Document 2RRevmmkrn9rLgeRDN82Q0YpL

TENNECO.nter. office memo CHEMICALS, INC. To P.A. Ketterer At Flemington V A Fpom W.C. Champion At Burlington Subject Analysis for VCM in Resin date November 21, 1974 COPY TO *P. L. Bogart H.B. Carr F.W. Kanzler R.A. Lojewski *Dr. M. Rosen ./File The attached B.F. Goodrich analytical method was obtained by Pete Bogart through the Vinyl Chloride Safety Association. Essentially, the method allows for determination of residual vinyl chloride in resin by analysis of the headspace of a vial of resin whose temperature has been raised to above the Tg to drive off the dissolved monomer. If this method is hs accurate and reproducible as claimed by Goodrich, considerable analysis time could be saved over our current dissolution method. We would request to you evaluate this method and comment upon it. Attachment, WCC/jst *without attachment COLORITE 013270 Gr, P, ScftAKF \ I' Tho S. Goodrich Company ' tiiMici n ii onuiMuii emu I12A MECKSVIUE ROAD BRECKSVIHE, OHIO Kill PHONE; 21-5!6-3U \ September 19, 1974 Dr, T. G. Fox Mellon Institute Pittsburgh, Pennsylvania 15213 Dear Dr. Fox: Enclosed are three copies of the manuscript "Analysis for Vinyl Chloride in PVC Powders by Head-Space Gas Chromatography", by A. R. Berens, L. B.' Crider, C. M. Tomanek, and J. M. Whitney. I hope you will consider this short paper for early publication in Polymer Betters Edition, Journal of Polymer Science. We believe that this note warrants speedy publication in view of the current concern about the possible toxicity of vinyl chloride. The rapid, simple, and reliable analytical procedure we report should quickly be noted and applied by the many producers and fabricators of PVC around the world. Furthermore, the general method -- analysis of vapor in equilibrium with a polymer above Tg -- may well prove useful in other polymer/volatilecontaminant systems, which are of increasing concern throughout the poly mer industry. As I will be out of the country until November 4, would you please address your reply and any requests for clarification or revision to my -^co-author: ------ L* B, Crider B, F."Goodrich Chemical Co. Technical Center ,. ' Avon Lake, Ohio 44012 Thank you very much for your prompt consideration of this paper. Sincerely yours, bak enclosures (3) Alan R. Berens Research Fellow COLORXTE 013271 Analysis for Vinyl Chloride in PVC Powders by Head-Space Gas Chromatography' by: A. R. Berens, Corporate Research, Th& B. F. Goodrich Co. , Brecksville, Ohio. --- L. B* Crider and C. M. Tomanek, Technical Center, B. F. Goodrich Chemical Co., Avon Lake, Ohio and J. M. Whitney, General Chemical Plantr~B. F. Goodrich Chemical Co., Avon Lake, Ohio. Recent concern about the possible health hazard of exposure to vinyl chloride monomer, VCM (1) has focused attention on the measurement of residual monomer contents of commercial PVC products. We report here a simple, rapid analysis for VCM in PVC through gas chromatography of the vapor phase over PVC powder samples. The basis of our method is the observation (2) that at a temperature --above the glass-transition point of PVC, the-solubility of VCM in PVC accurately follows Henry's Law behavior upTcTa VCM content of at least 4000 ppm. Writing Henry's Law as S = KPV (1) where S is the concentration of vfcM dissolved in the PVC in ppm by weight VCM/PVC, and Pv is the VCM partial pressure in mm. Hg, we find the Henry's Law constant, K, is 6. 52 ppm/mm at 90*C. The analytical proce dure simply involves sealing a weighed PVC sample containing VCM in a COLOR!TE 013272 2- suitablc container at room temperature, heating the container to 90'C to establish VCM equilibrium between PVC and vapor phases, then analyzing a samplc of the "head-space" vapor to determine its VCM content. Henry's Law is then applied to calculate the original VCM content of the PVC as follows: Let us say that the PVC sample of weight rn grams originally con- "tains Wt grams VCM. When equilibrated at 909C in a closed container, the same amount of VCM is now distributed between PVC