indicated asystematic effect related to
the stirring time, and thetime between sample
preparation and analysis.
Is the Cl- measurementsystem valid?
CoV study to determinethe levels of chloride indifferent lots of starting
material A
CoV study to determinethe variability in chloridelevels in different lots of
pure A.
Variability is less than thatof the MS (<12 ppm, 6
sigma)
Embed MSE in Cov study
ALL SAMPLES SHOULD BESTIRRED FOR AT LEAST
(TIME) AT (SETTING)BEFORE ANALYSIS.
Second MSE to evaluate theeffect of changes in
measurement procedure
Measurement error reducedto ~12 ppm (6 sigma) -
sufficient for thisapplication. N13.
Path 4
Can the standard variablesbe used to increase purity to
sufficient levels withoutfurther purification steps?
Path 5
Can Cl- be removedchemically by addition of
(reagent)?
Path 6
Can (person)’s method forchloride removal be
employed?
Could this route beimplemented at another
plant?
STANDARD VARIABLESCAN BE OPTIMIZED TO
REDUCE CHLORIDECONTENT OF PRODUCTBEFORE PURIFICATION.
THIS METHOD HAS BEENDEMONSTRATED FOR Br-,AND MAY WORK FOR Cl-AS WELL. SHOULD NOTAFFECT pH OR COLOR.
Stir all samples for (time) at(setting) before analysis.
THIS METHOD HAS BEENDEMONSTRATED FOR
RELATED CASES, BUT ISUNKNOWN WITH X AND A.
Best previous procedure typically saw <10000ppm chloride, but often as high as 50000 ppm
before purification. Had seen as low as 3000 ppmonce. APHA color ranged from 75-150 units. pH
was approximately 4.5.
47
WE CAN MAKE CRUDE XAND PURIFY BY
RECRYSTALLIZATIONAND STEAM
DISTILLATION
Path 1
This route has been fullydeveloped technically (lab
scale). However, capitalinvestiment required at site
makes price of productunacceptably high.
This path is not feasiblewith current customer and
specifications. Seemonthly reports of (people)
from (dates) for moreinformation.
How can the process for production of X from A be developed to meet customerspecifications for a 50% solution in water by (date)?
APHA color < 10pH 7.0-9.0
chloride content <1200 ppmcost < (price)
Others: metals, bromide, alkylhalide, etc. - refer to customer documentation.
Route currently under investigation for processdevelopment:
A + B + C --> X + Y
Other routes have been investigatedextensively (see monthly reports 1974-2002)
Can product from thecurrent lab process be
purified to meet thespecifications? IMPURITIES CONTAINING
Cl- (P, Q) WILL BEPRESENT IN ALL
SAMPLES of A
Path 2
CoV work showed that theamount of Cl- impuritiesdepends heavily on the
solvent used for storage.Variation in the range of10000-20000 ppm was
observed.
P, Q ARISE AS ACONSEQUENCE OF
EXTENDED STORAGE OFA IN SOLVENT. PURE A
SHOULD BE USEDRATHER THAN A THATHAS BEEN STORED INSOLVENT - THIS WILL
REDUCE THE MEAN ANDVARIATION IN IMPURITY
LEVELS.
Does the starting materialhave impurities?
MS IS “REPORTEDLY”VALID AND AGREES WITH
CUSTOMER MS, BUTSHOULD BE CHECKED.
Path 3
Initial MSE foundmeasurement error was
~500 ppm. This isunacceptable for this
application.
CoV study indicated asystematic effect related to
the stirring time, and thetime between sample
preparation and analysis.
Is the Cl- measurementsystem valid?
CoV study to determinethe levels of chloride indifferent lots of starting
material A
CoV study to determinethe variability in chloridelevels in different lots of
pure A.
Variability is less than thatof the MS (<12 ppm, 6
sigma)
Embed MSE in Cov study
ALL SAMPLES SHOULD BESTIRRED FOR AT LEAST
(TIME) AT (SETTING)BEFORE ANALYSIS.
Second MSE to evaluate theeffect of changes in
measurement procedure
Measurement error reducedto ~12 ppm (6 sigma) -
sufficient for thisapplication. N13.
Path 4
Can the standard variablesbe used to increase purity to
sufficient levels withoutfurther purification steps?
Path 5
Can Cl- be removedchemically by addition of
(reagent)?
Path 6
Can (person)’s method forchloride removal be
employed?
Consider optimizing:
mode of additionstoichiometry
stirringreaction temperaure
reaction timetype of solvent
amount of solventfiltration procedurerotavap procedure
others?
