ML20128N173
| ML20128N173 | |
| Person / Time | |
|---|---|
| Site: | Millstone  |
| Issue date: | 03/08/1996 |
| From: | Crone L NORTHEAST NUCLEAR ENERGY CO. |
| To: | |
| Shared Package | |
| ML20128N126 | List: |
| References | |
| CP-801-2801-380, NUDOCS 9610160316 | |
| Download: ML20128N173 (56) | |
Text
{{#Wiki_filter:. _. __ --_ ___ - _- __ - . - - _ _ - . _ - - - _ - _- - ... -. . 4 l* MILLSTONE NUCLEAR POWER STATION CHEMISTRY PROCEDURE J I l Routine Operation and Calibration of the 4 Laboratory Ion Chromatography Systems CP 801/2801/3801Y l j j Rev. 3 j j V 4 Approval: /M ent - Millstone P Station fo e Sr. Vice Presic SORC Mtg. No: 'Ecou,d hym Date: 3- R -9 c, Effective Date: I- L94
- Level of Use Subject Matter Expert:
lnformation L Q one 9610160316 961004 PDR ADOCK 05000245 P PDR
i j i~ Millstone All Units j Chemistry Procedure
- Routine Operation and Calibration of thelaboratoryIon Chroniatography i Systsms i
TABLE OF CONTENTS ! 1. PURPOSE . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2 j 2. PREREQUI SITES . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2 l 3. PRECAUTI O N S . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4 [ 4. INSTRU CTI ONS . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5 i 4.1 Procedure Entry Position . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5 l 4.2 Start-Up Aution 300 Software . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5 i 4.3 Running a Sample - Aution 300 Software . . . . . . . . . . . . . . . . . . . . 7
- 4.4 - Calibration of IC - Aution 300 Sofmare . . . . . . . . . . . . . . . . . . . . . 8
{ 4.5 Analysis of Control Standard - Aution 300 Software . . . . . . . . . . 10 l 4.6 Manual Integration of Peaks - Aution 300 Software . . . . . . . . . . 11 ' i 4.7 Start-Up Process 450 Software . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12 . l 4.8 Running a Sample - Process 450 Software orbkcetk%Je 14 4.9 Calibration of IC - Process 450 Software er.hkei tr 15 4.10 Analysis of Control Standard - Process 450 Software e t-N216 M twv 4.11 Manual Integration of Peak - Process 450 Software .s. acc.18 *[ 4.12 2 Method Develpment . . ........
- 5. M&A70Ti8NOW. 9.7. 0.f. .$. . . . . . . . . . . . . . . . . 2
- 6. R EFERE N C ES . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23 7.
)
SUMMARY
OF CHANGES . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23 l ATTACHMENTS AND FORMS ! Chem Form 801/2801/3801Y-1," Millstone Chemistry 1.aboratory Method i, 1.og For Ion Chromatograph" l Chem Form 801/2801/3801Y-2," Method Development For Ion Chromatograph" i Chem Form 80.1/2801/3801Y-3," Millstone Chemistry Laboratory Ion j Chromatograph Control Standard I.cg" $ Chem Form 801/2801/3801Y-4," Millstone Chemistry Department Ion Chromatograph Raw Data Log" l Level of Use 6 6.. /tc. u.- i CP 801/2801/3801Y gnformat. ion
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- 1. PURPOSE 1.1 Objective !
. Provide instruction for routine operation of Dionex lon bhromatographs
~
meluding:
- Instrument start-up
- Analysis of samples
- Instrument calibration
- Data manipulation
- Method development 1.2 Discussion The general term " chromatography" means the separation of components from a complex mixture by a technique based on selective absorption. All chromatography methods employ a mobile phase and a stationary phase to separate the analyte (s) ofinterest. The basic principle behind " Ion Chromatography" is the specific rate of ion exchange that exists between the sample ion and the counter-ion (cluent or mobile phase) with the stationary phase (resin). This rate of ion exchange determines the time necessary for the sample ion to pass through the separator (analytical) resin column and be detected.
I' 1.3 Frequency 1.3.1 When in use Ion Chromatographs are calibrated weekly, or when a control standard indicates a prob!em with existing calibration. 1.3.2 When in use a control standard is run daily, f
- 2. PREREOUISITES 2.1 General 2.1.1 Power available (115 volts) to instrument.
2.1.2 Valve actuating gas at 80 - 120 psi delivery pressure. f i i A CP 801/2801/3801Y Level of Use r -m m
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2.2 Documents 2.2.1 Control Chart 2.2.2 When specified by Chemistry management, Instrument
~
Performance Trend Chart. l l 2.2.3 IC notebook 2.3 Tools and Consumables l 2.3.1 Reagents, standards, eluents, and regenerates have been prepared. 2.3.2 High purity water, Nanopure or Super Q. 2.4 DeGnitions ACI - Advanced Computer Interface CIM - Computer Interface Module IC - Ion Chromatograph NOTE The followin definitions relate to the operation of the Process 450 Software w h is windows based. DOUBLE CLICK - When using a computer mouse, this means to press the left button twice in rapid succession. This will open a computer file. SINGLE CLI.CK - When using a computer mouse, this means to press the left button once. This is used to select a computer file, menu, or command.
. SINGLE CLICK-RIGHT - When using a computer mouse, this means to press the:ight button once.
- HOLD CLICK - When using a computer mouse, this means to press and hold the left button and not to release it until the desired taskis accomplished.
j
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I DRAO - When using a computer mouse, this means to move a , computer generated image from oce position to another. i For example - HOLD CLICK anc' DRAG Process 450 icon to j bottom of CRTscreen. , l
- 3. PRECAUTIONS 1
t
- 3.1 Bottles containing cluent and regenerate should not be pressurized beyond 15 psi as the bottles may explode causing serious injury to laboratory personnel.
3.2 Samples containing elevated levels (greater than 1.0 ppm) of hydrazine, metals, or organics should not be analyzed as damage to the resin columns and suppressor system may occur. 3.3 Care should be taken when tightening plastic fittings as to avoid damaging plastic threads. A torque wrench should be used if a torque value is specified. 3.4 Spilled or leaked eluents and regenerates should be cleaned up as soon as possible to avoid damage to system components. 3.5 Except during initial startup, eluent pumps should not be operated without first setting minimum and maximum pressure settings as damage may occur to the pumps if these settings are not set. 3.6 Care should be taken when working around system plumbing to ensure that gas lines cannot become kinked, punctured or otherwise damaged. l l l l l l l l e 4 t - CP 801/2801/3801Y Level of Use Information 4y 4. N^w$new Rev. 3 ps% ? f"% 4 of 24
!. l I
. l
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- 4. INSTRUCT 10NS j '
NOTE 7 ,
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i;
'1. The methods that have been created for Ion Chromatogr analyses ;
l are listed on Chem Form 801/2801/3801Y-1,
- Millstone emistry l Laboratory Method to ForIon Chromato . " Method parameters areident in Chem Form 80 1/3801Y-2," Method l
4 Development For lon Chromatograph." Each method will have its own completed Method Development Form. This form should be ! reviewed if there are any questions regarding execution of the subject 1 method. New r ethods can be created following the guidance
- provided in Sec.