and vapor phases, or Wt = Wv + Wp (2) where Wv and Wp are the weights of VCM in the vapor and polymer phases respectively. Henry's Law gives W KPV m and, assuming ideal gas behavior, (3) (4) ----- -wbere -Mv is the-molecular -weight of VCM, Vg is he volume of the vapor phase, (container volume less volume of PVC sample), R is the gas constant, t and Ts = 363K. Combining (2), (3) and (4) gives While the PVC and vapor are at 90C, a sample of vapor is taken by syringe and brought to room temperature, Tt, and pressure, PA where its volume is Z ml., then injected into the gas chromatograph. From'the VCM peak area, (or height), the weight, Y_, of VCM in the syringe sample is obtained by COLORITE 013273 -3- applying the appropriate response factor, peak area (or height) per g VCM. The response factor is determined through calibration of the GC response on known gas mixtures. The syringe sample thus contains Y/Mv mols VCM and PjZ/RTj total mols gas. The mol fraction VCM, <pv, in the vapor, both in the syringe at room temperature and in the vial at 90 is thus <Pv " Y/Mv Px Z/RTX _ YRT, MyPiZ (6) Since the gas sample was simply cooled in going from vial to syringe, Pj/Ta = P3/T3, o . <hf -- YRT2 MyPsZ (7) The partial pressure of VCM at 90 4 is thus PPv -` ,^P -' YTSRZTz* (8) Introducing (8) into (5) we have W't, YRTS MvVg m MVZ ( K+ ` (9) ____ This -expression, gives the VCM content of the PVC sample, W^/m, directly "from the GC analysis of the vapor phase. * The time required for equilibration of VCM between vapor and PVC phases can be estimated from recently reported diffusion data (3). From the solution of Pick's diffusion equation for spherical geometry (4), the time required for 99% of the original VCM dissolved in a PVC sample to diffuse Out into a VCM-free environment is given by % _ 0. 45 d' t.99 (10) COLORXTE 013274 -4- v/here d is the particle diameter in cm and D the diffusion coefficient in cm^/sec. For VCM in PVC at 90C, D is approximately 2xl0~^ cm^/sec (3), hence t gg will be less than 1 hour for PVC particles of less than 25 microns effective diameter. In our experience, a one-hour heating time at 90C has proven satisfactory for the analysis of most commercial PVC resins in the as-polymerized powder form. Our analytical method is less - satisfactory for molded, extruded, or otherwise fused PVC samples be- --cause of the very long-equilibration times required. "In developing the head space method of analysis, we have used a Hewlett Packard 5710 gas chromatograph equipped with a flame ionixation -detector. The column used for the analysis is a 6 ft. x 1/8 inch stainless steel column, packed with 80/100 mesh Porapak QS. The column oven is controlled at 140C, the detector at 250"C and the injection port at 150C. Carrier gas (helium) flow is 30 cc per minute. Under these conditions, vinyl chloride elutes from the chromatograph in approximately 280 seconds. __________ ./^response factor for the chromatograph is determined by injecting .--.known, standard mixtures of vinyl chloride and air. 4 .' -Samples for analysis are prepared by weighing approximately two grams of PVC powder into a 12 cc vial and sealing the vial with a fold-over septum. The sample vials are then placed in an air oven or water bath controlled at 90"C and allowed to equilibrate. After equilibrium is established an aliquot of the vapor'space in the m vial is removed with a gas-tight syringe. The volume of this vapor sample --at room temperature and pressure is noted. The sample is injected into COLORXTE 013275 \ -5- the chromatograph for analysis. Determination of the residual vinyl chloride in the sample is made using equation (9) above. \ To verify the accuracy of the head space analysis, a PVC resin was stirpped of all residual vinyl chloride via vacuum-thermal techniques. This "clean" resin was then weighed into sample vials which were then septum-sealed. Known amounts of vinyl chloride gas were injected into the vials and allowed to equilibrate for one hour at 904C. The vial head space -was then analyzed as described. Table 1 compares the head-space analyti cal results with the calculated ppm vinyl chloride. TABLE 1 Resin Weight (gms) 3.2 VC1 Charged (cc) 2. Calculated ppm VC1 1600 Head-Space Analy; ppm V Cl 1586 3.2 1. 