Document B5yOmbjdyxD5rwp830Y42Va28
ANALYTICAL PROCEDURES FOR PER/TRI PLANT LABORATORY
1. Test
Moisture Test (Cloud Point Method)
2. Samples
No. S-l Mixed Organic No. S-2 Recycle Tank No. S-3 DH Reflux No. S-4 DH Bottoms No. S-5 Dopp Condenser No. S-6 Heavies Reflux No. S-7 Per Reflux No. S-8 Per/Tri Reflux No. S*9 Tri Reflux Before No. S-10 Tri Reflux After No. S-ll Topping Reflux No. S-12 Dried Per No. S-13 Dried Tri
3. Apparatus and Reagents
a. Isopropyl Alcohol b. Dry Ice c. Thermometer, -36*C to 54*C, 0.2*C Divisions
4. Procedure
a. Place about 20 mL of sample in a clean, dry test tube and imme* diately stopper with a cork containing a thermometer. The thermometer bulb should reach within 1/4 inch of the bottom of the test tube.
b. The test tube should be cooled down until a cloud first appears in sample. It should then be wanned up and cooled down once or twice more to the cloud point to make the end point more defined.
5. Repppt
Temperature of initial cloud formation unless it is below -15*C. If the cloud point is below -15*C, report less than -15*C.
5/87 SL 020726
CON* to
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2
OPERATION OF MITSUBISHI MOISTURE METER MODEL CA-05
CONFIDENTIAL*
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1. Turn power switch on left side of instrument to the ON positioJJ?'
2. Move Speed Adjust control to on stirrer.
3. If titration speed (on left side of the display) indicates a negative number, inject 1/4 mL of the check solution or 1 ml of a sample and depress the titration button. The titration will begin indicating WAIT. After it has corrected the negative number, an electronic buzzer will sound and the display will display "END". After this, depress the CL button and you are now ready to go to-step 4.
4. At this point, depress the Sample button and then the ENT button until a V appears on the display. Then on the keyboard enter the size sample you intend to use (1 mL) and depress ENT again. This will cause to come up on the display which stands for specific gravity. Enter the desired specific gravity on the keyboard and depress ENT again. At this
point depress the SL button and display will indicate RDY.
Titration of Sample:
1. Rinse the syringe supplied with sample 4-5 times before drawing up the proper amount of sample to be injected into the titration flask.
2. Before injecting the sample into the titration flask, make sure the RDY is displayed on the display. If so, depress the Start button and "Add Sample" will come up on the display. At this point inject the sample into the titration flask. It will automatically start to count out the pg of HgO. When the buzzer sounds, it will display pg of H-O and also print out ppm H^O.
Changing Solutions:
1. Changing C Solution:
a. Move speed control (#8) to zero and allow stirring bar (#7) to come to a complete stop.
b. Remove drying tube (#1) from cathode solution cell (#3). Using a Dropper Pipette draw out all of the solution in the cathode solution cell (#3).
c. Using a funnel inserted into the hole for the drying tube (#1) on the cathode solution cell (#3), pour the contents of one ampule of Aouamlcron C.
d. Replace drying tube (#1) back into cathode solution cell. (Make sure drying tube has fresh Prlerite in it.)
e. Move speed control knob on stirrer back to 6 on scale. f. Depress titration button. The titration will begin indicating Walt.
After it has dried out the new solution, the buzzer will sound and
3
2. Changing A Solution:
a. Move speed control (#8) to zero and allow stirring bar (#7) to cone to complete stop.
b. Open drain port (#6) and allow all of the solution to drain out. c. Close drain port (#6). d. Remove blind plug (#10) from top of titration cell assembly (#4).
Using a funnel, add all of the contents from a Generator Solution A (Anode) bottle to the titration cell assembly (#4) and replace the blind plug (#10). e. Be sure to keep fresh Drierlte in drying tube #2. f. Move speed control knob on stirrer back to 6 on scale. g. Depress the titration button. The titration will begin indicating Wait. After it has dried out the new solution, the buzzer will sound and the display will display END. After this depress the button and you are now ready to go to step 1 of "Titration of Sample".
Troubleshooting:
1. Open detector indicated.
a. Unplug and plug back pis Jacks (11,12).
b. Turn power off and back on at Power Switch.
c. Depress formula key
then depress 2 on the keyboard and then
enter. (This will clear out any error in the calculation formula.)
d. Depress formula key (F) again, then depress on the keyboard and
then enter. (The correct formula is now in the instrument.)
e. Depress print key, then depress 3 on the keyboard and then enter.
f. You are now ready to go to step of starting conditions.
