ML20080E079
| ML20080E079 | |
| Person / Time | |
|---|---|
| Site: | Grand Gulf  |
| Issue date: | 08/25/1983 |
| From: | MISSISSIPPI POWER & LIGHT CO. |
| To: | |
| Shared Package | |
| ML20080E069 | List:
|
| References | |
| TASK-2.B.3, TASK-TM 08-S-04-133, 8-S-4-133, TAC-60187, NUDOCS 8308300715 | |
| Download: ML20080E079 (40) | |
Text
. - _ _ _ _ _
/ '
=
PLANT OPERATIONS MANUAL s
4 ,
Volume 08 08-S-04-133 Ssetion 04 Revision 0 Date:
CHEMISTRY INSTRUCTION OPERATION OF THE CAS CHROMATOGRAPF AND CONSOLE SAFETY RELATED Prepared: ~Mo __/
m_
((h 4 (b , ]p ,
Reviewed: /
Technical Independent Review Plant Chemist ,
l List of Effective Pages:
Prge 1-30 Actscheent I Attachtsent II List of TCN's Incorporated: .
Rcvision TCN No.
O None 88;?*188Foi888fg E
. . GRAND GULF NUCLEAR STATION CHEMISTRY INSTRUCTION
Title:
Oparation of ths Gas No.: 08-S-04-133 R3 vision: O Pags: 1
. , Chromatograph end Censole 1.0 PURPOSE i
The purpose of this instruction is to provide directions for operating the Perkin-Elmer Sigma 3B Gas Chromatograph and the Perkin-Elmer Sigma 15 Console.
2.0 REFERENCES
2.1 Perkin-Elmer Corporation; Instructions:
2.1.1 Sigma 3B Gas Chromatograph 2.1.2 Sigma Series Console 2.2 Practical Gas Chron'aloEraphy-for. the Users of Perkin-Elmer Gas Chromatographs; Perkin-Elmer 990-9389; 1973 3.0 DEFINITIONS j 3.1 Sigma 3B Gas Chromatograph - The Sigma 3B is a versatile, single or dual column, temperature programmable gas chromatograph equipped with an 1/8 inch stainless steel 5 Molar Sieve Column, 6 feet in length, and a Hot Wire Thermal Conductivity Detector (HWD) which compares the thermal conductivity of the components in an injected gas sample with the thermal conductivity of the carrier gas flowing continuously, through a reference cell.
3.2 Sigma 15 Console - The console is a versatile laboratory data system that functions as a data processor, a teletypewriter terminal, and a printer / plotter. The console features Read Only Memory (ROM) with a capacity of 15K two-byte (16 bit) words and Random Access Memory (RAM) with a capacity of 4K words. The system provides the means by which an operator can, by utilizing keyboard directives and conversation, operate the console to collect and reduce data from the chromatograph, print out analysis data reports, establish analyzer chromatographic conditions, initiate operation of auxiliary devices at the times required, and build and store methods and files for later use.
3.3 Default Method - Used to establish a data link between the chromatograph and the console, to adjust the baseline, to run unknown gases to determine peak elution times and areas, and to calculate area and base sensitivities for use in an analysis method.
3.4 Quantitative Analysis Methods - There are three different quantitative ,
analysis methods. These are:
l l
= ..
GRAND GULF NUCLEAR STATION CHEMISTRY INSTRUCTIOd
, i
. Titlo: Oparction of tha Gee Ns.: 08-S-04-133 Rsvision: O Paga: 2
, Chrom tegraph cnd Console 3.4.1 Normalization Analysis - In this method, the system automatically applies a factor of 100 so that the concentrations are expressed as percent. This method suffers from the disadvantage that the reported concentration of any one component depends upon the concentration of every other peak in the file, so that any change affecting the total peak area such as noise, baseline upset, or other factors can affect the concentration for a particular peak.
Directions for generating a normalization method are given by defaulting (0) the standard weight on the STD WT, SMP WT line.
3.4.2 Internal Standard Analysis - The analysis method presented fully in this instruction, is the preferred analysis method. Only two components affect the reported concentration of any component of interest, the internal standard component itself, and the internal standard component added (or present) in the sample. Directions o for generating an area normalization analysis method with an internal standard are given by omitting standard weight and l providing the standard name at the STD line, using the exact spelling as used in the component list for that standard.
3.4.3 External Standard (Corrected Area) Analysis - This method can be used when an internal standard cannot be added or is not present in a sample. This method is extremely susceptible to variations in the quantity of gas injected, since peak area is related directly to concentration in this technique. However, the concentration reported for a given peak is not related to the concentration of any other peak. Directions for generating an external standard analysis method are given by entering i for STD WT and defaulting (r.o name entred) STD NAME.
S Reference the three analysis methods above. When the standard weight is not entered (i.e. , 0), a Normalization Analysia will te performed, regardless of the entry for the standard name. If the standard weight is some value other than 0, the entry or omission ;
of the standard name determines whether an Internal (standard name entered) Standard Method or an External (standard name defaulted)
Standard Method will be generated.
, GRAND GULF NUCLEAR STATION CHEMISTRY INSTRUCTION v 8 Titto: Op3ratien of tha G o No.: 08-S-04-133 Rsvision: O Pega: 3
- , Chromatograph and Console 3.5 Method Characteristics - Each method has three sections and each section is divided into two portions. The sections and portions are as follows:
l 3.5.1 Analyzer Control Section
- a. Fixed Portion (INJ TEMP through INIT OVEN TEMP, TIME)
- b. Variable Portion (TENP RATE TIME) not applicable to this procedure 3.5.2 Data Processing Section
- b. Variable Portion (RT, RF, CONC, NAME) l 3.5.3 Even[ControlSection l
- a. Fixed Portion (ATTN - CHART - DELAY)
- b. Variable Portion (TIME DEVICE FUNCTION NAME)
The values entered or defaulted into the fixed portions remain constant, except where the Variabla Portion of the Event Control Section can change I the ATTN value and the CHART speed. The variable portion allows input or I variables which direct the system to act upon certain data at, or during specific times, and to use the values, especially the RT, RF, CONC, NAME '
of the standard, for calculating Response Factors and percents of gas molecules present in an injected gas.
3.6 Operator - The use of the term, operator, implies authorized and qualified chemists, chemistry technicians, I and C technicians or other .
authorized personnel qualified to operate or perform maintenance on the instruments.
- 4.0 PREREOUISITES 4.1 Assure that calibration due dates have not been exceeded.
4.2 Replace the sample injection septum when the GC is used daily, or when the integrity of the septum is doubtful.
4.3 Assure that the carrier gas supply is adequate and that carrier gas has
- been purging for 10 to 15 minutes before applying power to the l filaments.
4.4 Apparatus Required 4.4.1 Sample Injection Port septums l
GRAND GULF NUCLEAR STATION CEMISTRY INSTRUCTION t
I
Title:
Op3rctica of th3 Geo Ns.: 08-S-04-133 R2 vision: O Pcgo: 4
. Chromatograph and Console :
4.4.2 Gas tight (hypodermic) syringes with needles 4.4.3 Gas vials with rubber septums 4.4.4 Printer / Plotter paper 4.5 Reagents Required Various gas standards with varying concentration as required, including atmospheric air
- 4.6 Attachments 4.6.1 Attachment I - Summary of OperatinF Conversations and Directives (seven pages) 4.6.2 Attachment II - System Directives (three pages) 5.0 PRECAUTIONS Observe plant safety guidelines.
NOTE If the gas chromatograph and console are operating, and if acceptable, calibrated methods are programmed for a desired analysis, determine the desired method number according to Section 6.9, if necessary, then proceed to Section 6.11 to perform the analysis; or proceed as necessary, to any desired section or step.
6.1 SIGMA 3B Gas Chromatograph Start-up 6.1.1 Assure that the carrier gas supply is sufficient for performing the analyses.
6.1.2 Set the cylinder carrier gas supply regulator to 300 kpa.
I 6.1.3 On the top left control panel for the SIGMA 3B Gas Analyzer, set l' the carrier gas Flow Controller knobs for Channels A and B to exactly 30 cc/ minute for both channels.