793 759 3.2 . 5 397 379 3.2 .025 20 23. 3 The head-space method has also been compared to a direct method of analysis in which residual vinyl chloride is determined without relying on established method of polymer/vapor equilibrium. In this method, 20-30 mg of PVC re sin is weighed into a glass tube which fits into the injection port of the H-P 5710 chromatograph. The PVC powder is held in the heated sec tion of the tube with a glass-wool plug. The injection-port sep,tum is re'# moved, the sample tube dropped into the injection port, and the septum .replaced. The heat of the injection port (150*C) drives the volatiles out of COLOKITE 013276 -6- the polymer into the carrier gas stream. To produce plug flow through the column, its first 2 or 3 inches are chilled with dry ice before the sample is introduced. After sample insertion, the column oven is programmed at 16C per minute to 200C. Vinyl chloride elutes in approximately six minutes. The vinyl chloride peak area is a direct measure of the total VCl content of the PVC sample. While this method of analysis appears reliable, the small PVC sample size introduces a possible weighing error and the need to chill and program the column temperature makes the method some what lees convenient than the,head-space method. Table 2 compares data from the two methods. TABLE 2 Head-Space Analysis Direct Method of Analysis Sample ppm Residual VC1 ppm Residual VCl______ PVC Homopolymer "A" 30 30 31 29 31 20 29 24 PVC Homopolymer "B" 46 47 45 45 % 43 48 To demonstrate the reproducibility of the head-space analysis, a PVC homopolymer resin was divided into 20 samples each sealed in a glass jar. Two of these samples were analyzed by the head-space method each day for ten days. Table 3 shows the results of this experiment. COLORXTE 013277 TABLE 3 Head-Space Analysis Sample Identification First Day ppm Residual VC1 6.1 Second Day 5.9 6.4 7.2 .Third Day 5.2 5.4 Fourth Day 7.4 7.5 Fifth Day Sixth Day t 7. 5 7.4 7. 6 7.8 Seventh Day 5.8 b, 6 Eighth Day 7.5 8.4 Ninth Day 7.9 8.4 Tenth Day 8.4 7. 5* Average: 71. ppm Std. deviation: 1.0 ppm COLORITE 013278 8- In closing, we suggest that a similar analytical method might be generally applicable lor the determination of volatile components in polymers. To establish the method for a new polymer/penetrant system would require, first, the determination of conditions where Henry's Law applies and of the Henry's Law constant, and second, an estimate of the time required to establish vapor-polymer equilibrium. The authors gratefully acknowledge M. Mele's contribution of data in Table I and The B. F. Goodrich Company's permission to publish this note. COLORITE 013279 -y - References 1) Chem. Engr. News, Jan. 28, 1974, p. 6. 2) A. R. Berens, Polymer Preprints _1_5 (2) 197 (1974). 3) A. R. Berens, Polymer Preprints 15 (2) 203 (1974). 4) J. Crank, The Mathematics of Diffusion, Oxford Univ. Press, London, 1956. COLORITE 013280 B. F. GOODRICH CHEMICAL COMPART Standard Test Procedure No** 999"T TITLE: Residual Vinyl Chloride Monomer Content of Polyvinyl Chloride .Resins TYPE OF ANALYSIS: Vapor Space Equilibrium, Gas Chromatographic PRODUCT: Polyvinyl Chloride Resin, Finished Product I. SCOPE This procedure is suitable for determining the residual vinyl ___ chloride monomer content of polyvinyl chloride (PVC) resins. The method cannot be used for polymer in other forms such as compounds or final fused products, II. PRINCIPLE The basis for this method relates to the vapor equilibrium which is established between residual vinyl chloride monomer (RVCM), PVC resin and air in a closed system. It has been demonstrated that the RVCM in a PVC resin will equilibrate in a closed vessel quite rapidly, provided the temperature of the PVC resin is maintained above the glass transition temperature of that specific resin. III. INTERFERENCES 1) Normally this vapor will contain only air, vinyl chloride ___ _______ monomer.and traces of water. Any other volatile material present in the closed vessel could change this equilibrium -----relationship. Impurities in the low ppm range will generally have only a very small influence on this equilibrium rela tionship. 