2. No end point or stops titrating. a. Change solutions and as described in "Changing Solutions".
5/87 SL 020728
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Fig. 3 Cell Cnit
1-drying tube 2-drylng tude 3-cathode solution cell 4- titration cell assembly 5-sample injection port 6- drain port 7- stirring bar 8- speed control 1 for stirrer 9- electrode 10-blind plug
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SL 020729
SPECIFIC GRAVITY FOR HjO TITRATIONS
Sample
TBL
NPL
BLM
DME
EC
VCM
VDCM
EDC
Furnace Feed
MC -314
-324
-343
-348
-366
-368 PER -232
-208
-229
TRI
-230 -113
-127
-138 -143
-145
MeCl
-147
Unsyftetrical
Mix
DOL/SBL/DOX NRE/MC 366/208 366/230 Dowtherm
Heavies Still Bottoms
Specific Gravity
0.781 0.806 0.831 0.861 0.924 0.969 - 1.212 1.262 1.262 1.326 1.310 1.326 1.308 1.310 1.320 1.625 1.625 1.625 1.625 1.468 1.468 1.462 1.465 1.465 1.460 1.321 1.5536
0.930 1.124 1.385 1.460 1.022 1.330
5
5/87 SL 020730
t1eTcIAtLiv: e Order ' nt Cou
6
ANALYTICAL PROCEDURE FOR PER/TRI PLANT LABORATORY
1. Xe&t
pH of Dried Unstabilized Per
2. Sample
No. S-l Dried Unstabilized Per
3. Apparatus and Reagents
a. pH meter with electrode assembly b. 0.01 fi Sodium Hydroxide (approximately) c. 0.01 U Hydrochloric Acid (approximately) d. Neutral Distilled Water (pH * 7.0)
A. Procedure
a. Adjust pH of about 50 mL of neutral water to 7.0. (Note D) b. Measure 100 mL of sample into a 250-mL separatory funnel. Add 25 mL
of neutral water. Shake for two (2> minutes venting as required. c. Allow phases to separate and discard organic phase. d. Drain aqueous layer into a 150-mL beaker, place on stirrer and allow
water phase to stir for 30 seconds with electrode in solution and meter on before taking reading.
5. Report
Report pH of sample as read from meter.
6. Notes
a. Check standardization of pH meter once each shift. Use pH 7.0 buffer. The buffer should be changed each day, but it is not normally necessary to change it each time the meter is checked. Keep buffer in a tightly stoppered bottle.
b. Always keep pH electrodes in distilled water when meter is not being used.
c. Always keep saturated KC1 solution in the calomel electrode. Do not cover hole with rubber band.
d. Use fresh Neutral HgO each time a set of samples are run, and adjust pH of neutral H-0 just before using. There should be a slow drift through 7.0. Tnis drift should not be less than 10-15 seconds per 0.1 pH reading.
5/87
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SL 020731
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The pH instrument should be buffered once a shift.
1. Check and make sure the temperature is set at 25 degrees centigrade.
2. Buffer instrument with buffer 7 first. Then check with buffer 4 and buffer 10. A reading of 4.2 or lower and 9.8 or higher should be observed. If not, check (and fill if necessary) the KC1 solution in the reference electrode. If there is still a problem, check for crystals (which may be interfering) in the reference electrode. At this point an instrument person should be contacted to insure proper cleaning and refilling of electrode.
ANY TIME ELECTRODES ARE REMOVED FROM LIQUID, THE METER SHOULD BE IN THE STANDBY POSITION.
Keep the meter in the standby position when not in use.
Do not leave the electrodes immersed in the sample.
Keep the electrodes in clean distilled water when not in use.
It is very important to fallow the jab breakdown as written. (Shake the proper length of time, take a reading after 30 seconds, ect.) No exceptions.
Do not neutralize large quantities of "neutral" water and let sit. "Neutral" water should be neutralized just prior to use.
There should be a good response when .01 N NaOh is added to neutralize the "neutral" water. This means there should be noticable needle deflection. No more than a couple of drops (2-4) of .01 N NaOh should be needed to neutralize a volume of 100 mis. of water. If more is needed, the dropper bottle should be emptied, rinsed with distilled water, and filled with fresh .01 N NaOh. If there is still poor response, the "neutral" water is suspect and should be changed out.
FILENttMEi pHprob SL 020732
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7
ANALYTICAL.. ERQCEPURE FOR -EERZTRL, PLANT LABORATORY
1. last
pH of Dried Unstabilized Tri
2. gamble
No. S-l Dried Unstabilized Per
3. Apparatus and Reagents
a. pH meter with electrode assembly b. 0.01 J} Sodium Hydroxide (approximately) c. 0.01 fi Hydrochloric Acid (approximately) d. Neutral Distilled Water (pH - 7.0)
4. Procedure
a. Measure 75 mL of neutral water into a 250-mL beaker and adjust pH to 7.0 (Note D).
b. Raise electrodes and pipette 25 mL of sample into beaker and mix well with stirrer for one minute.
c. Slow stirrer and allow phases to separate. d. Lower electrodes into aqueous_phase but not into organic phase. e. Wait a few seconds and switch meter to proper range and read pH.
5. Report
Report pH of sample as read from meter.
6. Notes
a. Check standardization of pH meter once each shift. Use pH 7.0 buffer. The buffer should be changed each day, but it is not normally necessary to change it each time the meter is checked. Keep buffer in a tightly stoppered bottle.
b. Always keep pH electrodes in distilled water when meter is not being used.
c. Always keep saturated KC1 solution in the calomel electrode. Do not cover hole with rubber band.
d. Use fresh Neutral HgO each time a set of samples are run, and adjust pH of neutral H_0 just before using. There should be a slow drift through 7.0. This drift should not be less than 10-15 seconds per 0.1 pH reading.