Could this route beimplemented at another
plant?
STANDARD VARIABLESCAN BE OPTIMIZED TO
REDUCE CHLORIDECONTENT OF PRODUCTBEFORE PURIFICATION.
THIS METHOD HAS BEENDEMONSTRATED FOR Br-,AND MAY WORK FOR Cl-AS WELL. SHOULD NOTAFFECT pH OR COLOR.
Stir all samples for (time) at(setting) before analysis.
THIS METHOD HAS BEENDEMONSTRATED FOR
RELATED CASES, BUT ISUNKNOWN WITH X AND A.
Best previous procedure typically saw <10000ppm chloride, but often as high as 50000 ppm
before purification. Had seen as low as 3000 ppmonce. APHA color ranged from 75-150 units. pH
was approximately 4.5.
48
WE CAN MAKE CRUDE XAND PURIFY BY
RECRYSTALLIZATIONAND STEAM
DISTILLATION
Path 1
This route has been fullydeveloped technically (lab
scale). However, capitalinvestiment required at site
makes price of productunacceptably high.
This path is not feasiblewith current customer and
specifications. Seemonthly reports of (people)
from (dates) for moreinformation.
How can the process for production of X from A be developed to meet customerspecifications for a 50% solution in water by (date)?
APHA color < 10pH 7.0-9.0
chloride content <1200 ppmcost < (price)
Others: metals, bromide, alkylhalide, etc. - refer to customer documentation.
Route currently under investigation for processdevelopment:
A + B + C --> X + Y
Other routes have been investigatedextensively (see monthly reports 1974-2002)
Can product from thecurrent lab process be
purified to meet thespecifications? IMPURITIES CONTAINING
Cl- (P, Q) WILL BEPRESENT IN ALL
SAMPLES of A
Path 2
CoV work showed that theamount of Cl- impuritiesdepends heavily on the
solvent used for storage.Variation in the range of10000-20000 ppm was
observed.
P, Q ARISE AS ACONSEQUENCE OF
EXTENDED STORAGE OFA IN SOLVENT. PURE A
SHOULD BE USEDRATHER THAN A THATHAS BEEN STORED INSOLVENT - THIS WILL
REDUCE THE MEAN ANDVARIATION IN IMPURITY
LEVELS.
Does the starting materialhave impurities?
MS IS “REPORTEDLY”VALID AND AGREES WITH
CUSTOMER MS, BUTSHOULD BE CHECKED.
Path 3
Initial MSE foundmeasurement error was
~500 ppm. This isunacceptable for this
application.
CoV study indicated asystematic effect related to
the stirring time, and thetime between sample
preparation and analysis.
Is the Cl- measurementsystem valid?
CoV study to determinethe levels of chloride indifferent lots of starting
material A
CoV study to determinethe variability in chloridelevels in different lots of
pure A.
Variability is less than thatof the MS (<12 ppm, 6
sigma)
Embed MSE in Cov study
ALL SAMPLES SHOULD BESTIRRED FOR AT LEAST
(TIME) AT (SETTING)BEFORE ANALYSIS.
Second MSE to evaluate theeffect of changes in
measurement procedure
Measurement error reducedto ~12 ppm (6 sigma) -
sufficient for thisapplication. N13.
Path 4
Can the standard variablesbe used to increase purity to
sufficient levels withoutfurther purification steps?
Path 5
Can Cl- be removedchemically by addition of
(reagent)?
Path 6
Can (person)’s method forchloride removal be
employed?
Consider optimizing:
mode of additionstoichiometry
stirringreaction temperaure
reaction timetype of solvent
amount of solventfiltration procedurerotavap procedure
others?
Could this route beimplemented at another
plant?
STANDARD VARIABLESCAN BE OPTIMIZED TO
REDUCE CHLORIDECONTENT OF PRODUCTBEFORE PURIFICATION.
THIS METHOD HAS BEENDEMONSTRATED FOR Br-,AND MAY WORK FOR Cl-AS WELL. SHOULD NOTAFFECT pH OR COLOR.
Study factor effects usingsequential DOEs
Study this treament optionusing whole plot/split plot
DOE designs
Stir all samples for (time) at(setting) before analysis.
THIS METHOD HAS BEENDEMONSTRATED FOR
RELATED CASES, BUT ISUNKNOWN WITH X AND A.