2) Any material which elutes from the chromatographic column at approximately the same time as vinyl chloride will cause high RVCM results. * IV. PRECISION AND REPR0DUCI3ILITY Initial data obtained with this method, covering a range of O.CG25 to 0.2000 wt. percent, indicates that one standard deviation (determined from duplicate results) is approximately 2.l. Absolute accuracy has been checked by comparing results to another, totally independent method. In this case agreement between the two methods is + 5^ in the range 0.0025 to 0.2000 vt. These results were obtained by two operators in one laboratory. COLORXTE 013281 EFG Standard Test Procedure No. 999-T Page 2 of 7 V. SAFETY 1) Do not release vinyl chloride to the laboratory atmosphere during preparation of standards. Venting and purging with vinyl chloride - air mixtures must be held to an absolute minimum. Y.Tien venting and/or purging is required the vapor must be routed to outside air. Vinyl chloride, even at low ppm levels, must never be vented inside the laboratory. It can be vented into a properly functioning fume hood. 2) Be careful not to come into contact with heated parts of the chromatograph, such as the injection port, detector, heated column, etc. Handle all electrical connections with care. VI. APPARATUS 1) Gas Chromatograph, Hewlett Packard Model 57HA, dual flame ionization detector, equipped with following options: (a) 005 Dual flow controller to) 006 Substitute linear oven programmer (5702a) for isothermal oven controller (c) Oil Substitute auxiliary heated zone controller (5708a) <d) 017 Substitute universal heated injection port with disposable glass liners (18747) (e) 024 Rotometer kit for carrier gas *2) Integrator -- Hewlett Packard Model 3380A with built-in recorder Alternate Integrator -- AutoLab System 4 k 3) Chromatographic Column -- An 8 ft. x l/8 in. stainless steel column packed with 80/100 Poropak QS and conditioned at 200 C. Oven, forced draft capable of maintaining a constant temperature of 90 +_ 1.0 C. (Fisher Cat^. No. 13-244-176 Isotemp Oven) 5) Gas Sampling Bottles, 250 ml capacity equipped with glass stopcocks on both ends plus a septum fitting (Fisher Cat. No. 11-134-190) 6) Serum Bottles, 10 cc volume with rubber septums (Fisher Cat. No. 3-210B serum bottles and Cat. No. 3_215 rubber stoppers) 7) Analytical Balance, capable of weighing to +_ .0001 gram 8) Hydrogen Cylinder with regulator 9) Flowmeter, 0 to 2 liters per minute COLORITE 013282 BFC Standard Test Procedure No. 999-T \ VI. APPARATUS (continued) Page 3 of 7 10) Helium Cylinder with regulator 11) Clean air supply at 25 psig 12) Bubble Flow Indicator VII. REAGENTS Calibration gases, vinyl chloride in air mixtures 1) Low level between 15 and 25 parts per million 2) A high level between 800 and 1200 parts per million These can be obtained from: Precision Gas Products, Inc. P. 0. Box 538 Linden, New Jersey 07036 VIII. PREPARATION OF GAS CHROMATCGRAPH 1) Install the 8 ft. x l/8 in. Poropak QS column and condition at 200 C. 2) Adjust flow rates for the H. P. 57HA according to the operating manual (30 cc's per minute helium carrier gas, 30 cc's per minute hydrogen and 130 cc's per minute air.) 3) Set conditions for analysisas follows: Injection port - 150* C. Detector - 250* C. Oven - 160" C. 4 k) After these conditions have been reached and the chromatograph has stabilized it is ready for calibration. IX. CALIBRATION l) Fill the clean glass 250 ml' gas sample bottle with the low level (15 to 25 ppm) vinyl chloride air standard. The procedure for doing this is detailed in Attachment 1, Always use the same bottle for this low level standard. 