5/87
CONFIDENTIAL! Subject it? Protective Order of 14th Judicial District Court
No. 9.1 -1145
SL 020733
8
ANALYTICAL,PROCEDURE FOR PER/TRI PLANT LABORATORY
1. Te
Bromothymol Blue Test for Acidic Impurities
2. Samples
No. S-l Dried Per No. S*2 Tri Before Dryer
3. Apparatus and Reagents
a. 35-mL glass vials with plastic polyseal caps b. Bromothymol blue indicator solution
4. Procedure
a. Pipette 10 mL of sample into a clean glass vial containing 10 mL of the bromothymol blue solution.
b. Cap with the plastic cap and shake vigorously. c. Allow phases to separate. d. Compare the color of the aqueous (top) phase to the color standards.
5. Report
Sample Color
yellow - pH below 6.0; increase ammonia addition green - pH between 6.0 and 7.5 blue - pH greater than 7.5; decrease ammonia addition
6. Notes
a. The bromothymol blue indicator solution must remain green when placed in the empty glass vial. A change of color could indicate dirty glassware.
b. Any sample color in the green range (chartreuse through blue-green) indicates a good sample and no change is needed in the neutralizer.
5/87 SL 020734
COWFWBWTI^ order
Subject "
COOrt
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91-U45
M. ANALYTICAL CONTROL TEST
1. Test
Color of Product
2. Samples
a. Dry Per b. Dry Tri c. 1 Per Bottoms d. 2 Per Bottoms
3. Apparatus andJReagents
a. Hellige Aqua Tester b. Nessler Tube with Plunger c. Hellige Color Discs
4. Procedure
a. Fill one Nessler tube to mark with distilled water. b. Fill one Nessler tube to mark with sample. c. Place sample in the right position of comparator and distilled water
in left position of comparator.. d. Insert plunger in each tube, e. Rotate disc until color intensity matches. f. Record the APHA color of sample.
5/87
SL 020735
MCLANALYTICAL CONTROL TEST
1. lS
Sodium Iodide Test
2. Sample
No. S-l Dried Unstabilized Per No. S-2 Dried Unstabilized Tri
3. Apparatus and Reagents
a. 2.5% Sodium Iodide in Acetone b. 0.01 U Sodium Thiosulfate c. Acetic Acid
4. Procedure
a. Measure 50 mL of sample and pour into a 250-mL flask. Add 40 mL of
2.5% sodium iodide-acetone solution and 4 drops of acetic acid.
b. Loosely stopper and place in dark for 30 minutes.
c. At the end of 30 minutes observe for any yellow color formation. Add
50 mL of ice water to sample with color and place on magnetic
stirrer.
d. Titrate colored sample with 0:01 JJ Na-s-O*. The disappearance of all
color is the end point.
1
5. Calculations
a. ppm Perchlor-Oxide - T x N x 0.0491 x 10^ 50 x 1.62
- T x N x 1123.4
- T x 11.23
b. ppm Trichlor-Oxide - T x N x 0.0291 x 106 50 x 1.46
- T x N x 672.3
6. Typical Results
- T x 6.723
No Color Formation
5/87 SL 020736
jet 14th ot
91-
11
ANALYTICAL PROCEDURE FOR PER/TRI PLANT LABORATORY
1. Test
Iron Determination
2. Samples
a. Heavy Still Bottoms b. Still Bottoms c. Heavy Still Feed d. Heavy Still Reflux
3. Apparatus and Reagents
a. pH meter b. PC-600 c. 60-mL Separatory Funnel d. Filter Paper Whatman No. 541 e. 520 mm filter f. 0.03% ortho-phenanthroline (water matrix) g. 5% hydroxlamine hydrochloride (water matrix) h. 1:1 Solution of HC1 i. 6 N Solution of NH4.OH
4. Procedure
a. In a hood, pipet 25 mL of hydroxlamine hydrochloride into a 60-mL separatory funnel.
b. Pipet the appropriate sample size into the 60-mL separatory funnel also. (Note 2)
c. Shake separatory funnel vigorously for 3 minutes to extract the iron from the sample. (3 minutes)
d. Filter sample mixture through a No. 541 filter paper (that has been moistened with distilled water).
e. Dilute sample to 50 mL and adjust pH to 3 if necessary. f. Add 5 mL of ortho-phenanthroline to solution. g. Dilute to 80 mL and adjust pH again to 3.3-3.7 with either 1:1 HCl or
1:1 NH40H. h. Pour solution into a 100-mL volumetric and bring to volume with
distilled water. i. Let stand for 15 minutes. j. Blank PC-600 with a reagent blank. k. Place probe into sample, take reading and record.