Study this treament optionusing whole plot/split plot DOE
designs
Best previous procedure typically saw <10000ppm chloride, but often as high as 50000 ppm
before purification. Had seen as low as 3000 ppmonce. APHA color ranged from 75-150 units. pH
was approximately 4.5.
49
WE CAN MAKE CRUDE XAND PURIFY BY
RECRYSTALLIZATIONAND STEAM
DISTILLATION
Path 1
This route has been fullydeveloped technically (lab
scale). However, capitalinvestiment required at site
makes price of productunacceptably high.
This path is not feasiblewith current customer and
specifications. Seemonthly reports of (people)
from (dates) for moreinformation.
How can the process for production of X from A be developed to meet customerspecifications for a 50% solution in water by (date)?
APHA color < 10pH 7.0-9.0
chloride content <1200 ppmcost < (price)
Others: metals, bromide, alkylhalide, etc. - refer to customer documentation.
Route currently under investigation for processdevelopment:
A + B + C --> X + Y
Other routes have been investigatedextensively (see monthly reports 1974-2002)
Can product from thecurrent lab process be
purified to meet thespecifications? IMPURITIES CONTAINING
Cl- (P, Q) WILL BEPRESENT IN ALL
SAMPLES of A
Path 2
CoV work showed that theamount of Cl- impuritiesdepends heavily on the
solvent used for storage.Variation in the range of10000-20000 ppm was
observed.
P, Q ARISE AS ACONSEQUENCE OF
EXTENDED STORAGE OFA IN SOLVENT. PURE A
SHOULD BE USEDRATHER THAN A THATHAS BEEN STORED INSOLVENT - THIS WILL
REDUCE THE MEAN ANDVARIATION IN IMPURITY
LEVELS.
Does the starting materialhave impurities?
MS IS “REPORTEDLY”VALID AND AGREES WITH
CUSTOMER MS, BUTSHOULD BE CHECKED.
Path 3
Initial MSE foundmeasurement error was
~500 ppm. This isunacceptable for this
application.
CoV study indicated asystematic effect related to
the stirring time, and thetime between sample
preparation and analysis.
Is the Cl- measurementsystem valid?
CoV study to determinethe levels of chloride indifferent lots of starting
material A
CoV study to determinethe variability in chloridelevels in different lots of
pure A.
Variability is less than thatof the MS (<12 ppm, 6
sigma)
Embed MSE in Cov study
ALL SAMPLES SHOULD BESTIRRED FOR AT LEAST
(TIME) AT (SETTING)BEFORE ANALYSIS.
Second MSE to evaluate theeffect of changes in
measurement procedure
Measurement error reducedto ~12 ppm (6 sigma) -
sufficient for thisapplication. N13.
Path 4
Can the standard variablesbe used to increase purity to
sufficient levels withoutfurther purification steps?
Path 5
Can Cl- be removedchemically by addition of
(reagent)?
Path 6
Can (person)’s method forchloride removal be
employed?
Consider optimizing:
mode of additionstoichiometry
stirringreaction temperaure
reaction timetype of solvent
amount of solventfiltration procedurerotavap procedure
others?
Could this route beimplemented at another
plant?
STANDARD VARIABLESCAN BE OPTIMIZED TO
REDUCE CHLORIDECONTENT OF PRODUCTBEFORE PURIFICATION.
THIS METHOD HAS BEENDEMONSTRATED FOR Br-,AND MAY WORK FOR Cl-AS WELL. SHOULD NOTAFFECT pH OR COLOR.
Study factor effects usingsequential DOEs
Study this treament optionusing whole plot/split plot
DOE designs
This treatment had noeffect on chloride or pH
(DOE2), but removed colorto give final product thatbeat color specification.
Include this treatment instandard procedure from
now on.
Stir all samples for (time) at(setting) before analysis.
TREATMENT WITH(reagent) DOES NOTAFFECT CHLORIDE
CONTENT OR pH, BUTDOES REMOVE COLORED
IMPURITY.
THIS METHOD HAS BEENDEMONSTRATED FOR
RELATED CASES, BUT ISUNKNOWN WITH X AND A.
Study this treament optionusing whole plot/split plot DOE
designs
Best previous procedure typically saw <10000ppm chloride, but often as high as 50000 ppm
before purification. Had seen as low as 3000 ppmonce. APHA color ranged from 75-150 units. pH
was approximately 4.5.
50
WE CAN MAKE CRUDE XAND PURIFY BY
RECRYSTALLIZATIONAND STEAM
DISTILLATION
Path 1
This route has been fullydeveloped technically (lab
scale). However, capitalinvestiment required at site
makes price of productunacceptably high.