6.1.4 Allow the analyzer to purge for 10-15 minutes to prevent oxidation on the heating filaments. ..
6.1.5 Lift the hinged keyboard panel cover and do the following:
Titlo Oparcticn of tha Goo Na.: 08-S-04-133 Rsvisicn: O Pega: 5 Chrom tegrcph rnd Consolo
- a. Set the Oven Protect Switch (top left of keyboard) to 250.
- b. Set the Filament Control knob (top right of keyboard) as follows:
(1) N 2 Ar (65 mA)O if N2 /Ar carrier gas is used (2) Low (150 mA) if He carrier gas is used (Medium, 240 mA or High, 300 mA may be used when necessary)
NOTE Block temperatures should not exceed 450*C at the N2 /Ar setting, 325*C at the Low setting, 225*C at the Medium setting or 175'C at the High setting.
- c. Set the Polarity Switch to + if Channel A (upper sample injection port) will be used, or to , if Channel B will be used.
6.1.6 Lower the panel cover and turn the Power Switch to ON.
6.1.7 Lift the panel cover aFtin, press the RESET button to assure current to the filament, then lower the panel cover.
NOTE Beginning with Step 6.1.8, operator input is underlined.
6.1.8 Set up the Gas Chretatcgraph for Analycis.
NOTE l
Function Range Increments Remarks Actual ZONE 8 *C 0 to +449 1*C Temperature Not available TEMP INJ ZONE 9 *C 0 to +449 1*C Actual Use 50 to 200.
TEMP LRT Temperature 50 is recommended INIT *C -99 to +449 1*C Actual Use same as TEMP Temperature detector setting
GRAND CULF NUCLEAR STATION HEMISTR NSTRUCTION Titic: Oparctica of ths Gac Ns.: 08-S-04-133 Revision: O Peg 3: 6 Chromategrcph cnd Consoln l
FINAL 'C -99 to +449 1*C 70*C Use same as TEMP detetor setting INIT TIME min. O to 999 1 min. O min. O or 999 minutes equivalent to infinite time (or isothermal operation)
RAMP RATE degC/ min. O to 39.9 0.1 degC/ min. O min. Setting of 0 equivalent to isothermal operation FINAL TIME min. O to 999 1 min. O min. O or 999 minutes equivalent to ,
infinity (iso-thermal at final temperature)
NOTE In order for the desired values to be programmed into the analyzer, the Functicn key must be held down shile entering the values. Observe in the table above that Zone functions require that two Function keys be used, but only the ZONE TENT key is held throughout the entry for the detector temperature setting.
- a. Set temperateres for filament cleaning when the detector has been OFF, as follows:
NOTE If the detector has not been OFF, and changes in settings are desired, proceed to Steps 6.1.8.b(1) through (3).
(1) Press and hold the ZONE TENT key, then press 9 DET CE/ MOD 180 ENTER.
I NOTE Lower or higher settings may be used as deemed necessary.
Also, see Step 6.1.8.b.
I
.CRAND CULF NUCLEAR STATION CHEMISTRY INSTRUCTION
Title:
, Operation of the Gas No.: 08-S-04-133 devision: O Page: 7 Chromatograph and Console (2) Release the ZONE TEMP key.
(3) Press and hold the INIT TEMP key, then press CE/ MOD 180 ENTER.
(4) Release the INIT TEMP key.
(5) Using the keys in the same manner as in Steps (3) and (4) above, set FINAL TEMP to 180, INIT TIME to O_, RAMP RATE to O_ and FINAL TIME to O_.
(6) Allow two hours for cleaning the filaments.
- b. Change and set operating temperatures as follows:
(1) Use the keys in the same manner as Steps 6.1.8.a(1) and (2) to set the detector to the desired temperature.
NOTE Any temperatures from 50 to 200 is suitable, 2nd may be used, but when analyzing H 2 , 02 or N2 , 50 degrees C is sufficient. Since the temperature of 50 degrees is recommended, this procedure uses that value where applicable.
(2) Using the keys in the same manner as Steps 6.1.8.a(3) and , l (4), set the INIT TEMP and the FINAL TEMP to the temperature setting of the previous step. l l
(3) If not already set, use the keys in the same manner as Steps 6.1.8.e(3) and (4) to set, 1 NIT TIME to 0, RAMP RATE to O_ and FINAL TIME to O_.
NOTE Heat-up of the CC is rapid, but cool down is considerably slower. Proceed, as necessary, while the GC is adjusting to the desired temperature, however, do not complete the fine setting portion of Step 6.4.7 until the Sigma 3B READY LIGHT (located in front of Sample Injection Ports A -
and B) has illuminated.
,dR ND CULF NUCLEAR STATION CHEMISTRY INSTRUCTION
, Tit 10,: Op3retion of th3 Geo No.: 08-S-04-133 R3 vision: 0 Pcgs: H Chromatograph and Console 6.1.9 When necessary, condition (bake) or recondition the column as follows:
- a. Assure that carrier gas flow is set at 30 cc/ minute.
- b. Set the Oven Protect Switch to 350.
- c. Do Steps 6.1.8.a(1) through (5) at 300*C instead of 180*C.
- d. Allow 8 or more hours for conditioning.
6.2 Start up the Sigma 15 Console and set the system clock. ----- - --
6.2.1 Turn the Power Switch (bottom lef t of console) to ON and answer the following system prompts with the underlined responses:
- a. NO OF TERMINALS 1 ENTER
- b. NO OF ANALYZERS 0, ENTER
- c. NO OF INSTRUMENTS 1 ENTER NOTE Use the 24-hour clock format for setting the system clock.
NOTE It is noe necessary to set the system clock unless date and times are desired on data printcuts. Elution and er,tention times are not affected by the system clock settings.
6.2.2 Press / (slant) C and type Hour Numerals, ENTER Minute Numeral (s), FNTER Fonth Numerals, ENTER Day Numeral ('s), ENTER Year Numerals and wait for the second hand to reach the exact minute, then press FNTER.
NOTE Seconds, other than 0 may be used by pressing . after Minute Numerals, entering the value, and waiting for the exact second before pressing the last ENTER. For example:
11 ENTER 15.30 ENTER 10 ENTER 26 ENTER 82 ENTER ~~
for 30 seoends past 1115 on 10726/82.
6.2.3 When checking the time settings to affira Sey are correct, press
] C_, and if correct, press the CANCEL key u terminate the conversation and clear the backlighted display.
i
, GRAND GULF NUCLEAR STATION CHEMISTRY INSTRUCTION Titlo: Opsrction of tha Gco Ns.: 08-S-04-133 l Ravicion: O Pegs: 9 Chromatograph and Console l NOTE To take the console out of a mode, press the CANCEL ENTRY key, then press the CANCEL key. (This is not necessary for Step 6.2.3.)
NOTE j l
When the SHIFT
- A directive is used to illuminate the backlighted ~
display in sequ'ence, the system clock stops while the directive is in sequence, requiring that the clock be reset if correct clock time is desired.
NOTE .
The following default method (Seciton 6.3) is used to establish a link between the chromatograph and the console, and to obtain data for genreating an analysis method. Although there may be a necessity for recalling it for baseline setting, analyzing gases with unknown components etc. , the default method can be changed to an analysis method using the MODIFY program (Section 6.10), or it l can be deleted to save space, once another method has been generated. When desired, press VOID 1 ENTER to free the printer, then press DELETE 1 ENTER to delete the default method.
6.3 Default Method Generation 6.3.1 Press the GEN key, Method Number and ENTER.
6.3.2 When the INJ TEMP prompt appears, press the ACCEPT SECTN key three times to accept the defaulted valuer for the following sections of the method.
- a. INJ TEMP
- c. ATTN-CHART DELAY 6.3.3 Wait for the printout of the method.
6.4 Link the Plotter / Printer to the Chromatograph, set up the system to obtain a peak file and adjust the baseline as follows:
6.4.1 Press the PLOT key.
6.4.2 Press the SPACE BAR.
,GRANQ CULF NUCLEAR STATION CHEMISTRY INSTRUCTION Titlo: Oparction of tho Goo INo.: 08-S-04-133 Rsvisien: O Pagar 10 Chromatograph and Console 6.4.3 Answer the backlighted display prompts with the following underlined responses.