CfllCdUtjpn
Look up ppm FeClj on chart provided with electrophotometer (Note 3)
5/87
Su
coW ote<**-v<! J? court SL 020737
12
Iron Determination (Continued) NOTES
1. Blank: make blank same as the sample only do not use sample. 2. Sample Size
pom FeCl3 Ejmec.te.d_ in Sample
Sample Volume (mL) to Use
2 ppm
10 mL
2-15 ppm
5 mL
5-50 ppm
2 mL
10-70 ppm
1 mL
20-150 ppm
0.5 mL
100-1000 ppm
0.1 mL
3. If FeCl^ exceeds limits on chart. rerun sample using a smaller aliquot.
5/87 SL 020738
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)
ABSORBANCE READING
0.01 0.02 0.03 0.04 0.05 0.06 0.07 0.08 0.09 0.10 0.11 0.12 0.13 0.14 0.15 0.16 0.17 0.18 0.19 0.20 0.21 0.22 0.23 0.24 0.25 0.26 0.27 0.2 0.29 0.30
SAMPLE SIZE 0.1 0.2
, 0.3 0.4 0.5 1.0 2.0 5. 0
BRINKMAN PC/600 CHART FOR FECL3
25 ML HYDROXYLAMINE HCL 5 ML 0 - PHENANTHR'OL INE
MG FE
1 3 4 6 7 9 10 11 13 16 16 17 19 20 21 23 24 26 27 29 30 31 33 34 36 37 39 40 41 43
ABSORBANCE READING
0.31 0.32 0.33 0.34 0.35 0.36 0.37 0.38 0.39 0.40 0.41 0.42 0.43 0.44 0.45 0.46 0.47 0.48 0.49 0.50 0.51 0.52 0.53 0.54 0.55 0.56 0.57 0.58 0.59 0.60
FACTOR X MG FE = PPM FECL3
FACTOR 18.125 9. 063 6. 042 4.531 3.625 1.813 0.9063 0.3625
MG FE
44 46 47 49 50 51 53 54 56 57 59 60 61 63 64 66 67 69 70 72 73 74 76 77 79 so 82 83 84 86
ABSORBANCE
MG FE
READING
5.0 ML
0. 5 ML
1
0.36
3.63
3
1.08
10.88
4
1.45
14. 50
6
2. 17
21.75
7
2.53
25. 38
9
3.26
32.63
10
3.62
36.25
11
3.99
39.88
13
4.71
47. 13
16
5.80
58. 00
17
6. 16
61.63
19
6.89
68 88
20
7.25
72.50
21
7.61
76. 13
23
8.34
83.38
24
8.70
87. 00
26
9.43
94.25
27
9. 79
97.88
29
10.51
105.13
30
1 0.88
108.75
31
11.24
112.38
33
11.96
119.63
34
12. 33
123.25
36
13. 05
130.50
37
13.41
134.13
39
14. 14
141.38
40
14.50
145.00
41
14.86
148.63
43
15.59
155.88
ABSORBANCE READING
44 46 47 49 50 51 53 54 56 57 59 60 61 63 64 66 67 69 70 72 73 74 76 77 79 80 82 83 34 36
MG FE 5.0 ML 0,.5 ML
15.95 16.68 17. 04 17.76 IS. 13 18.49 19.21 19.58 20.30 20.66 21.39 21.75 22.11 22.84 23.20 23.93 24.29 25.01 25.38 26.10 26.46 26.83 27.55 27.91 28.64 29.00 29.73 30.09 30.45 31.18
159.50 166.75 170.38 177.63 181.25 184.38 192.13 195.75 203.00 206.63 213.88 217.50 221.13 228.38 232.00 239.25 242.38 250.13 253.75 261.00 264.63 268.25 275.50 279.13 236.38 290.00 297.25 300.88 304.50 311.75
SL 020740
13
ANALYTICAL PROCEDURE FOR PER/TRI PLANT LABORATORY
BEfflQS.A=LC.-ll
1. Ips_E
Dew Point Using Alnor Dew Pointer
2. Sample:
Plant Air
3. Apparatus:
Alnor Dew Pointer with dew point calculator
4. Procedure
a. Purge out sample line by opening sample valve to allow an air flow. b. Open instrument case. Pull out operating valve handle; open purging
valve; turn switch to battery position. c. Connect sample line to inlet connection and purge instrument with
plant air. Let purge under pressure for one minutes. Operate pump at last 5 times. d. Close purging valve. Operate pump until pressure ratio gauge read about 0.3. Press operating valve handle and then pull out. Open purging valve. Repeat this step at least 4 times. e. Disconnect sample line or complete close sample valve. f. With the index finger tip, depress the gauge valve. Wile the gauge is depressed, turn the unit adjuster to bring the bottom of the meniscus even with the 1 mark on the gauge. Release the gauge valve. g. Repeat Steps B, C and D.
h. Pump up sample to a pressure ratio of about 0.45; make test as in Step D. Look into the observation window as the operating valve handle is pushed in. Not whether a cloud is formed. If not, repeat this procedure by going to successively lower pressure ratios (0.45, 0.44, 0.43 ... 0.38, 0.37, 0.36 ... 0.33, 0.32, 0.31) each time a fog or cloud is noticed. Repeat at the same pressure ratio. If fog repeats, this is the end point. If not, continue until the end point is reached.
i. Read thermometer. j. Set arrow number 2 on dew point calculator opposite the end point
pressure ratio on Scale D. Find the thermometer temperature on Scale F. Read dew point on Scale E opposite thermometer temperature on Scale F. k. Leave a small purge on sample line.
5. Report:
Dew point temperature from dew point calculator
6. Plant air dew point of 40@F.
NOTE: Step j is to be used only when running dew points on plant air. Check with the Laboratory when other samples are to be run.