- on 4.12.
- 2. Names given in parenthesie in action steps are the software program j given names to compute .soction keys as displayed in the CRT. ;
- 4.1 Procedure Entry Position i ! ,
! 4.1.1 IE running IC m the operating software is Auto Ion 300, Go l
- To Section 4.2. I er Peukne ek3 ;
4.1.2 IE running IC M operating software is Process 450 for IBM #I l j compatible computers, Go To Section 4.7.
- 4.1.3 IE developing a method for IC, Go To Section 4.12.
I j 4.2 Start-Up Autolon 300 Software 4.2.1 Refer To Chem Form 801/2801/3801Y-2 and VERIFY the following is consistent with method to be run: l Eluent l 1 ! = ' Regenerant i l l
- Plumbing .
4 l
- Resin columns .
- Suppressor i
l Injection source: loop, or concentrator column i . i 4.2.2 ENSURE the following: 4 Level of Use 6 i ' CP 801/2801/3801Y i STOP THNK
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Rev. 3 REVIEW lnformation ; 1, f4 M -
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There is an adequate supply of regenerate and eluent to complete required analyses.
- Valve actuating gas is at desired delivery pressure.
l 4.2.3 IE IC has been turned off, PRESS power buttons to each , component as follows: NOTE is located on The "On" the back button of the CRT. for The the computer Aution will 300 automatically data station load t (computer)he operating software from the hard disk.
- a. Printer
- b. Chromatography Module
- c. Computer Interface Module ;
i
- d. Computer 4.2.4 VERIFY the following components are in " REMOTE" position: l
- Analytical Pump Module
- Conductivity Detector Module
- Chromatography Module 4.2.5 WHEN computer has finished booting up, PRESS "EhTER" :
to continue. 4.2.6 PRESS "K7." l 4.2.7 Using the keyboard, SET date. 4.2.8 PRESS " ENTER." ] 4.2.9 PRESS "K9." 4.2.10 Using the keyboard, SET time. 4.2.11 PRESS " ENTER." )
.( l / CP 801/2801/3801Y Level of Use Information W g W W^bes
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1 j- 4.2.12 WHEN date and time have been set, PRESS "K5"(CONTINUE)
- twice.
4.2.13 ENTER CIM address of 705. - 4.2.14 PRESS " ENTER." l 4.2.15 ENTER CIM default configuration file name. i 4.2.16 PRESS " ENTER." i
- 4.2.17 PRESS "K5" (CONTINUED) to display main menu.
l 4.2.18 PRESS "KO" (EXECUTE) to advance to auto-monitor page. s 4.3 Running a Sample-Antion 300 Software i , NOTE 1 4 Methods are run from the auto-monitor page displayed on the CRT. l Function keys are dis ed on the bottom of the screen. The first step of s runnmg a method is d the method into the CIM. After the CIM is 4 loaded, the method is initiated. Information defining method parameters such as system number and CIM address can be found on Chem Form 801/2801/3801Y-2," Method Development For Ion l Chromatograph" for method being run. Unit 3's software differs slightly from Unit l's as the exact number and order of computer prompts is not j identical. 1 i 4.3.1 PRESS "K2"(LOAD CIM). i 4.3.2 WHEN prompted, Refer To Chem Form 801/2801/3801Y-2 and i ENTER response as follows: PROMPT RESPONSE CIM address number? 705 or 706 j System 1 or 27 1 or 2 Use schedule? N Name of method file? Method name Sample name? Sample name Any additional prompts Default value j . 4.3.3 PLACE sample inlet tube in sample bottle.
; 4.3.4 PRESS "K7" (STAKT).
i Level of Use
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- lnformation g pg,ag .p .pq 4
- NOTE The analysis will automatically start and run through to completion after
. the system number has been entered into computer.
4.3.5 WHEN prompted, Refer To Chem Form 801/2801/3801Y-2, and
- ENTER response as follows
i PROMPT RESPONSE ! CIM address number? 705 or 706 ! System number? I or 2
- 4.3.6 WHEN sample analysis has finished, PERFORM the following
t
- a. REVIEW chromatogram for proper integration of peaks.
- b. IE any peaks are poorly integrated, Refer To Section 4.6, "ManualIntegration of Peaks."
i c. RECORD data and INITIAL j Chem Form 801/2801/3801Y-4. 1 i d. REMOVE sample inlet tube from sample bottle and PLACE in bottle containing DI water. 4.4 Calibration ofIC-Aution 300 Software 4.4.1 Before calibrating instrument, RUN at least one blank sample of Nanopure or Super Q water to insure that:
- Baseline is stable. !
- There is no contamination in system.
. No leaks in system.
. The sample intake pumps are properly primed and are delivering the expected sample volume. >
'4.4.2 VERIFY that auto-monitor page is displayed on CRT.
4.4.3 PRESS "K2"(LOAD CIM). Level of Use Information
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i i ! NOTE i i The calibration information is automatically updated when the sample name is entered as "AUTOCAL #." The "#"part of the name
- corresponds to the number of the standard as it relates to a multi-standard calibration curve. For example,if one standard was used to calibrate the instrument, the standard name would be "AUTOCAL."
If 2 standards were used to define the calibration curve, the names of the standards would be "AUTOCAL1," and "AUTOCAL2." If a third standard was used, its name would be "AUTOCAL3," and etc. 4.4.4 WHEN prompted, Refer To Chem Form 801/2801/3801Y-2, and ENTER response as follows: PROMPT RESPONSE CIM address number? 705 or 706 System 1 or 2? I or 2 Use schedule? N Name of method file? Method name Sample name? AUTOCAL # Any additional prompts Default 4.4.5 PLACE sample inlet tube in standard to be analyzed. 4.4.6 PRESS "K7" (START). 4.4.7 WHEN prompted, Refer To Chem Form 801/2801/3801Y-2, and ENTER response as follows: PROMPT RESPONSE CIM address number? 705 or 706 System number? I or 2 4.4.8 WHEN standard analysis is finished, PERFORM the following:
- a. COMPARE area or height of standard with previous standard run.
- b. IE difference exceeds plus or minus 5.0%, INVESTIGATE reason for difference.
- c. REVIEW chromatogram for proper integration of peaks.
- d. NOTIFY Chemistry supervision of any identified problems.