2) With the 1 cc gas syringe draw out of the calibration bottle, through the septum, in excess of 1 cc of the gas sample. After the plunger on the syringe is pulled all the way, wait five seconds before removing the syringe needle from the bottle septum. 3) After the five second delay remove the needle from the septum and move plunger to read exactly 1 cc on the syringe. COLORITE 013283 BFG Standard Test Procedure Mo. 999-T ' Page 4 of 7 IX. CALIBRATION (continued) M Immediately inject the 1 cc sample into the chromatograph injection port (as rapidly as possible). 5) Remove the needle from the injection port and start the chromatograph recorder and integrator. 6) In approximately three minutes the vinyl chloride will elute 7) 'Wait one minute after the VC1 elutes and starting at Step 2 above repeat Steps 2 through 6. Do this four times. -8) Fill in the data obtained in the four runs above on the calibration sheet (Attachment 2). 9) If the peak areas from these four runs do not deviate more than 5/> from the average of the four runs, this step is complete. If there is a deviation greater than 5'p from the average, repeat Steps 1 through 8. See Note 1. 10) After the above calibration is completed, recharge the second glass calibration cylinder with the high level (800 to 1200 ppm) vinyl chloride air standard. Starting at Step 2 above repeat this procedure through Step 9 using the high level standard. 11) This calibration is complete if the requirements of Step 9 are met. If Step 9 is not met, refer to Mote 1. 12) For the third calibration point use the high level standard, but in this case use only a 0.5 cc sample. 13) `Draw out an excess of 0.5 cc with the gas syringe. 1^) Wait five seconds after the plunger is pulled back before removing the syringe needle. 15) After the five second delay remove the syringe and adjust the plunger to read exactly 0.5 cc. 16) Inject this sample into the chromatograph and record the peak area on the calibration sheet. 17) Repeat Steps 13 through 16 four times. 18) If the peak areas from these four runs do not deviate more than % from the average of these four runs, this calibration is complete. If there is a deviation greater than 5^ from the average, repeat Steps 13 through 16. See Note 1. COLOR!TE 013284 BFG Standard Tent Procedure No. 999-T Page 5 of 7 IX. CALIBRATION (continued) 19) The data generated in the above calibration is used to calculate the response factor for the calculation of residual vinyl chloride in the san-.plcs analyzed. The response factor calculations are detailed on the cali bration sheet. Note 1: If the deviation is still greater than $>, shu-t down and locate the source of the problem. X. SAMPLE ANALYSIS (Samples must be run at same range and attenuation used for calibration standards. If range or attenuation is changed "for the sample, then new standards must be run at this range and attenuation. 1) All samples should be kept in tightly sealed glass jars. ""Samples must be run promptly (within 30 minutes) from the time they are received in the laboratory. Within 3 minutes the sample should be weighed into the serum bottle and placed in the oven. The exact total volume of the serum bottles must be measured. See Attachment 5* 2) Prepare duplicates for each sample. Take one serum bottle plus rubber septum, mark with identification and obtain a tare weight to four decimal places. Record tare weight on analysis work sheet. See Attachment 3* 3) Remove serum bottle from balance, remove septum and pour in the proper amount of resin to be analyzed. Replace rubber septum. Be certain that rubber septum is fully seated and sealed. ... ______ Approximate Bottle Volume Add 12 cc 2 grams + .5 A simple technique can be devised based on a volumetric resin addition. Small cups, having the proper volume, can be used to rapidly obtain the resin sample. This can then be added to the serum bottle with a tiny funnel. 4) Replace serum bottle on balance and record the weight to four decimal places. 5) Remove bottle from balance. 6) Place bottle in oven (at 90 + 1.0 C.) and allow it to remain 15 -0 +1 minutes. 