7. Change glass wool in Dew-Pointer filter weekly. V
5/87
of
l- Cout
SL 020741
14
ANALYTICAL EROCEDURE FOR PER/TRI PLANT LABORATORY METHOD A-LC-11
1. Test
Determination of Specific Gravity by Hydrometer
2. Saipplg
Refrigerated Brine
3. Interferences
Insoluble materials and suspended air bubbles
4. Apparatus
a. Hydrometer, 1.200*1.400 Specific Gravity b. Thermometer, -40* to 120*F
5. Procedure
a. Fill graduate with sample, being careful not to entrain air and form bubbles.
b. Place hydrometer in sample slowly. Do not allow hydrometer to sink much below the final reading. Read at the highest point the liquid comes on the hydrometer.
c. Measure temperature of sample. Leave thermometer in sample at least one minute.
6. Calculations
a. Determine the temperature correction for the sample from the correction table.
b. Determine the freezing point from the table using the corrected specific gravity.
c. Report corrected specific gravity and freezing point of sample.
7. Typical Results
Specific Gravity - 1.280*1.300
5/87 SL 020742
COWFIDEHTIAT*1 Order Sublet torroteetvw ct Court o* !*
Hydrometer Efigdlng
1.200 1.210 1.220 1.230 U!40 1.250 1.260 1.270 1.280
1A9Q 1.300 1.310 1.320 1.330 I,34p 1.350 1.360 1.370 1.380
1.32P 1.400
UOQ
ANALYTICAL PROCEDURE FOR PER/TRI PLANT LABORATORY Temnerature Corrections for Specific Gravity of Refrigerated Brine (Calcium Chloride^
Corrections to be applied to hydrometer readings of calcium
chloride solutions at various temperatures, using a hydrometer calibrated at 60*F/60*F
OIL--IQ1F .011 .010
.012 .011
20*F 39* F -40* F .50* F .009 .007 .005 .003
.009 .007 .005 .003
.012 .011 .009 .007 .005 .003
.013 .011 .009 .007 .005 .003
AL3.013 .012
.014 .012
.009 .010 .010
,997 .008
.008
.005 .003 .005 ~ .003 .005 .003
.014 .012 .010 .008 .005 .003
.015 .013 .010 .008 .006 .003
.015 .016 .016 .017
.013 .014 .014 .014
^011 .011
.011 .012
.012
.008 .008 .009 .009 .009
.006 .006 .006 .006 .006
.003 .003 .003 .003 .003
JU2_--lG15__ .012 ,099 .006 .003 .018 .015 .012 .009 .006 .003
.013 .009 .006 .004
.010 .007 .004
.007 .004
.004
60*F N 0
C 0 R R E C T I 0 N S
70*F .002 .002 .002 .002 .002 .003 .003 .003 .003 .003 .003 .003 .003 .003 .003 .003 .003 .003 .003 .004
80*F .004 .005 .005 .005 .005 .005 .005 .005 .005 .006 .006 .006 .006 .006 .006 .006 .006 .006 .007 .007
90* F 100*F
.007 .009 .007 .010 .007 .010 .007 .010 .008 .010 .008 .010 .008 .011 .008 .011 .008 .011 .008 .011 .009 .011 .009 .012 .009 .012 .009 .012 .009 .012 .009 .012 .010 .013 .010 .013 .010 .013 .010 .013
.004
.004 .007 .010 .013
.004 .007
Temperatures below 60*F Observed Hydrometer Reading MINUS Temperature Correction - Specific Gravity
Temperatures above 60*F
at 60*/60*F
Observed Hydrometer Reading PLUS Temperature Correction - Specific Gravity
------------------------- ---------------------------------------------------------- ---------------------------------- at 60*760*F
FREEZING POINTS OF REFRIGERATED BRINE
1.20 1.21 1.22 1.23 1.24 1.25 1.26 1.27 1.28 1.29 1.30 1.31
5/87
_2_ A.
-6 -7 8 -9 -9
-10 -11 -12 -12 -13
-14 -15 -15 -16 -17
-17 -18 -19 -20 -21
-22 -23 -24 -24 -25
-26 -27 -28 -29 -30
-31 -32 -33 -34 -35
-37 -38 -40 -42 -43
-45 -47 -49 -52 -55
-60 -56 -52 -48 -45
-42 -28
-40
-38, ., .
-35
-,r. KT ! t'*v 1 !^ I-1"-' "
" ,
.
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order
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SL 020743
ANALYTICAL PROCEDURE FOR PER/TRI PLANT LABORATORY
1. Test Determination of HC1 in Vent Gas
2. Sample Reactor Condenser Vent
3. Apparatus and Reagents a. Gas burette, 100 mL b. Confining solution
4. Procedure a. Put about 200 mL of confining solution in leveling bottle. Change confining solution once per week. b. Fill connecting tube by running a small amount of confining solution into burette. c. Connect burette to sample line. Purge at least 5 minutes. d. Close burette stopcocks and sample valve so as to leave a slight pressure in burette. Disconnect from sample line, and allow burette to come to room temperature. e. Equalize sample in burette to atmospheric pressure by rotating stopcock. f. Allow confining solution to enter burette and absorb the HC1. After absorption has taken place, read the amount of HC1 absorbed directly from gas burette.