- e. IE no further analyses are to be performed on calibration standard, REMOVE sample inlet tube from standard bottle and place in storage bottle containing DI water.
f A4 d CP 801/2801/3801Y Level of Use ,Q Information p% gggp% yN,"OV n Rev. 3 9 of 24
. _ . - - - - - . _ - - - - _ - _ - . - - . . - .. _ .. - - - _ - - . . - . - . - . . _ = . - _ . -
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[' 4.5 Analysis of Control Standard - Autolon 300 Software I 4.5.1 VERIFY that auto-monitor page is displayed on CRT. 4.5.2 PRESS "K2"(LOAD CIM). 4.5.3 WHEN prompted, Refer To Chem Form 801/2801/j801Y-2, and ENTER response as follows: PROMPT RESPONSE CIM address number? 705 or 706
- System 1 or 2? I or 2 i
Use schedule? N Name of method file? Method name
- Sample name? CTRL Any additional prompts Default j 4.5.4 PLACE sample inlet tube in control standard to be analv
- :ed.
2 4.5.5 PRESS "K7" (START). } 4.5.6 WHEN prompted, Refer To Chem Form 801/2801/3801Y-2, and j ENTER response as follows: 'd PROMPT RESPONSE
- CIM address number? 705 or 706 i System number? I or 2 h 4.5.7 WHEN control standard analysis is finished, PERFORM the i following
i
- a. RECORD data and INITIAL Chem Form 801/2801/3801Y-3.
- b. Refer To control chart and PLOT result.
! c. E trend chart is available, Refer To trend chart and PLOT value.
- d. REVIEW chromatogram for proper integration.
- c. E control standard value is outside of acceptance criteria, INVESTIGATE problem and NOTIFY Chemistry
) . supervision. 2 1 1 Level of Use A g g g h; p le CP 801/2801/3801Y g g-iu$sV Rev. 3 Information FN M P% f%. 10 of 24
l l 1 1 ) I
- f. IE applicable, PROVIDE brief explanation of problem and
! follow-up actions on the following: I
- control chart
- Chem Form 801/2801/3801Y-3 4.6 ManualIntegration of feaks - Antolon 300 Software
- NOTE i'
The followin g instruction is for integrating the last sample to be analyzed
- by the IC. Tl21s is the only chromatogram that can be reprocessed if the
! data is not stored. The cursor is moved left or right by rotating the " wheel" i on the keyboard. The cursor is moved up and down by hitting the " shift" key, then rotating the rth-9. ! 4.6.1 VERIFY that auto-monitor page is displayed on CRT. j - 4.6.2 PRESS "K4"(REPROCESS DATA). i j ! 4.6.3 PRESS "K5" (REPLOT). 4.6.4 MOVE cursor to a position on chromatogram that is slightly
. below and in front of area of interest.
t
! 4.6.5 PRESS "KO"(ANCHOR).
1 ! 4.6.6 MOVE cursor to form box surrounding area ofinterest. 4.6.7 PRESS "K1" (ZOOM).
! 4.6.8 MOVE cursor to beginning of peak to be integrated.
4.6.9 PRESS "K7"(PEAK START). 4.6.10 MOVE cursor to end of peak to be integrated. 4.6.11 PRESS "K8"(PEAK AREA / HEIGHT). 4.6.12 PRESS "K6"(REPORT RESULT). 4.6.13 PRESS "K3"(HARDCOPY). 4.6.14 PRESS "K4"(REPROCESS DATA) Level of Use . gf ., g ft g[ - g,s CP 801/2801/3801Y g,, 3 Information p p:\ # ft 11 of 24
4.6.15 IE additional peaks are to be re-integrated, Go To step 4.6.3. 4.6.16 PRESS "KO"(AUTO-MONITOR). 4.7 Start-Up Process 450 Software ' 4.7.1 Refer To Chem Form 801/2801/3801Y-2 and VERIFY following is consistent with method to be run:
- Eluent
- Regenerant
- Plumbing
- Resin columns
- Suppressor
- Injection source, loop, or concentrator column 4.7.2 ENSURE the following:
There is an adequate supply of regenerate and eluent to : complete required analyses. e Valve actuating gas is at desired delivery pressure. NOTE i Dionex Series 450 will automatically boot up to the main menu upon
- power-up.
l 4.7.3 IE IC has been turned off, PRESS power buttons to each ! i component as follows: l
- a. Printer ,
I
- b. Chromatography Module
)
i
- c. Advanced Computer Interface Module j
- d. Compute 4
i . 4 f f f b CP 801/2801/3801Y Level of Use gg gg7 g '- , n V Rev. 3 Information g pg pq g.% 12 of 24
- 4.7.4 VERIFY the following components are in " REMOTE" position
=
l Analytical Pump Module
- Conductivity Detector Module I.
Chromatography Module - 4 , 4.7.5 LOCATE " Analyze" icon. l 4.7.6 DOUBLE CLICK " Analyze" icon to open program. 1 l 4.7.7 SINGLE CLICK" File" pull down menu. i
- 4.7.8 SINGLE CLICK " Monitor."
! NOTE i The "Run" icon and " Trend" icon will appear at the bottom left corner of
- the screen when a analyzer has been selected and approved.
- 4.7.9 SELECT analyzer to be opened and SINGLE CLICK.
l 4.'i.10 SINGLE CLICK "OK."
- 4.7.11 To select additional analyzers, Go To 4.7.7.
i 4.7.12 MOVE mouse arrow to down arrow located in top right corner of analyze window and SINGLE CLICK to reduce window to icon.
- 4.7.13 HOLD CLICK and DRAG " Process 450" main menu icon to I bottom of screen.
} 4 i i Level of Use j <. J i_ .*%"QQ}jii / CP 801/2801/3801Y , lnformation $[20P", . INK Rev. 3 l g %q j,. :x. pr% [^% 13 of 24 l
I l 1 4.8 Running a Sample - Process 450 Software oc %knd 58%mre. i NOTE - 4 Samples are analyzed using the "Run Program." This srogram can ' ! momtor multip j selected under (real the tune) Analyze ems simultaneously. '"he analpers ram willhave their own
- child system
' windows (cation and amon1 when the run icon is opened. The
.ystems are selected by clicking Ir title bar, which highlights the bar in l blue. When the ACI starts sampling for the system i running) a real time chromatogram as displayed e systeminwindow; th(i.e.,the a method is
- status of the system is shown at the bottom of the window.
i 4.8.1 PIACE sample inlet tube in sample to be analyzed. 4.8.2 IE "Run Window"is not displayed on CRT, DOUBLE CLICK "Run" icon to display window. 4.8.3 SINGLE CLICK system title bar " Anion" or " Cation" at top of
, system window to select system to be run.