7) At the end of the heating cycle remove the bottle from the oven and immediately insert the needle from the 1 cc gas syringe into the bottle through the septum. (Bo not allow the needle to contact the resin sample.) COLORXTE 013285 o o o o o o OOO OOQOOOO "A BFG Standard Test Procedure No. 999~^ Page 6 of 7 X. SAMPI.5 ANALYSIS (continued) 8) Sample Size - Use a 1 cc sample volume when the RVCM content is expected to be less than 100 ppm. Use a 0.5 or 0.3 cc car.'-1.0 for expected higher concentrations. 9) Draw out the proper volume sample (plus slight excess) "from the bottle. Wait 5 seconds after pulling the plunger back before removing the needle from the sample bottle. 10) After the 5 second delay remove the syringe needle from the serum bottle and adjust plunger to read the proper volume. 11) Inject the sample into the chromatograph, start integrator and recorder. 12) The vinyl chloride peak will elute in approximately 3 minutes. 13) Wait one minute after the vinyl chloride peak elutes and repeat Steps 7 through 11 using a duplicate sample. iM Record sample peak area, gas sample size, attenuation, sample identification, etc. on work sheet (Attachment 3)- 15) One minute after the vinyl chloride elutes you are ready to run another sample. *. COLOR!TE 013286 BFG Standard Test Procedure No. 999"^ Page 7 of 7 , XI. CALCULATION OF RVCK IN SAMPLE The following information is needed to calculate the residual vinyl chloride content of the resin. 1) Response factor for vinyl chloride = R (counts/nanogram VCl) (as determined in the calibration step) 2) Weight pf polyvinyl chloride resin in vial = W (grams) 3) Volume of sample Injected into chromatograph = V (cc) 4) Area of the chromatograph peak for the vinyl chloride o A (integrator counts) 5) Volume of sample bottle (serum vial) = B (cc) 6) . Atmospheric Pressure = P (mm Hg) ppm KVCM A = 100 -1 A x 10 -9 X lp + (1.16 RV -3) x 10 --------------------------- -7 A x 10 X COLORITE 013287 This calculation can very easily be set up on a Monroe i860 Programmable Calculator. It should not b^ routinely performed on a hand calculator because of a high probability for errors Monroe i860 program for this method is attached. See Attachment 4 BFG Standard Test Procedure No. 999-T ATiYc;r:sN? 1 Method for Preparation of Standard VCM/Air Mixtures l) Clean the 250 ml gas sampling bottles vith acetone and blow tho roughly dry vith clean air or nitrogen. --2) -J\.pply lov vapor pressure stopcock grease to both stopcocks after washing and drying. 3) Attach a septum to the septum stem. 4) Using the proper standard VCM/air cylinder equipped vith regulator attach the sample bottle using a short piece of tubing. Attach the other end of the bottle to the rotometer. 5) Open both stopcocks on the gas sampling bottle. Open valve on gas cylinder. Very slowly and carefully open the regulator on the cylinder to provide a flow rate of approximately 1.5 liter per minute. 6) Purge for two minutes. Be certain that the VCM/air mixture is properly vented as stated in Section V. 7) At the end of the purge time turn off the valve at the cylinder and then both stopcocks to off, closing the stopcock closest ___ to the cylinder first. -_8) Has. sampling bottle is now ready to use. COLOR!T 013288 COLORITE 013289 BFO Standard Test Procedure No. 999~T - Run No. Sample Identification Injected Sample Size, cc ATTACHMENT 2 Calibration Data Sheet and Calculations Peak Area Avg. Peak Area Deviation from Avg. Counts per Nanogram VC1 1 19 ppm Std 2 3 4 11 tl 11 1.0 4600 . 4565 4690 4585 4610 .2 1.0 .4 .5 95*7 5 6 7 8 805 ppm Std tl 1 -1 J1 tl , 0.5 11 M. I | 95370 96485 ] 95732 f 96901 96122 .8 j-4 1 Uj .8 t 94.2 9 10 805 ppm Std 11 11 It 12 It 1.0 193946 1.4 190241 .5 189789 1.4 190916 191,223 .2 93*7 Us ins a 1.0 cc sample, each ppm VC1 in the standard contains 2.5352 nanograms VCM. Runs 1 through 4 each contain (19)(2.5352) = 48.17 nanograms VCM Runs 5 " JB n " (805){2.5352)(.5) = 1020.4 nanograms VCM Runs 9 " 12 " " (305)(2.5352) = 2040.8 nanograms VCM 4 ThenAverage Peak Area -f Nanograms VCM = Counts per Nanogram VCM The Response Factor = Avg, Counts per Nanogram VCM = 94*53 r Avg. Counts per Nanogram VC1 * 94.53 BFG Standard Test Procedure No. 999-T P* L GC Run No. 1 2 3 -4 5 6 Sample Identification Sample Weight (grams) W "A" 2.0012 "B" 1.9873 "C" * 2.1249 "D" 2.0141 "E" 1.9981 itpn 2.0476 ATTACHMENT 3 Analysis Work Sheet and Results Vapor Sample Volume (cc) V 1 3 5 5 ' 5 .5 GC Peak Area A 43,210 769,343 143,356 19,423 117,324 4,422 Atm. Pressure mm P 75>3 'r Response Fac tor Date Volume . of Serum Bottle PPM RVCM in Res i n R 94. 