5. Report % HCl absorbed by confining solution
5/87 SL 020744
17
ANALYTICAL PROCEDURE FOR PER/TRI PLANT LABORATORY
1. Test
Determination of % HC1
2. Sample
HC1 Absorber Bottoms
3. Reagents and Apparatus
a. 2.74 N Sodium Carbonate b. Xylene cyanole indicator c. 20-mL pipette d. 250-mL beaker
4. Procedure
a. Pipette 20 mL of sample into a 250 mL beaker. b. Add 50 mL of distilled HgO and 4 drops of xylene cyanole. c. Titrate with 2.74 N sodium carbonate to a steel blue end point and
record titer.
5. Calculations
20 L - T-
* 10 . , ,,d
or Titer x 0.50 - % HC1
5/87
i.. vG Protect! Sub 3^ of i4tVi wo.
ordGr court
SL 020745
18
ANALYTICAL PROCEDURE FOR PER/TRI PLANT LABORATORY
1. Test
Determination of Alkalinity of Water 2. Sample
Steam Drum Water 3. Apparatus and_Reaeents
a. 0.02 H2S0 b. Phenolphthalein Indicator c. Methyl Orange Indicator d. 10% Barium Chloride Solution (BaClg)
4. Procedure
a. "P" and "MO" Readings
(1) Measure 100 mL of sample and pour into casserole. Add 4 drops phenolphthalein indicator.
(2) Titrate with 0.02 N H.SO, to clear end point. Record this titration as "F".
(3) Add 4 drops of methyl orange indicator. Without refilling burette, titrate with 0.02 N H,,S0, to a reddish orange end point. Record this titration as "MO".
b. Hydrate "PHT" Reading
(1) Measure 100 mL of sample and pour into casserole. Add 10 mL of 10% BaCl. solution.
(2) Let stand 20 minutes.
(3) Add 4 drops of phenolphthalein indicator and titrate with 0.02 N HjSO^ to a clear end point. Record this titration as "PHT".
5. Calculations
a. P" Reading _ T ("?") x 0.02 x 0.05 x 10 _
ppm CaO^
100
T C r ) x 1U
b. ^0" Beading I,("MQ") x 0.02 x 0.05 x 10*
ppm CaCOj
100 - T ( MO ) x 10
c. "PHT"_Jteading _ J CffHT") x 0,02 x 0,0? X 10* _ T
x lf)
ppm CaCO^
100
T * raT ' x 10
VJ
5/87 SL 020746
19
ANALYTICAL ERQgEDURE fPR FER/TRI PUNT LABORATORY
1. Ift&S
Dissolved Solids in VaCer
2. Sample
Steam Drum Vater
3- Apparatus .apd Agents
a. Nalcometer b. Fhenolphthalein Indicator c. 0.02 N Sulfuric Acid d. 600 Micromho Standard (tfalco Solution 298)
4. Standardization
Pour 600 Micromho Standard into cell on nalcometer. Turn range, set knob to 100 and press button. Meter should read 6. If it does not, remove button on bottom of nalcometer and adjust to 6.
5. Procedure
a. Measure 50 mL of sample into a beaker. b. Add two (2) drops of phenolphthalein indicator to sample.
(1) If no pink color appears, add sufficient sample to fill cell. (2) If pink color appears, add 0.02 N lUSO,, one drop at a time until
the pink color disappears) then add sufficient sample until pink color just reappears. Add to cell and proceed with step "C".
c. Set range (10, 100, or 1,000) and push button.
6. Calculation
Reading x Range - Micromho
Look up ppm dissolved solids on chart provided using your known Micromho from meter.
0,
Cryatt
S^ectDistrict
of "14th
gl-1145 t5o.
5/87
SL 020747
MICROMHO/CM TO PPM TOTAL DISSOLVED SOLIDS CONVERSION CHART
MMHO/CM
PPM TDS
/iMHO/CM
PPM TDS pMHO/CM
21 4 2.1 6 3.2 8 4.2 10 5.2
12 6.4 14 7.4 16 8.5 18 9.6 20 11.0
25 13.5 30 16.0 35 19.0 40 22.0 45 24.5 50 27.5
60 33.0 70 39.0 80 45.0 90 51.0 100 56.0
120 140 160 180 200
220 240 260 280 300
350 400 450 500 550 600
650 700 750 800 850
68 80 91 100 115
127 139 150 164 176
210 240 270 300 335 370
400 435 470 500 530
900 950 1000 1500 2000 2500 3000 3500 4000 4500 5000
5500 6000 6500 7000 7500 8000 8500 9000 9500 10000
PPM TDS
560 600 630 970 1300 1700 2000 2400 2750 3150 3500
3900 4300 4700 5000 5400 5800 6200 6600 7000 7400
* Every 50 /xMHO/CM is approximately 30 ppm TDS
5/87 SL 020748
Protective Order of 14th Judicial District Cout
No. 91-1145
analytical procedure for per/tri plant Laboratory
1. Test
Determination of Calcium and Magnesium in Water as Calcium Carbonate
2. Sample
Steam Drum Feed
3. Apparatus and Reagents
a. Versenate Solution (EDTA) 1 mL - 0.001 g CaCO,
b. Monover Indicator
3
c. Hydrochloric Acid, 1 N (HC1)
d. Methyl Red Indicator
e. Ammonium Hydroxide, 6 N (NH^OH)
4. Procedure
a. Measure 100 mL of sample into the casserole and add 200 mL of distilled water.
b. Add 1-2 drops of methyl red.
c. Titrate with 1 N HCl to the red end point and add exactly 2 mL in excess.
d. Stir gently for 30 seconds. e. Add 2 mL of 6 N NH^Oh and stir to mix.
f. Add Monover indicator until wine-red color develops. g. Titrate with standard versenate until the solution changes from
wine-red to pure blue.