- a. INSTRUMENT: 1 ENTER
- b. MODE: 0 ENTER NOTE Mode codes are as follows:
0 = integration (tick) marks and peak crest times 1 = peak crest times only 2 = integration marks only 3 = no integration marks, no peak crest times 6.4.4 Press the . key to affirm the position of the Plotter plot head is at 10%. (The default value is 5%.)
6.4.5 If the plot head was not at 10%, press the 10_ 0 keys, then press the ENTER key.
NOTE LeavinF the plotter plot head at 5% is acceptable, if desired.
Simply press the CANCEL key, if 5% is acceptable to the operator.
6.4.6 Set up the system to obtain a Peak File as follows:
i
- a. Press the SET UP key.
- b. Answer the following prompts with the underlined responses:
(1) INSTRUMENT: 1 ENTER (2) ME" HOD: [UMERAL, ENTER (3) MODE: ENTER to accept a 0 value NOTE Mode codes are as follows: .
0 = short report 1 = long report (4) SAMPLE #/ID: ENTER ENTER (or sample number NUMERALS ENTER sample ID ENTER using up to 20 characters for the sample ID).
CRIND,CULF NUCLEAR STATION CHEMISTRY INSTRUCTION
Title:
Opsrction of tha Gas No.: 08-S-04-133 Rsvision: O Pega: 11 Chromatograph and Console l t
NOTE When the preceding step has been completed, the green portion of the READY /RUN button illuminaces and the system is ready to operate.
6.4.7 Adjust the Base Line.
NOTE Generally, baseline adjustments are not necessary each time a
._ sample / standard _is run. . _ . _
- a. If the GC ready light, directly in front of injections ports 'A -
l and B is illuminated, press the READY /RUN switch (without I
injecting sample).
1 NOTE Either the GC ready li ht F or the interface READY /RUN light may be pressed.
- b. Use the ZERO knob located at the top far right of the CC keyboard for gross adjustment, turning it slowly up and down '
until a response is detected.
- c. Slowly, adjust the ZERO knob to position the plotter head at the base of the plotter paper.
- d. Use the FINE ZERO knob to positien the plottar head at tne I pre-set plot head positica (6.4.4).
6.4.8 Press the DATA STOP key.
6.4.9 Press 1 ENTER to respond to INSTRUME:IT prompt, then allow
~'
sufficieht (Eme for che system to scop collecting data and printing a report.
NOTE Normally, the defaulted area and base sensitivities of 50 and 4 are adequate, but affirmation of this can be determined by doing Steps 6.4.10.a through 6.4.10.g(2). If area and base calculations are not desired, proceed to the last note preceding Section 6.5.
6.4.10 Detereine area and base sensitivity as follows:
- a. Press AT*N (H), - (minus) 4.
. GRAND GULF NUCLEAR STATION CHEMISTRY INSTRUCTION Titlo: Op3rctics of ths Geo Ns.: 08-S-04-133 Rsvision: O Paga: 12
. Chromatograph and Console l
- b. Press the READY /RUN switch.
! c. If the printer pen goes off scale, or if it appears that the pen will go off scale before two minutes have elapsed, do Step 6.4.10.a using a - 2, instead of -4.
l d. Allow the system to collect noise data for two (2) minutes.
- e. Envelope the noise peaks by drawing parallel lines across the top and bottom of the peaks.
- f. In millimeter measurements, measure the greatest distance from the bottom edge of the chart paper to the top parallel line and the shortest distance from the bottom edge of the chart paper to the bottom parallel line.
NOTE Use the following Attenuation vs Signal for Full Scale Plotter Head Deflection values to calculate Area and Base Sensitivity.
Attenuation Sfyg (uV) Attenuation Syg (uV)
-4 50 -2 200
-3 100 -1 400 6.4.11 Calculate Area and Base Sensitivity as follows:
(s) Area Sensitivity = 35Sys (H -HL)/PW H Where, S ys = signal for full scale plot head deflection in uV, corresponding to the applicable attenuatiott value given in the note following Step 6.4.10.f 1
HH = Highest point on a two-minute envelope in mm from the bottom edge of the printer / plotter paper HL = Lowest point on a two-minute envelope in mm
- from the bottom edge of the printer plotter paper PW = Width of plotter paper (ex. 180 mm) 1
. GRAND CULF NUCLEAR STATION CHEMISTRY INSTRUCTION
.Titlo; Operation of the Gas No.: 08-S-04-133 Revision: 0 Page: 13 Chromatograph and Console NOTE Round the answer to the nearest multiple of five.
(b) Base Sensitivity = 1.7 Sys (HH-HL )/180 using the same envelope as for area sensitivity.
NOTE Kound the answer to the next higher whole number.
NOTE Ideally, the noise trace obtained above should be flat (horizontal). If there is extensive drift, the values obtained in Step 6.4.11 will be high. If so, reconditioning of the column may be required.
NOTE When sample is injected in Step 6.5.2, the printer pen may go off scale, but the value is retained. Data is also retained during attenuation adjustment and even when I the Plotter has been disabled. If the Plotter was disabled, data will be printed out when the Plotter is reactivated.
5.5 Obtain Peak Area and Elution Times Utilizing the Default Method (Step 6.3) as follows:
NOTE Since percents of gases are determined by this procedure, sample volumes are not critical.
6.5.1 When the asdy (green) light ou the instrument interface illuminates, place the syringe needle into the gas sample / standard, w~ait approximatley 15 seconds for stabilization at the needle point, then' slowly fill the syringe to 1.0 cc with l the gas.
NOTE -
Inserting the needle all the way, each time, as in the following step, and proceeding rapidly, but smoothly, through the step assures that no sample, especially the hydrogen, is lost, and that ensuing injections will be consistent.
. GRAND GULF NUCLEAR STATION CHEMISTRY INSTRUCTION
,Titlo- Oparaticn of tha Gas No.: 08-S-04-133 Ravision: 0 lPage: 14 Chromatograph and Console l l l
6.5.2 Insert the needle as far as possible into the sample injection l port (Channel A), steadily inject the sample and simultaneously press the READY /RUN switch the moment the syringe plunger touches the plunger stop.
NOTE To assure high ouality analyses that will follow, consistency in f the performance of Step 6.5.2 is essential.
L 6.5.3 Press the ATTN (H) key, type 9 (or 10), then wait until the ligher molecules (ex H2 ) have eluted, then press ENTER.
6.5.4 Raise or lower the attenuation as desired according.co Step 6.5.3 or by pressing the f AT_TN or the SATTN keys.
NOTE During plotting of data, pressing (decreases the amplitude of a given$ peakATTN by a increases factor of attenuation two), and pressing YATTN decreases attenuation (increases the amplitude of a given peak) by a factor of two each time the keys are pressed.
The range of actual values extend from an expansion factor of X16 to an attenuation factor of 2048. This is equivalent to the displayed values of -4 to lie for example:
Displayed Numeral Incr./Decr. Displayed Numeral Incr. Decr.
-4 Exp. Fac. 16 4 Attenuation 16
-3 Exp. Fac. 3 5 Attanuation 32
-2 Exp. Fac. 4 6 Attenuation 64
-1 Exp. Fac. 2 7 Attenuation 125 0 Attenuatian 1 8 Attenur.cion 255 1 Attenuation 2 9 Attenuation 512 2 Attenuation 4 10 Attenuation 1024 3 Attenuation 8 11 Attenuation 2048 6.5.5 If necessary, change the position of the plotter head by pressing
. numeral (representing % of full scale) ENTER.
NOTE When . is pressed, the present plotter head position numeral wil be displayed. If no change is made, press CANCEL to remove the display.
Titlo: Op3rcticn of th3 G:s Ns.: 08-S-04-133 Revision: 0 Pega: 15 Chromitegrcph and Cens910 6.5.6 If necessary, adjust Chart Speed by pressing CHART desired am/ minute NUMERALS ENTER.
NOTE When CHART is pressed, the present chart speed (mm/ minute) will be-d is played. If the chart speed is not changed, the display is removed by pressing the CANCEL key.
6.5.7 When sufficient data has been collected, press DATA STOP 1 ENTER.
NOTE When the DATA STOP signal is accepted, the system will print out an Area Normalization Report. In the example that follows, the-run number is 2 because run I was used to adjust the baseline.