53 >' B 12 .0 \f 6.4 213 22.6 3.2 19.4 0.7 COLORITE 013290 A BFG Standard Test Procedure No. 999-T ATTACHMENT L Program for Calculating ^ RVCM in Res In - Monroe i860 Operating Procedure: 1) Br ( ) ( ); 0; 0 Program No. 133 prints 2) Enter A) Area Counts B) Response Factor, counts/nanogram VCM C) Syringe Volume, cc D) Atm. Pressure, mm E) Sample Weight, grams F) Volume of Serum Bottle, septum in place, cc 3) Prints answer in ppm RVCM in resin 1 33 0000 1 4 4,7 3 5 94 0 753 2 12 0000 5 300 3000 00 0 0 0 0 12 0000 39 8 6 4 1 A PROGRAM NO. -AREA COUNTS 'RESPONSE FACTOR -SYRINGE VOLUME -ATM. PRESSURE -SAMPLE WEIGHT -SERUM BOTTLE VOLUME COIiORXTE 013291 13 3* 0 0 0 0 0000 1 2 3 4 5 6 7 8 9 00 10 1 2 3 4 5 6 7 8 9 0020 1 2 3 4 5 6 7 8 9 00 30 1 2 3 4 5 6 7 a 9 1 1s 000 00 1 003 003 060 /I 7 6 056 1 10 00 1 060 056 1 10 002 060 056 1 10 00 3 . 060 056 1 10 004 060 056 1 10 00 5 060 056 110 010 060 065 ' 111 00 1 02 3 026 00 1 000 025 00 1 o ; t. J J ; i > i t . P 1* . J 1 i I i S r a \ f X ( / 0 ax t 0 0 A I) n1 3 l 027 2 020 '3 1 10 4 ..006 5 111 ___ J3 00 1 7 023 ___ J3 026 '9 0050 00 1 000 1 025 CM 01 1 01 3 --------4 --___ 5 027 020 6 02 1 : --7 1 ` .8 026 111 9 002 0060 02 3 --------- 1 111 ----- 2 00 3 3 02 3 4 012 5 ` 000 6 000 7 00 1 6 00 1 9 007 0 006 027 1 020 . 2 1.1 o 3 00 7 4 111 5 00 6 6 024 7 111 a 9 0080 007 020 1 10 1 ' 006 2* 1 1 1 3 00 1 4 , 023 5 02 6 6 00 1 7 000 8 025 9 ,, 007 ) = 1 6 t / X ( r* 0 a' 3 ) -- + ( t p X t 5 X 0 0 f / 5 ) 1 7 t 6 4 t 7 = + e t / X ( t 0 nx 7 COLORITE 0X3292 C o 0090 1 2 3 4 9 6 7 3 9 0 10 0 1 2 3 4 .5 6. 7 8 9 0 110 1 2 3 4 5 6 7. 8 9 0 12 0 1 2 3 4 .5 6 7 8 9 0 130 1 2 3 4 s 6 7 8 9 01 3 027 020 024 111 007 020 0 13 02 1 ' 00 1 000 000 0 20 1 1 10 0 07 111 006 -0 24 111 007 020 1 10 00 1 00 3 006 003 02 3 111 004 023 002 -0 1 1 0 20 024 026 002 01 1 005 02 3 006 002 012 00 5 027 020 1 10 002 006 002 012 - ) - r 7 + / 0 0 -- 4 7 t 6 v t 7 -- 4 f. J G 3 X t. * X 2 9 -- v. < l , . 1 9 S 'X Sy ) 4 6 2 1 2 3 4 i5 6 7 8 9 . 0 15 0 1 2 3 4 5 6 7 a ` 94 0 16 0 1 2 3 4 5 6 7 8 9 0 17 0 1 2 3 4 5 6 7 8 9 0 18 0 1 2* 3 4 5 6 7 a 9 o o 005 02 3 026 111 010 022 026 111 024 C0 1 01 2 004 027 027 020 024 026 111 00 5 023 006 00 2 004 000 000 023 003 006 0U3 027 -0 2 0 02 1 026 00 6 012 ' 005 023 012 000 000 '000 000 00 0 00 1 02 7 020 1 10 00 3 111 COLORITE 013293 s n I 0 190 1 2 3 4 5 6 7 8 9 0200 1 2 3 4 5 6 7 8 9 . 00 1 02 3 111 002 02 3 11 V 00 3 020 06 1 1 76 176 ' 065 065 06 5 1 27 000 000 000, 000 377 / X '1 .? X t J A Sr 0 0 0 0 COLORXTE 013294 o U <J U u W KJ KJ KJ V_> KJ KJ \ BFG Standard Test Procedure No. 999-T ATTACHMENT 5 Establishing True Volume of Serum Bottle 1) Clean serum bottle (water and detergent) and rinse with acetone. Air dry thoroughly, 2) Allow to condition for at least 15 minutes at room temperature. 3) Weigh serum bottle plus septum to 0.0001 gram on art analytical balance. U) Using distilled water which has been conditioned to within + 2 F. of room temperature fill the bottle to the very top. 5) Carefully insert and seal the septum. This will tend to force a small amount of water out of the bottle. 6) Dry the outside of the bottle and weigh again on the analytical balance. 7) Knowing the temperature of the water, determine, using a table of density of water at various temperatures,the volume of the bottle. 8) Check three bottles and average the results. Individual results should not differ more than +0.3 cc from the average. (Bottles normally have a volume of approximately 12.0 cc.) COLORITE 013295