Document dQq7E18bw40DojVxyrkRrdqEb

OATS IMUKO <t*K Monsanto Chemical Company W/' W. 0. KRUMMRICH PLANT LABORATORY jVHITTIR V' STANDARD ANALYTICAL METHOD aTTOnCInTT Lkodvct Arooloro, Pyrunola and Related Products? l>II |NUMBER ' OF - T ------------ 1JLFFB0P1STBT-------------- ;.'C7 Dielectric Constant und Power Factor' this com* P? 1 lUPtmiDEI METHOO 1160B | | revises instruction^ > IMUCO on l/fl/GC soon: mil. method lo uoed to noara/C' the dielectric oonataht and pewr-t I'uctOi- 01 dielectric fluids. " sq^xmay u. fee Page 2 for tho equipment Hot end connecting diagram. b The GE test cell 1 det'oribod as below. toot clectrodcr., concentric tileIce1 cylinders with .c.jet. In-, inner' electrode le 2.U': O.D. x 3-26" high. The outer eleotiode 1.3 >.0" l.D. 3.2b" high. General Electric Ot Pittsfield. Marie., Cot. No. 1,!j!,9,6G3, Drawing Mo. K-GtiBY'i. ' Spacer plate. Oeneral Electric Co., Drawing No. l4-Ool?r4-2... HOC ml. l>e..or Set the spacer plate In the bculco" with the concentric : lngo up. Set too concentric cylinders in the appropriate! rlngB. o. Oven, constant temperature. Fisher Jr. Cat. No. 13'2Gi-i:s, modified t> Include couplets Inner wall lining o .- ,033s eliiudnuBi, installation of motor and blower. Vcrmratnre roiwiiis fonntrjnt to 100*C (0.h*C). ' Hie even is also provided with General Radio Co. type 936 binding p:?>ta and Insula tors arranged to mutch terminals l'roii. tho oapacitanco and I'oslotivlfcy bridges. The ovun is mounted directly t' tlie aide of the cabinet containing the ;apacita :c: end power factor' apparatus. This pc tail ts short, direct connoctio.'u. Terminals and leads are inside Ucove.t lor connocfiiV! to the test cell. a. A 160 wet: heater Vo ot fcaohoO to tho underside of the Capacitans* nritlcc oh I eld to hold temperature aoout 20* C above ambient. Required to hold relative hrrG.dlty oeiev; kotf. MOWS 076954 -2\ Balance Capacitor - General ... Radio 1409F Oaclllator - General Radio 1302-A Bridge - Oeneral Radio 716-C Null Detector - Oeneral Radio 12J2-AJ Null Detector 60 Hz. Supply In out Oaollloacope - EICO 427 60 Ka Supply - 40 voltB R.M.S. with 3rd Harmonic Supprea-j elon Cell - Q.E. # 1,559.663 Oven - Modified Fisher iBotemp No. 13-245 Oscillo scope jr- leads for ,, Resistivity f Gen. Unknown Substitution _______ LI Det. Unknown Direct[* Cell Bridge Balance Capacitor Oven Oscillator - 1000 Hz ELECTRICAL PROPERTY APPARATUS MCNS 076955 Product: Aroclors, Py rands and Related Products Test: Dielectric Constant and Power Factor Methid No. T-B245 Page 3 of 10 pages e. The remaining units are UBed aa received after Interconnection as shown on page 2. f. Thermometer, -1 t6 101C., 0.1 division, 610 nmi, Fisher Cat. No. 15-000, or equivalent. REAGENTS a. Trl Sodium Phosphate, 10$ solution, Trl Sodium Phosphate, AP. Grade or equivalent. Hake the 10$ solution Immediately prior to uae. b. Trichlorobenzene, Commercial Grade. c. Methanol, 99.9+$ Pure, Carbon and Carbide Co., or equivalent. d. Benzene - ACS grade. SAFETY Chlorinated benzenes and diphenyl are Irritating to the skin. The vapors of the hot materials are irritating to the eyes and upper respiratory system. If aocldental contact is made with the eyes, flush Immediately with a large amount of water for at least 15 minutes and get immediate medical attention* Wash other affected areas with soap and water. Benzene and methanol are flammable. The voltages used In the determination of power factor and dielectric constant are low and present no unusual shook hazard. If It is neoesBary to open cabinet or remove any component, the line plug must be removed. Moot measurements are made at 100C. Therefore, gloves should be worn when making connections to the test cells when they are In the oven. DETERMINATION 1. Adjustment of Controls on Eleotrlcal Apparatus A. On Panel No. 1 (Top Panel, Amplifier and Null Detector) 1. Turn the 4-way (main power) switch on the upper right hand side to the 1000 position to determine the Dielectric Constant and power factor at .1000 Hz (cycles). Turn this switch to the 60 position for measurements at 60 Hz (cycles). 