5. Calculations
ppm Cl+2 and Mg+2 as CaCO- - Titer x 0.001 x 106 - Titer x 10 100
6. Typical Re$\ilt$
0 ppm
5/87
CfV tiO*
ot
iCt- *
SL 020749
22
ANALYTICAL PROCEDURE FOR PER/TRI PLANT LABORATORY
1. Test
Calcium
2. ?mnl$
Cooling Tower Water
3. Apparatus and Reagents
a. Burette, 25 mL b. Casserole, porcelain c. Cylinder, graduated, 50 mL d. Measuring dipper, brass e. Pipette, safety bulb, 2 mL f. Stirring rod, glass g. Calcium indicator h. Versenate 1 mL - 1 mg CaCo. i. Sodium hydroxide, 1.0 N
4. Procedure
a. Measure 50 mL of sample and transfer to a casserole. b. Add 2.0 mL of 1.0 N sodium hydroxide to sample and stir. c. With the brass measuring cup provided, add one (1) level measure of
calcium indicator and stir. d. Sample will turn salmon-pink if Ca is present. e*' Titrate with versenate until the color turns orchid-purple, f. Record titer and calculate ppm CaCO^.
5. Calculation
Titer x 10 - ppm CaCO^
5/87
SL 020750
ot 14 th
o. yju
order cact
23
ANALYTICAL_ PROCEDURE FOR PER/TRI PLANT LABORATORY
1. Ies_t
Determination of Sodium Sulfite in Vater
2. Sample
Steam Drum Vater
3. Apparatus and Reagents
a. Starch indicator b. 1.0 N HC1 c. 0.01587 N KI-KI03
4. Procedure
a. Cool sample to at least 70*F. b. Measure 100 mL of sample into casserole. c. Add 1 mL of starch indicator and 5 mL of 1.0 N HC1. d. Immediately titrate with 0.01587 N KI-KIO, until first permanent blue
color is obtained.
5. Calculation
Sodium Sulfite (NajSO^) ppm
ST x 0.01587 x 0.0630 x 10* - NT x 100 100
Where NT - (Sample Titer - Blank Titer)
5/87
l hi,:
ctive order istrict COUEt
SL 020751
24
ANALYTICAL PROCEDURE FOR PER/TRI PLANT LABORATORY
1-
Determination of Residual Chlorine (Cl2) 2. Sample
a. Well Water b. Cooling Tower Water 3. Apparatus and Reagents a. Wallace and Tieman Comparator b. Residual Chlorine Disc c. Ortho-tolidine 4. Procedure a. Select two clean comparator cells. Pill one to the mark with a
sample and place in right.cell space of comparator. b. Add .5 mis of 0 - tolidine.from the calibrated dropper into the -
other cell. Fill to the mark with sample. Place in left cell space. c. Immediately hold up to the light and match colors by revolving the disc. Read the value from upper left corner comparator. 5. Report Value read from comparator.
SL 020752
CONFlV.'-HNTT1I rM*: toct.ive Order
strict Court
Mo. 91--U45
ANALYTICAL PROCEDURE FOR PER/TRI PLANT LABORATORY
1. Test Determination of Ortho-Phosphate
2. Sample
Cooling Tower Water Make-up Water
3. Apparatus and Reagents
a. Amino Acid Reagent Powder Pillows (Code-2012) b. Molybdate Reagent for Phosphate (code-2044) c. Sulfuric Acid Solution, ION (Code-2033)
4. Procedure
UNFILTEREDI
)
a. Add 25 ml of sample to a 100-ml graduated cylinder with a ground glass stopper.
b. Add 1 ml of sulfuric acid solution (Code-2033) and mix. c. Add 1 ml of molybdate reagent (Code-2044) and mix. d. Add the contents of one amino acid reagent powder pillow
(Code-2012) and mix until dissolved. e. Allow 10 minutes for full color development which will be blue if
phosphate is present. Do not wait more than 15 minutes before taking the readings. f. Use an unfiltered cooling water blank to zero Sequoia - Turner spectrophotometer with a 600 nm wavelength setting. g. Place sample in instrument, take reading and look up ppm orthophosphate from chart provided.