4.8.4 SINGLE CLICK " Load" pull down menu located at top of "Run I Window." 4.8.5 SINGLE CLICK " Method" from pull down menu.
~
4.8.6 SELECT method to be run and SINGLE CL1CK. 4.8.7 IE correct method has been selected, SINGLE CLICK "OK." 4.8.8 SINGLE CLICK "Run" pull down menu located at top of run Window.
- i. .
4.8.9 SINGLE CLICK " Start" from pull down menu. NOTE For trending purposes, samples from the same system should always be named exactly the same. !
< 1 4.8.10 ENTER sample name inside sample box.
)
4.8.11 SINGLE CLICK "OK." , I Level of Use A I I$ f CP 801/2801/3801Y , Informat. ion
'NTOP P% 6
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9 l l l l 1 l 4.8.12 EHEN sample analysis has finished, PERFORM the following: ; j a. REVIEW chromatogram fot proper integration of peaks. )'
- b. IE any peaks are poorly integrated, Refer To Section 4.11,
" Manual Integration of Peak - Process 450 Software."
h i c. ededaet RECORD data and INITIAL 57Nart. I j Chem Form 801/2801/3801Y-4. i
- d. REMOVE sample inlet tube from sample bottle and PLACE i in bottle containing DI water.
i 4.9 Calibration ofIC - Process 450 Software em bbet-sadt wice C% w( l
- NOTE The calibration information is automatically updated when the sample ;
i name is entered as "AUTOCAL W." The "# part of the name ' j corres multi ponds to the number of the standard as it relates to a ! standard calibration curve. For example,if one standard was used
- to calibrate the instrument, the standard name would be "AUTOCAL." If 2 standards were used to define the calibration curve, the names of the {
i standards would be "AUTOCAL1," and "AUTOCAL2 " If a third standard ! was used,its name would be "AUTOCAL3," and etc. 1 L 4.9.1 Before calibrating instrument, RUN at least one blank sample of . j Nanopure or Super Q water to insure that: ! Baseline is stable. There is no contamination in system. No leaksin system. The sample pumps are properly primed and are delivering the expected sample vo, ume. 4.9.2 PLACE sample inlet tube in standard to be analyzed. 4.9.3 VERIFY that "Run Window," auto-monitor, for system to be calibrated is displayed on the CRT. 4.9.4 SINGLE CLICK syst m title bar " Anion" or " Cation" at top of system window to select syt tem to be run. t I g., g'g x ;.# 8y y N e w CP S01/2801/3801Y i Level of Use Rev. 3 Information p pg f:;( p.N 15 of 24
t-i
> - 4.9.5 SINGLE CLICK "Imad" pull down menu located at top of "Run j Window."
i l 4.9.6 SINGLE CUCK " Method" from pull down mend. l 4.9.7 SEECTmethod to be run and SINGLE CUCK. . { 4.9.8 SINGLE CUCK"OK." , 4.9.9 SINGLE CUCK "Run" pull down menu located at top of"Run j Window." 'i 4.9.10 SINGLE CUCK " Start" from pull down menu. j 4.9.11 ENTER standard name inside sample box. t
- 4.9.12 SINGLE CUCK "OK."
4.9.13 WHEN standard analysis has finished, PERFORM the following:
- a. COMPIRE area or height of standard with previous standard run.
- b. E difference exceeds plus or minus 5.0%, INVESTIGATE reason for difference,
- c. REVIEW chromatogram for proper integration of peaks.
- d. NOTIFY Chemistry supervision for any identified problems.
- e. E no further analyses are to be performed on calibration standard, REMOVE sample inlet tube from standard bottle and PLACE in storage bottle containing DI water.
4.10 Analysis of Control Standard - Process 450 Software o rblerd 15 4.10.1 PLACE sample inlet tube in control standard to be analyzed. 4.10.2 SINGLE CUCK system title bar " Anion" or " Cation" at top of system window to select system to be run. 4.10.3 SINGLE CUCK " load" pull down menu located at top of Run Windpw. 4.10.4 SINGLE CLICK " Method" from pull down menu.
! / '
CP 801/2801/3801Y Level of Use . 4, Nsv
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i i !' 4.10.5 SELECT method to be run and SINGLE CLICK. l ! 4.10.6 SINGLE CLICK "OK." 1 ... ! . _ 4.10.7 SINGLE CLICK "Run" pull down menu located at' top of"Run Window."
- i i 4.10.8 SINGLE CLICK " Start" from pull down menu.
4 NOTE f For trending purposes, samples from the same system should always be named exactly the r.ame. 1 4.10.9 ENTER control standard name inside sample box. 4.10.10 SINGLE CLICK "OK." I ' 4.10.11 WHEN control standard analysis is finished, PERFORM the following:
- a. RECORD data and INITIAL Chem Form 801/2801/3801Y-3.
- b. Refer To control chart and PLOT result.
- c. IE trend chart is available, Refer To trend chart and PLOT value.
- d. REVIEW chromatogram for proper integration.
i
- e. IE control standard value is outside of acceptance criteria, INVESTIGATE problem and NOTIFY Chemistry i supervision.
- f. PROVIDE brief explanation of problem and follow-up actions on the following:
i
. control chart
. Chem Form 801/2801/3801Y-3 I
- g. REMOVE sample inlet tube from calibration standard and place in bottle containing DI water. (
)
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V J i i 4.11 Manual Integration of Peak - Process 450 Software er P*Ane* kd%DtL E\ j , NOTE I t
' Chromatograms can be re-integrated from the Optimize Program. This pr ram can be used to fine tune the integration, assign peak names and to
-u ate method files and data files to include new parameters. This section d is with
- Set Baseline Manually" file of the Optunize Program,which only affects the chromatogram that is being worked on.
i J 4.11.1 DOUBLE CLICK "Procesr499" main menu icon. 4.11.2 DOUBLE CLICK
- Optimize" icon.
4.11.3 SINGLE CLICK " Ele" pull down menu. 1 4.11.4 SINGLE CLICK "Open Data File." l l 1 NOTE The list of file directories is located at the bottom left of window. 4.11.5 SELECT raw data file directory that contains chromatogram that is to be reprocessed. 4.11.6 SINGLE CLICK "OK." 4.11.7 SELECT data file name of chromatogram. 4.11.8 SINGLE CLICK "OK." 4.11.9 SINGLE CLICK " Operations" pull down menu. 4.11.10 SINGI.E CLICK" Set Baseline Manually." 4.11.11 SELECT peak to be re-integrated by one of the following methods:
. In box located in top left hand corner, SINGLE CLICK peak number that is to be edited.
- SINGLE CLICK-RIGHT peak on displayed chromatogram.