The injected sample was room air. The constituents are hydrogen at 0.39 minutes, oxygen at 0.84 minutes and nitrogen at 1.35 minutes. The printout is as follows:
INST I METH 1 FILE 9 RUN 2 14: 7.2 12 / 13 / 82 SENSITIVITIES 50 4 ,
' I 1
TIME AREA BC RRT RF C NAME l O.39 0.2023 0.039 1.000 0.0155 0.84 275.5788 0.084 1.000 21.0527 '
1.35 1033.2160 0.135 1.000 78.9219 6.5.8 If additional runs are desired, repeat Steps 6.5.1 through 6.5.7, as necessary.
NOTE The default nethod in Step 6.3 is useful for recalling for the i purpose of zeroing the chromatograph, running samples with unknown constituents to determine peak areas and times and other purposes; however, the procedure can be changed to an analysis procedure as per the Modify Section (6.10) of this procedure, if desired, or deleted as per the note preceding Step 6.3, if space is needed. .
- GRAND GULF NUCLEAR STATION CHEMIST'Y INSTRUCTION Titlo: Oparatica of tha Gco No.: 08-S-04-133 Revicica: O Pega: 16
. Chromatograph and Console
- 6. 6- Generate an Area Normalization Analysis Method for calibration with Relative Response Factors (Internal Standard Analysis) or with Absolute Response Factors (External Standard Analysie).
6.6.1 If the printer is linked to the GC (green ready light ON), press VOID 1 ENTER.
6.6.2 Press the GEN key, Method Number and ENTER key.
NOTE If default values in a complete section are acceptable, the ACCEPT {
) SECTN key may be used instead of the ENTER key. If the default values of a given line is acceptable, the NEXT LINE key may be used; however, using the ENTER key provides a printout of the default values used, as well as operator input.
NOTE Fixed and variable portions of the three sections of the method
! generation are not separated. See Step 3.5 and Section 6.10 for l more detail, if necessary.
6.6.3 Respond to the system conversation with the following underlined entries:
- a. ANALYZER CONTROL Section (1) INJ TEMP: ENTER (2) DET ZONE 1 & 2: ,5ftpfl%R,JOENjTF l (3) AUX TEMP: ENTER l (4) FLOW A, B; g ENTER H ENTER (5) ;XIT OVEN TEMP TIME: R ENTER (6) TEMP RATE TIME: ACCEPT SECTN
- b. DATA PROCESS Seetion EM ,
The following Step 6.6.3.b(1) and Step 6.6.3 b(8) are flags directing the generation of an area normalization, internal standard analysis method when zero (default) standard weight
GRAND GULF NUCLEAR STATION CHEMISTRY INSTRUCTION Titlo: Opsrctica of th3 Gao No.: 08-S-04-133 R3 vision: O Pega: 17
. . Chromatograph and Console is used and a standard name (internal standard) is entered in Step 6.6.3.b(8). An external standard analysis method is generated when a numeral of one, or greater, is used for standard weight, and the standard name defaulted (no standard name).
NOTE In the next step, decide whether the peak file of subsequent runs using this method are to be saved or erased to save space, before making the third entry. Also, decide whether an Internal Standard Method (Std We 0, less problems) or an External Standard Method (Std Wt 1) will be generated.
l (1) STD WT, SMP WT l a. For an Internal Standard Method, press ENTER, ENTER l and ENTER to save subsequent files, or 1 instead of the third ENTER, to erase subsequent files,
- b. For an External Standard Method, press 1, ENTER and ENTER or numeral 1 for reasons described in the
- previous step.
(2) FACTOR SCALE: ENTER ENTER (3) TIMES: type the desired run time NUMERAL (S) (2.0 to 3.0 minutes are sufficient for the analysis of hydrogen, oxygen and nitrogen), then press ENTER five times.
NOTE Normally, it is not necessary to change the defaulted I
values in the following step, but if values other than the default values are desired, enter those values where applicable as follows:
First Entry - Area Sensitivity - Use higher values to reduce coise, or lower values to detect smaller peaks.
Second Entry - Base Sensitivity - Use larger values to make it easier for the system to find and -
return to baseline sooner.
l l
l
GRAND GULF NUCLEAR STATION CHEMISTRY INSTRUCTION
Title:
Op3rcticn of ths Gco No.: 08-S-04-133 Rsvisien: O Paga: 18 Chroratsgraph cnd Censole The default values for the remaining entries are adequate for this method. The entries are:
Third Entry - Skim Sensitivity Four?.h Entry - Baseline Correction Code Fifth Entry - Detector Range Sixty Entry - Multiplex Detector Range is not applicable to the SIGMA 15.
(4) SENS-DET RANGE: Press ENTER six times if default values are satisfactory, or enter values as described in the preceding note, if necessary.
I (5) UNKNOWN AIR: ENTER ENTER At the first entry of the following step, entry of a 1 numerical value less than the lowest peak of interest, will prevent the printout of peaks with concentrations i less than the entered value. l (6) TOL: ENTER (or numerical value) ENTER ENTER NOTE The entered values in the following four steps are taken from the Default Analysis Report generated at Step 6.5.7.
For Step 6.6.3.b(7), select the largesc, centrally located peak as the reference peak. (When analyzing air, use the oxygen peak as the reference peak.)
(7) REF PK: Enter the four following vsluss for the selected reference peak as follows:
(a) RRT VALUE ENTER (usually same as TI:TE value)
(b) START TIME ENTER (a time prior to peak start)
(c) END TIME ENTER (a time af ter peak printout esturns to baseline)
(d) RT Value ENTER (8) STD NAME: Select either (a) or (b).
, GRAND GUI.F NUCLEAR STATION CFEMISTRY INSTRUCTION
Title:
Op3rction of the Gas No.: 08-S-04-133 Revision: O Page: 19 l Chromatograph and Console (a) Internal Standard Method: Enter the standard name using the exact spelling as the name of the reference standard in the component list, Step 6.6.3.b(9).
NOTE Up to 20 characters may be used. The name used must be spelled exactly the same at this step as on the component list in Step 6.6.3.b(9), otherwise the l system will be unable to perform the internal standard calculations or, during calibration, to compute response factors.
(b) External Standard Method: Press ENTER.
(9) RT RF CONC NAME: Type the first components RT value, press ENTER ENTER (to accept I as the response factor),
component's CONCENTRATION (%) ENTER and the component 's NAME ENTER.
CAUTION When entering the component representing the standard name, assure that the spelling is exactly the same as the spelling of the standard name at Step 6.6.3.b(8)(a) for the internal standard.
(10) Repeat the previous step for all desired components.
(11) Press the ACCEPT SECTN key.
- c. Event Centrol (1) ATTN-CHART-DELAY: Press ENTER for all acceptable default values and/or type attenuation value ENTER chart speed ~
rahoin, ENTER desireTchart delav time ENTER.
(2) TIME DEVICE FbNCTION NAME:
NOTE In this step, ATTN values and/or CHART speeds are entered -
in order that these values will change during the run.
When entering the ATTN and CHART speed values while generating a method, start with the lowest CHART speed
G
' RAND GULF NUCLEAR STATION CHEMISTRY INSTRUCTION
Title:
Opsration of ths Gas No.: 08-S-04-133 Ravision: O Paga: 20 Chromatograph and Console value, then the lowest ATTN value which must be at least
.01 higher than the CHART speed value, and work in ascending order of time, until all desired values are entered. When using the Modify program (Section 6.10) this technique is reversed, i.e., start with highest ATTN value, then the highest CHART speed value, and work in descending order to the lowest values.
(a) To change the chart speed and the attenuation values during the run, select a time just preceding the ATTN time value and type or press Time Numerals ENTER CHART sun / minute value ENTER ENTER (the Printer Head returns to zero) Time of ATTN change ENTER ATTN (H Key) ATTN Value NEXT LINE (or NAME ENTER), or (b) Enter only the ATTN values or the CHART speed l values, if desired, using the same dialog for each according to the previous step.
1 (3) When all values have been entered, press the ACCEPT SECTN l key.