2. Allow the equipment to warm up fcr t'.t leeist 10 minutes. HONS 076956 Product: Arc-clors, Pyranols and Related Products Test: Dielectric Constant and Fever I'&ctor Method No. Page 4 of K- pfige J>. Turn the gain control to the middle of the red area. 4. Turn the toggle switch to LOO position. 5. For 60 Hz (cycle) measurements, turn the filter frequency knob to 20-200 C position and then adjust the filter tuning dial for a maximum meter reading. This will be very close to a dial reading of 6. For 1000 Hz (cycle) measurements, turn the filter frequency knob to the 200C-2KC position. Then edJuBt the filter tuning dial for a maximum taster reading, litis will be very close to a dial reading of 10. D. On Panel No. 2 (Oscilloscope) CAUTION: Do not allow a high Intensity spot to remain stationary on the sex-sen for any length of r.ir.ie. 1. Turn "OFF PHASE" control to the 12 o'clock position (relative to the oscilloscope). 2. Turn the "MEN" control to about the 12 o'clock position (relative to the oscilloscope). NOTE: Always use the minimum trace Intensity " compat&ble with easy visibility. 3. Adjust the "FOCUS" and "ASTIO" controls for a sharp line. Use the vertical and horizontal positioning controls to center the image. A. Set the "SWEEP SELECTOR" to 10K . TOOK 5. Set the "SWEEP VERNIER" to 8. 6. Set the "VERT. ATTKN." v/cn. to 0.1. 7. Set the "VERTICAL GAIN" to 4. 8. Set the "VERT. AC-DC" to AC. 9. Set the "HORIZONTAL GAIN" to about 2 l/2. 10. Set the "SYNC SELECTOR" to (~).* *QNS 07695J rivu':i;U; A. .io.'Oib, Pyranols ano Related Produc te Test: Dielectric Constant and Power Factor wet- oo ilo, ... . Pagt Si of iv .rages C. On Panel No. 3 (Capaolt&roe Bridge) 1. Turn "RANQE SELECTOR" switch to "100c" for 60 Hz (cycle) measurements and to "1 Kc" for 1000 Hz (cycle) measure ments . 2. Turn "METHOD SWITCH" to SUBST. 3. Turn "DISSIPATION FACTO?." !ielector switch to "0". D. On Panel No. 4 (Oscillator) 1. Disregard this panel for not.sureaenta at 60 Hz (cyclofi). 2. On 1000 cycle measurements, depress the No. 10 "MULTIPLY BY" button. 3. Sot "FREQUENCY DIAL" to 100. 'I. Turn "OUTPUT" dial ec that jointer Is at tin end of the arrow. 5. Depress the "UNBAL. 6000 01HIS" button. II. Determination of Constants for the Apparatus 1. Carefully assemble the cell which has been cleared and dried within the last 8 hours. Refer to Seei.lor .TV. 2. Place the cell assembly In the Fisher oven which has been adjusted to 25*C. 3. Position the cell so that the thermometer hole in the over, top Is over the center of the cell. 4. Connect the clip on the lead from the oven QROUFD connection to the termini 1 on the outer cylinder of the o:ll. 5. a. Adjust the position of the oven HIGH clip sc- it Is close to (about 1/4") but not touching the terminal of the inner cylinder'. b. lioutove the therinoitfitcr from the coll. 6. To Balance the Bridge - Adjust the CAPACITANCE end DISSIPATION FACTOR dials alternately until a sharp balance Is obtained on both, adjusting the DISSIPATION' SWITCH if necessary. This condition will be Indicated on the oscilloscope when a sharp narrow traoe Is observed. , MCNS 076958 Product: Aroclors, Pyranols and Related Products Teat: Dielectric Constant and Power Factor Method No. T-2245 Page 6 of 10 pages 6. (Cont.) The capacitance balance usually must be made more closely than It oan be read In order to obtain a dissipation factor balanoe to a tenth division on the dial. CAPACITANCE value Is the sum of the readings of the dial and vernier. DISSIPATION FACTOR value Is the sum of the reading of the dial and switch. A. Balance the bridge and record the CAPACITANCE value. Call this value X. 7. Connect the clip from the HXQH lead to the Inner cylinder of the cell. 8. Again balanoe the bridge and record the CAPACITANCE value. Call this value X'. 9. Remove the beaker containing the cell from the oven and fl] 1 It with benzene (ACS grade} to a level 0.737 inches (ca. 3/4 Inch) above the top of the concentric cylinders of the cell. 10. Adjust the temperature of the benzene to stirring with a thermometer. while 11. Replace the cell In the oven (at 25C) and make the same electrical connections as In Steps 4 and 7. DO NOT Inter change connections. 12. Balance the bridge again, recording the CAPACITANCE value. Call this value Y. 13. Calculate the oell constant by the following equation: Cell Constant, K B -A , (this Is usually around 70 uuf). -rro Where A - X - X' B- X -Y 2.27 Is constant for benzene 0 (oell lead constant) A - K MOMS 076959 Product: Aioolors, Pyranols and Related Produoto Teat: Dielectric Constant and Power Factor- Method No. '.i'-Si'Jo Pago 7 of 10 pages 14. Tabulate the System Constant (A), the Cell lend Constant (a), and the Cell Constant (K) on a piece of stiff paper and post then near the Instrument Where they can be easily referred to for comparison and calculations. These constants must be checked at least once every three months and In all cases where the Dielectric Constant and/or Power Factor are out of specification. (A) - The System Constant Is th-; air capacitance of the entire syBtem. (K) - The Cell Constant Is the air capacitance of the measure ment portion of the cell alone, that In tiiat part of the oell completely surrounded by the material being tested. (0) - The Lead Constant Is the capacitance of the leads to the cell nob covered by the test material.. III. Measurement of Dlelectrio Constant and Power Factor on Aroelor3, Pyranols, Inerteens, and Trl-Tetrachlorobenzeue Blends. A. Test Hun on Cell to Determine Whether it la Clean and Properly Aligned. 1. Carefully assemble a oell which has been cleaned and dried within the p3t 8 hours. 2. Adjust the oven control to hold at a temperature of 1000C. 3. Position the oell so that the thermometer hole In the oven top Is over the center of the cell. 4. Conneot the ollp on the lead from the oven GROUND connection to the terminal on the outer cylinder. 5. a. Adjust the position of the oven HIGH clip so It Is close to (about l/4") but not touching the terminal of the inner cylinder. b. Allow 15 minutes for the oell to reach temperature equilibrium Inside the oven. c. Remove the thermometer from the top of the oven before talcing any measurements on tlieT"bridge. '~TtftB~Ts importrS. d. Hake all the adjustments on the electrical apparatus as directed In Part I of this method. HONS 076960 Product: Arocloi'3, Pyrariols and Related Produot8 Tesii Dielectric Constant and Power Factor Meb.iod So. 1-22-.5 Page 8 of 10 pages 6. Balance the bridge and record the readings. Call the CAPACITANCE value C* and the DISSIPATION value D. 7. Connect the RICH clip to the terminal of the Inner cylinder. 8. Again balance the bridge and reoord the readings. 