/
- _ % ,,,r/v A e CP 801/2801/3801Y Level of Use 'a . . -
symw-STOP D NK M CT Rev. 3 lnformation [% N /N /% 18 of 24
4.11.12 SINGLE CLICK " View" menu. 4.11.13 SINGLE CLICK " Start /Stop" markers option. l l 4.11.14 MOVE mouse cursor to a position that is slightly below and in front of area ofinterest. NOTE , The mouse cursor can be used to zoom in on the peak to be integrated. l This makes it very easy to see where a pak should begin and end. The scale tool box, located in the upper rig at hand corner of the baseline window, can also be used to enlarge and concentrate on the area of interest. The whole chromatogram can be moved by using the arrow keys
- (up, down, left and right) that mrder the chromatogram.
j ! 4.11.15 HOLD CLICK and MOVE cursor until area ofinterest is j contained in highlighted box. 4 I 4.11.16 RELEASE mouse button. i j 4.11.17 MOVE cursor along baseline of chromatogram in front of peak j until double arrow appears. 4.11.18 HOLD CLICK and MOVE cursor to position on chromatogram where peak should start. l 4.11.19 RELEASE mouse button. i ! 4.11.20 MOVE cursor along baseline of chromatogram in back of peak { until double arrow appears. I 4.11.21 HOLD CLICK and MOVE cursor to position on chromatogram where peak should end. . 4.11.22 RELEASE button. . 4.11.23 WHEN desired changes have been made, SINGLE CLICK " File" pull down menu. j '4.11.24 SINGLE CLICK " View Report." j 4.11.25 IE satisfied with report, SINGLE CLICK " Print." 4.11.26 SINGLE CLICK "OK." 1 Level of Use g_ g/:4 p
- r. N F %ew d CP 801/2801/3801Y Rev. 3 Information ,gg% PN k #% 19 of 24
i L f I. 4.11.27 SINGLE CLICK bar located in top left corner of baseline window. f 4.11.28 SINGE CLICK"Close." - 4 4.11.29 SINGE CLICK bar located in top left hand corner of l " optimise" window.
- 4.1130 SINGE CL1CK "Close."
t ! 4.1131 IEyou want to save desired changes, SINGLE CL1CK "Yes" 4.1132 IE you do not want to save chanses, SINGLE CLICK "No" to 1 l 4 leave data as is. l i i j 4.1133 IE "Yes" was selected, SINGLE CLICK "OK." - ! 4.11.34 SINGLE CLICK bar in upper left hand corner of"La 4.5^"
- window. {gk3g 4.1135 SINGLE CLICK " Minimize" to reduce window to icon.
' Cnemist. 4.12 Method Development Cnemistry Technician, or Cnemistry speciahst NOTE Chem Form 801/2801/3801Y-2 is the Method Development Form for the Ion Chromatograph. Completion of this form will document all the analytical parameters of the IC method being developed.
4.12.1 IE developing a method for Ion Chromatograph, COMPLETE Chem Form 801/2801/3801Y-2 as follows:
- a. RECORD following information in Section A:
Name of method I l Name of person (s) developing method i
+
Name of chemist that reviewed method Level of Use e i r CP 801/2801/3801Y Information s;g. Q-d %#h ~1dvinv Rev. 3 j.u. p.% W 20 of 24 1
.I
- b. RECORD following information in Section B:
Analytes to be detected Matrix of sample General description of analytical range .
- c. RECORD following information in Section C:
Instrument unit number
- System number ofIC,1 or 2 I CIM address >
1
- d. RECORD following information in Section D:
Description of separator column
- Description of guard column Concentrator column or sample loop
- e. RECORD description of suppressor system in Section E.
- f. IE desired, RECORD schematic of plumbing system in Section E j
- g. RECORD instruction on how to prepare cluent in Section G ;
including the following: l
- Typical flow rate Expected conductivity l 1
- b. RECORD instruction on how to prepare regenerate in {
Section H. l
- i. RECORD instruction on how to prepare standard in l Section I and COMPLETE calibration and control standard tables.
j i I Level of Use , ., /L, .J f M CP 801/2801/3801Y , Information EP ?NK ' '9 p " ?ENIE / Rev. 3 7% #1# FN /Ns. 21 of 24
- l
' I l i .
- j. RECORD following calibration data in Section J:
- Analytical range of method.
l
- Number of calibration standards used t$ define calibration curve.
l
- Type of curve fit.
- Ilmit of detection and limit of quantification.
4.12.2 ATTACH following to completed
- - Chem Form 801/2801/3801Y-2
- Computer hardcopy ofIC method.
l
- Calibration data,which includes graph and chromatograms.
- Examples of typical sample chromatograms.
4.12.3 IE not a chemist, SEND completed form to chemist for review. I cnemist l 4.12.4 REVIEW method, especially preparation of standards and reagents. 4.12.5 PLACE signature on method development form indicating approval of method. 4.12.6 RETURN form to method developer. I 1 chemist, 4.12.7 COPY method development form and attachments. ! Chemistry CN*ry
- 4.12.8 PLACE original in IC notebook and SEND copy to Analytical specialist Chemist.
4.12.9 RECORD method data on Chem Form 801/2801/3801Y-1. in r t- CP 801/2801/3801Y Level Of Use N& Mr Nicf ' hew Rev. 3 lnformStlOn jpg jg;g. gpq pg 22 of 24
- ' 4.13 Start-Up Process Peaknet Software
! 4.13.1 ENSURE there is an adequate supply of regenerate and eluent to j complete required analysis. - 1 NOTE j Dionex Series Peaknet will automaticaDy boot up to the main menu upon 4 power-up, i ! 4.13.2 IE IC has been turned off, PRESS power button to each j component as follows:
- a. Printer i
- b. Chromatography module I
- c. Conductivity detector
- d. Computer h >
#\
- e. Gradient pump module 4.13.3 Using mouse, LOCATE and DOUBLE CLICK on "Dionex Peaknet" icon.
4.13.4 Using mouse, LOCATE and DOUBLE CLICK on " Main Menu" icon. 1 1 l 1 Level of Use Information g- r[4- t T- Tum[sE' CP 801/2801/3801Y Rev.3
#4 % % P% 22: of 24
. . . _ _ _ . _ _ . . ~_ . _ _ _ _ . _ _. _ _ _. _ _ _ _ _ _ _ _ _ . . _
i i l l I
- 5. REVIEW AND SIGNOFF l 5.1 The review and signoff for this procedure is located on the following l Chemistry forms: -
1 i Chem Form 801/2801/3801Y-1 i i
- Chem Form 801/28013801Y-2 Chem Form 801/2801/3801Y-3 ;
Chem Form 801/2801/3801Y-4
- 6. REFERENCES I 6.1 Dionex Aution 300 Data Station Operator's Manual, Dionex Corporation, l Sunny Vale, CA i 6.2 AI-450 Chromatography Software User's Guide , Dionex Corporation, I Sunny Vale, CA G,3 464+ CMrenleynpy Shute. Llw/5 Guide; keg .