This path is not feasiblewith current customer and
specifications. Seemonthly reports of (people)
from (dates) for moreinformation.
How can the process for production of X from A be developed to meet customerspecifications for a 50% solution in water by (date)?
APHA color < 10pH 7.0-9.0
chloride content <1200 ppmcost < (price)
Others: metals, bromide, alkylhalide, etc. - refer to customer documentation.
Route currently under investigation for processdevelopment:
A + B + C --> X + Y
Other routes have been investigatedextensively (see monthly reports 1974-2002)
Can product from thecurrent lab process be
purified to meet thespecifications? IMPURITIES CONTAINING
Cl- (P, Q) WILL BEPRESENT IN ALL
SAMPLES of A
Path 2
CoV work showed that theamount of Cl- impuritiesdepends heavily on the
solvent used for storage.Variation in the range of10000-20000 ppm was
observed.
P, Q ARISE AS ACONSEQUENCE OF
EXTENDED STORAGE OFA IN SOLVENT. PURE A
SHOULD BE USEDRATHER THAN A THATHAS BEEN STORED INSOLVENT - THIS WILL
REDUCE THE MEAN ANDVARIATION IN IMPURITY
LEVELS.
Does the starting materialhave impurities?
MS IS “REPORTEDLY”VALID AND AGREES WITH
CUSTOMER MS, BUTSHOULD BE CHECKED.
Path 3
Initial MSE foundmeasurement error was
~500 ppm. This isunacceptable for this
application.
CoV study indicated asystematic effect related to
the stirring time, and thetime between sample
preparation and analysis.
Is the Cl- measurementsystem valid?
CoV study to determinethe levels of chloride indifferent lots of starting
material A
CoV study to determinethe variability in chloridelevels in different lots of
pure A.
Variability is less than thatof the MS (<12 ppm, 6
sigma)
Embed MSE in Cov study
ALL SAMPLES SHOULD BESTIRRED FOR AT LEAST
(TIME) AT (SETTING)BEFORE ANALYSIS.
Second MSE to evaluate theeffect of changes in
measurement procedure
Measurement error reducedto ~12 ppm (6 sigma) -
sufficient for thisapplication. N13.
Path 4
Can the standard variablesbe used to increase purity to
sufficient levels withoutfurther purification steps?
Path 5
Can Cl- be removedchemically by addition of
(reagent)?
Path 6
Can (person)’s method forchloride removal be
employed?
Consider optimizing:
mode of additionstoichiometry
stirringreaction temperaure
reaction timetype of solvent
amount of solventfiltration procedurerotavap procedure
others?
Could this route beimplemented at another
plant?
STANDARD VARIABLESCAN BE OPTIMIZED TO
REDUCE CHLORIDECONTENT OF PRODUCTBEFORE PURIFICATION.
THIS METHOD HAS BEENDEMONSTRATED FOR Br-,AND MAY WORK FOR Cl-AS WELL. SHOULD NOTAFFECT pH OR COLOR.
Study factor effects usingsequential DOEs
Study this treament optionusing whole plot/split plot
DOE designs
This treatment had noeffect on chloride or pH
(DOE2), but removed colorto give final product thatbeat color specification.
Include this treatment instandard procedure from
now on.
Stir all samples for (time) at(setting) before analysis.
TREATMENT WITH(reagent) DOES NOTAFFECT CHLORIDE
CONTENT OR pH, BUTDOES REMOVE COLORED
IMPURITY.
THIS METHOD HAS BEENDEMONSTRATED FOR
RELATED CASES, BUT ISUNKNOWN WITH X AND A.
Study this treament optionusing whole plot/split plot DOE
designs
See path 6 detail
This treatment had no effect onchloride under a wide variety of
conditions.
Best previous procedure typically saw <10000ppm chloride, but often as high as 50000 ppm
before purification. Had seen as low as 3000 ppmonce. APHA color ranged from 75-150 units. pH
was approximately 4.5.
51
WE CAN MAKE CRUDE XAND PURIFY BY
RECRYSTALLIZATIONAND STEAM
DISTILLATION
Path 1
This route has been fullydeveloped technically (lab
scale). However, capitalinvestiment required at site
makes price of productunacceptably high.
This path is not feasiblewith current customer and
specifications. Seemonthly reports of (people)
from (dates) for moreinformation.
How can the process for production of X from A be developed to meet customerspecifications for a 50% solution in water by (date)?