NOTE The other available devices whi S can be changed by prograssning these changes into the run are EXT, NO INT, WIDTH and SENS. Changes of these devices are not necessary for this procedure. Refer to Appendix I, Pages Al-15 through Al-19, Sigma 15 SERIES CONSOLE Instruction Manual for an in depth discussion.
6.6.4 Press the PLOT key and if:
- a. INSTRUMENT 1 is displayed, press the CANCEL key.
- b. INSTRUMFNT 0 is displayed, press the SPACE BAR, numeral i and ENTER, to link the I'lotter to the GC.
6.6.5 Press the . key to affirm the pcsition of the Plotter plot head is at 10%. (The default value is 5% and can be used if desired.)
6.6.6 If the plot head was not at 10%, press the 10 keys (if desired),
then press the ENTER key, or if 5% is displayed and desired, press the CANCEL key.
GRAND GULF NUCLEAR STATION CHEMISTRY INSTRUCTION
Title:
Opsrcticn of the Gco Ns.: 08-S-04-133 Rsvision: O Paga: 21 Chromatograph and Console 6.6.7 Set up the system to obtain data by pressing SET UP 1 ENTER method Numeral ENTER, and ENTER again to accept mode 0.
l 6.6.8 Place the point of the syringe into the gas sample source and allow approximately 15 seconds for stabilization, then slowly draw one cc of gas into the syringe.
6.6.9 Place the syringe needle into sample port A as far as it will go, steadily eject the sample while simultaneously pressing the READY /RUN button as the syringe plunger touches the plunger stop.
NOTE The system will analyze the sampla and print out an analysis report, but the following steps are necessary for ascertaining the accuracy of the analysis and calibrating the analysis rethod.
6.7 Response Factor Calculation and Calibration 6.7.1 When the printout from Step 6.6.9 is completed, press or type, ~
CALIB FILE NUMBER (listed at the heading of the run) ENTER METHOD NUMBER ENTER and ENTER again to accept numeral 0.
6.7.2 After RUN NO, enter the number corresponding to the amount of runs made for the Fiven method, then wait for the Calibration Report.
6.7.3 Observe that no Response Factor value is less than 0.500, nor greater than 32.767 (indicated as .001), and that each response factor has three or more significant figures.
6.7.4 If the criteria of Step 6.7.3 were met, proceed to Step 6.7.6.
6.7.5 Shculd any one or more Response Factors fall outside the criteria'
, of Step 6.7.3 (a likely condition with Absolute Response Factors in External Standard Analyais Mecheds), change the sample size injected to :hange the peak areas in the peak files or use the Mcdify Sectica (6.10) of this procedure and take any of the following steps:
- a. Change the range (sensitivity) seting of the chromatograph to l change the peak areas in the peak files (i.e., reduce to I obtain smaller peak areas and larger response factors, or, l vice versa). -
l l
\
[ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ - - _ _ - _ - _ _ _ _ _ - - _ _ - - - _ - - - _ - . _
GRAND, GULF NUCLEAR STATION -
/ CHEMISTR'l INSTRUCTION
Title:
Oparction of tha Gno No.: 08-S-04-133 Rnvision: O Pcga: '52
. . Chromatograph and Console -
~
- b. Change the concentration entries in the' component list as follows: -
(1) HiFh Response Factors - divide by 10 (2) Low Response Factors - multiply by 10
- c. If 6.7.5.b above was done, enter values at th'e FACTOR SCALE line as follows: , .
(1) ENTER (to accept default factor '1), then enter 1 if the -
concentrations were divided by 10, or (2) ENTER (to accept default factor 1), then enter -1,if the concentrations were multiplied by 10. -
6.7.6 When all of the criteria of Step 6.7.3 are satisfactory, calibrate -
as follows:
- a. Press CALIB FILE NUMBER ENTER METHOD NUMBER ENTER 1 ENTER. '
- b. After RUN NO, enter the number of runs made. -j NOTE ^ ~ ,
^
The method is now calibrated to those acceptable values.
There will be'no printout. d i N, 6.8 Initiate a Report Conversation, if necessary: 'i -
6.8.1 If the RUN/ REAM light ia ON, press VOID D 1, EjnJT to free the printer. {
' {
t 6.8.2 Press PLOT and observe that INSTRUMENT l'.is displayed, t
6.8.3 If INSTRUMENT 1 vas diaplcyeri, press'the CARL 3 key. l' -
l l
6.8.4 If INSTRUMENT 0 was displayed, presa SPACE Bq l EtrIER .and 0 ENTER after MODE display.
6.8.5 Press REPRT FILE NUMER ENTER METHOD NUMBER ElrfER. ,- , l 6.8.6 If the Standard Weight and' Sample Weights are to be changed, type STANDARD WEIGHT NUMERAL (S) ENTER SAMPLE WEIGHT NUMERAL (S)#NEXT -
LINE.
t
' V,-
/
4 w ,
~J g
,#~
GRAllD GULF NUCLEAR STATION CHEMISTRY INSTRUCTION
Title:
Op3raticn of ths Gao No.: 08-S-04-133 Rsvision: Pcge:
O 23
. Chromatograph and Console l
1 6.8.7 If the weights are not to be changed, press ENTER ENTER NEXT LINE.
- 6.9 Determine data space, number of methods, files, etc. to determine which method is satisfactory for ,the desired ane. lysis, or for any other rasson.
l- 6.9.1 Press the STAT key ENTER to determine the amount of methods in the system and the available space in the computer.
6.9.2 Press LIST METHOD NUMBER ENTER. ,
! 6.9.3 Repeat 6.9.2 until the desired method is located.
6.10 Modification NOTE l When minor, changes to an existing mehtod :cre required, the user can use the Modify Conversation; however, if extensive changes are required, it is generally faster to generate a new method. {
. NOTE Each section (Analyzer Control,iData Processing, and Event Control) has two parts each, a . fixed portion and a variable portion. Each portion may be nadified,~but the technioue for modifying the fixed and variable
, portions differ as will be shown in the proceeding steps.
6.10.1 Press' HOD METHOD NUMBER ENTER.
6.10.2 Analyzer Control Modification f
- a. Fixed Portion (INJ TEMP through.INIT OVEN TEMP, TIME)
NOTE ~
l Select (1), (2), (3), (4), or (5), following, or any w combination of (2), (3), (4) or (5) as recaseary.
- (l). Press ACCEPT SECTN to accept the existir.g vslues of the
, entire section (including both the Fixed and variable Portione).
_ (2) Press NEXT LINE when there are to be no changes made on cl.at particular line. ~
I' .(3 ) Press ENTER when a value within the line is not to be f
changed. '. e l
- ' 1 e.
& 7
'l "
~
^
J sk * . " ' ' '
_2
{' L,,
NUTThOs"L@lU CHEMISTRY INSTRUCTION Titlo: Opsrctica of ths Geo Ns.: 08-S-04-133 Rzvision: O Pcgs: 24 I Chrom-tegrcph end Concola (4) Type the changes followed by ENTER for each change.
(5) Do (3) or (4) until the line is completed,
- b. Variable Portion, TEMP RATE TIME is not applicable in this procedure, so press ACCEPT SECTN.
6.10.3 Data Proceaaing Modification NOTE Although STD NAME falls within the fixed portion of this section,
, ' l
-- . the_ ACCEPT SZCTH. command does not function for STD NAME.
Entry j for STD NAME will be given at Steps 6'.10.3.4(2) and (3). l
. I (1) Select 6.10.2.a(1), (2), (3), (4), (5) or a combination of 6.10.2.a(2), (3), (4) or (5) for all lines except STD NAME.
(2) To delete the standard name, press . NEXT LINE.
(3) To accept the present standard name, press NEXT LINE.
- b. Variable Portion (RT, RF, CONC, NAME)
CAUTION To avoid ERROR re'sponses, and to program the method correctly, the following three ' con ~ditions hust apply:
- 1. Do not use ENTER following a D. I or R command.