- 7.
SUMMARY
OF CHANGES het corp. 3 Su ey %le , C A , l 7.1 Change calibration frequency from daily to weekly, step 1.3.1. , 7.2 Added instruction concerning the following: l How to manually integrate a peak on a chromatogram, Section 4.6. How to operate " Process 450 Software"in the following Sections:
- 4.7 \. ,
- 4.8
- 4.9
- 4.10
- 4.11 -
How to complete Chem Form 801/2801/3801Y-2," Method Development For Ion Chromatograph," Section 4.12 l t ... A - CP 601/2801/3801Y l Level of Use s. m < . , ,e . x . lnformation Y_' "" r% p% yy f?%, 13og24 4
I 7.3 The content of this procedure was modified to incorporate new format criteria specified in Revision 0 of the " Millstone Procedure Writer's Guide." l l l l l I l l I 1 i CP 801/2801/3801Y Level of Use i lnformation ._A[ HE~ M 7)) i Rev. 3
,?,q pg pg peg u ,, ,
1 A A
/ /-8-9Y 93-3W j Form Approved by !
sr. vce President [ Millstone station Effective Date SORC Mtg. No.
- Millstone Chemistrv Ymboratory i
Method Img For Ion Chromatorranh I j METHOD NAME ANALYTES RANGE BY i i i i i i i i l i
.s., -
I - l i i
- Chem Form 801/2801/3801Y-1 i Rev.1 l Page1 of1
- . . _ . - - - . = .. . . - . . _ - . - . . - - . - . . - . . . . , . . . . . - . - _ . - . . . _ . .
. 0 /)
C l' 8 ' W VS*6Y ! Form Approved'by Sr. Mce Pr'esident - $11 stone Station Effective Date SORC Mtg. No. Method Develonment For Ion Chromatorranh I A. Method Name-t j l ! Developed By: / l (Pnnt) (Signature) j Reviewed By: / j (Print) (Signature) l B. Objective of Method-i i t C. Instrument Identification-(Unit, System, CIM) D. Columu Separator: Guard: Concentrator: E. Suppressor: Chein Form 801/2801/3801Y-2 Rev. I 1 Page 1 of 5
J E Plumbine Descriotion/ Schematic-
~
. (Ontional) M i t J I i i 4 ) i l Chem Form 801/2801/3801Y-2 ! Rev.1 Page 2 of 5
4 G. Einent l Preparation: i
. ~
l l l l 1 l l l Bow Rate: ! Conductivity: H. Renenerate: l Preparation: ; 1 How Rate: Chem Form 801/2801/3801Y-2 Rev.1 Page 3 of 5
i 9 I. Standards: i Calibration Standards ! 4 1 Chemical Specie Concentration 1 Concentration 2* Concentration 3* l 1)- - l I 2)
- 3) l
- 4) i 5)
- 6) j 1
I
- Optional I l
i Control Standards ! j Chemical Specie Concentration 1 Concentration 2* Concentration 3* 1)
- 2) {
1 3)
- 4) ,
- 5) I
- 6) )
l
' Acceptable deviation should E letermined by statistical analysis.
Preparation: l I i 4 Chem Form 801/2801/3801Y-2 Rev.1 Page 4 of 5 2
I l J. Calibration Data' )
- 1. Range of Method:
- 2. Number of Standards Used:
- 3. Type of Curve Fit:
- 4. LOD:
- 5. LOQ:
Chem Form 801/2801/3801Y-2 Rev.1 ; Page 3 of 5
)
l
a,_A_,__4.___ - _au_. a >.-an, gad _iA.1-ma E_mm.-a.-S a- 4..s .4 ..m.*amae*.h a u. u a.%%.t4m_mme m#m _..6a._.,_m_a..w_--- -_m..m ._ *,w -w. - --a w- -,. - __.,__a- - , , , I l 1 * \- \ 7 i t { \ 4 - . i%
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Fonn Approved by 8. Vee Presidentf/Mi nstone Station EWettve Das hg. No. t . LaboraL% t j Millstone Chemistn Denartment lIN Ion Chromatorraph Raw Data f mg ' RANGiE. ~
~
i Daternme Sample I.D. Coi> Eel lon Concentration 'E rW6als Number PPB) Area or _. j Mhpht - g a -- 1 .. _ i 1 - i ,, j _
- j _
.. ~
i . 1 8 1
- Chem Form 801/2801/3EbWm4Fon- 31-Rev.1 Rev. 3 Page1of1 Page.1 of1 m- - - - . w=-- ,- =m - __ - -
i . , O A a.~ C I Y /* 8'VY $5-64/ l Form Approveriby Sr. % ice Pr'esident - $listone Station 'ffective Date SORC Mtg. No. I { Method Develonment ForIon Chromatorranh l A. Method Name: AEoM / k' b Developed By: A EEWL,2_ /d.4cdc /_ /' { (Print) \. (Signature) Reviewed By: hb / /M M j (Signature) ' / G(Print) i l 1 B. Obiective of Method: AJ+c.N6r1 af L.ow uvec seas u A,J h Nw 4 C R t._ (Tot fet & L tcd04L/
- wd6 al G k n9LL[ IA_% i n G
- , SA m f (L j doic eMdt J n CLA d aA f 50 C Nks C.
t w A. i i C. Instrument Identification: (44 : T'~ 2 ,4-c-T I b VS / !
- (Unit, System, CIM)
D. Columns: Separator: AS / 2-l Guard: C6 /t l ' Concentrator: A6 l'L l l
- E. Suppressor
- Owno/ ata l
1 i j l Chem Form 801/2801/3801Y-2 Rev.1 , Page 1 of 5 l
1 1 . i 1 - I i i - l 1. Standards-1 Calibration Standards Chemical Specie Concentration 1 Concentration 2* Concentration 3* $ 1) Gob w . Tab TO ,, b / D. o srb
- 2) t. rua,4ot. A ua @0 esb 2fbo Y/ b 900 py 6 3) l l 4) l 5) j 6)
- 1'
- Optional I
Control Standards I Chemical Specie Concentration 1 Concentration 2* Concentration 3*
- 1) 5obiu 2.0eeb
, 2) q 7 ,44,s.c 9 ,u. 2, o 'j % ! 3)
- 4)
{ 5) j 6) t - i
=
- Acceptable deviationghould be determined by statistical analysis.