APHA color < 10pH 7.0-9.0
chloride content <1200 ppmcost < (price)
Others: metals, bromide, alkylhalide, etc. - refer to customer documentation.
Route currently under investigation for processdevelopment:
A + B + C --> X + Y
Other routes have been investigatedextensively (see monthly reports 1974-2002)
Can product from thecurrent lab process be
purified to meet thespecifications? IMPURITIES CONTAINING
Cl- (P, Q) WILL BEPRESENT IN ALL
SAMPLES of A
Path 2
CoV work showed that theamount of Cl- impuritiesdepends heavily on the
solvent used for storage.Variation in the range of10000-20000 ppm was
observed.
P, Q ARISE AS ACONSEQUENCE OF
EXTENDED STORAGE OFA IN SOLVENT. PURE A
SHOULD BE USEDRATHER THAN A THATHAS BEEN STORED INSOLVENT - THIS WILL
REDUCE THE MEAN ANDVARIATION IN IMPURITY
LEVELS.
Does the starting materialhave impurities?
MS IS “REPORTEDLY”VALID AND AGREES WITH
CUSTOMER MS, BUTSHOULD BE CHECKED.
Path 3
Initial MSE foundmeasurement error was
~500 ppm. This isunacceptable for this
application.
CoV study indicated asystematic effect related to
the stirring time, and thetime between sample
preparation and analysis.
Is the Cl- measurementsystem valid?
CoV study to determinethe levels of chloride indifferent lots of starting
material A
CoV study to determinethe variability in chloridelevels in different lots of
pure A.
Variability is less than thatof the MS (<12 ppm, 6
sigma)
Embed MSE in Cov study
ALL SAMPLES SHOULD BESTIRRED FOR AT LEAST
(TIME) AT (SETTING)BEFORE ANALYSIS.
Second MSE to evaluate theeffect of changes in
measurement procedure
Measurement error reducedto ~12 ppm (6 sigma) -
sufficient for thisapplication. N13.
Path 4
Can the standard variablesbe used to increase purity to
sufficient levels withoutfurther purification steps?
Path 5
Can Cl- be removedchemically by addition of
(reagent)?
Path 6
Can (person)’s method forchloride removal be
employed?
Consider optimizing:
mode of additionstoichiometry
stirringreaction temperaure
reaction timetype of solvent
amount of solventfiltration procedurerotavap procedure
others?
Could this route beimplemented at another
plant?
See path 4 detail
Current best conditionsproduce chloride levels of1100 ppm with variation of
~50 ppm (6 sigma) andsuccessfully meet color and
pH specifications.
STANDARD VARIABLESCAN BE OPTIMIZED TO
REDUCE CHLORIDECONTENT OF PRODUCTBEFORE PURIFICATION.
THIS METHOD HAS BEENDEMONSTRATED FOR Br-,AND MAY WORK FOR Cl-AS WELL. SHOULD NOTAFFECT pH OR COLOR.
Study factor effects usingsequential DOEs
Study this treament optionusing whole plot/split plot
DOE designs
This treatment had noeffect on chloride or pH
(DOE2), but removed colorto give final product thatbeat color specification.
Include this treatment instandard procedure from
now on.
Stir all samples for (time) at(setting) before analysis.
TREATMENT WITH(reagent) DOES NOTAFFECT CHLORIDE
CONTENT OR pH, BUTDOES REMOVE COLORED
IMPURITY.
THIS METHOD HAS BEENDEMONSTRATED FOR
RELATED CASES, BUT ISUNKNOWN WITH X AND A.
Study this treament optionusing whole plot/split plot DOE
designs
See path 6 detail
This treatment had no effect onchloride under a wide variety of
conditions.
Best previous procedure typically saw <10000ppm chloride, but often as high as 50000 ppm
before purification. Had seen as low as 3000 ppmonce. APHA color ranged from 75-150 units. pH
was approximately 4.5.
52
WE CAN MAKE CRUDE XAND PURIFY BY
RECRYSTALLIZATIONAND STEAM
DISTILLATION
Path 1
This route has been fullydeveloped technically (lab
scale). However, capitalinvestiment required at site
makes price of productunacceptably high.
This path is not feasiblewith current customer and
specifications. Seemonthly reports of (people)
from (dates) for moreinformation.
How can the process for production of X from A be developed to meet customerspecifications for a 50% solution in water by (date)?
APHA color < 10pH 7.0-9.0
chloride content <1200 ppmcost < (price)
Others: metals, bromide, alkylhalide, etc. - refer to customer documentation.