- 2. When using the i key,. where there are no existing lines in the method, start with the RT value of the last constituent to elute and work backward to the RT value of the first elutant. l
- 3. When using the I key, where lines alrecdy exist in the method, the RT value of. the line to be inserted must be lower than the lowest existing RT value.
c i
N
,y' s
Titlo: Opsrction of ths Gao No.: 08-S-04-133 Rsvicion: 0 Pega: 25
. Chromatograph and Console NOTE The variable portion of this section can be modified in three ways:
- 1. Use the D key to delete one or all lines in the method, 6.10.3.b(4),
- 2. Use the I key to insert lines when no lines exist in the method, 6.10.3.b(1) or when lines alredy exist in a method, 6.10.3.b(2), or
- 3. Use the R key to replace an existing line or to modify the values in an existing line, 6.10.3.b(3).
Select one or a combination of the following steps to perform the desired modification. Additionally, the T key can be used to return the dialog to the top of the list, 6.10.3.b(5). The T key can be used at any time during Steps 6.10.3.b(1) through 6.10.3.b(4)(e), provided the ACCEPT SECTN key has not been pressed.
(1) Use the I key to insert lines when there are no existing lines in the method, starting with the last constituent to elute, and working backward to the first elutant, as follows:
(a) At the RT print out, press NEXT LINE, then when the printer head returns to zero, press I RT Value ENTER RF Value ENTER (or ENTER to accept 1~000)
Concentration Value ENTER Constituent Name ENTER.
(b) Repeat the preceding step, workinF backward, until all constituents are entered.
(c) Prece ACCEPT SECTN when all entries have been made.
(2) To use the I key when lines already exist in the method, select either (a) or (b) as follows:
(a) When the RT value of the line to be inserted is lower than the lowest existing RT value, do Steps 6.10.3.b(1)(a) through (c). ~
(b) When the RT value of the line to be inserted is Freater than the lowest existinF RT vlaue, delete all RT values that are lower than the new RT value that is to be inserted, according to Step 6.10.3.b(4), insert the new RT value, then re-enter the lower values in descending order according to Steps 6.10.3.b(1)(a) and (b).
. _ _ _ _ _ . - . - . = .
. . l
. GRAND GULF NUCLEAR STATION CHEMISTRY INSTRUCTION l
, Title,: Oparation of the Gas No.: 08-S-04-133 Revision: O Page: 26 Chromatograph and Console (c) Press ACCEPT SECTN when completed.
NOTE When any existing value, including the RT values, is acceptable, simply press ENTER to accept that value.
(3) Use the R key to replace an existing line or to modify the values in an existing line.
(a) At the RT print out, press KEXT LINE until the line that is to be changed is printed out, or type the RT value of the line followed by ENTER.
(b) Press R RT Value ENTER RF Value ENTER CONC Value ENTER NAME ENTER.
j (c) After each recurring RT printout, repeat Steps 6.10.3.b(3)(a) and (b), above until all modifications are complete.
I (d) When all modifications have been completed, press l ACCEPT SECTN. l (4) Use the D key to delete a line as follows: l l
(a) At RT, press NEXT LINE until the line that is to be deleted is printed out, or type the RT Value of the line followed by ENTER.
(b) Press the D key following the printout of the selected line.
(c) When the next line in the method is printed out, either prcss NEXT LINE to accept that line, or D to ""
delete the line.
(d) Repeat the previous step as desired.
(e) If desired, enter new values according to Steps -
6.10.3.b(1)(a) through (b), or 6.10.3.b(2)(a) and (b) as applicable.
," . GRAND CULF NUCLEAR STATION CHEMISTRY INSTRUCTION
Title:
Op2 ration of the Gas No.: 08-S-04-133 Revision: 0 Page: 27 Chromatograph and Console (f) Press ACCEPT SECTN when completed.
(5) If it is necessary to work from the top of the list, press the T key and do any of the following:
(a) direct the dialog to the top of the list by pressing NEXT LINE, then use the D, I or R directives as per i Steps 6.10.3.b(1) through (4) as necessary, or (b) type the RF Value for one of the existing lines, then use the D, I or R directives as per Steps 6.10.3.b(1) through (4) as necessary, or (c) add ?. new line by , pressing NEXT LINE once, and when the printer head returns to zero, press _I an RT Value lower than the lowest existing RT value, l ENTE 1ETF Value ENTER (or simply, ENTER to accept 1.000) CONC Value ENTER NAME ENTER, repeating this step with lower RT vlaues for each successive entry.
until all entries are made, or (d) if, er when no further entries are to be made, press NEXT LINE and ACCEPT SECTN.
6.10.4 Event Control Modification
- a. Fixed Portion (ATTN-CHART-DELAY), do either (1) or (2).
(1) If all values in the line are acceptable, press NEXT LINE, or (2) Press ENTER for all acceptable values and/or type ATTN Value ENTER Chart Speed ENTER Desired Chart Delay Time ENTER.
NOTE The T key [6.10.3.b(5)] can be used at any time during Steps 6.10.4.b through 6.10.4.b(2)(c), provided the ACCEPT SECTN key has not been pressed.
- b. Variable Portion (TIME DEVICE FUNCTION NAME)
O
~
. GRAND GULF NUCLEAR SfATION CFEMISTRY INSTRUCTION
Title:
Operation of the Gas No.: 08-S-04-133 ' Revision: O Page: 28 Chromatograph and Console NOTE l
Use Steps 6.10.4.b(1)(a) through (d) when there are no l existing values in the list, or Steps 6.10.4.b(2)(a) through (d) when there are existing values in the list.
(1) When no values exist in the TIME DEVICE FUNCTION NAME portion list, add ATTN values and CHAPT speed values as per (a) and (b), or ATTN values only or CHART speed values only as per (a) and (c).
(a) Press NEXTLINrand wait for the printer head to -
Zero.
(b) Starting just prior to the peak start time of the last constituent to elute and working backward in descending order of time to just prior to the peak j start ime of the first elutant, enter the values I into the list by pressing I Time ENTER ATTN (R key) I ATTN value NEXT LINE (or NAME ENTER), then when the printer head returns to zero, and if CHART speeds are to be entered, press I a time value just prior to the ATTN time value ENTER CHART nun / min. ENTER ENTER, or (c) Enter only the ATTN values, or the CHART speeds according to the previous step for each.
(d) Press ACCEPT SECTN when completed.
(2) Use the R key to replace any existing values requiring change, as follows:
NOTE The R key cannot be used for replacing an ATTN value with a CHART value, and vice-versa.
(a) Af ter TIME print out, type the latest Time Value ENTER, and af ter that line is printed out, press][
New Time Value ENTER (or simply, ENTER to accept present value) ATTN (H key) New ATTN Value Name.
ENTER or NEXT LINE for the last two functions.
(b) If further changes are to be made, repeat the previous step working backward, through the lowest time value as necessary.
' GRAND GULF NUCLEAR STATION ' CHEMISTRY INSTRUCTION Titlo: Oparation of th2 Gac No.: 08-S-04-133 R:vicion: O Pcgs: 30 Chromatngrcph end Cent: ole NOTE Numeral 1 ENTER will provide a long report.
- d. SAMPLE f/ID: ENTER ENTER or type of the sample number ENTER, the sample ID (up to 20 characters) ENTER.
6.11.4 When the " Ready" light on the system interface illuminates, fill the hypodermic syringe to 1.0 cc of sample and insert the needle as far as it will go.into the sample injection port.
- 6.11.5 Eject the sample steadily, and as the plunger of the syringe strikes it's stop, simultaneously press the READY /RUN button, then wait for the analysis and report.
l
- 6.11.6 Repeat Section 6.11 as necessary for additional analyses.
4
, GRAND GULF NUCLEAR STATION CHEMISTRY INSTRUCTION 08-S-04-133 lRivision 0 Attachment I lPage 1 of 7
SUMMARY
OF OPERATING CONVERSATIONS AND DIRECTIVES LEGEND Push buttons, consoie panel dispeeys, and terme pnnted out on the Pnnter/ Plotter' Labeled pusa tuttoets -
u "* I, 8, ' -e * - I Unlabeled pusn buttens -
8 Display panel indications -
i.~d f ** *""*1 N
~
Print-out. Printer / Plotter - !NJ *EMP, FLOW A.S. E
~~_
User entry, Printer / Plotter
- NY:RoCAABCN RUN, SAMPI.E 1 Entnee to be mode by user from keyboere:
om t (D,,, )
LRRCRS
!! A is displayed, push t = * '= t , then enter correct value andspush i s 'r*!