Preparation: sobu- Ah EN- M Acu#f A rd " " L Zk77o 4 e; esTbce am Mws ee cww' < n 2 *o+1 .4 1 . A+ aad loo al u f * *
- ap ,
L'T'* %t k Tu tw A t Chem Form 801/2801/3801Y-2 Rev.1 Page 4 of 5
1 i
.l
^ t
- F. Plumbing Description / Schematic-(Ontional) . , pg j
g EI *** . p+ O O k . Ii m L*lran" l l i vwt 3, 1 ' 1
/}
w
~
etM Sr _ 1 ( J -- L ;gt ~ p~ (& 4
'cc IL
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If i c5 (L i wf el - useatwT *" j f**t* fa nsit.c.ah t u_. 9 C s it. 5 i- \ i n testat w r , pg pyo ed II s E /4t_/C
'/ i Er i
J J Chem Form 801/2801/3801Y-2 Rev.1
- Page 2 of 5
) , i !o , G. Eluent
- Preparation
- Iru Af AsA c,mrc (, o J ..f r,o j 4
_M s,
- vu 4O.L+a ..w >z x.+u-i i
1 i 1 i i a T i l Flow Rate: /. o l./~ m i l Conductivity: l 0W H. Regenerate:
- Preparation
- . d M o d 5 4,1 t/0 t tac. t so- a; 2 i
lA t s nc
/
br wmt for- /tg,edt w r i 1 l 1 . i ( . 4 i d . 1 Flow Rate: //+ 1 l l 1 ? I )
- Chem Form 801/2801/3801Y-2 1 Rev.1 Page 3 of 5
i J. Calibration Data:
- 1. Range of Method: .Ippb - lopff cm St g g - [),.
- 2. Number of Standards Used: 3 ( z.ceo Ar- uc+L 8) l
] 3. Type of Curve Fit: Qu A44-n c_ l l 011 l
- 4. LOD: A .*'r# (* 4 so vb j 1
- 5. LOQ: Me- - oS'ffb crs pgge 4
J 4 i i T Chem Form 801/2801/3801Y-2 Rev.1 Page 5 of 5 1
- . - - . _ - ..- --...~... - _ _.-. - .. .- . . - . - - . - . . . - - . . _ . - . - . . . . . . - , ,4,, O A l-l' 3'VY TE-6Y j ', Form Approved'by Sr. Oce Pr'esident - $11 stone Station Effectrve Date SORC Mtd. No.
I i Method Development ForIon Chromatorraph l A. Method Nang f74-WC 7 - ! Developed By: &cEsEd. /diedr /K / j (Print) N (Signature) '/ -
- Reviewed By: DN-
/ /M6 (Signaturt)
~
f (Print) B. Objective of Method: A f dAt.Ys t s os- //sM wu. 1;w w w ,Je : ks/de Leo to s M rc77aeJ M1 & J SeGL A M 7c. Aud i i C. Instrument Identification: tv,r 2 #c / c%s / (Unit, System, CIM) I D. Columns: Separator: _f.s / 2 Guard: # d6 /2-
~
Concentrator: M4
- E. Suppressor: /M/od 54_s i
l l Chem Form 801/2801/3801Y-2 Rev.1 Page 1 of 5
\
E Plumbing Description /Schematie- - l (Ontionan
#0 1 3
11-0 O
't i LAfMC'T 1 f' $ ( -gz. g, V&t. Jf- '
M ls l l
"# Sr - )
( CGIL [h_ c
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ch
%f ti < $ ,ys t4wT *6 l f**f pasTL r- c A u.u- l 7 0.S it. 5 F H
W f'*# ;
,, Ar d,,o
^ '
m E /4t/C
, '/ii ar 2" Chem Form 801/2801/3801Y-2 Rev.1 v a ') nr <
D G. Eluent I Preparation: IG~u Ai AA Da wrc (, o d d I.o A Ms. h tu Y O A+rr ,n .W )z w. -i e_r-l 4 i Flow Rate: /. o .*f/~ m Conductivity: 10 W H. Renenerate:
~
Preparation: # #flod 5 #_1 t/otTM-c.t Sts- =i Z. (A r i n c br wmc for- /t Gurwr
/
1 l l
' Flow Rate: //+
1 Chem Form 801/2801/3801Y-2 Rev.1 Page 3 of 5
- MomE
- AM*4 A obeo
! la-t-95 l A/ok: nym rW l "WWed en f/h/9*/ sm I
- 1. Standards- y, j f
) Calibration Standards I Chemical Specie Concentration 1 Concentration 2* Concentration 3* { i 1) ETA . T/ r" 2. S~ n~ /d mM 1
- 2) 4 mmtsam O O S" De w Osl Den O.1 DDA 3) 4)
5) , 6) 1
' Optional Control Standards Chemical Specie Concentration 1 Concentration 2* Concentration 3*
l 1) tru /. o M*~ l l 2) 4_ o,, e,e,y ,,,s
' l l 3) l 1
' 4) 5)
- 6) l
- Acceptable deviation should be determined by statistical analysis.
Preparation: 7e.o~ /oo o y- er r u s.ca n=4/ 6, uv r As Au.ws 7s /oo As a,K A r w+rt t-t+oerr- per p S #0h int 37Ec k. enn- sit NH t th e_ d% s ID ra A .s~n s fool coo h J. f~ Ar^ 1o00 , eoc ppk 7eou , s l'O f" goso A s es pph
/. e al to y qso ) mgp h Chem Form 801/2801/3801Y-2 Rev.1 Page 4 of 5
J. emlibration Dag 4 7, .
- 1. Range of Method: 0IA o- . M.^r % r/3N/ N'
- 2. Number of Standards Used: J i 2m eo'd b'-
- 3. *Pype of Curve Fit: G u.% 4.+ 5 i c_
- 4. LOD: u.A m m,m i
- 5. LOQ: -~ am u.s u l
1 l l 1 ( 1 e d Chem Form 801/2801/3801Y-2 Rev.1 Page 5 of 5
! i
-- t ,
i
. - 4
- 5 3
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=
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l l Nh' lh2/f/
~
Form Approved by Sr. Nice President - $11 stone Station
/ 3-W Effective Date
%-S%I SORC Mtd. No.