9. ThlB checks cell element alignment and spacer as following example > reading from step 6 reading from atep 8 capacitance 997.0 922.0 total cell capacitance 75.0 If value Is the same as "A" in cell constant determination, cylinder alignment Is acceptable. reading from Btep 6 reading from step 8 dissipation factor -0.041 -0.039 dissipation factor difference 0.002 Dissipation factor difference should be loos than 0.004 when teflon spacer Is used. 10. Remove the oell from the oven and fill the beaker with the material to be tested to a levol 0.737 Inches (ca. 3/4 inch) above the cylinders of the cell. 11. Adjust the temperature of the sample to 100C. (use hot plate). MOTEs Stir sample continuounly with a thermometer ~ while adjusting the temperature. 12. Flaee the oell and sample In the oven and make the sane connections from the oell to the bridge aa In StepB 4 arid 7. DO NOT Interchange connections. 13. Allow fifteen minutes for the cell to reach temperature equilibrium Inside the oven. 14. Remove thermometer from the oven before taking a measuremend this le "Important;. HONS 076961 Product] Arocloi-B, Pyranola and Related Products Tests Dielectrio (instant and Power Factor Method No. T- 22'lf, Page 9 of 10 pages 15. Balance the bridge and record the readings. Oall CAPACITANCE value C DISSIPATION value D 16. CALCULATIONS Dielectric Constant C*"C-0 Where Ca C 0 X Capaoltance value from step 6. Capacitance value from step 35. Cell lead value from part II, Btep I?. Cell constant from part II, step 13. # Power Factor - Ca /jjs.nf j Where C* CAPACITANCE value from step 6. AC > Step 6 minus step 15 - 0. D* DISSIPATION value from Btep 15. D DISSIPATION value from step 6. f TEST frequency. Fo FREQ from Range Seleotor Switch. A Stands for change In. 0 Cell lead valve from part II step 13. NOTE: Dissipation factor Is numerically equal to power factor within 2% for all values less than 20$. IT. PRECISION (Reference: General Radio Manual for Model 716-C Capacitance Bridge) a. Capacitance readings are precise to 2 uuf x multiplier reading (0.2^ of full scale for each range) when the dissipation factor is less than 0.01. b. Dissipation Factor (Power Factor) readings are precise to 0.0005 or 2% of the dial reading whichever is larger, for values less than 0.1 for D (Dissipation Factor).. IV. Cell Cleaning A. The Electrodes Cleaning Procedure 1. Remove the electrodea from the tested material while hot and allow them to drain. MONS 076962 Producti Aroeloro, Pyranols and Related Products Test) Dlelectrlo Constant and Power Factor Method No. T-224JPagt 10 of 10 pages 2. Place the eleotrodes In hoc TCB for 10 minutes. 3. Wash with unheated TCB. 4. Rinse twice with methanol and twice with tap water. 5. Place the electrodes in hot 10$ T.S.P. solution. Soak and heat for 10 ulnute3. 6. Wash thoroughly with tap water. 7. Place the electrodes in hot top water for 11 rainuteo. CAUTION: After Step 6 -- DO NOT TOUCH THE EJ^C'l'RpDES with Hands i ............. ' 8. Wash with dlBtilled water twice. 9. Dry in drying oven for at least two hour:-, t.t 120c. B. TheO.E. Cell Cleaning 1. Reclean the Cell before use, if more than 8 hours have elapsed since the previous cleaning. 2. Follow the procedure for the electrodes starting at Step 4. C. Cleaning of the Accessories 1. Apply the same cleaning procedure as given for the eleotrodes (Steps 1 to 8) to prepare the glass spacer and beaker for next test. 2. Clean the thermometer in the same manner as the electrodes, except for Step 8. 3. Place the wet theraoinetsr (after Step 7) directly in position In the Temperature Keating Unit (Modifier. Fisher Isotemp Oven) and allow to dry. MOMS 076463