Operating Conversations 1 SETTING SYSTEM CLOCK (1) < c 0 : 28.7 0/ 0/ 0 (System prints out current clock reading.)
(3} If clock setting CK: l usca l (3a] If hour and minutes not OK, but month, day, year OK:
(M.ut) l tett. i (Manusee) i f art. l i tuft. i
. to 23 . t. $. 9 (3b} If month, day, or year not CK:
(N . .e n
) it.<t i ( .-e) ....
i rm. i (..
.n
) i te. i (o.7)
. .i irm.i (v t.
) i E=. i i
2 SETTING MAXIMUM OVEN TEMPERATURE N.ot- r.
\ ..
_ _ ~ - - - -
~
e GRAND GULF NUCLEAR STATION a CHEMISTRY INSTRUCTION 08-S-04-133 IRavision 0 Attachment I {Page 2 of 7
SUMMARY
OF 0?fRATING CONVERSATIO.MS A'ID DIRECTIVES 3 METHOD GENERATION (A) ANALYZER CCNTROt.
- w. o.<..a
- t-Q h" . 213) l(*fte }
t ANALYTER CONTROL as
- NJ TEMP ( p gj .e) {*1 tun I l 23 o e64 GS 23 DET 20NE 1,2 (in".;450-J;.
25 t
.4) ii nlai i.(ga..c)im--ei ene
. as AUX TEMP (?,";,.$c'") I "" u=a I 88 * ***
l Note Valve settings on " Read-a-Flow" units FLOW A*3 (EU' 53..) l ****l (ED* lN ) l**" u"< l must be entered or " Ready" indicator
'. own o m .. won't light.
- ) n ...
INIT OVEN "'EMP, TIME ,(-El'.",'.0"c") l a 'ta l (yg . ) t =<p un i stoo i. So - o is u.
TEMP RATE TIME
- i
@ ..c) :< n i (74:o!t.'.T)
. . . . . .. m ... i< a i (R."* .. ) i <a
. i.
(Repeat TEMP, RATE, TIME entries as required.}
I .ca- se: = i IND TIME MAX mR 'End time max = maximum allowable data end time in' Data Processing section.
1 3 METHOD GENERATION (B) DATA PROCESSING DATA PROC o a o (W, *,'f*) I t"t' l (5"$) I t"n' t (c$ "'**""")
STD WT, SMP WT I *'" ' '** l jgjjjg *gjj,'; 81 ' Tile Dispo- I 0 = Save File
, ,sition Code FAC"'OR , SCALE (l = Delete File.
($*""",'"'O) I t'"' I (f.".'uE,'c .) I "*" u*' I i
- i. to ee. .i.
L _
GRAND GULF NUCLEAR STATION CHEMISTRY INSTRUCTION
- . 08-S-04-133 IRevision 0 Attachment I {Page 3 of 7
SUMMARY
OF OPERATING CONVERSATIONS AND DIRECTIVES 3- METHOD GENERATION (9) DATA PROCESSING (Cent'd) 327.47 0 327.47 327.37 327.67 TIMES *(9.l Ji- ) i on i (g==t,sua,,.) n n ! (y;,afr) ion 1 (ggrafr) in ni (g;,*fr) inn t 0to 327.47 0toDET DSTtoDET PSPtoDET PEP to DET 221*$7
'DET = Data End Time (N"*[.'II)
. I "" '" I DST = Data Start Time PSP te DET , PSP = Previous Forced Base Point Time. l
= . . . .
l sEss-oET RAncE (; ,,,,,,) in u., g,2,,,,,) n.,. i ( =,,,,,,) nm. , g:ees.;,,) n. ,., ( g ) n,....,
t is un i se tu o ie too.co o. s. 2 e ie .
!O = Draw B.L.
N Baseline (B.L.) to next valley (Da" amas*) l arn v=< l <
1 = Project 3.L. horizontally o ie . , Correction Code [2 = Craw B.L. to next base point, i.ooo o UNK, AIR I wn un 1
- **,,*) I < ="- l ($i "**)
(,7,*M".*147 0 to 32 4to 327.87
. .. n. .
3
/
oL Gr, e) n n t G"J~.e) I a'"i G.w_) i-- va i
. t. . . u. . ? . to io..
0 0 0 0 REF PK RRT '
(Ref. Pt.) l ta'te j (T'Line. 'aus.R ' P M) l nrta Ref.} Pt. End (T&ame. enas. g g,,,g g ( Roses. T1sne W I
\ Ref. Pt. as - ',
o to 32.787 DST to DET RPS se DET R.pg to nFE NoName
'RPS = Ref. Pk. Start Time'
,RPE = Ref. Pk. End Time
(","e,jg) Inn un i STD NAME d 2o smar. cure RT RF CONC NAME 1 0 No Namne RT. Com. gg.gg Response 1Facter.) g g,.g, g { Caecentrataan, g gorg, g(panees / Name.
Carnpanens t Caet.)
/ I ,,,p ,,, I ponent & Censpeneet 1 O to 327.47 0 to 32.787 0 to 8990.9990 to cascacters (RepeatRT, RF, CONC, NAME entries as required.]
i .c:r- ic: = 1
- Data end time must be equal to or less than total run time required for temperature program designated in Analyzer Control Section, above.
GRAND, GULF NUCLEAR STATION CHEMISTRY INSTRUCTION 08-S-04-133 IRsvision 0 Attachment I {Page 4 of 7 3
SUMMARY
OF OPERATING CONVERSATIONS AND DIRECTIVES 3 METHOD GENERATION (C) EVENT CONTROL EVENT CONTROL
, i. ...,
xT N-CHART-DEuv ( *4 **_) it-i (r.$.:-) ice.i (I;;. ) i=<nu...
II 0 n.100 l
0 t. 327.47 ,
TIME DEVICE FUNC" ION NAME J' 8'"'*"
($@ ,) Icet.1 [o.**?I CHART C, (CM j ,,,,) Ie m at ([^ , ,"***" ) Iw n u=II Ot 327.sf 0 t.100 20 m ;
H* 8 8* "e="8 (5=m. ., ) i-i i n i arrN x, (0=- -) i- i (E:l=~~) iw- ew i
- t. . . _ . -
X* * "* "**
- t (52 = ) I'*t L'") GLX, (!".J. ) l '" ' (E,"7) l at" wa< l 0 = Multiplexer
- o w m.st e t.e 7 so .,,, ,
f* 27 = Hot Wire Polarity
,21 to 26 = Relays .
I
] ,
s ($",",'l ,,,,) I tera l l ae .=t l NO INT ' taNI, (e",;'**) t rete l (y,7) l=en uw l
- w. up.e
' Integrate f0= Integrate )
a te m.st
, Code l
- o. : 3. w,. (. = No Integrate
~
- g. n. o.s n. up
($Q ) lietet (=p i WIDTH W, (s ,g ,) , ,,, , [ Q4 m.n) .g , ,y uy , ** S p ,1 e s t *"-
0 n. 337.67 1 t. 4 20.a r w , "'
k I. .. .. u (j@ m ) Itet.1 its I E , (,T*****) Itntel ([=',,","")
e i. m. st i nn uw ] , Detector No. is dummy entry. )
t e. se - , Has no of fact on operation..
,* , , .. . n .
(5@ . ) I set'l I === 1 SENS S A ', B ' S , BC ,( ^C ,,,,) I ret.1 (,,",,,) l am.1 (sg,) , em. , ( o.
) , ,m. ,
. m. .,
x.ups . . . = , t. m - . t.
0o.De (E**
g, 7 )1.<nuni Baseline (B.L.) ,0 = Draw B.L. to next valley i.c:, u ,,, Correction Code 1 = Project B.L. horirontally 2 = Draw B.L. to next base point.
l
- *Lotter or symbol above Device push button represents equivalent key on auxiliary keyboard.
- Chenge in WICTH must be entered when NO INT is in effect so System is on baseline.
Otherwise, WIDTH may not change. .