Route currently under investigation for processdevelopment:
A + B + C --> X + Y
Other routes have been investigatedextensively (see monthly reports 1974-2002)
Can product from thecurrent lab process be
purified to meet thespecifications? IMPURITIES CONTAINING
Cl- (P, Q) WILL BEPRESENT IN ALL
SAMPLES of A
Path 2
CoV work showed that theamount of Cl- impuritiesdepends heavily on the
solvent used for storage.Variation in the range of10000-20000 ppm was
observed.
P, Q ARISE AS ACONSEQUENCE OF
EXTENDED STORAGE OFA IN SOLVENT. PURE A
SHOULD BE USEDRATHER THAN A THATHAS BEEN STORED INSOLVENT - THIS WILL
REDUCE THE MEAN ANDVARIATION IN IMPURITY
LEVELS.
Does the starting materialhave impurities?
MS IS “REPORTEDLY”VALID AND AGREES WITH
CUSTOMER MS, BUTSHOULD BE CHECKED.
Path 3
Initial MSE foundmeasurement error was
~500 ppm. This isunacceptable for this
application.
CoV study indicated asystematic effect related to
the stirring time, and thetime between sample
preparation and analysis.
Is the Cl- measurementsystem valid?
CoV study to determinethe levels of chloride indifferent lots of starting
material A
CoV study to determinethe variability in chloridelevels in different lots of
pure A.
Variability is less than thatof the MS (<12 ppm, 6
sigma)
Embed MSE in Cov study
ALL SAMPLES SHOULD BESTIRRED FOR AT LEAST
(TIME) AT (SETTING)BEFORE ANALYSIS.
Second MSE to evaluate theeffect of changes in
measurement procedure
Measurement error reducedto ~12 ppm (6 sigma) -
sufficient for thisapplication. N13.
Path 4
Can the standard variablesbe used to increase purity to
sufficient levels withoutfurther purification steps?
Path 5
Can Cl- be removedchemically by addition of
(reagent)?
Path 6
Can (person)’s method forchloride removal be
employed?
Consider optimizing:
mode of additionstoichiometry
stirringreaction temperaure
reaction timetype of solvent
amount of solventfiltration procedurerotavap procedure
others?
Could this route beimplemented at another
plant?
See path 4 detail
Current best conditionsproduce chloride levels of1100 ppm with variation of
~50 ppm (6 sigma) andsuccessfully meet color and
pH specifications.
STANDARD VARIABLESCAN BE OPTIMIZED TO
REDUCE CHLORIDECONTENT OF PRODUCTBEFORE PURIFICATION.
THIS METHOD HAS BEENDEMONSTRATED FOR Br-,AND MAY WORK FOR Cl-AS WELL. SHOULD NOTAFFECT pH OR COLOR.
Study factor effects usingsequential DOEs
Study this treament optionusing whole plot/split plot
DOE designs
This treatment had noeffect on chloride or pH
(DOE2), but removed colorto give final product thatbeat color specification.
Include this treatment instandard procedure from
now on.
Stir all samples for (time) at(setting) before analysis.
TREATMENT WITH(reagent) DOES NOTAFFECT CHLORIDE
CONTENT OR pH, BUTDOES REMOVE COLORED
IMPURITY.
THIS METHOD HAS BEENDEMONSTRATED FOR
RELATED CASES, BUT ISUNKNOWN WITH X AND A.
Study this treament optionusing whole plot/split plot DOE
designs
See path 6 detail
This treatment had no effect onchloride under a wide variety of
conditions.
STILL ROOM FORIMPROVEMENT IN THIS
AREA. (SEE PATH 4 DETAIL)
Best previous procedure typically saw <10000ppm chloride, but often as high as 50000 ppm
before purification. Had seen as low as 3000 ppmonce. APHA color ranged from 75-150 units. pH
was approximately 4.5.
53
54
55
56
57
Conclusions
• Thought maps are a viable alternative to DMAIC. There are probably others.
• The Cytec Six Sigma program may not look like Six Sigma programs at other companies, but it meets our needs, matches our culture, and achieves excellent results.
• It is necessary to both learn from others and innovate.
58
Guiding Thoughts
1. To make more money, we should learn more about our products and processes.
2. To learn, we should employ the scientific method (a.k.a. induction/deduction).
3. To employ the scientific method, we should select a tool set and methodology based on critical thinking.
59
Guiding Thoughts
TOOLS LEARNING PROFIT
60
Thank You
andrew.downard@cytec.com
top related