FILTERED:
a* Filter 25.0 ml of sample through a 0.20 micron filter paper. b. Use steps a-e above.
c. Use distilled water to zero the spectrophotometer. d. Place sample in instrument, take reading and look up ppm
orthophosphate from chart provided.
of S1u4btjhecJt utdoicLi-arKlCn-eicstit.vricOt rCdeoruit
f
020753 SL
)
ORTHOPHOSPHATE 0-25 ppm as PO4
APPARATUS REQUIRED
Comparator, Taylor test tube model, complete with 0-25 ppm phosphate. as PO4, slide
Measuring Dipper, brass Mixing tube, graduated 10 and 14 ml Millipore filter paper 50 cc syringe and filter paper holder
code 401 113 170
CHEMICALS REQUIRED
Molybdate Reagent Stannous Reagent, dry
PROCEDURE FOR TEST
code 236 239
Filt red Phosphate The temperature of the sample should be in the range of 70-100 F. sample through the millipore filter paper, using the 50 cc syringe.
Filter the
Using the mixing tube graduated at 10 and 14 ml, fill the tube to the first mark (10 ml) with the filtered sample. Add molybdate to the second mark (14 ml). Stopper and mix well. Add one (1) level measure of stannous reagent. Again stopper and mix well. A blue color develops, the intensity of which is proportional to the phosphate present.
Place the mixing tube in the middle compartment in the base. Fill the two test tubes on either side with filtered sample. With the color slide on the base, hold the in strument toward a source of daylight and move the slide in front of the test sample until a color match is obtained. Read the phosphate value within one (1) minute.
CALCULATIO N O F RESULTS
When a match is obtained, the phosphate in parts per million as PO4 is read directly from the color standard slide.
Unfilt red Phosphate Same as above, deleting the filtering step.
SL 020754
Subject
Of 14th J
Cooling Water Test for - Phosphate
Unfiltered
1. Pour 25.0 ml of sample into a 50 ml mixing graduate.
2. Add 1 ml 10N H2S04 and swirl to mix (1 dropper full).
3. Add 1 ml of molybdate reagent for phosphate using the calibrated dropper (1 dropper full) .
4. Add 1 amino acid reagent powder pillow, mix well.
5. Read after 10 minutes but wait no longer than 15 minutes at 660 nm.
6. Using unfiltered cooling water zero the spectrophotometer.
7. Read the absorbence of the developed sample and convert obsorbance to ppm phosphate using the chart provided by the PPG Laboratory personnel.
Filtered
1. Filter 25.0 ml of sample through a .22 micron filter paper.
2. Use steps 1-5 above.
3. Use distilled water to zero the spectrophotometer.
4. Read the absorbence of the developed sample. Convert absorbence to ppm phosphate using the chart provided by PPG Laboratory personnel.
Control Filtered Phosphate Unfiltered Phosphate - Filtered
Phosphate
15 - 20 ppm less than 3
Cooling Water Test for - Betz 2020
1. Pour 50 ml of sample into a 50 ml mixing graduate.
.2 Add 5 ml of Polymer Buffer and swirl to mix.
3. Set wavelength drive to 420 and zero the spectrophotometer with this solution.
4. Add 1 ml of Polymer Reagent and stir for 5 seconds EXACTLY.
5.
Absorbence
x
120 = ppm
2020. S?*??
^1 Judicial
D...it si1t1vr/e0icotroco*urt
of 11'4tn " No. 91-U43 SL 020755
\
ANALYTICAL PROCEDURE FOR- PER/TRI PLANT LABORATORY
26
r \
1. Test
BETZ 2020
2. Sample
Cooling Tower Water Make-up Water
3. Apparatus and Reagents
a. Spectrophotometer b. Beaker, 150 ml c. Cylinder, graduated, 50 ml d. Pipette, 1 ml e. Pipette, 5 ml f. Stirring Rod g. Polymer Buffer, Code 1254 (pints) h. Polymer Reagent, Code 1253 (pints)
4. Procedure
a. Using to 50-ml graduate, measure 50 ml of sample into a 150-ml beaker.
b. Add 5 ml of Polymer Buffer by pipette and stir for 10 seconds. c. Use a wavelength setting of 420 nm for the Sequoia-Turner
Spectrophotometer. d. Fill sample cell with water solution and use to set photometer to
zero absorbance. e. Pour solution back into beaker. f. Add 1 ml of polymer reagent by pipette and start timing
simultaneously. Stir solution for 30 seconds. g. Then set timer for 4 1/2 minutes. After 4 1/2 minutes, transfer
solution to sample cell and read absorbance. Note that total lapsed time of solution since polymer reagent addition should b exactly 5 minutes before taking reading.
5. Calculation of Results
Determine Betz 2020 treatment concentration in ppm 2020 from calibration curve.
CCWWEHTTM.: l to Protect'-ve Order
subjec Sudiciel oi.trrot Court of 14th Wo. 9l~U4
SL 020756
27
ANALYTICAL PROCEDURE FOR PER/TRI PLANT LABORATORY
1. Test pH
2. Sample Cooling Tower Uacer
3. Ap,pamvs,j?nd Rgpgentg
a. pH meter with Calomel and glass electrodes b. Buffer solution (pH 7.0)
* ProgyflMrs
a. Standardize pH meter with buffer solution. b. Rinse electrodes thoroughly with the sample. c. Read pH of the sample on a portion sufficient to cover the tips of
the electrodes. 5. Report
Direct reading for pH meter
f
5/87
tec^ SuMy-*1*utaojcio91i -V. *"i-a455 of
Court.
SL 020757