' *** Entry of WIDTH 1 for a time of 0.00 results in data collection at the maximum rate througnout intervals areasuspended.
run. Automatic rate reductions to slower, optimum rates at appropriate tChenges to A and B occur when NO INT is in effect or System is on baseline.
GRAND* GULF NUCLEAR STATION CHEMISTRY INSTRUCTION 08-S-04-133 Rwision 0 Attachment I Page 5 of 7
)
J
(
SUMMARY
OF OPERATING CONVERSATIONS AND DIRECTIVES 4 LINKING PRINTER / PLOTTER TO ANALYZER OR INSTRUMENT
,- 4,,, g ' Current linkage = 0 if Printer / Plotter (1) - - - - - - - - - - - -
is not linked.
(2} If link OK: I c4=en 1 (3} If plotter is linked to another device, push space bar and answer questions displayed?
~
' O = integration marks, peak crest times '
l Mode Code , 1 = peak crest times only (default) -
2 = integration marks only
,3 = no integration marks, no peak crest times ,
[4] To return to print mode (break link between Plotter and Analyzer or Instrument:
- To change link from Analyzer to Instrument, enter 0 for Analyzer number.
5 POSITIONING' PRINTER / PLOTTER BASELINE (1} Q !'~I (2) If baseline 1ccation displayed (as percent of full scale) it. CK:
(3) If baseline location displayed is C4,rvus value (I.* *.u" s r,s) l'*l a w too 6 SETUP PROCEDURE (1) lic . I 0
(2) i 5~.(~t9. (.ss.".*',r") l a ta l (3) If Analyzer No. entered is 1 or 2, go to step 4a. If 0, go to ste3_4b__
GRAND* GULF NUCLEAR STATION CHEMISTRY INSTRUCTION 08-s-04-133 IRsvision 0 Attachment I lPage 6 of 7
SUMMARY
OF OPERATING CONVERSATIONS AND DIRECTIVES 6 SETUP PROCEDURE (conro M. w.a n. w.a (4a) iwms: (p.=,) ic i (43) r- - < n (y:- ~ ) i ri i
., i.
- n. w.a (5) (-r=3( - )ii*ot n i. ass 0
(6) I E ( l." ) le=vr.t
- 0. i (Mode Code 0=shortreport}
1 = long report , .
(7) l as tacm ) (Not requested when Analyzer no. is 0. Push Ita'"!
if no other detector is to be used; otherwise, enter next detector no. , then repeat steps 5 and 6.)
i
- n. m (8) ; sa-u .,. ;
(ww ) icmaI (s in) iema1 (Sampie no. is eun no. in eeport]
i i. m.,
gg I 1
'g * [9] : m ason ; (Prm e w ) Itat
] i. 2 (Printer No. 1 = Printer'/ Plotter]
~
(10] : aat "$*'t appears unless Analy:er is at flows and temperacures" required by method, all specified detectors and any external devices are '72ady". When all con,ditions required by Method are established at Analyzer, !=o Maave goes out and Analyzer temperatures stabilize 2 minutes. The n l a==a l at Analyzer -
, _ lights. _.
(11l Inj ect sample, push la===1 (12) (*wa==53 or i ~~a (13) When analysis end time occurs repeat steps 10 through 12 to run another sample by the same Method.
' Step 9 omitted if Printer / Plotter is only terminal on System.
ATTENUATION VALUES Value Entered Attenuation Value Entered Attenuation
-4 X16* 4 16
-3 X 8* 5 32
-2 X4* 6 64
-l X 2* 7 128 0 1 8 256
, 1 2 9 512 2 4 10 1024 3 8 11 2048
- Expansion factor
GRANIT GULF NUCLEAR STATION CHEMISTRY INSTRUCTION
. . 08-S-04-133 l Revision 0 Attachment I IPage 7 of 7
SUMMARY
OF OPERATING CONVERSATIONS AND DIRECTIVES 7 CALIBRATE CONVERSATION
- x. o.r.a x. o.s.a
(1) t =.i CAL (ru. s ) Icarta l (w.ia.e x..) I r=rt ! ({gJr) I r=re.1 i St. 33187 1 t. ISS g, g 0 = calculate response factors,'
report, do not change Modify Code 4 stored Method 1 = calculate response factors, g modify stored Method ,
t 'Run nc. is used to calculate averace response (2) , RUN NO. (a n ) I carte t factors based on current and previous runs s i. toe of standard sample.
.j 6
- A
- l oGRAND GULF NUCLEAR STATION CHEMISTRY INSTRUCTION l
o . 08-S-04-133 Revision 0 Attachment II .Page 1 of 3 SYSTEM DIRECTIVES KEY DIRECTIVE Console Aux.
Kevboard Kevboard
- 1. CONVERSATION CONTROL KEYS ENTER ESC Store the entry just made CANCEL CTRL C Abort Conversation or terminate Method modification CANCEL ENTRY ] Cancel entry REPEAT LINE ! Ignore entries just entered on line (not terminated) and accept new entries
^) NEXT LINE : Proceed to next line in Conversation; use default values for any entries net made on line just entered ACCEPT _SECTN ; Accept default values for entries 1 j
in remainder of section in Method I being generated and go to next.
section, or terminate GEN
- 2. SYSTEM INTERACTION DIRECTIVES SET UP I Set up Analyzer or Instrument to run a chromatogram (link Analyzer / Instrument to Method)
Not DISPLY SETPNT Avanacle Display setpoint for parameter designated DISPLY ACTUAL Not Display actual value for parameter Avanacle designated l
RESET R Reset Instrument or Analyzer designated to initial condttions.
All data deleted unless directive s
is preceded by DATA STOP
~
DATA STOP E Terminate acquisition of data, j save data VOID V Void Analyzer or Instrument designated (remove Analyzer or Instrument
__ _ _ _-___ w _ - A _s _-
, GRAND GUIS NUCLEAR STATION CHEMISTRY INSTRUCTION 08-S-04-133 IRavision 0 Attachment II lPage 2 of 3 SYSTEM DIRECTIVES
, KEY DIRECTIVE l
Console Aux.
Keyboard Kevboard I
- 2. SYSTEM INTERACTION DIRECTIVES (Cont'd)
For Analyzers only OVEN ["%
, Display maximum oven temperature
- 3. DIRECTIVES AFFECTING STORED INFORMATION l GEN ,
G Generate Method LIST L List Method designated CALIB C Calibrate Method designated (calculate component response factors)
~
MODIFY M Modify Method designated-
'NOR$ N -
Provide normalization report for File designated DELETE D Delete Method designated -
FILE F Erase File designated
- F *F Erase all Files in group designated..
Enter numbers of first and last Files in the group to be erased STAT S Print status report
/S /S Print System configuration status
/C /C Set clock
/T /T Print time and date REPRT A To File indicated, apply Method designated and provide report
- 4. PLOTTER CONTROL KEYS ATTN ( ) Not Display attenuation. To modify Available Value displayed, enter new Value, push ENTER
,GRAN3 GULF NUCLEAR STATION CHEMISTRY INSTRUCTION
- 08-S-04-133 Revision 0 1 Attachment II Page3of3l SYSTEM DIRECTIVES KEY DIRECTIVE Console Aux.
Keyboard Keyboard t
_4_ . PLOTTER CONTROL KEYS (Cont'd) I I
ATTN t or + Not Increase (t) or decr ease- ( + )_ ____ __ j i
Avanabla attenuation by'a factor of 2 CHART Not Display chart speed. To modify Avanable value displayed, enter new value, push ENTER PPR FD
- Na Feed chart paper 8 inches or Availabl*
until CANCEL is pushed I
PLOT Not Available Link Plotter to the Instrument or Analyzer / detector designated PRINT ACTUAL Not Print actual values of Analyzer Avanable Control parameters when Analyzer
,. is ' Ready', setpoints for Instrument.
. During run, print elapsed time, attenuation, oven temperature for Analyzer -
g Not Position Plotter baseline at Avanable designated % of full scale.
- 5. CONSOLE DIAGNOSTICS Not Avanable Put Printer / Plotter in local mode. Keyboard / printer behave as typewriter
- A Not Illuminate backlighted display Available legends in sequence in groups
- of eight. All Analyzers, Instruments, must be voided, peak Files idle)
.)
I
_ - - - - - - - - - - - - -