Method Development ForIon Chromatograph A. Method Name: /1 Me o tJ f Developed By: to diedE / h_f>
/ (Signature) '
(Print) -- Reviewed By: bb b [d - / 3I[ M (Print) (Signat r B. Objective of Method: 4 at<_ysis o f uo au~l<.cf m Ah .. & H,a k i osN F1, HJ luLl m'h' M , n , a n i e r~ So S 16 we.+ /~vag LonA.4ie c , YkJ s is R l oo 7 , ;e,-t ,0 ,sc,c m-{,e uto a . C. Instrument identification: na ri z e> # oo os_im c d45 2 sys h - i (Unit, System, CIM) D. Columns: Separator: 65 Io Guard: N/A Concentrator: dl* L-oo p , ancnod E. Suppressor: dwe s 2r Chem Form 801/2801/3801Y-2 Rev.1 l Dnen 1 et C
J G. Eluent Preparation: 3G d Hel /.Ifm M b A? l 2. o as do ne.e&da 6Lih H d I awd i4 emi i F tu.k' 'b A > 4u 4 1. h br wcrt .2. Flow Rate: /o Conductivity: I 2- m H. Regenerate: Preparation: 100 m A Ta A. n 4 fo J m es,& w-&c.d i a .4.e 4 d . ImM 4e i L % ,- br h Semc w.4L ej.h een ik% ms
/
# r"'s o r'- b 4 C.- C4M N 001 EEG f eJOfAd T
? L A. C t. Ma RLGtdct.M T ,J down+-s dt 2 i M b7+LL- >Jt>J As 7~7 o eJ AW t' F*L.o e ~3 o Wo A Yo 'Tb f. fA s/rdi c.'7~ C L k1t/ L / k{. ?O [O10 0 9" A M T~ltb A r. S 4G t. Shu A1 k L GtA tr2 d 7Nt n dra cu.n o h a t. dc m.ic FM W Lidt kh dodnte r 7b MA .LT sdLL 7 f.s Ht l
l Flow Rate: //+ Chem Form 801/2801/3801Y-2 Rev.1 Paoeinf4
I E Plumbing Description / Schematic: (Ootionan 3444 HLI ! GPA 1 fI , gj g C a 1i O LokhlIa.TccT 2. / '~ q ( L 2.. N/A-V4-uK ~ ,/ M3 smT.g i} r ' c, '. ~ 1', 7
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- 65 'o swe ie l fwf \
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- unos t l
C - ro[ l Ha% j v ktL)tf :4 t b l5 C- ggggg g 7 f"P l I 1 i I Chem Form 801/2801/3801Y-2 R ev 1
. . -.- .. _ . . = . _ . - . . -.- . - .-. . . . . _ . - - . - . - . . . - - - - -
4 4 i j I. Standards-Calibration Strndards l Chemical Specie Concentration 1 Concentration 2* Concentration 3*
- 1) es,m . or o e,- . o so ppn .juu pp n
- 2) w,+ .io. e, - . s a e,- i. o pp~ j l 3) e7y u t, ,,sc f, , g_ 3. o g. 3;o y . ;
)
- 4) dibiu ziac rs~~ o p ~ / u~ n ~ > So px 5)
! 6)
- Optional
].
- Control Standards 1
! Chemical Specie Concentration 1 Concentration 2* Concentration 3* i i I) So b /ww . 02.o p w [ 2) h , , u a zoo pp - } 3) 17pg , ,g, s c 2,o ,p ~ 4)pyy ,,, ,,, ,,_ l 5) 4 i 6) l ' Acceptable deviation should be determined by statistical analysis. j Preparation: NA z<se es recrx<J how ard u vat 2 < escor<<>t i
- Mr- o rutt soce.1cs u t perm a mas a i
- 1 o txr7oa o r 6 deea ru-Tzh .3% so wns e i
4 h i 1 i _ _ . i ' 1 l I ) i i Chem Form 801/2801/3801Y-2 j Rev.1 t Page 4 of 5 _
1 i t 1 J. Calibration Data: [ 1. Range of Method: s e c_ acto a i
- 2. Number of Standards Used: 3 Cuzo u srch 53 i>'g+d
- 3. Type of Curve Fit: Quet wic.
- 4. LOD: sacouru rr 4
1 j 5. LOQ: , s e. % p a rr-l I i i2 M 6 LS l NO l g- s oo(( b l l N%* z o (fb
- I ff m l Erw Ico((b - S~pf-~
? j tJtdy sy~ - I 9f p+ i N i l 1 l .i l i 4 l Chem Form 801/2801/3801Y-2 Rev.1 Page 5 of 5 l l 1
~
-Method Updated: 14:17 on Thu c 09 Jun 1994 j Component: Sodium Fit Type: Quadratic r' = 0.999991 Amt = ( 3.158047e-015
- Resp * )+
( 7.460499e-008
- Resp )+ -0.0001 i Standardization: External I Calibration: Height
/
/
/
m.! 1.25e+006 -
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/
/
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/
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Method: C:\DXNMETHODNCATIONS. MET Component: Ammonium Fit Type: Quadratic r 8 = 0.998920 Amt = ( 8.449920e-014
- Resp 2 )+ l
( -2.671342e-008
- Resp )+ 0.0062 i Standardization: External Calibration: Height I i
I
, ./
-, /
- 3. 5e+006 -- /
/
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/
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/
m, 2.5e+006 - t e . S l n 2e+006 -
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/
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. . I 1
I l-i Mathod: C:\DX\ METHOD \ CATIONS. MET l Component: Ethanolamine l Fit Type: Quadratic r' = 0.999725 Amt = ( 4.434428e-014
- Resp * )+
( 2.990569e-007
- Resp )+ 0.0164 Standardization: External I Calibration: Height 1
l 8e+006 -
-_ / ,
/
7e+006 - , i l , f"
/
l Ge+006 - l _ l ! t I
/
( l Se+006 -
/
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l l ======.===================================================================== 1 Sample Name: CONTROL Date: 06/09/1994 14:23:62 ; i Data File : C:\DX\ DATA \ CATIONS \ DATA 0061.D01 l Method- : C:NDX\ METHOD \ CATIONS. MET l l ACI Address: 2 System: 1 Inject #: 1 Detector:CDM-2 l Analyst : Column: l
================================================================
dalibration = Volume Dilution Points Rate Start Stop Area Reject
.ternal 1 1 3529 SHz 0.00 11.76. 10 ********************* Component Report: All Components ******************+****
Pk. Ret Component Concentration Height Area Bl. % Delta Num Time Name Code , .. - - - - _ - . _ - _ - - - - - _ - - - - - A b_'L - _!- _ - _ - _ - _ p_---_-__--_-_-_ pm ___--_--_------_-_--- 1 3.48 Sodium .ozo 0.020 262402 2327176 1 0.00 2 4.62 Ammonium 2.*
- 0.268 1889880 19885931 2 0.00
- 3. 5.13 Ethanolamine 2* 1.920 3996034 47926058 2 -4.69 4 6.03 Hydrazine /** 109.080 4858884 393765727 2 0.00 Totals 111.276 11007200 463904892 -
F//e: DA 7~ A OO61.001 Samp/e: CON 7ROL 9.0 , l y 8.0 7.0 C.O HyWhvne 5.0 l ahan.Namine l , < 4.0. uS 3.0 m.g,., gng , 2.0 i 1.0
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- te rr.a 1 ', 1 3760 SH 0.00 12.60 10
.....e,4+,,.,,,++,,. . Component. Report: All Components +++++'+'****++ ********
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